CN105837214B - A kind of preparation method of graphene product - Google Patents
A kind of preparation method of graphene product Download PDFInfo
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- CN105837214B CN105837214B CN201610164587.9A CN201610164587A CN105837214B CN 105837214 B CN105837214 B CN 105837214B CN 201610164587 A CN201610164587 A CN 201610164587A CN 105837214 B CN105837214 B CN 105837214B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
Abstract
The invention discloses a kind of preparation methods of graphene product, include the following steps：Graphene powder is mixed with SiC powder, mixed-powder addition organic solvent dispersion is uniform, obtain supersaturated graphene dispersing solution slurry；Supersaturated graphene dispersing solution slurry is uniformly mixed with organic adhesive under the conditions of being protected from light, mixed slurry is obtained；Mixed slurry is fitted into 3D printing former, is successively printed according to three-dimensional part model by the way of face exposure or spot scan using controllable UV Line beam, graphene product crude green body is made；Graphene product crude green body is subjected to low-temperature defatted processing and hip treatment, obtains fine and close graphene product.This method utilizes photocureable rapid shaping principle, and the shape of graphene product is unfettered, preparation method fast and easy, and product compactness is preferable, has filled up the blank for preparing graphene product in the market.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of preparation method of graphene product.
Background technology
Graphene is both most thin material, and most tough material, fracture strength more taller than best steel 200
Times.It has good elasticity, stretch range that can reach the 20% of own dimensions again simultaneously.It is that current nature is most thin, intensity
Highest material.Graphene most potential application at present is the substitute as silicon, ultra micro transistor npn npn is manufactured, for producing
Following supercomputer.Replace silicon with graphene, the speed of service of computer processor will be hundreds times fast.In addition, graphite
Alkene is almost fully transparent, only absorbs 2.3% light.These features make it be highly suitable as the original of transparent electron product
Material, such as transparent touch display screen, luminescent screen and solar panel.
Currently, being seldom seen in document for the manufacturing method of graphene product, most of application about graphene also stops
Laboratory stage is stayed in, lacking a kind of can easily and fast prepare the variously-shaped graphene product with high-compactness
Method.
Invention content
The object of the present invention is to provide a kind of preparation methods of graphene product, solve and there is no a kind of preparation method at present
The problem of variously-shaped graphene product with high-compactness can easily and fast be prepared.
The technical solution adopted in the present invention is that a kind of preparation method of graphene product includes the following steps：
Step 1, raw material is prepared
Graphene powder is mixed with SiC powder, organic solvent is added in mixed-powder, makes mixed-powder using ultrasonic wave
It is uniformly dispersed in organic solvent, obtains supersaturated graphene dispersing solution slurry；By supersaturated graphene dispersing solution slurry with have
Machine bonding agent uniformly mixes under the conditions of being protected from light, and obtains mixed slurry.
Step 2, crude green body manufactures
Mixed slurry is fitted into 3D printing former, using controllable UV Line beam, using face exposure or spot scan
Mode, successively printed according to three-dimensional part model, graphene product crude green body be made.
Step 3, it post-processes
Graphene product crude green body is subjected to low-temperature defatted processing, so that the organic adhesive in crude green body is evaporated and overflows；It carries out again
Hip treatment obtains fine and close graphene product.
The features of the present invention also characterized in that：
Preferably, the additive amount of SiC powder is the 0.1~1% of mixed-powder total volume.
Preferably, organic solvent is NN- dimethylformamides, N-Methyl pyrrolidone or tetrahydrofuran.
Preferably, organic adhesive is epoxy acrylic resin, urethane acrylate, polyester acrylate, polyester third
One of olefin(e) acid resin or amino acrylic resin.
Preferably, per 10mL organic solvents in be added 2mg~20mg mixed-powders, supersaturated graphene dispersing solution slurry with
The volume ratio of organic adhesive is 3:2~3:7.
Preferably, for the layer thickness control successively printed at 20~80 μm, optical source wavelength is 200~400nm.
Preferably, when being exposed using face, time for exposure 0.1-3s；When using spot scan, spot diameter be 0.1~
0.15mm, hot spot movement speed 1-300mm/min.
