CN109503187A - A kind of precursor dipping/cracking process prepares the preparation process of carbon/carbon compound material PECVD boat - Google Patents

A kind of precursor dipping/cracking process prepares the preparation process of carbon/carbon compound material PECVD boat Download PDF

Info

Publication number
CN109503187A
CN109503187A CN201811527766.XA CN201811527766A CN109503187A CN 109503187 A CN109503187 A CN 109503187A CN 201811527766 A CN201811527766 A CN 201811527766A CN 109503187 A CN109503187 A CN 109503187A
Authority
CN
China
Prior art keywords
carbon
compound material
dipping
sample
carbon compound
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811527766.XA
Other languages
Chinese (zh)
Inventor
吴彪
贾林涛
邵忠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujian Kang Carbon Composite Technology Co Ltd
Shanghai Kang Carbon Composite Mstar Technology Ltd
Original Assignee
Fujian Kang Carbon Composite Technology Co Ltd
Shanghai Kang Carbon Composite Mstar Technology Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fujian Kang Carbon Composite Technology Co Ltd, Shanghai Kang Carbon Composite Mstar Technology Ltd filed Critical Fujian Kang Carbon Composite Technology Co Ltd
Priority to CN201811527766.XA priority Critical patent/CN109503187A/en
Publication of CN109503187A publication Critical patent/CN109503187A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • 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
    • C04B35/56—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 carbides or oxycarbides
    • C04B35/565—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 carbides or oxycarbides based on silicon carbide
    • C04B35/571—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 carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
    • 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
    • C04B35/806—
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite
    • 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
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

The invention proposes a kind of techniques that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat, compared with the bearing frame of conventional graphite material, carbon/carbon compound material mechanical property is better than graphite, and it can adapt to PECVD high temperature, condition of high vacuum degree, the severe film coating environment such as plasma sputtering, and take CVI (chemical vapor deposition) although technique preparation carbon/carbon plate material mechanical property more preferably, service life is longer, but since the complexity of process control procedure causes manufacturing cost higher.Therefore, the present invention prepares carbon/carbon compound material green body and SiC coating using precursor dipping/cracking technology, and the bearing frame of technique preparation significantly reduces the manufacturing cost of bearing frame under the premise of meeting pecvd process.

