CN106187192A - The preparation method of a kind of glass-like carbon goods and glass-like carbon goods - Google Patents
The preparation method of a kind of glass-like carbon goods and glass-like carbon goods Download PDFInfo
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- CN106187192A CN106187192A CN201610561829.8A CN201610561829A CN106187192A CN 106187192 A CN106187192 A CN 106187192A CN 201610561829 A CN201610561829 A CN 201610561829A CN 106187192 A CN106187192 A CN 106187192A
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- C—CHEMISTRY; METALLURGY
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- 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
- C04B35/524—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 obtained from polymer precursors, e.g. glass-like carbon material
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- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention discloses the preparation method of a kind of glass-like carbon goods.The method includes: step 1, disperse graphene in deionized water first with surfactant, obtains graphene solution；Then being sufficiently mixed with described graphene solution by high molecular polymer powder, obtaining mass ratio between Graphene and high molecular polymer is (0.1～1): the mixed slurry of 100；Step 2, described mixed slurry is dried after carry out dry ball milling, and the material powder after ball milling is carried out conditioning；Step 3, the powder after conditioning is carried out compression molding, then carry out low-temperature setting, obtain glass-like carbon green compact；Step 4, in anaerobic or inert environments, glass-like carbon green compact are carried out carbonization process；Step 5, graphitization processing.The invention also discloses the glass-like carbon goods making to prepare in aforementioned manners.Compared to existing technology, the present invention can significantly shorten the production cycle, improves the performance of glass-like carbon goods, and the specification of fertile glass-like carbon goods, shape unrestricted.
Description
Technical field
The preparation method that the present invention relates to a kind of glass-like carbon goods and the glass-like carbon goods using the method to prepare.
Background technology
Glass-like carbon is because having low-density, high intensity, high rigidity, high connductivity and high-termal conductivity, corrosion-resistant, wear-resistant, almost
The excellent properties such as airtight and isotropism, be widely used in electronics industry, semi-conductor industry, metallurgical industry, chemical industry,
Nuclear industry and medical domain etc..Prepare the macromolecule prepolymer presoma of glass-like carbon material mainly have phenolic resin, furfuryl alcohol resin,
Poly furfuryl alcohol, polrvinyl chloride, polyimides etc..At present, preparing glass-like carbon and mainly use cast shaping process, its basic technology is by height
Molecularly Imprinted Polymer is dissolved in alcohols solvent, through low-temperature setting molding or add firming agent molding and prepare green compact, afterwards in anaerobic or
Person's inert environments carries out 1000oThe carbonization of about C processes, and prepares glass-like carbon goods；Through 2000-3000 afteroAt the high temperature of C
Reason prepares purity more preferable glass-like carbon goods.With high molecular polymer for the material that sets out, cast shaping process is used to prepare glass
The process route of charcoal can be summarized as: solution allocation → curing molding → carbonization → graphitization.During curing molding, resin is molten
Escape within subordinate after the little molecule absorption energy such as solvent in liquid, moisture.Along with the further increase of curing molding temperature, tree
Fat will proceed by condensation polymerization, discharge gas and the energy of flouring generation.Because of the volume contraction in glass-like carbon forming process
Occur mostly in the curing molding stage, for improving the quality of goods, preventing the destruction that volume contraction causes, it is desirable to curing molding
Stage uses slowly heating rate (0.5-1oC/h).Use cast shaping process to prepare glass-like carbon goods and generally produce week
Phase length, production cost height, the specification of formed glass carbon product and shape are limited.
Summary of the invention
The technical problem to be solved is to overcome prior art not enough, it is provided that the preparation of a kind of glass-like carbon goods
Method, can significantly shorten the production cycle, improve glass-like carbon goods performance, and fertile glass-like carbon goods specification,
Shape is unrestricted.