Preferably, 100 DEG C~800 DEG C of the temperature of low-temperature defatted processing, time 1-2h.
Preferably, 1000 DEG C~1350 DEG C of hip treatment temperature, pressure 100MPa~200MPa, time 0.2-3h.
The invention has the advantages that the present invention manufactures graphene product using 3D printing technique, can easily and fast make
The problem of standby variously-shaped graphene product for providing high-compactness, and the shape of graphene product is unfettered, process
Simply, the defects of manufacture efficiency is high, graphene product interior solid obtained, pore-free, slag inclusion.
Specific implementation mode
The present invention is described in further detail With reference to embodiment, but the present invention is not limited to these realities
Apply mode.
The present invention provides a kind of preparation methods of graphene product, include the following steps：
Step 1, raw material is prepared
SiC powder is added in graphene powder to be uniformly mixed, SiC powder addition is the 0.1 of mixed-powder total volume
~1%, the addition of SiC powder can enhance the binding force inside graphene product.Then organic solvent is added in mixed-powder
Disperseed, adding proportion is：2mg~20mg mixed-powders are added in per 10mL organic solvents.Made using high-power ultrasonics
Mixed-powder is uniformly dispersed in organic solvent, obtains supersaturated graphene dispersing solution slurry；Organic solvent is preferably three kinds following：
DMF, i.e.,：NN- dimethylformamide (boiling points：153 DEG C, self-ignition point：445℃)；NMP, i.e.,：N-Methyl pyrrolidone (boiling point：
203 DEG C, burn point：346℃)；THF, i.e.,：Tetrahydrofuran, (boiling point：203 DEG C, burn point：346℃).
Then supersaturated graphene dispersing solution slurry is uniformly mixed with organic adhesive, obtains mixed slurry.It is organic viscous
Agent is connect for bonding/solidified forming graphene product three-dimensional structure in 3D printing forming process, it is ensured that graphene product
Structural strength before crude green body sintering, while can be overflowed rapidly in low-temperature defatted sintering process.In order to ensure being solidified into form quality
Amount and precision, it is necessary to select that laser curing velocity is very fast and the lower organic adhesive of viscosity, preferably epoxy acrylic resin, poly- ammonia
Ester acrylate, polyester acrylate, polyester acrylate resin or amino acrylic resin.Supersaturated graphene dispersing solution slurry
Volume ratio with organic adhesive is preferably 3:2~3:7.In addition, to ensure the good mobility of slurry, mixed process and storage
Process should avoid light-exposed, particularly avoid ultraviolet light.
Step 2, crude green body manufactures
Mixed slurry is fitted into 3D printing former, using controllable UV Line beam, using face exposure or spot scan
Mode, successively printed according to three-dimensional part model, graphene product crude green body be made.The layer thickness control successively printed is 20~80
μm, optical source wavelength is 200~400nm.It is exposed according to face, time for exposure 0.1-3s；According to spot scan, spot diameter is
0.1~0.15mm, hot spot movement speed 1-300mm/min.
Step 3, it post-processes
Made graphene product crude green body is placed in low-temperature sintering stove, it is low-temperature defatted at a temperature of 100 DEG C~800 DEG C
1-2h is handled, so that the organic adhesive in crude green body is evaporated and overflows；It is placed in again in hot isostatic pressing stove, in temperature 1000 DEG C~1350
DEG C, carry out hip treatment under the conditions of pressure 100MPa~200MPa, obtain fine and close graphene product.
The graphene product consistency that the present invention prepares is higher, stable quality, high to the utilization rate of raw material, and makes
Make that speed is fast, can especially complex, the especially fine part of forming shape, be suitble to small lot production.
