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• Published: 18 March 2022

Large-scale synthesis of graphene and other 2D materials towards industrialization

• Soo Ho Choi   ORCID: orcid.org/0000-0002-9927-0101 1 , 2   na1 ,
• Seok Joon Yun 1 , 2   na1 ,
• Yo Seob Won 2 ,
• Chang Seok Oh 2 ,
• Soo Min Kim 3 ,
• Ki Kang Kim   ORCID: orcid.org/0000-0003-1008-6744 1 , 2 &
• Young Hee Lee   ORCID: orcid.org/0000-0001-7403-8157 1 , 2  

Nature Communications volume  13 , Article number:  1484 ( 2022 ) Cite this article

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• Electronic devices
• Synthesis and processing
• Synthesis of graphene
• Two-dimensional materials

The effective application of graphene and other 2D materials is strongly dependent on the industrial-scale manufacturing of films and powders of appropriate morphology and quality. Here, we discuss three state-of-the-art mass production techniques, their limitations, and opportunities for future improvement.

Two-dimensional (2D) van der Waals (vdW) layered materials including graphene, transition metal dichalcogenides (TMDs), hexagonal boron nitride (hBN), and MXenes have attracted much attention in recent years. This is due to their distinctive physical and chemical properties, such as their quantum Hall effects and quantum valley Hall effects, indirect-to-direct bandgap transition, and strong spin-orbit coupling 1 , which have not been accessible with conventional 3D bulk materials. In addition, vertical vdW heterostructures constructed by layer-by-layer stacking enable interesting applications for atomically thin quantum wells, p-n junctions, Coulomb drag transistors, and twistronic devices 1 , 2 , 3 . However, applications based on such structures are limited by the fact that most vdW materials are currently only available with a lateral size of up to a few tens of micrometers. Techniques for the large-scale synthesis of 2D materials will therefore be required for industrialization. Moreover, since specific applications of these materials are strongly dependent on characteristics such as their morphology and quality, mass production techniques should also be developed that can accommodate such requirements (Fig.  1 ). In general, most applications rely on either films or powders of vdW materials. Films require high crystal quality, and can be used in the context of electronics, spintronics, optoelectronics, twistronics, or solar cells, whereas powders exhibit large surface areas and are employed in the construction of batteries, sensors, and catalysts. At present, only large-area graphene films and graphite oxide powders are currently available in the commercial market 4 . In this Comment, we briefly examine research trends in synthesis techniques and their associated challenges for the industrialization of 2D layered materials.

2D films and heterostructures require high crystal quality and homogeneous thickness for applications such as electronics and spintronics, whereas high-porosity powders with vast specific surface area can be used in contexts such as catalysts and energy storage.

Three representative synthesis techniques

There are currently three representative synthesis techniques available for the large-scale synthesis of 2D materials. The first is chemical vapor deposition (CVD); although a variety of thin-film deposition techniques have been investigated for growing large-area 2D films, including pulsed laser deposition (PLD) 5 , atomic layer deposition (ALD) 6 , and molecular beam epitaxy (MBE) 7 , CVD is most feasible for industrialization when one takes into account the uniformity and crystallinity of 2D films as well as requirements of high throughput, cost effectiveness, and scalability. The other two techniques being investigated for mass production are top-down liquid exfoliation of 2D materials and bottom-up wet chemical synthesis.

CVD for growing large-scale 2D thin films

There are multiple examples of CVD synthesis of thin films at wafer scale (Fig.  2a ). For example, wafer-scale polycrystalline monolayer and multilayer graphene films have been successfully synthesized by CVD on polycrystalline Cu and Ni foils since 2009 8 , 9 , 10 , 11 , and wafer-scale single-crystal monolayer graphene has been synthesized by using single-crystal substrates such as H–Ge (110) and Cu (111) 12 , 13 . Single-crystal multilayer graphene films have been also grown on Si–Cu alloys at wafer scale 14 . In 2012, centimeter-scale polycrystalline monolayers of hBN and TMDs were grown on polycrystalline Cu foils and SiO 2 /Si substrates, respectively 15 , 16 . And more recently, single-crystal hBN and TMD films were successfully synthesized on liquid Au, high-index single-crystal Cu surfaces, and atomic sawtooth Au surfaces 17 , 18 .

Lefthand panels show timelines of milestones for a chemical vapor deposition (CVD), b liquid exfoliation, and c wet chemical synthesis methods. The abbreviations correspond to: metal-organic CVD (MOCVD), graphene (Gr), graphite oxide (GO), reduced GO (rGO), and molybdenum disulfide (MoS 2 ). Righthand panels show the corresponding strengths and weaknesses of these methods in terms of mass production (MP), thickness controllability (THK), temperature variation (TEMP), uniformity (UNI), material diversity (MAT), crystal quality (QLTY), morphology (MORPH). Panel a reprinted from refs. 9 , 17 , American Association for the Advancement of Science, ref. 15 , Nature, refs. 7 , 10 , 12 , Wiley, ref. 5 , American Institute of Physics, ref. 6 , Royal Society of Chemistry, and ref. 11 , World Scientific. Panel b reprinted from refs. 26 , 27 , American Association for the Advancement of Science, refs. 22 , 23 , Wiley, refs. 19 , 20 , 21 , Elsevier, and ref. 24 , Institute of Electrical and Electronic Engineers. Panel c reprinted from ref. 28 , Elsevier, ref. 30 , American Chemical Society, ref. 31 , Elsevier, and ref. 32 , Royal Society of Chemistry.

CVD produces relatively high-quality 2D films under atmospheric or low pressure, and the size of the film can easily be scaled up by increasing the chamber size. However, high temperature reactions (above 500 °C) are required, which could be a drawback for industrialization. The growth of a vast range of 2D materials, including graphene, hBN, and TMDs, is still limited by the absence of appropriate precursors. Perhaps the most important technical challenge presented by this method is the poor control over the number of synthesized layers, because the absence of dangling bonds on the surface of 2D vdW materials makes epitaxial growth difficult.

Liquid exfoliation

Liquid exfoliation is a powerful process for the mass production of pristine 2D bulk materials by dispersing them into individual sheets. Bulk materials have been synthesized by chemical vapor transport (CVT) (Fig.  2b ) since the late 1960s, but most 2D bulk materials are currently only available in small quantities. Nanodispersion into monolayers is often required to manifest the unique 2D nature, but the strong vdW energy of micron-scale materials hinders facile exfoliation. Thus, two additional steps should be considered for liquid exfoliation processes: (i) weakening the layer-layer interaction by expanding the interlayer distance, and (ii) physical agitation for dispersion 19 , 20 . In 1958, it was demonstrated that the interlayer distance can be increased from 3.4 to 7.0 Å by the oxidation of graphite, known as “graphite oxide”, and such an expansion of the interlayer distance made it possible to disperse the individual graphite oxide layers by sonication. Graphite oxide layers can subsequently be reduced to graphene nanosheets through chemical treatment with reducing agents and thermal annealing treatment 21 , 22 , 23 .

The lattice of graphene nanosheets is often severely damaged during oxidation and reduction processes. To prevent this, the interlayer distance can be increased by intercalating ions and molecules between layers. Electrochemistry enables effective intercalation of both cations and anions in an electrolyte solution by applying negative and positive bias, respectively 24 . Alkali metals, organic solvents, and surfactants with similar surface energies to those of the 2D materials can also be directly intercalated in liquid or vapor phase 25 , 26 . After intercalation, agitation methods such as sonication, homogenization, and microwave treatment can be employed to exfoliate materials into individual 2D layers 27 . Liquid exfoliation enables mass production of 2D nanosheets under atmospheric pressure at room temperature. However, this approach also leads to presumably unavoidable damage and non-uniform nanosheet thickness.

Wet chemical synthesis

Hydrothermal and solvothermal syntheses are representative wet chemical synthesis methods, in which materials are respectively solubilized in aqueous solution and organic solvent under high vapor pressure at elevated temperatures (~300 °C). A variety of nanomaterials have been synthesized in this fashion since the first report of hydrothermal synthesis of microscopic quartz crystals in 1845 (Fig.  2c ). The wet chemical synthesis of pure 2D materials such as graphene and MoS 2 surged in the early 21st century 28 , 29 , and more recently, doped 2D materials, nanocomposites, and their heterostructures have been synthesized in this fashion by adding various precursors and dopants in solvent to enhance the material properties for specific applications 30 , 31 , 32 , 33 . For example, the hydrogen evolution reaction in graphene oxide was dramatically enhanced by introducing boron dopants 33 .

The strengths of wet chemical synthesis include the controllability of surface morphology, crystallite size, and dopants in 2D materials for catalyst, energy storage, and chemical/biological sensor applications. Reaction temperatures, precursors, and additives have been optimized for various types of 2D materials and their composites, enabling essentially unlimited mass production. The direct synthesis of 2D materials on a desired substrate is also possible, although such synthesis takes a relatively longer time—up to a few days. Growth temperature is often limited to below 300 °C due to the limited durability of equipment under harsh conditions including high pressure and exposure to corrosive chemicals. It is worth noting that bottom-up synthesis tends to yield low-quality 2D materials with defects, but it is still possible to employ these for catalytic applications.

Perspectives and challenges toward industrialization

The abovementioned techniques enable mass production of 2D materials, but considerable further advances will be required for some specific applications. Single-crystal graphene films have been successfully synthesized at wafer scale with layer control, but the synthesis of other 2D materials such as hBN and TMDs are limited exclusively to single-crystal monolayer films. Thickness control of such materials is essential for tunneling barrier and high-performance electronics. The combination of tunable bandgap semiconductors, metals, and insulators in 2D systems can generate versatile heterostructures with remarkable physical properties. Several planar and vertical heterostructures have been generated to date, but these remain limited to micron scale 34 , 35 . More generally, the growth of various heterostructures at wafer scale is still challenging (Fig.  3a ). Atomic sawtooth surfaces could be ideal as a growth platform for single-crystal 2D materials including graphene, hBN, TMDs, and their heterostructures, but surface facet control remains elusive. The formation of wrinkles in 2D films after high temperature growth is another important issue, originating from the thermal expansion coefficient mismatch between 2D materials and growth substrate. Recently, the growth of fold-free single-crystal graphene films at 750 °C has been reported 36 , but further investigation will be required to see if this method is applicable for other 2D materials, and lower-temperature growth methods should be established.

a Single-crystal homo/heteroepitaxial growth, wrinkle formation by thermal expansion coefficient mismatch between 2D materials and growth substrates, and cracking/contamination during the transfer process are all issues presented by the CVD technique. b Inhomogeneous size and thickness of 2D nanosheets and poor production yield are problems associated with liquid exfoliation. c Low durability and instability of 2D materials by defects and environmental pollution remain challenges for wet chemical synthesis.