The present invention solves above-mentioned technical problem the most by the following technical solutions:
The preparation method of a kind of glass-like carbon goods, comprises the following steps:
Step 1, disperse graphene in deionized water first with surfactant, obtain graphene solution；Then by high score
Sub-polymer powder is sufficiently mixed with described graphene solution, and obtaining mass ratio between Graphene and high molecular polymer is (0.1
～1): the mixed slurry of 100；
Step 2, described mixed slurry is dried after carry out dry ball milling, and the material powder after ball milling is carried out conditioning；
Step 3, the powder after conditioning is carried out compression molding, then according to following process conditions carry out low-temperature setting,
To glass-like carbon green compact: with 1oThe heating rate of C/h is warming up to 80oC, is incubated 2～5h；Again with 1oThe heating rate of C/h is warming up to
110oC, is incubated 2～5h；Again with 2oThe heating rate of C/h is warming up to 130oC, is incubated 2～5h；Again with 2oThe heating rate liter of C/h
Temperature is to 150oC, is incubated 2～5h；Cooling；
Step 4, in anaerobic or inert environments, glass-like carbon green compact are carried out carbonization process；
Step 5, graphitization processing.
Preferably, by macromolecule polymer solution carries out ball milling with described graphene solution, to mix realization the most mixed
Close.
Preferably, between Graphene and the high molecular polymer in described mixed slurry, mass ratio is 0.7:100.
Preferably, the process conditions that described carbonization processes are: with 10oThe heating rate of C/h is warming up to 350oC, is incubated 10h；
Again with 10oThe heating rate of C/h is warming up to 750oC, is incubated 10h；Again with 20oThe heating rate of C/h is warming up to 1000oC, insulation
10h；Cooling.
Preferably, when the material powder after ball milling is carried out conditioning, by the moisture control of powder 8～12%.
Preferably, the treatment temperature of described graphitization processing is 2500oC, the process time is 2h.
Described high molecular polymer can use phenolic resin, furfuryl alcohol resin, poly furfuryl alcohol, polrvinyl chloride, polyimides etc.
The existing macromolecule prepolymer presoma used when preparing glass-like carbon, preferably phenolic resin, furfuryl alcohol resin, poly furfuryl alcohol.
A kind of glass-like carbon goods, use as above either method to prepare.
Compared to existing technology, the method have the advantages that
The present invention has used for reference ceramic powders metallurgical technology, and to glass-like carbon, preparation technology is greatly improved, use powder preparation with
The mode that compression molding combines carries out follow-up low-temperature setting, carbonization, graphitization processing again after producing glass-like carbon base substrate, and
Improve the fracture toughness of glass-like carbon semi-finished product and finished product as modifying agent by adding Graphene, the present invention can significantly shorten glass
The production cycle of glass carbon product, improve conforming product rate.
The inventive method owing to have employed powder die press technology for forming, therefore fertile glass-like carbon goods specification,
Shape is unrestricted.
The performances such as the density of glass-like carbon goods prepared by the inventive method, the porosity, fracture toughness compare traditional handicraft
Improve a lot, especially fracture toughness.
Detailed description of the invention
The present invention is directed to the deficiency of traditional glass charcoal preparation technology, by using for reference the correlation technique in ceramic powders metallurgy,
To glass-like carbon, preparation technology is greatly improved, and the mode using powder preparation to combine with compression molding produces glass-like carbon base
Carry out follow-up low-temperature setting, carbonization, graphitization processing after body again, and improve glass-like carbon half by adding Graphene modifying agent
Finished product and the fracture toughness of finished product, thus can significantly shorten the production cycle of glass-like carbon goods, improve conforming product rate, and institute
The glass-like carbon goods prepared have the performances such as excellent density, the porosity, fracture toughness.
The preparation method of glass-like carbon goods of the present invention, specifically includes following steps:
Step 1, disperse graphene in deionized water first with surfactant, obtain graphene solution；Then by high score
Sub-polymer powder is sufficiently mixed with described graphene solution, and obtaining mass ratio between Graphene and high molecular polymer is (0.1
～1): the mixed slurry of 100；
Described high molecular polymer can use phenolic resin, furfuryl alcohol resin, poly furfuryl alcohol, polrvinyl chloride, polyimides etc. existing
The macromolecule prepolymer presoma used when preparing glass-like carbon, it is preferred to use phenolic resin or furfuryl alcohol resin or poly furfuryl alcohol.