Embodiment 1
A kind of preparation method of graphene product, specifically includes following steps：
(1) prepared by raw material
The synthesis of epoxy acrylic resin：Acrylic acid and epoxy resin molar ratio are 1:1~1.05, epoxy resin is slightly
Micro- excess can prevent the acrylic acid of remaining from having harmful effect to base material and cured film, but remaining epoxy group can also influence to set
The bin stability of fat.Bisphenol-a epoxy acrylate selects E-51 or E-44, phenol aldehyde type epoxy resin to select F-51 or F-
44.Catalyst selects catalytic activity high, the low triphenylphosphine of product viscosity, antimony triphenyl, chromium acetylacetonate, dosage (quality point
Number) it is 0.1%~3%.Acrylic acid is exothermic reaction with epoxy ring-opening esterification, therefore initial reaction stage control temperature is very heavy
It wants, epoxy resin is usually heated to 80~90 DEG C, acrylic acid, catalyst and inhibitor mixture, controlling reaction temperature is added dropwise
100 DEG C, while acid value is measured by sampling, 110~120 DEG C are warming up to the reaction later stage, acid value is made to be decreased to less than 5mgKOH/g stoppings
Reaction, it is spare to be cooled to 80 DEG C of dischargings.Since epoxy acid esters viscosity is larger, 20% activity dilution can be added when being cooled to 80 DEG C
Agent and appropriate polymerization inhibitor.Common reactive diluent is three glycerine diacrylates, trimethylolpropane trimethacrylate, often
Polymerization inhibitor is p methoxy phenol, hydroquinone, 2,5- dimethyl hydroquinones, 2,6- toluene di-tert-butyl phenols etc.,
Polymerization inhibitor addition is about the 0.01%~1% of resin quality.
198g graphene powders and 2gSiC powder mixings are weighed, 1000L DMF is added into, utilizes high-power ultrasonics
Mixed-powder is evenly dispersed uniformly, obtain supersaturated graphene dispersing solution slurry.Again by supersaturated graphene dispersing solution slurry
The epoxy acrylic resin prepared is added under the conditions of being protected from light and is sufficiently mixed, obtains mixed slurry.Supersaturated graphene point
Dispersion liquid slurry is 3 with epoxy acrylic resin volume ratio:7.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing Stereolithography equipment, using controllable UV Line beam, using face exposure
Mode is successively printed according to three-dimensional part model, and thickness is 80 μm, optical source wavelength 400nm, time for exposure 3s and successively makes
At graphene product crude green body.
(3) it post-processes
By in made graphene product crude green body merging low-temperature sintering stove, low-temperature defatted processing 2h is carried out at 800 DEG C, is made
Organic adhesive overflows, volatilizees.Again by after degreasing graphene product crude green body merging hot isostatic pressing stove in, 1350 DEG C,
Under 200MPa, hip treatment 3h is carried out, obtains fine and close graphene product.
Embodiment 2
A kind of preparation method of graphene product, specifically includes following steps：
(1) prepared by raw material
The synthesis of urethane acrylate is anti-using polyisocyanates, long chain diol, crylic acid hydroxy ester and catalyst
Answer synthesis of polyurethane acrylate.Tertiary amines, metallic compound and organophosphor can be selected in catalyst.Different polyisocyanate cyanogen can be selected
Acid esters and long chain diol obtain the urethane acrylate of different structure.The synthesis of urethane acrylate is to utilize isocyanates
Prepared by middle isocyano and hydroxyl reaction in long chain diol and crylic acid hydroxy ester, formation ammonia ester bond.
Synthesis of polyurethane acrylate method is in the present embodiment：By 2mol diisocyanate and a certain amount of lauric acid two
Butyl tin is added in reactor, is warming up to 40~50 DEG C, and 1mol glycol is slowly added dropwise, and after reacting 1h, is warming up to 60 DEG C, measure-
Nco value is added 2mol crylic acid hydroxy esters and a certain amount of hydroquinone of polymerization retarder, is warming up to 70~80 DEG C, directly to calculated value
Extremely-nco value is zero.There is larger toxicity in view of-NCO, when reaction, can suitably make crylic acid hydroxy ester slightly excessive, make-
The reaction was complete for NCO group.