High temperature processes (above 400 °C) are not compatible with current Si technology, and 2D thin films grown by CVD at high temperature must therefore be transferred onto a target substrate. A conventional transfer process can give rise to serious problems such as folding and cracking of 2D films, ultimately degrading film homogeneity and device performance. Furthermore, the polymer contaminants that are commonly introduced as a supporting layer for the transfer process can give rise to unintentional doping and high contact resistance in heterostructure interfaces and devices. Therefore, methods for the direct growth of large-area 2D films by CVD or advanced roll-to-roll transfer technique would be highly desirable. For industrialization, the manufacturing process including scalable techniques (roll-to-roll, batch-to-batch, etc.), production capacity/cost, reproducibility, and large-area uniformity are further considered 37 .

Wet chemical processes including liquid exfoliation and wet chemical synthesis also face several challenges for the mass production of 2D materials. Liquid exfoliation employs pristine 2D bulk materials synthesized by CVT or flux methods for the mass production of 2D nanosheets. Those synthetic methods typically take at least one week, lowering the throughput of production, and companies need the capacity to provide these bulk materials at a larger scale. Additionally, the production yield of liquid exfoliation generally remains poor, and although some materials show relatively high yield, most 2D materials like hBN and telluride are not effectively exfoliated with current techniques. In addition, it is difficult to obtain 2D nanosheets of uniform size and thickness with this method (Fig.  3b ). In order to remedy this, improved techniques for sorting the synthesized nanosheets in terms of size and thickness (e.g., density gradient ultracentrifugation) are needed.

Bottom-up chemical synthesis typically produces 2D materials with low crystal quality. The defect sites (i.e., edges) often serve as active sites for 2D catalyst, but also give rise to low durability and instability issues. Moreover, 2D materials generated by chemical synthesis are not uniformly distributed in terms of size and thickness, requiring special care during synthesis. In addition, the byproducts frequently generated during chemical synthesis can inhibit catalytic activity. To resolve these material quality and byproduct issues, post-treatments such as thermal annealing and purification have been suggested, but a simple process without post-treatment would greatly improve productivity. Another important issue is the environmental pollution caused by the large amount of hazardous chemical wastes used in synthesis (Fig.  3c ), and the use of supercritical fluid regions could be considered as a shortcut to minimize chemical use 38 .

In addition, rapid and reliable non-destructive characterization tools are highly required to evaluate the wafer-scale 2D materials in terms of sample quality and uniformity. The current state-of-the-art terahertz image, phase-shift interferometry, and wide-field Raman imaging could be adopted to analyze the electrical and optical properties of 2D films with short acquisition time of a few seconds per mm 2 and high spatial resolution of an order of micrometers 39 , 40 , 41 . It still requires a prolonged period to thoroughly inspect 12-inch wafer-scale sample, and therefore, the development of advanced characterization tools is further desired.

From a materials point of view, there is plenty of room for unexplored novel 2D materials and their vdW heterostructures. Since it is almost impossible to explore all such materials experimentally, artificial intelligence-based material design could prove useful for the industrialization and large-scale manufacture of such newly-developed 2D materials 42 .

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Acknowledgements

K.K.K. acknowledges support by Samsung Research Funding & Incubation Center of Samsung Electronics under Project Number SRFC-MA1901-04, the Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Science, ICT & Future Planning (2018R1A2B2002302 and 2020R1A4A3079710). K.S.M. acknowledges support by the Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Science, ICT & Future Planning (2022R1A2C2009292). Y.S.J., C.S.H., K.K.K., and L.Y.H. acknowledge support by the Institute for Basic Science (IBS-R011-D1).

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These authors contributed equally: Soo Ho Choi, Seok Joon Yun.

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Center for Integrated Nanostructure Physics, Institute for Basic Science (IBS), Suwon, 16419, Republic of Korea

Soo Ho Choi, Seok Joon Yun, Ki Kang Kim & Young Hee Lee

Department of Energy Science, Sungkyunkwan University, Suwon, 16419, Republic of Korea

Soo Ho Choi, Seok Joon Yun, Yo Seob Won, Chang Seok Oh, Ki Kang Kim & Young Hee Lee

Department of Chemistry, Sookmyung Women’s University, Seoul, 14072, Republic of Korea

Soo Min Kim

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C.S.H., Y.S.J., K.S.M., K.K.K., and L.Y.H. designed and developed this work. W.Y.S., O.C.S., Y.S.J., and C.S.H. investigated the history and technical issues of the various production methods. All authors participated in the writing manuscript.

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Correspondence to Soo Min Kim , Ki Kang Kim or Young Hee Lee .

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Choi, S.H., Yun, S.J., Won, Y.S. et al. Large-scale synthesis of graphene and other 2D materials towards industrialization. Nat Commun 13 , 1484 (2022). https://doi.org/10.1038/s41467-022-29182-y

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DOI : https://doi.org/10.1038/s41467-022-29182-y

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Mass Production of the Black Soldier Fly, Hermetia illucens (L.), (Diptera: Stratiomyidae) Reared on Three Manure Types

Chelsea d. miranda.

1 EVO Conversion Systems, LLC, College Station, TX 77845, USA; moc.sysnocove@kcammacaj

Jonathan A. Cammack

Jeffery k. tomberlin.

2 Department of Entomology, Texas A&M University, College Station, TX 77843, USA; ude.umat@nilrebmotkj

Simple Summary

The black soldier fly (BSF) has gained a considerable amount of attention globally for its ability to convert organic material into valuable biomass for waste management and food and feed purposes. As the industry of producing BSF expands, connecting research and application is necessary to optimize mass-production facilities. Historically, research on the BSF has been conducted at a benchtop scale. Expanding these results to industrial practices is challenging, as results typically are not scalable. This study investigates the production of BSF fed animal manure (swine, dairy, and poultry) at a larger scale (thousands of larvae fed kg of diet) than what has been previously published (small-scale studies with hundreds of larvae fed g of diet).

Recent interest in the mass production of black soldier fly (BSF) larvae has resulted in many studies being generated. However, a majority of the studies are benchtop, or small-scale, experiments. Results generated from such studies may not translate to large-scale/industrial production. The current study was conducted at a conventional large-scale (10,000 larvae/treatment fed seven kg) to determine the impact on selected life-history traits when BSF were fed seven kg of manure (swine, dairy, or poultry) or a control diet (Gainesville diet: 50% wheat bran, 30% alfalfa meal, and 20% corn). Results showed larvae fed dairy manure took one to two days longer to develop to prepupation, with lower survivorship (45%) compared to those fed poultry or swine manure (>70%). Furthermore, the maximum larval weight was reached on day six for those fed swine manure, while other treatments achieved the maximum weight on day seven. However, larvae fed swine manure averaged 150 mg, while those fed the other diets ranged between 175 and 200 mg. Data from this study may be valuable for the industrialization of BSF. Companies using a scale varying from previously published work, including this study, should conduct pilot studies to optimize their system prior to implementation.

1. Introduction

Insects provide a variety of goods and services for human exploitation [ 1 ]. They may be reared for medicinal purposes, such as wound therapy [ 2 ], or to engineer antibodies [ 3 ] and vaccines [ 4 ]. They may be cultivated for other well-known purposes, such as honey [ 5 ], silk [ 6 ], and dye production [ 7 ], or can be used to control insect pest populations [ 8 ]. Insects may also be used for food and feed purposes [ 9 ]; however, this industry is still in its infancy in terms of operating on an industrial scale. Recent interest in exploiting insects in this manner has prompted numerous studies [ 10 , 11 , 12 , 13 , 14 ], which helps progress the idea and refine the industry; however, a majority of the published studies are based on small-scale (benchtop) experiments, which may not truly represent what occurs on a larger industrial scale.

The black soldier fly (BSF), Hermetia illucens (L.), (Diptera: Stratiomyidae) has gained a considerable amount of attention. As discussed in previous publications, this species is distributed globally throughout temperate and tropical regions and is an ideal candidate for industrialization purposes, because it offers a means to manage a variety of wastes [ 15 , 16 , 17 ] and provides multiple revenue streams, such as the production of animal feed [ 9 ], biofuel [ 18 , 19 ], and fertilizer [ 20 ]. In systems using manure as a resource, the BSF reduces dry matter [ 21 ], pathogens [ 22 , 23 ], and odors [ 24 ]. However, most previously published work on BSF was performed on a small scale (e.g., several hundred larvae per replicate), which may not translate to an industrial scale.

Methods used in small-scale studies are typically different than those employed by mass-production facilities (larval numbers in the thousands and fed kilograms of substrate rather than hundreds of larvae consuming grams over time). Both factors are known to impact development. For example, Banks et al. [ 25 ] showed that bulk feeding increased the development time and larval weight across three densities (1, 10, and 100 larvae) compared to those fed incrementally. Similarly, Barragán-Fonseca et al. [ 26 ] found that, with small-scale densities (50, 100, 200, or 400 larvae), an increased larval density lead to greater delays in development (up to 45 days) on low-nutrient diets but not on high-nutrient diets. Variations in the development time, larval and adult weights, and survivorship have also been reported across different larval densities (500–2000 larvae) of BSF fed the same diet [ 27 ]. Even the authors of the study being presented here have conducted such studies [ 28 , 29 ]. However, all of these studies are considered small-scale when compared to practices in the industry, and it is not known if similar results would occur on a larger scale.

