CN106431498B - A method of preparing graphite/carbon SiClx densified composite - Google Patents
A method of preparing graphite/carbon SiClx densified composite Download PDFInfo
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- CN106431498B CN106431498B CN201610803513.5A CN201610803513A CN106431498B CN 106431498 B CN106431498 B CN 106431498B CN 201610803513 A CN201610803513 A CN 201610803513A CN 106431498 B CN106431498 B CN 106431498B
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
Abstract
The invention discloses a kind of methods for preparing graphite/carbon SiClx densified composite, before the depositing silicon silicon of graphite piece surface, first in one layer of silicon-carbide particle layer of graphite piece external coating as transition zone, then CVD deposition coat of silicon carbide.The present invention by one layer of silicon-carbide particle of graphite piece external coating as transition zone, CVD deposition coat of silicon carbide again, because silicon-carbide particle transition zone, there are small hole, the silicon carbide deposited on surface penetrates into hole so that coating in conjunction with matrix more closely;Meanwhile of the invention method period is short, power consumption is low, effectively solves the problems, such as the purity and coating binding force of graphite piece, prevents from giving subsequent workshop section introducing impurity.
Description
Technical field
The present invention relates to technical field of inorganic non-metal material preparation, and in particular to a kind of to prepare graphite/carbon SiClx densification
The method of composite material.
Background technique
In graphite piece surface depositing silicon silicon, generalling use methyl trichlorosilane is presoma, and chemical vapor deposition occurs
Coat of silicon carbide, by-product HCl gas are obtained after reaction.In certain specific applications, it is desirable that coat of silicon carbide combines densification, can
To prevent the partial impurities of graphite piece from entering reaction system;In addition, also coat of silicon carbide is required to be tightly combined, wear-resisting property is good.
For example, the fluidized-bed reactor of preparation grain silicon, which usually has, uses graphite liner, and in graphite liner surface coating silicon carbide coating.
Purification of graphite generallys use high temperature removal of impurities process, including longer heating and temperature-fall period, and not only the period is long, and power consumption is also high.And
Graphite surface after purification is smooth, relatively poor with the silicon carbide layer binding force that then deposits.
Summary of the invention
Goal of the invention: it is an object of the invention to the graphite/carbon SiClx densification for proposing that a kind of new period is short, power consumption is low is multiple
The method of condensation material solves the problems, such as the purity and coating binding force of graphite piece, prevents from introducing impurity to subsequent workshop section.
Technical solution: to realize the above-mentioned technical purpose, graphite/carbon SiClx densification composite wood is prepared the invention proposes a kind of
The method of material, by first making in one layer of silicon-carbide particle layer of graphite piece external coating before the depositing silicon silicon of graphite piece surface
It is realized for transition zone, then CVD deposition coat of silicon carbide.
Preferably, the coating layer thickness of the silicon-carbide particle layer is 30-80 μm, the carbonization in the silicon-carbide particle layer
1-20 μm of the particle size range of silicon particle.
In one embodiment, the silicon-carbide particle layer is by including silicon-carbide particle in graphite piece external coating
Slurry then be dried to obtain, the slurry include silicon-carbide particle, graphite glue, diluent, the silicon-carbide particle: graphite
Glue: mass ratio=3~5 of diluent: 3~5: 1, it is preferable that the silicon-carbide particle: graphite glue: the mass ratio of diluent
=3: 3: 1.It is highly preferred that the graphite glue is phenolic resin and graphite powder mixture, wherein graphite powder accounts for graphite colloids quality
The 3%-25% of content, it is preferable that graphite powder accounts for the 10% of graphite colloids mass content.The ash content of the graphite powder 2ppm with
Under, particle size range be 1-20 μm, the diluent be high-purity alcohol or absolute alcohol.
Wherein, the drying condition is the dry 2h or more at 90 DEG C -200 DEG C.
Preferably, the graphite piece is first cleaned by ultrasonic before brushing one layer of silicon-carbide particle layer.