20g graphene powders and 0.02g SiC powder mixings are weighed, 100L NMP is added into, utilizes large power supersonic
Wave is evenly dispersed uniformly by mixed-powder, obtains supersaturated graphene dispersing solution slurry.Again by supersaturated graphene dispersion slurry
Material is added the urethane acrylate resin prepared and is sufficiently mixed under the conditions of being protected from light, and obtains mixed slurry.Supersaturated graphene
Dispersion liquid slurry is 3 with urethane acrylate resin volume ratio:5.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, in such a way that face exposes, root are utilized
It is successively printed according to three-dimensional part model, thickness is 60 μm, optical source wavelength 350nm, time for exposure 2s and graphene is successively made
Product crude green body.
(3) it post-processes
By in made graphene product crude green body merging low-temperature sintering stove, low-temperature defatted processing 1.5h is carried out at 500 DEG C,
Organic adhesive is set to overflow, volatilization.Again by after degreasing graphene product crude green body merging hot isostatic pressing stove in, 1200 DEG C,
Under 150MPa, hip treatment 1h is carried out, obtains fine and close graphene product.
Embodiment 3
A kind of preparation method of graphene product, specifically includes following steps：
(1) prepared by raw material
20g graphene powders and 0.2g SiC powder mixings are weighed, 100L THF is added into, utilizes high-power ultrasonics
Mixed-powder is evenly dispersed uniformly, obtain supersaturated graphene dispersing solution slurry.Again by supersaturated graphene dispersing solution slurry
Urethane acrylate is added under the conditions of being protected from light and is sufficiently mixed, obtains mixed slurry.Supersaturated graphene dispersing solution slurry
It is 3 with urethane acrylate volume ratio:2.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, by the way of spot scan, root are utilized
It is successively printed according to three-dimensional part model, thickness is 40 μm, optical source wavelength 350nm, spot diameter 0.15mm, hot spot movement speed
1mm/min is spent, graphene product crude green body is successively made.
(3) it post-processes
By in made graphene product crude green body merging low-temperature sintering stove, low-temperature defatted processing 1h is carried out at 200 DEG C, is made
Organic adhesive overflows, volatilizees.Again by after degreasing graphene product crude green body merging hot isostatic pressing stove in, 1000 DEG C,
Under 120MPa, hip treatment 1h is carried out, obtains fine and close graphene product.
Embodiment 4
A kind of preparation method of graphene product, specifically includes following steps：
(1) prepared by raw material
2g graphene powders and 0.006g SiC powder mixings are weighed, 10L THF is added into, utilizes high-power ultrasonics
Mixed-powder is evenly dispersed uniformly, obtain supersaturated graphene dispersing solution slurry.Again by supersaturated graphene dispersing solution slurry
Polyester acrylate resin is added under the conditions of being protected from light and is sufficiently mixed, obtains mixed slurry.Supersaturated graphene dispersing solution slurry
It is 3 with polyester acrylate resin volume ratio:3.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, by the way of spot scan, root are utilized
It is successively printed according to three-dimensional part model, thickness is 20 μm, optical source wavelength 300nm, spot diameter 0.1mm, hot spot movement speed
300mm/min is spent, graphene product crude green body is successively made.
(3) it post-processes
By in made graphene product crude green body merging low-temperature sintering stove, low-temperature defatted processing 1h is carried out at 100 DEG C, is made
Organic adhesive overflows, volatilizees.Again by after degreasing graphene product crude green body merging hot isostatic pressing stove in, 1000 DEG C,
Under 100MPa, hip treatment 20min is carried out, obtains fine and close graphene product.
Embodiment 5
A kind of preparation method of graphene product, specifically includes following steps：
(1) prepared by raw material
2g graphene powders and 0.014g SiC powder mixings are weighed, 10L NMP is added into, utilizes high-power ultrasonics
Mixed-powder is evenly dispersed uniformly, obtain supersaturated graphene dispersing solution slurry.Again by supersaturated graphene dispersing solution slurry
Polyester acrylate resin is added under the conditions of being protected from light and is sufficiently mixed, obtains mixed slurry.Supersaturated graphene dispersing solution slurry
It is 3 with polyester acrylate resin volume ratio:4.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, by the way of spot scan, root are utilized
It is successively printed according to three-dimensional part model, thickness is 25 μm, optical source wavelength 200nm, spot diameter 0.15mm, hot spot movement speed
150mm/min is spent, graphene product crude green body is successively made.