Larval BSF density can hinder or, in some instances, enhance their performance. Bryant and Sokal [ 30 ] showed that low densities (80 eggs/18,000 mg of diet) and high densities (640 eggs/18,000 mg of diet) of house flies, Musca domestica L., (Diptera: Muscidae) faced different consequences during development. Low densities may result in poor conditioning of the diet (via metabolites produced by larvae), which impacts yeast growth and, ultimately, the availability of food [ 30 ]. However, an increased larval density may intensify the effects of competition, leading to reduced survivorship [ 30 , 31 ]. Larvae feed in aggregates generate heat [ 32 ], which, in turn, impacts BSF development and survivorship. Black soldier fly larvae reared at 30 °C developed the fastest (13 d), had the shortest prepupal development (8–10 d), and had the highest larval survivorship (90%) compared to those reared on temperatures that ranged from 10–42 °C [ 33 ]. Additionally, it is possible that higher densities produced more oral secretions (gut microbiota) that aided in the cooperative digestion of a resource [ 34 ]. As such, the larval density is a major factor that influences BSF performance.

The purpose of this study was to evaluate selected life-history traits of BSF fed swine, dairy, or poultry manure by using methods based on industrial standards [ 35 ]. Most of the data available on this species originates from small-scale studies, which may not translate to a larger production scale, as previously discussed. Results from this study may be valuable by providing a basis to compare findings from previous small-scale studies, as well as a paradigm to help optimize the mass-rearing conditions of BSF fed manure.

2.1. Acquisition of BSF

Methods for this study were based on those conducted by Miranda et al. [ 29 ]. Black soldier flies were obtained from a colony that is maintained at the F.L.I.E.S. (Forensic Laboratory for Investigative Entomological Sciences) Facility at Texas A&M University in College Station, TX, USA. The colony originated from a colony maintained in Tifton, GA, USA and was maintained following modified methods proposed by Sheppard et al. [ 36 ].

2.2. Acquisition of Manure

Manure less than 12-h-old was used in this study. Swine manure was collected from a farm in Anderson, TX, USA, dairy manure was collected from a commercial dairy located in Stephenville, TX, USA, and poultry manure was collected from layer hens housed at the Poultry Science Research, Teaching and Extension Center at Texas A&M University, College Station, TX, USA. Manure was placed into 18.9 L buckets, covered with lids (Home Depot ® , Leaktite™, Leominster, MA, USA), and transported to the F.L.I.E.S. Facility, where it was homogenized by hand-mixing for 5 min, transferred to 3.7 L Ziploc ® Freezer bags (S.C. Johnson & Son, Inc., Racine, WI, USA), and stored at −20°C until used. Before initiation of the experiment, the manure was allowed to thaw at room temperature for 24 h. Moisture contents of manure were measured gravimetrically with three 10 g samples following the methods described by Franson [ 37 ]. Initial moisture content for swine, dairy, and poultry manure were 72%, 83%, and 77%, respectively.

2.3. Experiment Design

Black soldier fly adults were maintained at the F.L.I.E.S. (Forensic Laboratory for Investigative Entomological Sciences) Facility in a 260 × 116 × 129 cm wooden cage lined with a fiberglass window screen (18 × 16 mesh size) in a greenhouse (25 °C, >50% relative humidity (RH)). To collect eggs, a 5.7 L Sterilite ® container (Sterilite ® , Townsend, MA, USA) was filled with 500 g Gainesville diet (50% wheat bran, 30% alfalfa meal, and 20% corn meal) [ 38 ] saturated with RO (reverse osmosis) water (70%). Corrugated cardboard was cut into 5.0 × 2.0 × 0.5 cm pieces with five taped together to form a bundle, which was placed on the lid of the container described above. The lid of the container had a 15 × 7 cm hole cut in the center of the lid and was covered with wire mesh. The container remained in the wooden cage for 8 h, after which the cardboard was removed from the cage and placed in a 0.9 L Ball ® mason jar (Ball Corporation, Broomfield, CO, USA) covered with a paper towel, which was secured with the metal ring of the mason jar lid. The jar with the cardboard containing the eggs was stored in a Rheem Environmental Chamber (Asheville, NC, USA; 29 °C, 60% RH, and 16L:8D (light:dark)) until larvae were enclosed. Ten replicates of 100 newly-hatched larvae were hand counted and then weighed on an OHaus ® Adventure ™ Pro AV64 balance (OHaus ® Corporation, Pine Brook, NJ, USA) to get the average weight of an individual larvae, which was then used to weigh approximately 10,000 larvae per replicate. Larvae were placed in 0.5 L deli food storage containers (Amazon.com Inc., Seattle, WA, USA) without a lid and were fed 150 g of Gainesville diet (70% moisture) for four days to decrease larval mortality prior to use in the experiment.

Treatments consisted of 10,000 4-d-old larvae fed 7 kg of swine, dairy, or poultry manure. Larvae in control groups were fed 7 kg of Gainesville diet (70% moisture). Larval diets were placed in the center of a 30 L Sterilite ® ClearView Latch ™ storage container, with 700 g of dry Gainesville diet [ 38 ] placed around the perimeter of the wet diet to serve as a pupation substrate and to prevent developing larvae from escaping. Larvae were weighed prior to placement on the manure or Gainesville diets to determine that their weights were not significantly different. The deli containers with developing larvae were poured on top of the diets, and the containers (with the larvae and diets) were placed inside the environmental chamber (via complete randomized block design) described above. Three replicates of each treatment and control were used, and two trials were conducted.

Larvae were allowed to feed on the manure or Gainesville diets for two days prior to measuring the daily larval weight, as they were too small to find without significantly disturbing the media. The daily larval weight was measured by attempting to select 10 of the largest larvae for nine days, and a different set of larvae was selected each day. The development time to first prepupation was recorded upon observation of the first prepupa within a given container. On the day the first prepupa was observed, larvae were sifted from the media, and survivorship was calculated by dividing the total weight of all living larvae from each replicate by the average final larval weight. After the total larval weight was recorded, larvae were placed in 30 L Sterilite ® containers with 1 kg of dry Gainesville diet. The prepupal weight was measured by selecting 10 of the largest prepupae from each replicate when 40% reached the prepupal stage. All weights were measured using the balance described above.

2.4. Statistical Analyses

Larval weight, development time from placement on the manure to prepupation, percent prepupation (survivorship), and prepupal weight were analyzed across treatments and trials. An ANOVA was performed for each parameter listed. Statistics were performed using JMP ® PRO 14 (SAS Institute Inc., Cary, NC, USA). Normality was checked using a Shapiro-Wilk test, and equality of variance was checked using a Bartlett’s test. Tukey’s HSD (honest significant difference) was used for mean separation ( p ≤ 0.05).

3.1. Larval Weight

Larval weight did not differ significantly across larval diets (F 3,142 = 1.9318; p = 0.1263). A significant trial effect was found (F 1,142 = 163.6540; p < 0.0001), but no significant treatment by trial interaction was found (F 27,142 = 0.7314; p = 0.8178). In general, individuals in trial two weighed 22% more than those in trial one. Larvae reared on swine manure reached a maximum weight on day six, while those fed the other diets did so on day seven. Furthermore, the maximum weight of larvae fed swine manure (150 mg) was less than those fed the other diets (175 to 200 mg) ( Figure 1 ).

Mean larval weight (mg) ± SEM ( 1 n = 6) of black soldier flies fed 7 kg of swine, dairy, or poultry manure or the Gainesville control diet [ 38 ] at 29 °C, 60% relative humidity (RH), and 16L:8D. 1 n = number of replicates per treatment.

3.2. Development Time to First Prepupation

Development time to first prepupation differed significantly (F 3,16 = 16.9048; p < 0.001) across the larval diets. No trial effect (F 1,16 = 0.1429; p = 0.7104) or treatment by trial interaction (F 3,16 = 0.5238; p = 0.6721) was found. The shortest development time was found for those fed the Gainesville diet (13 d). In regard to those fed manure, the shortest development time was found for those fed poultry (14 d) and swine manures (15 d), whereas those fed dairy manure took an additional day (16 d) to reach prepupation ( Figure 2 ).

Development time (d) to first prepupation (mean ± SE, 1 n = 6) of black soldier fly larvae fed 7 kg of swine, dairy, or poultry manure or the Gainesville control diet [ 38 ] at 29 °C, 60% RH, and 16L:8D. Different letters (A–C) indicate significant differences between treatments (α = 0.05) and ANOVA, followed by Tukey’s HSD. 1 n = number of replicates per treatment.

3.3. Percent Prepupation

Survivorship to prepupation was significantly different (F 3,16 = 22.2899; p < 0.0001) across the larval diets. No trial effect (F 1,16 = 0.6001; p = 0.4498) or treatment by trial interaction (F 3,16 = 1.2535; p = 0.3235) was found. The highest percent prepupation across all diets was found for those fed the Gainesville diet (88%). Survivorship to prepupation was significantly lower in dairy manure (45%), but not in poultry (78%) or swine (73%) manures, relative to the Gainesville diet ( Figure 3 ).

Percent prepupation (mean ± SE, 1 n = 6) of black soldier fly larvae fed 7 kg of swine, dairy, or poultry manure or the Gainesville control diet [ 38 ] at 29 °C, 60% RH, and 16L:8D. Different letters (A, B) indicate significant differences between treatments (α = 0.05) and ANOVA, followed by Tukey’s HSD. 1 n = number of replicates per treatment.

3.4. Prepupal Weight

Prepupal weight did not differ significantly (F 3,16 = 0.5997; p = 0.6245) across the larval diets. No trial effect (F 1,16 = 3.5717; p = 0.0770) or treatment by trial interaction (F 3,16 = 0.0837; p = 0.9679) was observed. Larvae fed the Gainesville diet weighed approximately 173 mg, and those fed poultry, swine, and dairy weighed 163, 152, and 167 mg, respectively ( Figure 4 ).

Prepupal weight (mg) (mean ± SE, 1 n = 6) of black soldier fly larvae fed 7 kg of swine, dairy, or poultry manure or the Gainesville control diet [ 38 ] at 29 °C, 60% RH, and 16L:8D. Different letters (A) indicate significant differences between treatments (α = 0.05) and ANOVA, followed by Tukey’s HSD. 1 n = number of replicates per treatment.

