Source: ACADIAN RESEARCH & DEVELOPMENT LLC submitted to NRP
VALUE-ADDED GRAPHENE MATERIALS FROM WOODY RESOURCES
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
COMPLETE
Funding Source
Reporting Frequency
Annual
Accession No.
1029958
Grant No.
2023-51402-39207
Cumulative Award Amt.
$175,000.00
Proposal No.
2023-00747
Multistate No.
(N/A)
Project Start Date
Jul 1, 2023
Project End Date
Jun 30, 2024
Grant Year
2023
Program Code
[8.1]- Forests & Related Resources
Recipient Organization
ACADIAN RESEARCH & DEVELOPMENT LLC
1482 COMMERCE DR
LARAMIE,WY 82070
Performing Department
(N/A)
Non Technical Summary
This project will demonstrate the utilization of wood biomass feedstock to produce graphene products through a less expensive, more environmentally friendly process. The wood feedstock is first pyrolyzed to biochar, then our synthesis process converts the biochar to graphene oxide, a viable product. Further treatment produces reduced graphene oxide and graphene nanosheets, also viable products. Graphene materials are useful in a number of applications such as battery manufacturing, pharmaceuticals, concrete, optics, filtration, and composites, but these materials can be prohibitively expensive. Graphite can be used to produce graphene, but the process often uses multiple harmful reagents, and the lack of domestic graphite production equates to reliance on foreign supply. The development proposed in this project uses a single reagent, can reduce synthesis costs, and increases availability of these powerful and important materials while helping to utilize the estimated 82-88 million dry tons of woody biomass available annually in the United States.Biochar will be produced from pine wood at various temperatures and processed to synthesize the graphene products. Materials will be characterized at every step to track product evolution and determine optimal biochar characteristics. This project aligns with USDA Strategic Goals and Research Priorities through development of value-added products using forest resources to expand markets for emerging technologies, as well as climate change mitigation through retention of feedstock carbon in final products.
Animal Health Component
20%
Research Effort Categories
Basic
(N/A)
Applied
20%
Developmental
80%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
12306502020100%
Goals / Objectives
The overall goal of this STTR Phase I project is to demonstrate the production of graphene products originating from woody biomass (pine wood). The graphene products include graphene oxide, reduced graphene oxide, and graphene nanosheets. This encompasses further goals of combatting climate change and expanding the market for the sustainable technology of graphene production from wood biochar. The use of biochar to produce graphene can help combat climate change by effectively sequestering carbon in the final product, and removal and processing of standing dead wood and other woody resources will result in a forest that is ready to produce new growth which will consume CO2 directly from the atmosphere. In addition, this project will develop materials to expand market opportunities and drive innovation of commercially viable products. The graphene products have application to emerging markets sectors such as energy storage via new battery technologies, and production of strengthened concrete.The four Objectives of this Phase I STTR project are as follows:Determine optimal biochar pyrolysis temperature to produce the highest quality graphene products when using our established conversion process.Demonstrate that our process can successfully convert biochar to graphene oxide.Show that biochar-derived graphene oxide can be reduced to produce reduced graphene oxide.Produce graphene nanosheets from reduced graphene oxide.
Project Methods
The methods for the projects are organized by the project tasks.Produce biochar and characterize:Biochar synthesis - Biochar will be synthesized under flowing N2 atmosphere in the range of 300 - 1000 °C using a heating rate of 20 °C/min, and temperature will be maintained for 1 hour once the target is reached.Biochar characterization - The produced biochar will be characterized via scanning electron microscope (SEM) to examine morphology and composition, N2 gas sorption to determine surface area and pore volume, thermogravimetric analysis (TGA) for thermal decomposition and proximate analysis of moisture, volatiles, fixed carbon, and ash, and X-ray diffraction to examine the crystal structure of the materials.Convert biochar to GO and characterize:Conversion of biochar to GO - To convert biochar to graphene oxide, the method developed at UW will be used. This method of producing stable GO uses aqueous nitric acid in the reactant slurry as oxidizing agent. The HNO3 is added very slowly to the carbon source in an ice bath. The mixture is then sonicated for 4 h at 70 °C, diluted 1:10, and filtered/washed until pH is ~6.5. The synthesized GO is furthered filtered and finally freeze-dried.GO characterization - Raman spectroscopy will be used to examine the GO and the characteristic bands. To determine carbon and oxygen content, bonding information, and sp2/sp3 ratio, X-ray photoelectron spectroscopy (XPS) will be used. Further bonding and structural data will be collected using Fourier-transform infrared spectroscopy (FTIR) and XRD will be used to examine crystal structure properties. Morphology will be investigated via SEM, thermal decomposition via TGA, and surface area will be measured via N2 sorption. Conductivity will be measured using a standardized method used in our previous work and by others where columns of material of consistent height, under pressure (30 MPa), are compressed by plungers with electrodes connected to a precision meter.Convert GO to rGO and characterize:Conversion of GO to rGO - To convert graphene oxide to reduced graphene oxide, samples are annealed under argon atmosphere with a heating rate of 20 °C/min to 1100 °C which is maintained for 30 min.rGO characterization - To characterize the produced rGO, the suite of tests used to characterize the GO will be used. This enables the direct comparison of the GO to the resultant rGO.Convert rGO to graphene nanosheets and characterize:Conversion of rGO to graphene nanosheets - Graphene nanosheets are produced through further thermal treatment of rGO by using an induction furnace to reach temperatures up to 2500 °C under argon atmosphere. The temperature does not need to be maintained for long to produce the graphene nanosheets.Graphene nanosheets characterization - To characterize the produced graphene nanosheets, the suite of tests used to characterize the GO and rGO will be used, allowing thorough comparison of all graphene materials produced in this project.