(3) it post-processes
By in made graphene product crude green body merging low-temperature sintering stove, low-temperature defatted processing 1h is carried out at 120 DEG C, is made
Organic adhesive overflows, volatilizees.Again by after degreasing graphene product crude green body merging hot isostatic pressing stove in, 1000 DEG C,
Under 100MPa, hip treatment 20min is carried out, obtains fine and close graphene product.
The defects of compactness for the graphene product that 1-5 of the embodiment of the present invention is prepared is good, internal pore-free, slag inclusion,
Market product requirement can be met, and different, can meet the needs of different shape part.
The present invention manufactures graphene product using 3D printing technique, and shape is unfettered, can easily and fast prepare and provide
The variously-shaped graphene product for having high-compactness, has filled up blank in the market, has prodigious market value.
Above description of the present invention is section Example, and but the invention is not limited in above-mentioned embodiment.
Above-mentioned specific implementation mode is schematical, is not restrictive.Every material using the present invention and method are not taking off
In the case of present inventive concept and scope of the claimed protection, it is all it is specific expansion belong to protection scope of the present invention it
It is interior.
Claims (3)
1. a kind of preparation method of graphene product, which is characterized in that include the following steps：
Step 1, raw material is prepared
Graphene powder is mixed with SiC powder, organic solvent is added in mixed-powder, so that mixed-powder is being had using ultrasonic wave
It is uniformly dispersed in solvent, obtains supersaturated graphene dispersing solution slurry；Supersaturated graphene dispersing solution slurry is glued with organic
It connects agent uniformly to mix under the conditions of being protected from light, obtains mixed slurry；
The additive amount of the SiC powder is the 0.1~1% of mixed-powder total volume；The graphene powder with it is described organic molten
The proportionate relationship of agent is：2mg~20mg graphene powders are added in per 10mL organic solvents；The supersaturation graphene dispersing solution
The volume ratio of slurry and the organic adhesive is 3:2~3:7；
The organic solvent is NN- dimethylformamides, N-Methyl pyrrolidone or tetrahydrofuran；
The organic adhesive is epoxy acrylic resin, urethane acrylate, polyester acrylate, polyester acrylate resin
Or one of amino acrylic resin；
Step 2, crude green body manufactures
Mixed slurry is fitted into 3D printing Stereolithography equipment, using controllable UV Line beam, is exposed or is put using face and swept
The mode retouched successively prints according to three-dimensional part model, graphene product crude green body is made；
Step 3, it post-processes
Graphene product crude green body is subjected to low-temperature defatted processing, so that the organic adhesive in crude green body is evaporated and overflows；Heat etc. is carried out again
Static pressure processing, obtains fine and close graphene product；
1000 DEG C~1350 DEG C of the hip treatment temperature, pressure 100MPa~200MPa, time 0.2-3h；
100 DEG C~800 DEG C of the temperature of the low-temperature defatted processing, time 1-2h.
2. the preparation method of graphene product according to claim 1, which is characterized in that the thickness control successively printed
For system at 20~80 μm, optical source wavelength is 200~400nm.
3. the preparation method of graphene product according to claim 1, which is characterized in that the printing type is exposed using face
Light time, time for exposure 0.1-3s；When the printing type uses spot scan, spot diameter is 0.1~0.15mm, hot spot movement
Speed 1-300mm/min.
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| CN110028329B (en) * | 2018-01-11 | 2021-10-29 | 航天特种材料及工艺技术研究所 | High-thermal-conductivity ceramic matrix composite and preparation method thereof |
| CN109825087B (en) * | 2019-01-31 | 2021-08-03 | 江南大学 | Protective material for 3D printing of high-negative Poisson ratio interwoven structure |
| CN115403390B (en) * | 2022-09-20 | 2023-03-31 | 吉林大学 | Method for preparing porous carbon skeleton by photocuring 3D printing through high-solid-content/low-transmittance carbon-based slurry |
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| CN103769586A (en) * | 2013-11-26 | 2014-05-07 | 王利民 | Metal 3D printing product production method by means of low-power laser sintering |
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