In order to solve Graphene dispersion problem in aqueous phase and the sex chromosome mosaicism of mixing homogeneously with high molecular polymer thereof,
Need to use surfactant；Described surfactant can use cetyl trimethylammonium bromide, dodecylbenzene sodium sulfonate,
The existing surfactant such as Tween-80.
Preferred mass between Graphene and high molecular polymer is than for 0.7:100.
By the most frequently used alr mode, high molecular polymer powder can be sufficiently mixed with described graphene solution, in order to
Improve the uniformity of mixing, present invention preferably employs the mode of ball milling mixing, i.e. utilize ball mill to high molecular polymer and stone
Ink alkene solution carries out abundant ball milling mixing.
Step 2, described mixed slurry is dried after carry out dry ball milling, and the material powder after ball milling is carried out conditioning；
First being dried by described mixed slurry, preferably drying temperature is 65oC, drying time can be according to slurry volume, baking oven merit
The practical situations such as rate, slurry water content set flexibly.Utilize ball-grinding machine that the material block after drying is carried out dry ball milling, block will be expected
Ball milling is uniform powder, as the raw material of follow-up compression molding.In order to ensure the quality of compression molding smoothly, the most first by ball
Powder after mill sieves (such as 200 mesh or 180 mesh sieves), to reject the biggest block material；Then to the powder after sieving
Carry out conditioning, by the moisture control of powder 8～12%, using water as follow-up compression molding during lubricant and
Binding agent.
Step 3, the powder after conditioning is carried out compression molding, then according to following process conditions carry out low-temperature solid
Change, obtain glass-like carbon green compact: with 1oThe heating rate of C/h is warming up to 80oC, is incubated 2～5h；Again with 1oThe heating rate liter of C/h
Temperature is to 110oC, is incubated 2～5h；Again with 2oThe heating rate of C/h is warming up to 130oC, is incubated 2～5h；Again with 2oThe intensification speed of C/h
Rate is warming up to 150oC, is incubated 2～5h；Cooling；
First according to the finished product corresponding mould of true form size Selection, press device can use hydraulic press, air pressure press
Or mechanical press.The base substrate suppressed is put into baking box, carries out low-temperature setting according to process above condition, obtain glass-like carbon raw
Base.Can be seen that from process above parameter, compare traditional handicraft, the heating rate needed for low-temperature setting in present invention process flow process
Can be greatly improved, temperature retention time significantly shortens, and total low-temperature setting time is greatly decreased.
Step 4, in anaerobic or inert environments, glass-like carbon green compact are carried out carbonization process；
The carbonization of the present invention processes and existing carbonization can be used to process technological parameter, but modified owing to present invention employs Graphene
Agent and have employed stamping of powder moulding process, the overall time that therefore carbonization processes also can shorten, and carbonization of the present invention processes
Preferred processing condition is: with 10oThe heating rate of C/h is warming up to 350oC, is incubated 10h；Again with 10oThe heating rate of C/h heats up
To 750oC, is incubated 10h；Again with 20oThe heating rate of C/h is warming up to 1000oC, is incubated 10h；Cooling.
Step 5, graphitization processing；
Graphitization processing can use existing technological parameter, preferred treatment temperature to be 2500oC, the process time is 2h.
Below in conjunction with specific embodiment, technical solution of the present invention and effect thereof are described further.Should be understood that following reality
Execute example and be merely to illustrate the present invention not for limiting the scope of the present invention.
Embodiment 1
It is that 0.05:100 configures slip by the mass ratio of Graphene Yu phenolic resin, and puts into ball milling 5h in ball mill, ball mill
Rotating speed is 400rpm.