4. Discussion

The results from this study demonstrate that diet can impact the production of BSF. Larvae fed the Gainesville diet [ 38 ] had the shortest development time (13 d) ( Figure 2 ), the highest survivorship (88%) ( Figure 3 ), and produced the heaviest prepupae (173 mg) ( Figure 4 ). In regard to those fed manure, variations in development time and survivorship were found across manure types. Although larval ( Figure 1 ) or prepupal weights ( Figure 2 ) did not differ across treatments ( p < 0.05), a longer development time (one to two days) was required for larvae to reach the prepupal stage, and fewer larvae survived (45%) when fed dairy manure. Similarly, in regard to the maximum weight, those fed swine manure reached their peak weight one day earlier than those fed dairy or poultry manures but weighed 25–50 mg less. These differences are important in respect to production efficiencies and bioconversion and may be explained by variations in the manure types.

Manure from different animals varies in chemical and physical compositions [ 39 ]. Poultry manure is typically higher in nutrients and lower in fiber than dairy manure [ 40 ], and these differences may explain differences in development and survivorship in the current study. Variation in development time and survivorship could translate to variation in production efficiency and bioconversion yields. Although prepupal weights were not significantly different across the treatments ( Figure 4 ), slower developments for those fed dairy manure ( Figure 2 ) and lower survivorship ( Figure 3 ) may have implications in higher costs of rearing (longer development time) and lower revenue (less yield). It is possible that those fed dairy manure were able to reach similar prepupal weights to those fed swine or poultry manures because the larvae were fed on the resource longer and were subject to reduced intraspecific competition because of high mortality. Additionally, BSF are thought to be generalist feeders, capable of digesting various wastes [ 15 , 17 , 41 ]. Compared to house flies, BSF have a larger arsenal of digestive enzymes that helps them acquire adequate nutrition from a variety of substrates to sustain their adult stage [ 41 ]. It is possible that the larval and prepupal weights did not differ significantly because BSF have such a wide range of digestive enzymes.

Previous studies that focus on BSF fed manure have been performed on a smaller scale (i.e., lower number of larvae per replicate) than the current study. Myers et al. [ 21 ] were the first to examine BSF development on dairy manure. Specifically, this study fed three hundred four-day-old larvae 27, 45, 54, or 70 g of dairy manure daily and found that the larval development to prepupation was significantly different ( p ≤ 0.05) between the lower feed ration and the other rations and lasted 26–30 d, which was up to two weeks longer than the findings from the current study (16 d). Survivorship to prepupation was not significantly different across the treatments for the aforementioned study (71–77%) but was greater than the survivorship found in the current study (45%). The prepupal weight was significantly different ( p ≤ 0.05) across the treatments in the small-scale dairy study (89–137 mg), and this was less than that observed in the current study (167 mg). However, when comparing the current study to another small-scale study that used a different manure type, such as poultry manure, impacts on the prepupal weight and development time were similar, but survivorship differed across the scales. For example, Lalander et al. [ 17 ], fed two hundred 10-d-old larvae poultry manure (40 mg DM/larva/d) and found prepupae weighed 165 mg, and those from the current study weighed 163 mg with the same development time to prepupation from the placement on manure (14 d). However, the current study found a lower survivorship (78% in the current study vs. 92% in Lalander et al. [ 17 ]). Yet, when we examine findings from our own small-scale study [ 29 ], which used larvae that were derived from the same colony as the current study, less time was needed for development in the small-scale study for those fed poultry manure (11 d vs. 14 d in the large-scale study), but more time was required in the small-scale study for those fed swine manure (17 d vs. 15 d in the current study), and larvae fed dairy manure required 16 d to develop, regardless of the scale. Although the percent prepupation was similar for those fed swine manure (84% vs. 73% in the current study), differences were more obvious for those fed dairy (93% vs. 45% in the current study) or poultry manures (78% vs. 95% in the current study). Additionally, differences in prepupal weight across the scales are apparent for swine, dairy, and poultry manures, as those in the small-scale study weighed 83, 99, and 114 mg compared to 152, 167, and 163 mg, respectively, in the current study.

Based on a comparison between this study and others conducted at a smaller scale, scale likely impacts the production of the BSF. Despite the fact that some aspects of the methodologies from some of the small-scale studies differed (such as rearing conditions and age of larvae at the initiation of the experiment) from the current study, there is overlap in methodologies among the studies that helps eliminate these factors from consideration as potential reasons for variation across the scales. For example, the rearing temperature for Myers et al. [ 21 ] (27 °C), and Lalander et al. [ 17 ] (28 °C) differed from the current study (29 °C); however, it is unlikely that this factor is largely responsible for differences across the scales, as Miranda et al. [ 29 ] used the same rearing temperature described by the current study, and differences in the development time, survivorship, and weight were found. The relative humidity should also not be considered influential, as most studies reared larvae at or around 60% RH. Additionally, although the age of the larvae at the initiation of the experiment differed between Lalander et al. [ 17 ] and the current study, it is also unlikely that this factor is responsible for the variations among the studies, because Myers et al. [ 21 ], Miranda et al. [ 29 ], and the current study conditioned larvae on the same diet (Gainesville diet [ 38 ]) for the same amount of time (four days) prior to the initiation of the experiment, and differences were found between these studies as well.

Interestingly, diet compositions across the manure types likely impacts the variation across the scales. For example, the development time did not differ for larvae fed dairy manure between Miranda et al. [ 29 ] and the current study, but differed for those fed poultry manure. Yet, when we compared the findings from Myers et al. [ 21 ] for dairy manure and those from Lalander et al. [ 17 ] for poultry manure to the current study, we saw that the opposite occurred, with delayed development reported by Myers et al. [ 21 ] for those fed dairy manure (26–30 d vs. 16 d) and the same development time as the current study for those fed poultry manure by Lalander et al. [ 17 ] (14 d). As previously discussed, manure types vary in chemical and physical properties and can vary within the same type, which may explain the differences observed between our study and previous small-scale studies. The development time is influenced by weight and survivorship, and so, the diet composition impacts those parameters as well. Furthermore, we find when comparing our study to Miranda et al. [ 29 ], which used larvae from the same colony with the same rearing conditions, and manure collected from the same facilities as the current study; differences across the manure types for development time, prepupal weight, and survivorship do not follow the same pattern across the scales. For example, for development time, the results were similar regardless of the scale, with swine and dairy not significantly different ( p ≤ 0.05) from each other but significantly different from poultry manure in either study. Larvae from the small-scale experiment developed faster on poultry manure (by three days) than those in the large-scale study, and these findings correlate with those from Barragán-Fonseca et al. [ 26 ], which found that lower densities and higher nutrient concentrations accelerated development. However, the pattern of differences across manure types for prepupal weights differed across the scales, with more pronounced differences among the manure types at the smaller scale compared to the larger scale. Specifically, larvae fed swine manure in the small-scale study were significantly different ( p ≤ 0.0001) in regard to prepupal weights from those fed poultry manure, but larvae fed swine, dairy, or poultry manure in the large-scale study were not significantly different ( p = 0.0624). Barragán-Fonseca et al. [ 26 ] found that the weights increased with the increased nutrient concentrations, and this was the case for the small-scale study but not for the large-scale study, as those fed dairy manure weighed more (167 mg) than those fed poultry (163 mg) or swine (152 mg). Although dairy manure is generally considered a lower-quality manure compared to swine or poultry manure, higher prepupal weights for larvae fed dairy manure may be explained by the lower survivorship, as previously discussed. Finally, the pattern of differences across manure types for percent of pupation differed across the scales, with more pronounced differences on the larger scale ( p ≤ 0.0001) than in the smaller scale ( p = 0.0004), but the findings from our studies do not agree with Barragán-Fonseca et al. [ 26 ] that survivorship increases with higher densities, as fewer individuals were produced from the large-scale study (45–78% survivorship) compared to the small-scale study (84–95% survivorship); however, our findings do agree that survivorship increases with increasing nutrient concentrations. The extent of the impact of diet compositions on differences across the scales is poorly understood due to a lack of large-scale studies; therefore, small-scale studies should include a large-scale component when possible.

Other factors known to influence BSF development are moisture [ 28 , 42 , 43 ], pH [ 44 , 45 ], species strain [ 46 ], and size of the rearing container [ 47 ]. However, because most studies are conducted with a few-hundred larvae, the impact of these factors is not necessarily the same at higher scales. It may thus be difficult for individuals interested in mass-producing BSF to extrapolate and apply information with expectations similar to those reported from studies that use methods that differ from industrial standards. It should be noted that the authors of this paper have also performed small-scale studies [ 28 , 29 ] but recognize that the outcomes of these studies may differ at a larger scale. Additionally, there are facilities that produce larvae at higher densities than 10,000 larvae and provide larvae more than 7 kg of diet, and so it is possible that the results from this study may not translate on a higher production scale. For these reasons, future studies should investigate BSF life-history parameters at larger scales than the current study.

5. Conclusions

The current study shows differences in the development time and survivorship for larvae fed different manure types. Although no significant difference was found across the manure types for prepupal weight, those provided dairy manure took one to two days longer to develop, with fewer individuals surviving to the prepupal stage (45% vs. >70%) when compared to those provided swine or poultry manures. Additionally, this study highlights the potential differences likely to exist across the production scales and urges future studies to perform their work on larger scales to advance the industrialization of BSF.

Acknowledgments

The authors wish to thank Melanic Osegueda and Sydney Busch for their assistance in maintaining the fly colonies as well as their efforts during the experiment. We also would like to thank Brittny Jones, Zanthé Bruce, and Aline Malawey for their efforts maintaining the BSF colony.

Author Contributions

Conceptualization, C.D.M. and J.K.T.; investigation, C.D.M; methodology, C.D.M. and J.K.T.; supervision, J.K.T.; writing—original draft preparation, C.D.M.; and writing—review and editing, C.D.M., J.A.C., and J.K.T. All authors have read and agreed to the published version of the manuscript.

The F.L.I.E.S. Facility at Texas A&M University would like to thank Fluker Farms (Port Allen, LA, USA) and EVO Conversion Systems, LLC (College Station, TX, USA) for their partial financial support of this project.

Conflicts of Interest

The authors declare no conflicts of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results.

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Article Contents

Introduction, structure and definition of graphene, basic properties and applications proposed in laboratory-scale research, mass production of graphene materials, some commercial applications of graphene materials on the market, summary and outlook, acknowledgement, declarations.

