# US 10,767,062 B2 · System and method for forming activated carbon aerogels and performing 3D printing

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- Number: US 10,767,062 B2
- Document ID: US10767062B2
- Status: Granted
- Kind: B2
- Application number: 15/613,630
- Filed: 2017-06-05
- Published: 2018-12-06
- Granted: 2020-09-08
- Earliest claimed: 2017-06-05
- Assignees: Lawrence Livermore National Security, LLC
- Applicants: Lawrence Livermore National Security, LLC
- Inventors: Swetha Chandrasekaran; Theodore F. Baumann; Marcus A. Worsley
- Web page: https://patentgrep.com/patent/US10767062B2

## CPC

- C09D 11/103: of aldehydes, e.g. phenol-formaldehyde resins
- B33Y 70/00: Materials specially adapted for additive manufacturing
- B33Y 70/10: Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
- C01B 32/00: Carbon; Compounds thereof (C01B21/00, C01B23/00 take precedence; percarbonates C01B15/10; carbon black C09C1/48)
- C08G 8/22: Resorcinol
- C09D 11/03: characterised by features other than the chemical nature of the binder
- B29C 64/106: using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29K 2061/04: Phenoplasts
- B29K 2401/00: Use of cellulose, modified cellulose or cellulose derivatives, e.g. viscose, as filler
- B29K 2509/02: Ceramics
- B29L 2031/3406: {Components, e.g. resistors}
- B33Y 10/00: Processes of additive manufacturing
- B33Y 80/00: Products made by additive manufacturing
- C01B 32/05: Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
- H01G 11/32: Carbon-based
- H01G 11/52: Separators
- H01G 11/86: specially adapted for electrodes (carbonisation or activation of carbon for the manufacture of electrodes H01G11/34)
- Y02E 60/13: Energy storage using capacitors
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- B33Y: ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- B29K: INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR {MOULDS, } REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29L: INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- H01G: CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE (selection of specified materials as dielectric H01B3/00; capacitors having potential barriers H10D1/62, H10K10/10)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

Making a carbon aerogel involves 3-D printing an ink to make a printed part, removing the solvent from the printed part, and carbonizing the printed part (with the solvent removed) to make the aerogel. The ink is based on a solution of a resorcinol-formaldehyde resin (RF resin), water, and an organic thickener. Advantageously, the RF resin contains an acid catalyst, which tends to produce carbon aerogels with higher surface areas upon activation than those produced from methods involving an ink composition containing a base catalyzed resin.

## Claims

### Claim 1

A 3-D printing ink, comprising:
water;
an organic thickener selected from the group consisting of water soluble cellulose derivatives, polyoxyalkylene compounds, polyvinyl alcohol, and mixtures thereof;
a resin that comprises resorcinol and formaldehyde;
an acid catalyst that catalyzes a reaction between the resorcinol and formaldehyde; and
a thixotropic additive;
wherein the 3-D printing ink does not contain graphene oxide; and
wherein the 3-D printing ink is a viscous thixotropic ink that is operable to gel after printing to form a printed part.

### Claim 2 (depends on 1)

The 3-D printing ink of claim 1, wherein the thixotropic additive comprises fumed silica.

### Claim 3 (depends on 1)

The 3-D printing ink of claim 1, wherein the organic thickener comprises hydroxypropylmethylcellulose.

### Claim 4 (depends on 1)

The 3-D printing ink of claim 1, wherein the organic thickener comprises a polyoxyalkylene compound.

### Claim 5 (depends on 1)

The 3-D printing ink of claim 1, comprising 10% to 60% by weight of the resin.