Wherein, the CVD deposition coat of silicon carbide includes the following steps:
(1) graphite piece for being coated with silicon-carbide particle layer is sent into CVD reactor as substrate, is passed through nitrogen to vacuum degree
130-180mbar, furnace tube are warming up to 500-800 DEG C, start to be passed through hydrogen, keep vacuum degree in furnace to reach 0.9-1.2bar, hold
It is continuous to be warming up to 1200-1600 DEG C;
(2) it maintains temperature at 1200-1600 DEG C, starts to be passed through unstripped gas MTCS (methyl trichlorosilane), hydrogen and argon gas,
It deposits 4-10 hours at this temperature;
(3) stop being passed through unstripped gas MTCS and argon gas after the reaction was completed, and start to cool down, in vacuum degree to 130-
Stop being passed through hydrogen after 180mbar;
(4) after temperature is down to 200 DEG C, stopping is passed through nitrogen, starts to be evacuated to 0.1-1mbar, then inflated with nitrogen is extremely
1bar;
(5) after substrate is completely cooling, substrate is taken out.
The utility model has the advantages that the present invention by one layer of silicon-carbide particle of graphite piece external coating as transition zone, then CVD deposition
Coat of silicon carbide, because silicon-carbide particle transition zone, there are small hole, the silicon carbide deposited on surface penetrates into hole,
So that coating in conjunction with matrix more closely;Meanwhile of the invention method period is short, power consumption is low, effectively solves the pure of graphite piece
Degree and coating binding force problem prevent from introducing impurity to subsequent workshop section.
Detailed description of the invention
Fig. 1 graphite/carbon SiClx densified composite scanning electron microscope schematic diagram prepared by the present invention.
Specific embodiment
The present invention provides a kind of methods for preparing graphite/carbon SiClx densified composite, by heavy on graphite piece surface
Before carbon distribution SiClx, first in one layer of silicon-carbide particle layer of graphite piece external coating as transition zone, then CVD deposition coat of silicon carbide
It realizes.
Below by specific embodiment, the present invention will be described in detail.
Graphite glue used in following embodiments is phenolic resin and graphite powder mixture, wherein graphite powder accounts for graphite glue
The 10% of weight content, the ash content of graphite powder are 1-20 μm in 2ppm or less, particle size range.
Embodiment 1
A kind of preparation method of graphite/carbon SiClx densified composite, includes the following steps:
(1) after ultrasonic clean graphite piece, the slurry made of certain silicon-carbide particle, silicon-carbide particle dynamics range are brushed
1-20 μm, slurry is mixed by silicon-carbide particle, graphite glue, diluent according to mass ratio 3: 3: 1 and is uniformly brushed in graphite
The surface of part is then transferred in drying box at least 90 DEG C dry 2h or more, and fine and close silicon carbide is formed on graphite piece surface
Granulosa.60 μm of coating layer thickness, the graphite piece that surface is coated with silicon-carbide particle layer is obtained, is then sent into CVD as substrate
Reactor depositing silicon silicon coating.
(2) CVD deposition stage process condition:
1) flange in the bottom is fallen, furnace tube is opened, is put into substrate;
2) flange is promoted, furnace tube is closed;
3) displacement, vacuum degree 0.5mbar are vacuumized;
4) evaporator heats, and feeding line preheating starts to be passed through nitrogen to vacuum degree 150mbar;
5) furnace tube is warming up to 600 DEG C, starts to be passed through hydrogen, keeps vacuum degree in furnace to reach 1.0bar, persistently overheating is extremely
1500℃;
6) after maintaining 1500 DEG C of a period of times, start to be passed through unstripped gas (MTCS, hydrogen, argon gas), deposit 6 at this temperature
Hour;
7) stop being passed through unstripped gas (MTCS, argon gas) after the reaction was completed, and start to cool down (about 3 DEG C/min of rate of temperature fall),
Stop being passed through hydrogen after vacuum degree is down to 150mbar, maintains this state for a period of time;
8) after temperature is down to 200 DEG C, stopping is passed through nitrogen, starts to be evacuated to 0.5mbar, then inflated with nitrogen is to 1bar.
9) it after substrate is completely cooling, takes out substrate and carries out packing and selling.
Embodiment 2
A kind of preparation method of graphite/carbon SiClx densified composite, includes the following steps:
(1) after ultrasonic clean graphite piece, the slurry made of certain silicon-carbide particle, silicon-carbide particle dynamics range are brushed
1-20 μm, slurry is mixed by silicon-carbide particle, graphite glue, diluent according to mass ratio 3: 4: 1 and is uniformly brushed in graphite
The surface of part is then transferred in drying box at least 90 DEG C dry 2h or more, and fine and close silicon carbide is formed on graphite piece surface
Granulosa.80 μm of coating layer thickness, the graphite piece that surface is coated with silicon-carbide particle layer is obtained, is then sent into CVD as substrate
Reactor depositing silicon silicon coating.