Progress 07/01/23 to 06/30/24

Outputs
Target Audience:Audience includes proactive sustainability managers at cement companies responsible for improving sustainability practices and company image. This customer profile is expressly interested because our materials can strengthen concrete and are made using sustainable materials. The second audience profile includes sustainability minded, forward thinking architects responsible for selecting building materials. They are influencers as an expert on the latest materials who is selecting and recommending materials to the client. For battery anode materials, the target audience is materials purchasers. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Nothing Reported How have the results been disseminated to communities of interest?The knowledge gained from this research project is currently confidential, and as such has not been shared with the public. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? All objectives of the project were completed. In terms of project tasks, the following items were completed: Task 2. Produce biochar and characterize 2.1 Biochar synthesis Biochar has been produced at six temperatures in the range of 300 - 1000 °C. 2.2 Biochar characterization The produced biochar has been characterized via N2 gas sorption to determine surface area and pore volume, thermogravimetric analysis (TGA) for thermal decomposition and residue determination, Raman spectroscopy to examine bonding, and X-ray diffraction to examine the crystal structure of the materials. Scanning electron microscope (SEM) is to be performed in January 2024 due to equipment issues at UW. Task 3. Convert biochar to GO and characterize 3.1 Conversion of biochar to GO GO was produced from all six biochar materials. 3.2 GO characterization Raman spectroscopy was performed to examine the GO and the characteristic bands. Bonding and structural data were examined via Fourier-transform infrared spectroscopy (FTIR), and XRD was performed to examine structure properties. Thermal decomposition was examined using TGA, and surface area and pore characteristics were measured via N2 sorption. Conductivity was measured using a standardized method, morphology investigated via SEM, and carbon and oxygen content as well as bonding information was studied using X-ray photoelectron spectroscopy (XPS). Task 4. Convert GO to rGO and characterize 4.1 Conversion of GO to rGO To convert graphene oxide to reduced graphene oxide, samples were annealed under argon atmosphere at 1100 °C. The rGO was produced from all six GO materials. 4.2 rGO characterization Raman spectroscopy, FTIR, XRD, TGA, and N2 sorption was performed on all rGO samples from comparison to the biochar and GO precursor materials. Conductivity, SEM, and XPS was performed with the GO samples. Task 5. Convert rGO to graphene nanosheets and characterize 5.1 Conversion of rGO to graphene nanosheets Graphene nanosheets synthesis was performed using high temperature processing. 5.2 Graphene nanosheets characterization To characterize the produced graphene nanosheets, the suite of tests used to characterize the GO and rGO was used, allowing thorough comparison of all graphene materials produced in this project. ?

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