The slip of the high molecular polymer prepared in above-mentioned steps is taken out and puts into drying baker, 65oDry under the conditions of C
10h。
The material block dried in above-mentioned steps is put into ball milling 5h in ball mill, crosses 200 mesh sieves.
Powder body after sieving in above-mentioned steps is put into climatic chamber and is carried out conditioning, controls the moisture content of powder
It is 10%.
The powder body obtained in above-mentioned steps is loaded in molding jig (cavity dimension is 50 × 50 × 10mm) compressing,
Dwell time 5min, briquetting pressure is 90MPa, matched moulds speed 0.2mm/s.
Base substrate after compressing in above-mentioned steps is carried out low-temperature setting process.During low-temperature setting, with 1oThe intensification of C/h
Ramp is to 80oC, is incubated 2h；With 1oThe heating rate of C/h is from 80oC is warming up to 110oC, is incubated 2h；With 2oThe intensification speed of C/h
Rate is warming up to 130oC, is incubated 2h；Again with 2oThe heating rate of C/h is warming up to 150oC, is incubated 2h；Cooling, prepares glass-like carbon raw
Base.
Glass-like carbon green compact after solidification in above-mentioned steps are carried out carbonization process.During carbonization, with 10oThe heating rate of C/h
It is warming up to 350oC, is incubated 10h；With 10oThe heating rate of C/h is from 350oC is warming up to 750oC, is incubated 10h；Again with 20oThe liter of C/h
Temperature ramp is to 1000oC, is incubated 10h；Cooling.
Glass-like carbon above-mentioned steps prepared is put in high temperature graphitization process stove and is carried out graphitization processing.Treatment temperature
It is 2500oC, the process time is 2h, i.e. obtains final glass-like carbon material.
The density of the glass-like carbon prepared in embodiment 1 is 1.42g/cm3, porosity is 2.71%, and fracture toughness is
0.96MPa·m1/2。
Embodiment 2
It is that 0.1:100 configures slip by the mass ratio of Graphene Yu phenolic resin, and puts into ball milling 5h in ball mill, rotating speed
400rpm。
The slip prepared in above-mentioned steps is taken out and puts into drying baker, 65o10h is dried under the conditions of C.
The material block dried in above-mentioned steps is put into ball milling 5h in ball mill, crosses 200 mesh sieves.
Powder body after drying in above-mentioned steps is put into climatic chamber and is carried out conditioning, controls the moisture content of powder
It is 10%.
The powder body obtained in above-mentioned steps is loaded in molding jig (cavity dimension is 50 × 50 × 10mm) compressing,
Dwell time 5min, briquetting pressure is 30MPa, matched moulds speed 0.2mm/s.
The low-temperature setting of the base substrate after compressing in above-mentioned steps is processed.During low-temperature setting, with 1oThe intensification speed of C/h
Rate is warming up to 80oC, is incubated 2h；With 1oThe heating rate of C/h is from 80oC is warming up to 110oC, is incubated 2h；With 2oThe heating rate of C/h
It is warming up to 130oC, is incubated 2h；Again with 2oThe heating rate of C/h is warming up to 150oC, is incubated 2h；Cooling, prepares glass-like carbon green compact.
Glass-like carbon green compact after solidification in above-mentioned steps are carried out carbonization process.During carbonization, with 10oThe heating rate of C/h
It is warming up to 350oC, is incubated 10h；With 10oThe heating rate of C/h is from 350oC is warming up to 750oC, is incubated 10h；Again with 20oThe liter of C/h
Temperature ramp is to 1000oC, is incubated 10h；Cooling.
Glass-like carbon above-mentioned steps prepared is put in high temperature graphitization process stove and is carried out graphitization processing.Treatment temperature
It is 2500oC, the process time is 2h, i.e. obtains final glass-like carbon material.