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Mass production and industrial applications of graphene materials

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Yanwu Zhu, Hengxing Ji, Hui-Ming Cheng, Rodney S Ruoff, Mass production and industrial applications of graphene materials, National Science Review , Volume 5, Issue 1, January 2018, Pages 90–101, https://doi.org/10.1093/nsr/nwx055

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Graphene is considered a promising material for industrial application based on the intensive laboratory-scale research in the fields of physics, chemistry, materials science and engineering, and biology over the last decade. Many companies have thus started to pursue graphene materials on a scale of tons (for the flake material) or hundreds of thousands of square meters (for the film material) for industrial applications. Though the graphene industry is still in its early stages, very significant progress in mass production and certain industrial applications has become obvious. In this report, we aim to give a brief review of the mass production of graphene materials for some industrial applications and summarize some features or challenges for graphene in the marketplace.

Graphene has attracted attention worldwide and is considered a promising material for industrial applications. Before the exfoliation of graphene with Scotch tape was reported in 2004 [ 1 ], several groups had exfoliated graphite to thin platelets [ 2 , 3 ], and identified ‘single-layer graphite’ on noble metal surfaces as grown by chemical vapor deposition (CVD) [ 4 ]. Properties and applications of graphene have been the subject of studies by the physics, chemistry, materials science, biology, biomedical and energy research communities, among others [ 5–7 ]. The 2010 Nobel Prize in Physics was awarded for “groundbreaking experiments regarding the 2D material, graphene” [ 1 ]. Around 2009, several research groups achieved breakthroughs in developing macro-scale CVD synthesis of graphene [ 8–10 ]. Earlier research on graphite oxide [ 6 , 11 ], its exfoliation in water and manipulation of the chemical properties of the resulting ‘graphene oxide’ sheets led to breakthroughs in its use in conductive polymer composites at a low loading level [ 12 ], to the generation of ‘paper-like’ films [ 13 ], and then later to their use as an electrode material in supercapacitors, their first use in electrical energy storage [ 14 ] and in many other applications [ 5 , 6 , 15–20 ]. These laboratory-scale pioneering results triggered intense interest in the mass production and industrial applications of graphene materials.

Many start-up companies as well as existing industrial enterprises have thus pursued graphene materials on a scale of tons (for the flake material from either graphite oxide or graphite itself), or hundreds of thousands of square meters (for graphene films made by CVD). They and other companies have also started to develop graphene-related products. In this report, we aim to give a brief summary of the mass production of graphene materials for some industrial applications. It is not our intent to exhaustively cover every application. We first define what is meant by graphene and ‘graphene-like’, briefly outline some of the basic properties of graphene and then introduce actual applications and some commercial products on the current market.

Graphene by definition is a single layer of carbon atoms organized in a 2D, atom-thick, ‘honeycomb’ lattice by sp 2 hybridized C–C bonds between two adjacent carbon atoms (IUPAC, 1995) [ 21 ]. It is worth noting, however, that the term is used more liberally to also include materials that have multi-layer graphene or few-layer graphene, that is, more than one layer of graphene stacked on top of each other. Various microscopy techniques have allowed observation of the atomic lattice of suspended graphene, as well as defects such as adatoms, vacancies, holes and so on [ 22 ]. In graphene samples the atom-thick layer is mechanically compliant and so sheets (also called platelets) are often wrinkled and/or crumpled, and, in many applications, the carbon atoms in the basal plane are functionalized with various chemical groups to enable the commercial application of interest. That is, almost all ‘graphene materials’ are different from the idealized 2D ‘graphene structure’ as proposed in 1947 [ 23 ]. What is now referred to as graphene was originally obtained by surface scientists by CVD on a variety of substrates; for example, see the perspective by Ruoff [ 24 ]. Thus with reference to commercial products, it should be appreciated that ‘graphene’ or ‘graphene-like’ refers to atom-thick layers that might be chemically functionalized and contain various sorts of defects, and are used in real applications.

Here we briefly summarize the basic properties and potential applications of graphene, and note that several review articles are provided here [ 15 , 25–27 ].

A perfect graphene sheet is a zero-bandgap semiconductor with a cone-like band structure near the Dirac point that displays an ambipolar electric field effect in which charge carriers (electrons or holes) show a linear dispersion relationship in concentrations of up to 10 13 cm −2 [ 1 , 5 ]. In addition, graphene has a half-integer quantum Hall effect (QHE) for both electron and hole carriers and also a high electron mobility of 1.5 × 10 4 cm 2 ·V −1 ·s −1 at room temperature, which is nearly independent of temperature between 10 K and 100 K [ 28–31 ]. Each additional graphene layer adds an optical absorption of ∼2.3% in a broad wavelength ranging from ultraviolet to near infrared, as a consequence of graphene's electronic structure [ 32 ]. The absorption becomes saturated when the input optical intensity is above a threshold value, leading to a nonlinear optical behavior [ 33 , 34 ]. The thermal conductivity of suspended graphene was stated to be in the range of ∼(4.84 ± 0.44) × 10 3 to (5.30 ± 0.48) × 10 3  W/mK at room temperature from Raman measurements [ 35 ], and it remains as high as about 600 W/mK when graphene is supported on SiO 2 , exceeding the value for metals such as copper and conventional thin-film electronic materials [ 36 ]. With a Young's modulus of 1060 GPa, and an intrinsic strength of 130 GPa, a free-standing graphene membrane has a breaking strength of 42 N/m, much stronger than steel's if one assumes a similar thickness [ 37 , 38 ]. Graphene is impermeable to all atoms and molecules under ambient conditions [ 39 , 40 ]. Hydrogen, the smallest atom, is predicted to take billions of years to penetrate graphene [ 41 , 42 ]. Monolayers of graphene, however, are permeable to thermal protons under ambient conditions, whereas no proton transport has been detected for bilayer graphene [ 43 ]. Although graphene is structurally stable and moderately chemically inert, chemical processing such as oxidization or fluorination may break the carbon bonding and introduce functional groups in graphene, thus bringing more variety in the properties and functions [ 44 , 45 ]. When functional groups are covalently attached to graphene, its highly extended pi electron cloud is disrupted, changing its electronic properties [ 46 ].

Graphene has been considered a good candidate for many applications, ranging from electronics [ 47 , 48 ], photonics [ 17 , 49 , 50 ], energy generation and storage [ 51–53 ], thermal management [ 54 , 55 ] and functional materials [ 12 , 56 ] to bio-applications [ 57 , 58 ], and many others. It is worth noting that potential applications of graphene can depend on the morphology and structure, which are mostly determined by the production methods and subsequent processing techniques. In the following, the techniques for preparing graphene, especially by mass production, are reviewed.

Many reviews have been published on the preparation of graphene materials on a laboratory scale [ 16 , 25 , 59 , 60 ], and here the focus is on the industrial-scale production of graphene materials and related issues. The techniques for the mass production must be able to meet the needs for the scale of testing in industry, which is typically a kilogram of powder or suspension containing graphene flakes (typically of micrometer scale), or a thousand pieces for continuous graphene films (usually larger than millimeter size). Considering the following factors: (i) the demands of attaining the desired properties and form/morphology for target graphene products; (ii) the quality and applications of the graphene materials; (iii) the scalability from laboratory to industry; and (iv) the stability and controllability of manufacturing, we note that the current production techniques used in industry are mainly the exfoliation of graphite, exfoliation/reduction of graphite oxide and CVD.

Direct liquid-phase exfoliation of graphite

Graphite is cheap and abundant, and the key to its exfoliation is overcoming the van der Waals interaction between graphene layers while maintaining the size of the graphene platelets. In addition to the energy input such as sonication, stirring, shearing forces, ball milling and so on, proper selection of solvents and surfactants is helpful in improving the yield of graphene platelets from graphite [ 61–63 ]. More importantly, the graphene platelets that are obtained by mechanical exfoliation potentially maintain the conjugated structure that exists in graphite, and may thus have good electrical conductivity and other properties predicted or measured for graphene. Since exfoliation is usually carried out in a solvent, its removal may cause severe restacking of the graphene platelets due to the van der Waals forces and (if present) capillary forces between them upon drying. Thus, the typical graphene products obtained from the direct exfoliation of graphite are suspensions or slurries, and the presence of solvents and other additives needs to be considered when the graphene suspensions are later used.

We have identified several companies that have reported producing graphene-containing suspensions/slurries based on the exfoliation of graphite (or similar precursors such as expanded graphite). Applied Graphene Materials plc in the UK was set up in 2010 and is advertising graphene dispersions on their website. Several companies (e.g. Ningbo MORSH, Qingdao Haoxin New Energy Technology, Dongguan SuperC Technology, Deyang Carbonene Technology) in China claim to use ‘physical exfoliation’ to produce graphene materials on the scale of hundreds to thousands of tons (of suspensions or slurries). For example, Dongguan SuperC Technology Ltd has announced a production capability of 10 000 tons of graphene suspension per year. As the exfoliation of graphite typically leads to a wide distribution of number of layers for the flakes, the suspensions have to be subjected to harsh separation processing to obtain graphene with a certain number of layers; chemical additives such as surfactants are often needed to keep the suspension stable for a long time. With better control of the thickness uniformity and stability, graphene materials from the direct exfoliation of graphite may have promise for use in paints and inks, as conducting additives in battery electrodes, as conducting fillers in composites and so on.

Oxidization of graphite and the subsequent exfoliation and/or reduction

Another well-known approach to exfoliate ‘graphitic layers’ is through oxidative intercalation using oxidizing agents such as sulfuric and nitric acids, and potassium permanganate. The oxygen functional groups in oxidized graphite are prevalent in the individual layers and thus sp 3 -hybridized carbon atoms are prevalent in the sp 2 -hybridized carbon network of the layers in graphite, leading to the product called graphite oxide [ 11 , 64–66 ]. Graphite oxide was first prepared by Brodie about 150 years ago [ 67 ], and was used by Boehm et al. for the preparation of thin graphene-containing platelets in 1962 [ 68 ]. With the increased interlayer distance including that due to adsorbed water, which is present as interlamellar (interlayer) H 2 O molecules that are bonded both to themselves and to the epoxide and hydroxyl functional groups on the layers, a small energy input such as stirring or bath-ultrasonication could break the interaction between oxidized graphene layers and yield dispersed individual layers: ‘graphene oxide’. A subsequent process to eliminate the majority of the oxygen functional groups, often called reduction but sometimes referred to as deoxygenation, can be used to partially recover the conjugated structure and electrical conductivity. Many approaches, e.g. using reducing regents to react with the oxygen functional groups, or ‘burning’ off the oxygen with thermal/microwave heating, irradiation, plasma/ion bombardment, have been developed to reduce graphite oxide or graphene oxide in the past decade [ 69–73 ]. Ruoff's group has demonstrated the impressive properties and potential applications of ‘paper-like’ materials made from graphene oxide and composites containing reduced graphene oxide mixed with polymer [ 12 , 13 ].