(2) CVD deposition stage process condition:
1) flange in the bottom is fallen, furnace tube is opened, is put into substrate;
2) flange is promoted, furnace tube is closed;
3) displacement, vacuum degree 1.0mbar are vacuumized;
4) evaporator heats, and feeding line preheating starts to be passed through nitrogen to vacuum degree 180mbar;
5) furnace tube is warming up to 500 DEG C, starts to be passed through hydrogen, keeps vacuum degree in furnace to reach 1.2bar, persistently overheating is extremely
1600℃;
6) after maintaining 1600 DEG C of a period of times, start to be passed through unstripped gas (MTCS, hydrogen, argon gas), deposit 4 at this temperature
Hour;
7) stop being passed through unstripped gas (MTCS, argon gas) after the reaction was completed, and start to cool down (about 2 DEG C/min of rate of temperature fall),
Stop being passed through hydrogen after vacuum degree is down to 130mbar, maintains this state for a period of time;
8) after temperature is down to 200 DEG C, stopping is passed through nitrogen, starts to be evacuated to 0.1mbar, then inflated with nitrogen is to 1bar.
9) it after substrate is completely cooling, takes out substrate and carries out packing and selling.
Embodiment 3
A kind of preparation method of graphite/carbon SiClx densified composite, includes the following steps:
(1) after ultrasonic clean graphite piece, the slurry made of certain silicon-carbide particle, silicon-carbide particle dynamics range are brushed
1-20 μm, slurry is mixed by silicon-carbide particle, graphite glue, diluent according to mass ratio 4: 3: 1 and is uniformly brushed in graphite
The surface of part is then transferred in drying box at least 90 DEG C dry 2h or more, and fine and close silicon carbide is formed on graphite piece surface
Granulosa.30 μm of coating layer thickness, the graphite piece that surface is coated with silicon-carbide particle layer is obtained, is then sent into CVD as substrate
Reactor depositing silicon silicon coating.
(2) CVD deposition stage process condition:
1) flange in the bottom is fallen, furnace tube is opened, is put into substrate;
2) flange is promoted, furnace tube is closed;
3) displacement, vacuum degree 1.0mbar are vacuumized;
4) evaporator heats, and feeding line preheating starts to be passed through nitrogen to vacuum degree 130mbar;
5) furnace tube is warming up to 800 DEG C, starts to be passed through hydrogen, keeps vacuum degree in furnace to reach 1.1bar, persistently overheating is extremely
1200℃;
6) after maintaining 1200 DEG C of a period of times, start to be passed through unstripped gas (MTCS, hydrogen, argon gas), deposit at this temperature
10 hours;
7) stop being passed through unstripped gas (MTCS, argon gas) after the reaction was completed, and start to cool down (about 1 DEG C/min of rate of temperature fall),
Stop being passed through hydrogen after vacuum degree is down to 180mbar, maintains this state for a period of time;
8) after temperature is down to 200 DEG C, stopping is passed through nitrogen, starts to be evacuated to 0.1mbar, then inflated with nitrogen is to 1bar.
9) it after substrate is completely cooling, takes out substrate and carries out packing and selling.
Embodiment 4
A kind of preparation method of graphite/carbon SiClx densified composite, includes the following steps:
(1) after ultrasonic clean graphite piece, the slurry made of certain silicon-carbide particle, silicon-carbide particle dynamics range are brushed
1-20 μm, slurry is mixed by silicon-carbide particle, graphite glue, diluent according to mass ratio 4: 4: 1 and is uniformly brushed in graphite
The surface of part is then transferred in drying box at least 90 DEG C dry 2h or more, and fine and close silicon carbide is formed on graphite piece surface
Granulosa.50 μm of coating layer thickness, the graphite piece that surface is coated with silicon-carbide particle layer is obtained, is then sent into CVD as substrate
Reactor depositing silicon silicon coating.