The density of the glass-like carbon prepared in embodiment 2 is 1.34g/cm3, porosity is 4.34%, and fracture toughness is
1.17MPa·m1/2。
Embodiment 3:
It is that 0.3:100 configures slip by the mass ratio of Graphene Yu phenolic resin, and puts into ball milling 5h in ball mill, rotating speed
400rpm。
The slip of the high molecular polymer prepared in above-mentioned steps is taken out and puts into drying baker, 65oDry under the conditions of C
10h。
The material block dried in above-mentioned steps is put into ball milling 5h in ball mill, crosses 200 mesh sieves.
Powder body after drying in above-mentioned steps is put into climatic chamber and is carried out conditioning, controls the moisture content of powder
It is 10%.
Pretreated powder body in above-mentioned steps is loaded (cavity dimension is 50 × 50 × 10mm) compacting in molding jig
Shaping, dwell time 5min, briquetting pressure is 60MPa, matched moulds speed 0.2mm/s.
The low-temperature setting of the base substrate after compressing in above-mentioned steps is processed.During low-temperature setting, with 1oThe intensification speed of C/h
Rate is warming up to 80oC, is incubated 2h；With 1oThe heating rate of C/h is from 80oC is warming up to 110oC, is incubated 2h；With 2oThe heating rate of C/h
It is warming up to 130oC, is incubated 2h；Again with 2oThe heating rate of C/h is warming up to 150oC, is incubated 2h；Cooling, prepares glass-like carbon green compact.
Glass-like carbon green compact after solidification in above-mentioned steps are carried out carbonization process.During carbonization, with 10oThe heating rate of C/h
It is warming up to 350oC, is incubated 10h；With 10oThe heating rate of C/h is from 350oC is warming up to 750oC, is incubated 10h；Again with 20oThe liter of C/h
Temperature ramp is to 1000oC, is incubated 10h；Cooling.
Glass-like carbon above-mentioned steps prepared is put in high temperature graphitization process stove and is carried out graphitization processing.Treatment temperature
It is 2500oC, the process time is 2h, i.e. obtains final glass-like carbon material.
The density of the glass-like carbon prepared in embodiment 3 is 1.38g/cm3, porosity is 3.47%, and fracture toughness is
1.23MPa·m1/2。
Embodiment 4:
It is that 0.5:100 configures slip by the mass ratio of Graphene Yu phenolic resin, and puts into ball milling 5h in ball mill, rotating speed
400rpm。
The slip of the high molecular polymer prepared in above-mentioned steps is taken out and puts into drying baker, 65oDry under the conditions of C
10h。
The material block dried in above-mentioned steps is put into ball milling 5h in ball mill, crosses 200 mesh sieves.
Powder body after drying in above-mentioned steps is put into climatic chamber and is carried out conditioning, controls the moisture content of powder
It is 10%.
Pretreated powder body in above-mentioned steps is loaded (cavity dimension is 50 × 50 × 10mm) compacting in molding jig
Shaping, dwell time 5min, briquetting pressure is 60MPa, matched moulds speed 0.2mm/s.
The low-temperature setting of the base substrate after compressing in above-mentioned steps is processed.During low-temperature setting, with 1oThe intensification speed of C/h
Rate is warming up to 80oC, is incubated 2h；With 1oThe heating rate of C/h is from 80oC is warming up to 110oC, is incubated 2h；With 2oThe heating rate of C/h
It is warming up to 130oC, is incubated 2h；Again with 2oThe heating rate of C/h is warming up to 150oC, is incubated 2h；Cooling, prepares glass-like carbon green compact.
Glass-like carbon green compact after solidification in above-mentioned steps are carried out carbonization process.During carbonization, with 10oThe heating rate of C/h
It is warming up to 350oC, is incubated 10h；With 10oThe heating rate of C/h is from 350oC is warming up to 750oC, is incubated 10h；Again with 20oThe liter of C/h
Temperature ramp is to 1000oC, is incubated 10h；Cooling.
Glass-like carbon above-mentioned steps prepared is put in high temperature graphitization process stove and is carried out graphitization processing.Treatment temperature
It is 2500oC, the process time is 2h, i.e. obtains final glass-like carbon material.