Products derived from graphite oxide include reduced graphite oxide and reduced graphene oxide powders as well as suspensions of graphene oxide made by exfoliating graphite oxide in solvents, and suspensions of reduced graphene oxide. The detailed morphology, structure and chemical components of the graphite-oxide-derived products are sensitive to the processing parameters and the equipment used, because the manufacturing processes involve chemistry and chemical engineering. This has several implications for production of ‘graphene’ based on graphite oxide. First, since the products are highly dependent on the manufacturing technique, products made by different companies may be very different in terms of physical morphology and chemical properties, although the companies may use similar techniques for manufacturing the graphite oxide. Second, due to the different and complicated morphological, structural and chemical features of graphene materials based on graphite oxide, the use (application) of such products often needs to be coordinated with the manufacturer. The complex relationship between the graphene materials and their applications may mean that most of the products from graphite oxide must be ‘custom-built’ and are definitely not ‘one type fits all’ applications. In addition, standardization for future industrial use will be difficult (but, of course, still important) because of differences in raw materials, subtle differences in manufacturing and the difficulties in its control, and the role of graphene materials in their final applications. Oxidation of graphite has been used by a few start-up companies to produce graphene materials, because the chemical processing is scalable. The Sixth Element Materials Technology (Changzhou) Co. Ltd announced a production capability of 100 tons of graphene oxide per year in 2012 (Fig.  1 a). Yan Qu, CEO of The Sixth Element notes, “… we are surprised by the wide range of applications of graphite-oxide-derived materials, from thermal dissipation films, to composites, and a conducting additive in the electrode of Li-ion batteries.” Further understanding of the chemistry during the materials processing of graphite oxide and of applications will be helpful in achieving products and performance with better stability and controllability.

(a) Graphene powder production line in The Sixth Element Materials Technology Co. Ltd. (b) Graphene film production line of Wuxi Graphene Films Co. Ltd. All photos are used with permission of copyright.

Chemical vapor deposition (CVD)

The CVD technique used in producing industrial graphene films is mainly based on the research published in Science in 2009 by Ruoff's group [ 74 ], namely, the growth of graphene on Cu foil from methane and hydrogen. In 2010, Hong, who cooperated with Samsung Tech., demonstrated a prototype manufacturing line that was able to produce rectangular graphene films 30 inches along a diagonal [ 75 ]. The CVD production of graphene typically has four steps: (i) synthesis of graphene films on metal foils such as Cu foils by CVD, (ii) removal of the metal, (iii) transfer of the graphene films onto a desired substrate, and (iv) doping the graphene film for reduced sheet resistance if needed. The CVD process can be carried out at either a low pressure (∼0.1 Torr) or at ambient pressure [ 76 ] and both have been applied in pilot lines for the industrial production of graphene. Currently, removing the Cu by chemical etching has been intensively used for graphene production. However, Cu accounts for more than 50% of the cost. There are several other potential methods available on a laboratory scale, e.g. electrochemical bubbling transfer [ 77 ] and electrostatic-force-assisted transfer [ 78 ], and these or other methods might be useful in the future on the industrial scale. To avoid breaking the graphene during transfer, it is protected with a covering polymer film that is removed after the graphene film has been transferred onto the target substrate. Alternatively an adhesive can be applied between the target substrate and the graphene on Cu, and the subsequent Cu etching leaves graphene on the target substrate with the adhesive layer in between. Both techniques are currently used for CVD graphene production in industry. To reduce the sheet resistance of the as-prepared CVD graphene to below 1000 ohm/sq, doping is often required, especially for the use of graphene in applications such as transparent conductors. The most popular doping agents used in industry are inorganic salts, for example, Fe(NO) 3 , HNO 3 and AuCl, because of their processability, stability and price.

Among companies actively involved in CVD graphene production are 2D Carbon (Changzhou) Tech. Inc. Ltd, Wuxi Graphene Films Co. Ltd and Chongqing Graphene Technology Co. Ltd in China; Graphene Square Inc. in Korea; Graphenea Inc. in Spain; BGT Materials Ltd in the UK; and Graphene Laboratories Inc. in the USA (one example is shown in Fig.  1 b). Graphene Square provides graphene films with a size of up to 8 × 8 cm 2 that are produced on Cu foil and then transferred onto a SiO 2 /Si wafer or quartz glass. Graphene films on polyethylene terephthalate (PET) with a size of 100 × 100 cm 2 are available to custom order. Changzhou 2D Carbon, Wuxi Graphene Films and Chongqing Graphene Technology have announced that their annual production capacities for graphene film on Cu foil are 150 000, 100 000 and 1 000 000 m 2 , respectively, and all are able to provide graphene films with sizes of up to 300 × 30 cm 2 on Cu foil or PET film. BGT Materials provides graphene film on SiO 2 /Si or PET with sizes in the range of 1 × 1 to 20 × 25 cm 2 . In January 2017, Graphenea announced an annual production capability of 7 000 wafers of CVD graphene with a wafer size of up to 8 inches. Graphene Laboratories are able to provide graphene on PET with sizes of <20 × 20 cm 2 . This information was obtained from the websites of each company.

For the further development of the CVD graphene industry, achieving (i) a wafer-scale size (or larger) of single crystal graphene and (ii) its nondestructive and clean transfer from the Cu foil (or other growth substrate if others are found) to a dielectric substrate (or other, arbitrary substrate) that satisfies the needs of industrial applications, e.g. fast processing, low price, high reliability and automatic control, are relevant. (Of course, there may be applications where polycrystalline graphene will serve sufficiently well and if it is less expensive than single-crystal material, of course it will be used.) Other challenges such as the controllable preparation of multi-layer graphene on metals and the direct growth of graphene on dielectric substrates with a quality comparable to that on Cu should also be targeted. An example is the recently reported growth of graphene on glass [ 79 , 80 ].

Although most graphene applications are still in the demonstration stage in R&D laboratories, a few commercial applications of graphene materials have emerged onto the market. In this section, some examples in which graphene materials have demonstrated advantages over their conventional counterparts will be reviewed. We have chosen to discuss those examples that we are particularly familiar with. (As stated above, this article is not intended as an exhaustive review of all commercial applications.) It is worth noting that studies indicate that graphene holds promise for applications in electronics, optoelectronics and sensors of various types [ 17 , 20 , 49 , 81 ]. As the focus of this paper is on topical areas that already have products in the marketplace, we do not review these topics.

Conducting additives in electrode materials for batteries

Graphene materials have been intensely investigated as active materials or important components in electrodes for energy storage. A number of challenges need to be met before commercial products are achieved. Graphene can act as a conducting additive in electrodes to replace (at least partially) the conventionally used carbon black or carbon nanotubes. News has indicated that one of the main applications of exfoliated graphite suspensions is as a conductive additive in battery electrodes, especially for those electrode materials with an intrinsically low electric conductivity like LiFePO 4 . Some of the reasons for this come from the fact that N-methyl-pyrrolidone (NMP) is a solvent suitable for both graphite exfoliation [ 82 , 83 ] and the electrolytes in Li-ion batteries. In addition, graphene flakes from the exfoliation of graphite usually contain less impurity and preserve most of the conjugated structure of graphene [ 84 , 62 ]. With higher surface areas and reasonably good electric conductivity, the amount of graphene flakes can be minimized to a value of 2 wt.% or less in the electrode, demonstrating a higher efficiency than carbon black, to achieve a similar performance of the electrode [ 85 ]. A few battery manufacturers are considering increasing the use of graphene suspensions as a conducting additive and more than hundreds of tons of graphene suspensions or slurries have been sold for this purpose. In addition, in situ introduction of graphene (or graphene oxide) materials in the procedures of fabrication of active materials may bring other advantages such as the better control of particle size of the active materials and the interface between graphene and active materials [ 86 , 87 ]. Given the huge development of Li-ion batteries worldwide, the market for using graphene as a conducting additive is expected to dramatically increase. One uncertainty, however, includes the choice of active materials, especially cathode materials, in batteries. Promising cathode materials, such as LiNiCoMnO 2 [ 88 , 89 ], have an electric conductivity much higher than LiFePO 4 so that the need for conducting additives could be further reduced or even eliminated. On the other hand, as stated above, the difficulty in controlling the number of layers and the size distribution in exfoliated graphite could lead to problems in the stability of the additive; the effects of number of layers and flake size still need further study; and how significant the improvement in electrochemical performance of the batteries with the use of graphene additive is still under study [ 90 ]. It is worth noting that some recently developed high-capacity electrode materials, e.g. sulfur cathodes [ 91 ] or Li metal anodes [ 92 ], may provide opportunity for graphene to play other roles than purely as conducting additives.