Description

A kind of precursor dipping/cracking process prepares the preparation of carbon/carbon compound material PECVD boat Technique
Technical field
The present invention relates to a kind of techniques that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat.
Background technique
As sustainable development tourism deepens continuously the popular feeling in countries in the world, solar energy is classified as by many countries to be given priority to New industry.Solar cell module system also receives more and more attention.In monocrystalline/polycrystalline silicon battery production technology It needs in silicon chip surface plated film, this is because when light is radiated at silicon chip surface, reflection can make light loss fail to keep an appointment one third.If Silicon face has one layer of suitable film, using film interference principle, the reflection of light can be made to be greatly reduced, and this film becomes the sun The antireflective coating (ARC, antireflection coating) of energy battery.It is generally used using more silicon nitride film at present Plasma reinforced chemical vapour deposition (PECVD) technique.This technique has depositing temperature low, and speed is fast, and process spread is good, The advantages that coating defects are few.PECVD process is carried out in the vacuum chamber vacuumized, will be as much as possible during PECVD Wafer, which is placed on PECVD boat, carries out coating process.In view of the process environments of PECVD complexity, usually used PECVD boat or boat plate Mainly it is made of graphite.Graphite product has impurity content low, high-purity high corrosion resistant, and thermal conductivity is high, and electric conductivity is moderate, physical chemistry The features such as property is stablized, but lead to graphite boat since the mechanical property of graphite is poor in practical applications in plated film and cleaned It is easily damaged in journey, service life is shorter.Traditional graphite bearing frame (boat) is after being machined out on monolith graphite sheet It is aided with related accessory.Therefore, researcher mainly constantly optimizes graphite bearing frame CONSTRUCTED SPECIFICATION, to wish to improve carrying Ability improves PECVD production efficiency.As utility model patent " a kind of graphite frame for board-like PECVD " (application number: CN201720071874.5), which is changed to 5*11 by graphite grid by original 5*10, makes holding for graphite frame Loading capability increases 10%, and production efficiency also increases 10%, reduces energy consumption and supplies consumption, reduces production cost.It is real With a kind of new patent " graphite frame " (application number: 201320758895.6) equipped with carbon fiber at the both sides of the edge up and down of graphite frame Tie up stiffening plate.The carbon fiber stiffening plate being generally aligned in the same plane with graphite frame ontology, both played a supporting role, while also avoiding existing There is rubescent blushing caused by influence of the graphite fixed plate to plated film airflow homogeneity, ensure that the product of cell piece plated film Matter.
Existing graphite bearing frame is aided with respective accessory after mainly being machined by graphite sheet and is made, and is limited to bearing frame certainly The structure of body designs and the material property of graphite material itself.Graphite bearing frame is limited in the room for promotion of silicon slice loading amount, In addition in severe film coating environment and acid cleaning process, graphite bearing frame is highly prone to destroy, and substantially increases graphite carrying The replacement frequency and pecvd process cost of frame.The carbon/carbon compound material bearing frame of chemical vapor deposition process preparation, although solution The low problem of graphite frame service life of having determined, but its relatively high cost allows many photovoltaic enterprises to hang back.
Summary of the invention
The purpose of the present invention is to propose to the works that a kind of precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat Skill, to solve the above problem of the existing technology.
To achieve the above object, the present invention can be resolved by the following technical programs:
A kind of technique that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat, comprising the following steps:
1) prefabricated body formed, polypropylene cyanogen carbon cloth and laminated cloth are subjected to laying according to mass ratio, Z-direction is then carried out and wears Precast body plate is made in thorn；
2) by the precast body plate graphitization processing；
3) precursor solution is prepared, and phenolic resin, furane resins is mixed according to certain mass ratio, hybrid resin is made Acetone or alcohol solution for standby；
4) it impregnates for the first time, the precursor solution is placed in dipping hot pressing furnace, the precast body plate is embedded in described It in precursor solution, vacuumizes, is kept the temperature after being warming up to specific temperature, apply certain pressure to precast body, certain time takes out Sample；
5) cracking for the first time, by above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, at carbonization Weighing is taken out after reason, measures its bulk density；
6) step 4) and step 5) are repeated until density of material reaches 1.2g/cm3Terminate to impregnate for the first time after above/crack week Phase；
7) siliceous precursor solution is prepared；
8) double-steeping, by above-mentioned steps 6) in sample obtained be impregnated in the siliceous precursor solution of step 7 and carry out Double-steeping；
9) second pyrolysis；By above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, at carbonization Weighing is taken out after reason, measures its bulk density；
10) step 4) and step 5) are repeated until density of material reaches 1.6g/cm3Terminate double-steeping/cracking after above Period；
11) mechanical process sets the resulting carbon/carbon fiber reinforced silicon carbide matrix composite of step 10) according to bearing frame final structure Meter is finely machined.
Due to using the technology described above, a kind of precursor dipping/cracking process of the invention prepares carbon/carbon compound material The technique of PECVD boat, compared with chemical vapor deposition process, the technological forming is fast, and heat treatment temperature is lower, and process costs are low In chemical vapor deposition, PECVD process consumptive material use cost can be greatlyd save, the bearing frame prepared under the process equally has There is the features such as mechanical property is strong, and plasma resistant sputtering is strong, and acid resistance is good.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of bearing frame in the present invention.