The density of the glass-like carbon prepared in embodiment 4 is 1.42g/cm3, porosity is 2.92%, and fracture toughness is
1.31MPa·m1/2。
Embodiment 5:
It is that 0.7:100 configures slip by the mass ratio of Graphene Yu phenolic resin, and puts into ball milling 5h in ball mill, rotating speed
400rpm。
The slip of the high molecular polymer prepared in above-mentioned steps is taken out and puts into drying baker, 65oDry under the conditions of C
10h。
The material block dried in above-mentioned steps is put into ball milling 5h in ball mill, crosses 200 mesh sieves.
Powder body after drying in above-mentioned steps is put into climatic chamber and is carried out conditioning, controls the moisture content of powder
It is 10%.
Pretreated powder body in above-mentioned steps is loaded (cavity dimension is 50 × 50 × 10mm) compacting in molding jig
Shaping, dwell time 5min, briquetting pressure is 90MPa, matched moulds speed 0.2mm/s.
The low-temperature setting of the base substrate after compressing in above-mentioned steps is processed.During low-temperature setting, with 1oThe intensification speed of C/h
Rate is warming up to 80oC, is incubated 2h；With 1oThe heating rate of C/h is from 80oC is warming up to 110oC, is incubated 2h；With 2oThe heating rate of C/h
It is warming up to 130oC, is incubated 2h；Again with 2oThe heating rate of C/h is warming up to 150oC, is incubated 2h；Cooling prepares glass-like carbon green compact.
Glass-like carbon green compact after solidification in above-mentioned steps are carried out carbonization process.During carbonization, with 10oThe heating rate of C/h
It is warming up to 350oC, is incubated 10h；With 10oThe heating rate of C/h is from 350oC is warming up to 750oC, is incubated 10h；Again with 20oThe liter of C/h
Temperature ramp is to 1000oC, is incubated 10h；Cooling.
Glass-like carbon above-mentioned steps prepared is put in high temperature graphitization process stove and is carried out graphitization processing.Treatment temperature
It is 2500oC, the process time is 2h, i.e. obtains final glass-like carbon material.
The density of the glass-like carbon prepared in embodiment 5 is 1.46g/cm3, porosity is 2.21%, and fracture toughness is
1.39MPa·m1/2。
Embodiment 6:
It is that 0.9:100 configures slip by the mass ratio of Graphene Yu phenolic resin, and puts into ball milling 5h in ball mill, rotating speed
400rpm。
The slip of the high molecular polymer prepared in above-mentioned steps is taken out and puts into drying baker, 65oDry under the conditions of C
10h。
The material block dried in above-mentioned steps is put into ball milling 5h in ball mill, crosses 200 mesh sieves.
Powder body after drying in above-mentioned steps is put into climatic chamber and is carried out conditioning, controls the moisture content of powder
It is 10%.
Pretreated powder body in above-mentioned steps is loaded (cavity dimension is 50 × 50 × 10mm) compacting in molding jig
Shaping, dwell time 5min, briquetting pressure is 120MPa, matched moulds speed 0.2mm/s.
The low-temperature setting of the base substrate after compressing in above-mentioned steps is processed.During low-temperature setting, with 1oThe intensification speed of C/h
Rate is warming up to 80oC, is incubated 2h；With 1oThe heating rate of C/h is from 80oC is warming up to 110oC, is incubated 2h；With 2oThe heating rate of C/h
It is warming up to 130oC, is incubated 2h；Again with 2oThe heating rate of C/h is warming up to 150oC, is incubated 2h；Cooling prepares glass-like carbon green compact.
Glass-like carbon green compact after solidification in above-mentioned steps are carried out carbonization process.During carbonization, with 10oThe heating rate of C/h
It is warming up to 350oC, is incubated 10h；With 10oThe heating rate of C/h is from 350oC is warming up to 750oC, is incubated 10h；Again with 20oThe liter of C/h
Temperature ramp is to 1000oC, is incubated 10h；Cooling.