Additives in anti-corrosion primers

Electrochemical corrosion causes considerable damage and loss worldwide every year. Various coatings have been used to prevent it, among which zinc-rich epoxy is an important primer to protect less active metals such as iron. The global market for zinc-rich epoxy primers is on the scale of a few tens of millions of tons a year, leading to the consumption of a similar amount of zinc powders since the zinc content is usually more than 70 wt.% [ 93 ]. The processing of so much zinc has caused many problems in the environment and has been said to be injurious to the health of workers in related industries [ 94 ]. A few strategies, e.g. replacing some of the zinc with graphite or carbon black, have been considered in order to reduce the use of zinc in the primer. Collaborative research between The Sixth Element Materials Technology Co. (Changzhou) Inc. Ltd and the Jiangsu Toppen Technology Co. Ltd has shown that the introduction of 1 wt.% reduced graphene oxide in the primers could replace up to 50 wt.% of zinc, leading to a graphene-based zinc epoxy primer with a much lower zinc content. With the 1 wt.% graphene content (plus ∼20 wt.% zinc), the epoxy primer has shown a nearly 4 times longer anti-corrosion life than the conventional zinc-rich epoxy primer (70 wt.% zinc) when coated on the same substrates and measured under the same conditions. Importantly, the cost of the 1 wt.% graphene powder is lower than that of the 50 wt.% of zinc that is replaced, even for the current production scale of graphene materials. The advantage of graphene in the epoxy primer is considered to be related to its effective bridging between zinc particles, resulting in an electrically conducting 3D network of zinc and graphene. During etching (corrosion), current reaches the zinc through the network of graphene platelets and the reaction of zinc protects the iron in the base. It is also perceived to be important that the distribution and stacking of graphene platelets in the epoxy physically hampers the diffusion of water or ions into the primer, thus increasing the anti-corrosion lifetime of the primer. A demonstration of such a primer coating was carried out on a tower of a power-producing windmill in the East China Sea in December 2014, and the feedback seems satisfactory so far (Fig.  2 a). Encouraged by this success, the Jiangsu Toppen Technology Co. Ltd has announced a plan to scale up the production of graphene-based zinc epoxy primers to 5000 tons per year in 2017.

(a) Graphene-based anti-corrosive paint applied to offshore wind turbine equipment. (b) Thermal conduction film made from graphene oxide. (c) Bracelets with double-edge curved touch sensor made of CVD graphene film. (d) Attires clothing with a heating function made of CVD graphene-based components. (e) A graphene-doped rubber tire. (f) CVD graphene films used in touch panels. All photos are used with permission of copyright.

A precursor for thermal dissipation films

Obviously, the current cost of graphene powder materials, compared to other bulk raw materials like steel or plastics, is still too high for them to be used as a major component in many large-scale industrial applications. This is one reason that graphene materials in the form of powders or suspensions are currently mostly used as additives. Thermal dissipation films are one area in which graphene can be used while being cost-competitive with other films, such as those from polyimide. Changzhou Fuxi Technology Co. Ltd has started to develop thermal dissipation films based on the high-temperature annealing of graphene oxide membranes (Fig.  2 b). Heat treatment up to 2800 °C converts the graphene oxide membranes into high-quality ‘graphite-like’ membranes, but with less AB stacking due to the partial exfoliation of the graphite oxide and crumpling/folding in some of the layers in this material that is in some ways similar to graphite. The in-plane thermal conductivity of such ‘graphite from graphene oxide’ is as high as 1500 W/mK, close to that of graphite films made from polyimide films. This high thermal conductivity has allowed heat dissipation films made from graphene oxide to be used in mobile electronics such as mobile phones or pads, with potential use in laptops and other devices in the future. In addition, graphite membranes (also referred to as films) can be produced in a thickness range from a few to hundreds of micrometers, depending on the processing of the graphene oxide membrane precursors. How the structure of the graphene platelets in the graphene oxide membranes (films) evolves during the heat treatment and affects the thermal conductivity of the as-made films is an important topic for fundamental study.

Touch panels and thermal heaters

Touch panels and thermal heaters based on CVD graphene are two functional components available for market. The Graphene Square, Changzhou 2D Carbon, Wuxi Graphene Films and Chongqing Graphene Technology can apparently produce graphene films having a size of up to meter-scale, with a sheet resistance in the range of 50–400 ohm/sq and a transmittance of >85% on substrates, which makes the production of graphene-based touch sensors and thermal heaters possible. The excellent flexibility and chemical stability of graphene compared to its competitors, e.g. indium tin oxide (ITO) and silver nanowires, also make it an attractive conductive film for use in wearable electronics. In 2016, Wuxi Graphene Films released a bracelet with double-edge curved touch sensor made of CVD graphene film (Fig.  2 c). A single-layer graphene film with a width of centimeters can conduct an electrical current of ∼1 A when a voltage of 3.5 V is applied, and this can provide a heating surface with a tunable temperature of 40–120°C and thus find use in, e.g. personal-care products or clothing (Fig.  2 d). The process for the production of CVD graphene-based components includes patterning of the graphene films, printing wires, and sealing with a cover, all of which require optimized processing because of the atomic-thin graphene, which is much less than that of conventional counterparts. On the other hand, the consumer electronic market, e.g. graphene touch panels, has ‘cut-throat competition’ and it will be of interest to see if graphene can significantly penetrate this market.

A complete industrial chain of graphene materials is very important. As stated above, the highly preparation-sensitive structure and properties have meant that applications need very close ‘communication’ with production of the graphene materials. It could be helpful to the growth of industrial applications of graphene if graphene manufacturing companies could be more specific about the graphene materials being sold. Depending on the preparation methods, the industrial chains, including the providers of raw materials and the downstream businesses, are likely to be different. Such factors will influence the investment cycle, profit model(s) and competitive positions of the companies that are involved.

In addition to the applications listed above, many more graphene-related products have been proposed (some more examples are shown in Figs. 2 e and f), although most of them are still in development. (However, one must note that not all of them have used the advantages of graphene materials and this has raised debate about the actual role of graphene in some of the products.)

History has witnessed the rise and sustained use of many ‘new’ materials. Achieving stable mass production and a wide range of applications for new materials takes time. It will be of great interest to see how quickly graphene materials can penetrate into other commercial applications, in addition to further penetration into the applications that are being commercialized now and that are described in this article.

Some commercially available graphene products (summarized based on the information provided on their websites).

Finally, we would like to note that there is often a ‘virtuous circle’ or feedback loop between applied R&D and fundamental research. The intense efforts to commercialize graphene in suitable applications are already leading to observations during the course of such efforts, which spur on further work on the fundamental side. We expect this aspect of fundamental research on graphene and related materials to also grow as a result of commercialization in existing and new areas.

Help from Runli Tang is appreciated.

This work was supported by the Ministry of Science and Technology of China (2016YFA0200102) and the National Natural Science Foundation of China (51521091).

YZ is a board member of The Sixth Element Materials Technology (Changzhou) Co. Ltd. HJ is the Chief Scientist of Wuxi Graphene Films Co. Ltd. RSR is the senior member of the Expert Advisory Committee of The Sixth Element Materials Technology (Changzhou) Co. Ltd. HMC’s team has transferred its technology to set up the Deyang Carbonene Technology Co. Ltd.

Conflict of interest statement. None declared.

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Mass customization vs. mass production: Variety and price competition

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Mass Production Technologies for Underground Coal Mining in India: Status, Challenges, and Prospects

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• Arvind Kumar Mishra   ORCID: orcid.org/0000-0002-1921-2973 7  

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The current trend in coal production in India shows that underground mining contributed less than 5–8% of the total coal produced. On the other side, the contribution of opencast mining to coal production is at its peak. This trend is not sustainable in the Indian scenario due to environmental issues, coal quality problems, and socio-economic stresses due to opencast mining. The solution lies in the adoption of Mass Production Technology (MPT) in underground mining which can compete with opencast mining in terms of OMS and production rate. Furthermore, Coal India Limited (CIL) has also launched a mission to upscale the coal production from underground mines to 100 million tonnes by 2027–28. Therefore, to advocate MPT and its diffusion in the Indian mining industry, this keynote discusses the existing mining methods and potential MPTs for exploiting deep-seated coal deposits in India. The MPT for underground mining has been defined and the eligible technologies are presented. The focus has been made on Longwall Technology which is one of the finest candidate technologies for MPT in India. Furthermore, the challenges in adoption in the Indian coal mining industry have been elaborated with real cases. Finally, the prospects in R&D, testing, and policymaking for smooth adoption in Indian coal mining have been deliberated. In sum, this keynote can enrich the knowledge of practising mining engineers, mine planners, and policymakers in adopting MPT for underground coal mining in future.

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Acknowledgement

The author is sincerely thankful to Dr. Ranjan Kumar and other scientists of CSIR-Central Institute of Mining and Fuel Research Dhanbad for their contributions in preparing this keynote. The views expressed in this paper are the view of the author and do not necessarily reflect those of the institute.

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Mishra, A.K. (2023). Mass Production Technologies for Underground Coal Mining in India: Status, Challenges, and Prospects. In: Sinha, A., Sarkar, B.C., Mandal, P.K. (eds) Proceedings of the 10th Asian Mining Congress 2023. AMC 2023. Springer Proceedings in Earth and Environmental Sciences. Springer, Cham. https://doi.org/10.1007/978-3-031-46966-4_5

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Experimental research on breakage characteristics of feed pellets under different loading methods.

1. Introduction

2. materials and methods, 2.1. samples and preparation, 2.2. experimental equipment, 2.3. experimental methods, 2.3.1. repeated compression, 2.3.2. repeated impacts, 2.4. evaluation of breakage characteristics, 2.4.1. size distribution function, 2.4.2. pulverization rate, 2.4.3. mass-specific energy, 2.4.4. fitting model, 3. results and discussion, 3.1. breakage behaviors of feed pellets, 3.2. particle size distribution, 3.3. energy and pulverization rate, 3.3.1. the influence of loading cycles, 3.3.2. relationship between energy and pulverization rate, 4. conclusions, supplementary materials, author contributions, institutional review board statement, data availability statement, conflicts of interest.

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Kong, X.; Cao, Q.; Niu, Z. Experimental Research on Breakage Characteristics of Feed Pellets under Different Loading Methods. Agriculture 2024 , 14 , 1401. https://doi.org/10.3390/agriculture14081401

Kong X, Cao Q, Niu Z. Experimental Research on Breakage Characteristics of Feed Pellets under Different Loading Methods. Agriculture . 2024; 14(8):1401. https://doi.org/10.3390/agriculture14081401

Kong, Xianrui, Qing Cao, and Zhiyou Niu. 2024. "Experimental Research on Breakage Characteristics of Feed Pellets under Different Loading Methods" Agriculture 14, no. 8: 1401. https://doi.org/10.3390/agriculture14081401

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• Library of Congress
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Technical Reports & Standards Collection Guide

Introduction.