(2) CVD deposition stage process condition:
1) flange in the bottom is fallen, furnace tube is opened, is put into substrate;
2) flange is promoted, furnace tube is closed;
3) displacement, vacuum degree 0.5mbar are vacuumized;
4) evaporator heats, and feeding line preheating starts to be passed through nitrogen to vacuum degree 160mbar;
5) furnace tube is warming up to 700 DEG C, starts to be passed through hydrogen, keeps vacuum degree in furnace to reach 1.0bar, persistently overheating is extremely
1400℃;
6) after maintaining 1400 DEG C of a period of times, start to be passed through unstripped gas (MTCS, hydrogen, argon gas), deposit 5 at this temperature
Hour;
7) stop being passed through unstripped gas (MTCS, argon gas) after the reaction was completed, and start to cool down (about 3 DEG C/min of rate of temperature fall),
Stop being passed through hydrogen after vacuum degree is down to 150mbar, maintains this state for a period of time;
8) after temperature is down to 200 DEG C, stopping is passed through nitrogen, starts to be evacuated to 0.8mbar, then inflated with nitrogen is to 1bar.
9) it after substrate is completely cooling, takes out substrate and carries out packing and selling.
Fig. 1 shows the graphite/carbon SiClx densified composite scanning electron microscope spectrogram of the method preparation using embodiment 1,
It can be seen that there is the silicon-carbide particle transition zone brushed on graphite matrix, the silicon carbide deposited on surface penetrates into carbon
Hole existing for silicon carbide particle transition zone simultaneously coats silicon-carbide particle so that coating in conjunction with matrix more closely, it is final to prepare
Fine and close coating structure out.In addition, the method for brushing transition zone is more simple, efficiently, so that the coating process period is short, power consumption
It is low, it effectively solves the problems, such as the purity and coating binding force of graphite piece, prevents from introducing impurity to subsequent workshop section.
Claims (4)
1. a kind of method for preparing graphite/carbon SiClx densified composite, which is characterized in that in graphite piece surface depositing silicon silicon
Before, first in one layer of silicon-carbide particle layer of graphite piece external coating as transition zone, then CVD deposition coat of silicon carbide, wherein institute
The coating layer thickness for the silicon-carbide particle layer stated is 30-80 μm, the particle size range of the silicon-carbide particle in the silicon-carbide particle layer
1-20μm;The silicon-carbide particle layer by include in graphite piece external coating silicon-carbide particle slurry it is then dry
It arrives, the slurry includes silicon-carbide particle, graphite glue, diluent, the silicon-carbide particle: graphite glue: the quality of diluent
Than=3 ~ 5:3 ~ 5:1.
2. the method according to claim 1, wherein the drying condition is the dry 2h at 90 DEG C -200 DEG C
More than.
3. the method according to claim 1, wherein the graphite piece brush one layer of silicon-carbide particle layer it
It is preceding to be first cleaned by ultrasonic.
4. the method according to claim 1, wherein the CVD deposition coat of silicon carbide includes the following steps:
(1) graphite piece for being coated with silicon-carbide particle layer is sent into CVD reactor as substrate, is passed through nitrogen to vacuum degree 130-
180mbar, furnace tube are warming up to 500-800 DEG C, start to be passed through hydrogen, and vacuum degree in furnace is kept to reach 0.9-1.2bar, lasting to rise
Temperature is to 1200-1600 DEG C;
(2) maintain temperature at 1200-1600 DEG C, start to be passed through unstripped gas MTCS(methyl trichlorosilane), hydrogen and argon gas, herein
At a temperature of deposit 4-10 hours;
(3) stop being passed through unstripped gas MTCS and argon gas after the reaction was completed, and start to cool down, after vacuum degree to 130-180mbar
Stopping is passed through hydrogen;
(4) after temperature is down to 200 DEG C, stopping is passed through nitrogen, starts to be evacuated to 0.1-1mbar, then inflated with nitrogen is to 1bar;
(5) after substrate is completely cooling, substrate is taken out.
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CN113151800A (en) * | 2021-04-25 | 2021-07-23 | 宜兴市海飞陵电子科技有限公司 | Silicon carbide coating, transition layer thereof and preparation method |
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CN115595659A (en) * | 2022-11-02 | 2023-01-13 | 深圳市志橙半导体材料有限公司(Cn) | Surface coating of graphite matrix, preparation method and application |
CN116590708B (en) * | 2023-07-18 | 2023-10-31 | 湖南泰坦未来科技有限公司 | Graphite material with silicon carbide coating and preparation method and application thereof |
CN117328036B (en) * | 2023-12-01 | 2024-04-05 | 成都超纯应用材料有限责任公司 | Graphite silicon carbide composite material and deposition process of graphite surface silicon carbide |
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