Glass-like carbon above-mentioned steps prepared is put in high temperature graphitization process stove and is carried out graphitization processing.Treatment temperature
It is 2500oC, the process time is 2h, i.e. obtains final glass-like carbon material.
The density of the glass-like carbon prepared in embodiment 6 is 1.47g/cm3, porosity is 2.01%, and fracture toughness is
1.32MPa·m1/2。
Claims (8)
1. the preparation method of glass-like carbon goods, it is characterised in that comprise the following steps:
Step 1, disperse graphene in deionized water first with surfactant, obtain graphene solution；Then by high score
Sub-polymer powder is sufficiently mixed with described graphene solution, and obtaining mass ratio between Graphene and high molecular polymer is (0.1
～1): the mixed slurry of 100；
Step 2, described mixed slurry is dried after carry out dry ball milling, and the material powder after ball milling is carried out conditioning；
Step 3, the powder after conditioning is carried out compression molding, then according to following process conditions carry out low-temperature setting,
To glass-like carbon green compact: with 1oThe heating rate of C/h is warming up to 80oC, is incubated 2～5h；Again with 1oThe heating rate of C/h is warming up to
110oC, is incubated 2～5h；Again with 2oThe heating rate of C/h is warming up to 130oC, is incubated 2～5h；Again with 2oThe heating rate liter of C/h
Temperature is to 150oC, is incubated 2～5h；Cooling；
Step 4, in anaerobic or inert environments, glass-like carbon green compact are carried out carbonization process；
Step 5, graphitization processing.
2. preparation method as claimed in claim 1, it is characterised in that by molten with described Graphene to macromolecule polymer solution
Liquid carries out ball milling mixing realization and is sufficiently mixed.
3. preparation method as claimed in claim 1, it is characterised in that the Graphene in described mixed slurry and high molecular polymer
Between mass ratio be 0.7:100.
4. preparation method as claimed in claim 1, it is characterised in that described high molecular polymer is phenolic resin, or furfuryl alcohol resin
Fat, or poly furfuryl alcohol.
5. preparation method as claimed in claim 1, it is characterised in that the process conditions that described carbonization processes are: with 10oThe liter of C/h
Temperature ramp is to 350oC, is incubated 10h；Again with 10oThe heating rate of C/h is warming up to 750oC, is incubated 10h；Again with 20oC/h's
Heating rate is warming up to 1000oC, is incubated 10h；Cooling.
6. preparation method as claimed in claim 1, it is characterised in that when the material powder after ball milling is carried out conditioning, by powder
The moisture control of material is 8～12%.
7. preparation method as claimed in claim 1, it is characterised in that the treatment temperature of described graphitization processing is 2500oC, processes
Time is 2h.
8. glass-like carbon goods, the method as described in any one of claim 1～7 of use prepares.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000275208A (en) * | 1999-03-25 | 2000-10-06 | Mitsubishi Pencil Co Ltd | Carbon material for electrochemical measurement and manufacture thereof |
| CN104411630A (en) * | 2012-06-15 | 2015-03-11 | 陶氏环球技术有限责任公司 | Vitreous carbon composition |
| CN105692589A (en) * | 2016-03-14 | 2016-06-22 | 中国科学院上海应用物理研究所 | Preparation method of glassy carbon material based on modified phenolic resin precursor |
-
2016
- 2016-07-18 CN CN201610561829.8A patent/CN106187192B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000275208A (en) * | 1999-03-25 | 2000-10-06 | Mitsubishi Pencil Co Ltd | Carbon material for electrochemical measurement and manufacture thereof |
| CN104411630A (en) * | 2012-06-15 | 2015-03-11 | 陶氏环球技术有限责任公司 | Vitreous carbon composition |
| CN105692589A (en) * | 2016-03-14 | 2016-06-22 | 中国科学院上海应用物理研究所 | Preparation method of glassy carbon material based on modified phenolic resin precursor |
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| Title |
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| 尹彩流等: ""粘结剂种类对模压成形制备呋喃树脂类玻璃炭的影响"", 《功能材料》 * |
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