• Technical Reports Collections
• Standards Collection
• American Documentation Institute (ADI)
• Office of Scientific Research and Development (OSRD) Collection
• Synthetic Rubber Project
• Technical Translations (TT) Series
• Locating Technical Reports and Standards
• Research Assistance and Reproductions
• Online Resources and Databases
• Using the Library of Congress
• Jennifer Harbster, Head, Science Section, Researcher Engagement & General Collections Division
• Sean Bryant, Reference Librarian, Researcher Engagement & General Collections Division
• Ashley Fielder,  Librarian for Medicine and Life Science. Science Section, Researcher Engagement & General Collections
• Created:  September 22, 2023

Last Updated: May 7, 2024

Science & Technical Reports : Ask a Librarian

Have a question? Need assistance? Use our online form to ask a librarian for help.

Get connected to the Library’s large and diverse collections related to science, technology, and business through our Inside Adams Blog. This blog also features upcoming events and collection displays, classes and orientations, new research guides, and more.

The Library of Congress is completing a project to update and modernize Library reading room websites. As a part of the process, “The Technical Reports and Standards Collection” is in the process of being updated and migrated to this new platform. The process has not yet been completed and the guide remains subject to change.

Researchers with questions about the collection are encouraged to contact a science or business librarian using the Ask-a-Librarian: Science and Technical Reports or Ask a Librarian: Business online form, by phone, at (202) 707-5639, or in person, at the reference desk, in the Science and Business Reading Room, on the fifth floor of the Library's John Adams Building.

Technical Reports

Technical reports are designed to quickly alert researchers to recent findings and developments in scientific and technical research. These reports are issued for a variety of purposes:

• to communicate results or describe progress of a research project
• to convey background information on an emerging or critical research topic
• to provide lists of instructions or procedures for current practices
• to determine the feasibility of a technology and recommend if research should be continued (and how to evaluate any further progress made)
• to detail technical specifications (materials, functions, features, operation, market potential, etc.)

Technical reports first appeared in the early part of the 20th century. The U.S. Geological Survey (USGS) published a series of professional papers beginning in 1902, and the National Advisory Committee for Aeronautics (NACA) issued its first report in 1915. But, the format gained importance during World War II, emerged in the postwar era, and remains, to this day, a major tool for reporting progress in science and technology, as well as in education, business, and social sciences research. The names given to series of these publications vary, but are often such generic terms as "technical reports," "working papers," "research memoranda," "internal notes," "occasional papers," "discussion papers" or "gray (or grey) literature." In the physical and natural sciences, "technical report" seems to be the preferred designation. For reports dealing with business, education, and the social sciences, on the other hand, the terms "working paper," "occasional paper," and "memorandum" are often the designations of choice. Other, more specific types of technical reports include "preprints" and "reprints." Preprints generally are versions of papers issued by researchers before their final papers are published by commercial publishers. Preprints allow researchers to communicate their findings quickly, but usually have not been peer reviewed. Reprints are typically released to heighten awareness of the research being conducted in a particular field or at a single institution. The term, "technical report" encompasses all of these designations.

Since many of these publications are intended to provide just a temporary snapshot of current research in a particular field or topic, they may contain the some of following distinctions:

• Rapid communication of new research results
• Dissemination to a targeted audience.
• Detailed methodologies, in order to facilitate review of research results by others
• No peer review, though there is often another selection process for publication (grant, contract, or institutional affiliation)
• Not published by typical commercial publishers (instead reports are issued or sponsored by government agencies, professional associations, societies, councils, foundations, laboratories, universities, etc.)
• Corporate authorship, where present, is typically emphasized

Unfortunately, uncertain availability, limited print runs, and decentralized distribution patterns with little bibliographic information are also often characteristics of this literature.

The Federal Government issues many different types of technical reports. An overview of some of these can be found in a May 2001 GAO report, " Information Management: Dissemination of Technical Reports ." Government issued or sponsored reports contain an additional characteristic - they may be subject to distribution restrictions linked to their classification status. Although references to classified reports may be found in technical reports literature, the security status or limited distribution of reports may make them unavailable to the general public and to the Library as well, as the Library holds only titles in the public domain. Those interested in locating such materials can consult the U.S. Department of Justice's Freedom of Information Act  site for guidance in obtaining these reports.

To enable them to be identified and located, technical reports are assigned report codes by agencies or organizations involved in their production or distribution. These codes may be referred to as "accession numbers," "agency report series numbers," "contract numbers," "grant numbers" or by other names, and include dates and individual report numbers. Typically, reports are assigned multiple codes and these codes help to identify the sponsoring agency, the organization performing the research or the organization disseminating the report.  Most technical reports held by the Library of Congress are not cataloged, and, for these reports, one or more report codes is required for Library staff to check the collections for a report or to locate and retrieve it. For more information about the current Standard Technical Report Number format (STRN) see ANSI/NISO Z39.23- 1997 (S2015) Standard Technical Reports Number Format and Creation . 

Standards are specifications which define products, methods, processes or practices, and are known to have existed as early as 7000 B.C., when cylindrical stones were used as units of weight in Egypt. According to  Office of Management and Budget (OMB) Circular A-119 , as revised in 2016, the term "standard" or "technical standard" refers to:

• common and repeated use of rules, conditions, guidelines or characteristics for products or related processes and production methods, and related management systems practices;
• the definition of terms; classification of components; delineation of procedures; specification of dimensions, materials, performance, designs, or operations; measurement of quality and quantity in describing materials, processes, products, systems, services, or practices; test methods and sampling procedures; or descriptions of fit and measurements of size or strength; and
• terminology, symbols, packaging, marking or labeling requirements as they apply to a product, process, or production method.

Technical standards are not "professional standards of personal conduct; or institutional codes of ethics." (p. 15).

Standards are typically generated by governments or by professional associations and organizations interested in or affected by the subject matter of particular standards. For example, U.S. government standards mandated by the  Fair Packaging & Labeling Act (FPLA)  have standardized the labeling required for packaging in which consumer commodities is sold. Standards set the basis for determining consistent and acceptable minimum levels of reliability and safety, and are adhered to either voluntarily or as mandated by law. For a more complete overview, see the NIST report  " The ABC's of Standards Activities " by Maureen A. Breitenberg (2009).

The Library of Congress standards collection includes military and other federal standards, industry standards, and a few older international standards from Russia, China, and South Africa. Material from the collection is available in various formats, including digital, print, and microform materials. The majority of the Library's standards collection held in the Science Section's Technical Reports and Standards Collection. The collection remains largely uncatalogued, and as a result, most items from this collection are not discoverable in the Library's online catalog. Inquires on Library holdings can be sent to the Science Section using the Science and Technical Reports Ask-a-Librarian form . Some standards, however, are housed in the Library's general collections and discoverable by searching the  online catalog -- the ASTM standards are one example. Other standards are in custody of appropriate specialized research centers, such as the Law Library , which maintains  OSHA standards and some building codes.

About the Science Section

Part of the  Science & Business Reading Room  at the Library of Congress, the Science Section is the starting point for conducting research at the Library of Congress in the subject areas of science, medicine and engineering. Here, reference specialists in specific subject areas of science and engineering  assist patrons in formulating search strategies and gaining access to the information and materials contained in the Library's rich collections of science, medicine, and engineering materials.

• Next: Technical Reports Collections >>
• Last Updated: Jul 3, 2024 11:51 AM
• URL: https://guides.loc.gov/technical-reports

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Why Canada has become a critical supplier of crude oil to the U.S.

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In the car-centric United States, we have a bit of a love affair with oil. And that romance is really an international love story — one where our neighbors to the north play a starring role, accounting for a growing share of oil that the U.S. refines and imports.

If Canadian crude and U.S. refineries were in a rom-com, Canadian crude would be the boy next door, the one U.S. refiners overlooked when they were courting Latin American oil back in the late 1980s and early ’90s.  

“So, you can think of Venezuela, Mexico,” said Kevin Birn with S&P Global Commodity Insights, alluding to when the world thought we were running out of oil. “The Gulf Coast refineries were looking for security of supply. A lot of these refiners entered into long-term joint-venture agreements with the suppliers to get access to security of that heavy barrel supply.” 

Big money was put into refining capacity that catered to the heavy Latin American oil, which is more expensive to refine into diesel or gasoline, Birn said.

“You need the ability to reach higher temperatures, and you need to have specially designed facilities that can handle that as well,” Birn said. “And so those joint ventures led to an expansion in U.S. refining capacity to process heavy barrels, first in the Gulf Coast region in the early ’90s, and that continued through to the early 2000s.” 

Those refineries had really invested in their relationship with heavy Latin American oil.

“But as we entered this century, millennia, we saw that kind of slow down,” Birn said. “A lot of those deals were rolling off, and the Latin American supply began to slow.” 

And even though we saw fracking and horizontal drilling transform the Permian Basin in West Texas into one of the most significant oil producing regions in the world, the oil there was not as compatible with the expensive new U.S. refineries, said Ryan Kellogg with the University of Chicago. 

“All of that capacity was built before the shale boom started. And all of a sudden, we had all this really nice, light, sweet crude available in the U.S.,” Kellogg said. “So, we’re now in this position where we have these very high-tech refineries that can process the really heavy crude.” 

We needed to get that heavy crude from somewhere else.  

“Think about the oil sands or tar sands of Alberta. Basically, this is like really thick, heavy, goopy crude oil,” Kellogg said.

And Chuck Mason with the University of Wyoming said Alberta’s oil sands also had a geographical advantage.

“In the grand scheme of things, not super-duper far away from the refining sector,” Mason said.

And for Canada, exporting heavy crude by pipeline and rail to its oil-hungry southern neighbor made sense. 

“This source of production that we’re talking about is the very epitome of land a landlocked resource,” Mason said. “U.S. refiners were just better buyers, because they were there easier to connect. The transactions costs associated with connecting up with them are massively smaller.”

It was a sensible match. 

“The relationship was very symbiotic,” Birn said, and that has only strengthened over the years. “Canadian growth occurred at such a rate and scale that it overwhelmed that region, and additional infrastructure was designed to deliver that crude oil into the Gulf Coast region of the United States, and increasing volumes and then making it to the U.S. Gulf Coast.” 

Many miles of new pipeline later, 60% of   U.S. crude oil imports come from Canada, according to the U.S. Energy Information Administration.   A decade ago, it was just 33%.

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