Specific embodiment
Illustrate embodiments of the present invention below by way of particular specific embodiment, those skilled in the art can be by this theory The bright revealed content of book is understood other advantages and efficacy of the present invention easily.
Embodiment 1
A kind of technique that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat, comprising the following steps:
1) prefabricated body formed, PAN (polypropylene cyanogen) carbon cloth and laminated cloth are subjected to laying according to mass ratio 1, then carry out Z To puncture, it is made with a thickness of 5mm, a length of 1200mm, width is the precast body plate of 500mm；
2) precast body plate graphitization processing selects the precast body plate of corresponding size to be placed in high temperature according to preparation product specification In 2200 DEG C of DEG C of graphitization processing 2h in furnace；
3) precursor solution is prepared, and phenolic resin is mixed with furane resins according to 0.1 mass ratio, hybrid resin is made 50% acetone soln；
4) it impregnates, the precursor solution that above-mentioned steps 3 prepare is placed in dipping hot pressing furnace, by prefabricated carbon fiber for the first time Body plate is embedded in precursor solution, is evacuated to 1KPa, and with 10 DEG C/h heating rate, after being warming up to 250 DEG C, sample applies pressure 1000 kilograms of power, heat preservation 5h obtains sample；
5) it cracks, the sample that the dipping of above-mentioned steps 4 is completed is placed in carbide furnace under 1200 DEG C of environment, anaerobic ring for the first time Weighing is taken out under border after carbonization treatment 2h, measures its bulk density；
6) step 4 is repeated, step 5 reaches 1.2g/cm until density of material3Terminate dipping/lytic cycle；
7) polycarbosilane precusor solution is prepared, and Polycarbosilane and acetone (analysis is pure) are prepared according to 0.05 mass ratio and gathered Carbon silane precursor solution is spare；
8) sample in above-mentioned steps 6 is impregnated in the polycarbosilane precusor solution of step 7 and carries out two by double-steeping Secondary dipping, impregnating autoclave are evacuated to 1KPa, and with 10 DEG C/h heating rate, after being warming up to 150 DEG C, it is public that sample applies pressure 1000 Jin, after keeping the temperature 3h, sample is taken out in cooling；
9) second pyrolysis；By above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, at carbonization Weighing is taken out after reason, measures its bulk density；
10) step 4) and step 5) are repeated until density of material reaches 1.61g/cm3After terminate double-steeping/cracking week Phase；
11) mechanical process sets the resulting carbon/carbon fiber reinforced silicon carbide matrix composite of step 10) according to bearing frame final structure Meter (such as Fig. 1) is finely machined.
Embodiment 2
A kind of technique that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat, comprising the following steps:
1) prefabricated body formed, PAN (polypropylene cyanogen) carbon cloth and laminated cloth are subjected to laying according to mass ratio 4, then carry out Z To puncture, it is made with a thickness of 30mm, a length of 2000mm, width is the precast body plate of 2000mm；
2) precast body graphitization processing selects the precast body plate of corresponding size to be placed in high temperature furnace according to preparation product specification In in 2600 DEG C of graphitization processing 5h；
3) precursor solution is prepared, and phenolic resin is mixed with furane resins according to 10 mass ratio, hybrid resin is made 55% acetone soln；
4) it impregnates, the precursor solution that above-mentioned steps 3 prepare is placed in dipping hot pressing furnace, by prefabricated carbon fiber for the first time Body plate is embedded in resin, is evacuated to 50KPa, and with 30 DEG C/h heating rate, after being warming up to 400 DEG C, sample applies pressure 5000 Kilogram, heat preservation 50h obtains sample；
5) it cracks, the sample that the dipping of above-mentioned steps 4 is completed is placed in carbide furnace under 1800 DEG C of environment, anaerobic ring for the first time Weighing is taken out under border after carbonization treatment 10h, measures its bulk density；
6) step 4 is repeated, step 5 reaches 1.2g/cm until density of material3After terminate dipping/lytic cycle；
7) trichloromethyl silane precursor solution is prepared, by trichloromethyl silane and acetone (analysis is pure) according to 0.5 mass It is more spare than preparing trichloromethyl silane precursor solution；
8) double-steeping, by the sample in above-mentioned steps 6 be impregnated in the trichloromethyl silane precursor solution of step 7 into Row double-steeping, impregnating autoclave are evacuated to 50KPa, and with 30 DEG C/h heating rate, after being warming up to 400 DEG C, sample applies pressure 10000 kilograms, after keeping the temperature 10h, sample is taken out in cooling；
9) second pyrolysis；By above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, at carbonization Weighing is taken out after reason, measures its bulk density；
10) step 4) and step 5) are repeated until density of material reaches 1.65g/cm3After terminate double-steeping/cracking week Phase；
11) mechanical process sets the resulting carbon/carbon fiber reinforced silicon carbide matrix composite of step 10) according to bearing frame final structure Meter (such as Fig. 1) is finely machined.
Embodiment 3
A kind of technique that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat, comprising the following steps:
1) prefabricated body formed, PAN (polypropylene cyanogen) carbon cloth and laminated cloth are subjected to laying according to mass ratio 3, then carry out Z To puncture, it is made with a thickness of 5mm, a length of 2000mm, width is the precast body plate of 1000mm；
2) precast body plate graphitization processing selects the precast body plate of corresponding size to be placed in high temperature according to preparation product specification In 2300 DEG C of graphitization processing 3h in furnace；
3) precursor solution is prepared, and phenolic resin is mixed with furane resins according to 8 mass ratio, hybrid resin is made 60% acetone soln；
4) it impregnates, the precursor solution that above-mentioned steps 3 prepare is placed in dipping pressure furnace, by prefabricated carbon fiber for the first time Body plate is embedded in resin, is evacuated to 200KPa, and with 15 DEG C/h heating rate, after being warming up to 260 DEG C, sample applies pressure 2000 Kilogram, heat preservation 10h obtains sample；
5) it cracks, the sample that the dipping of above-mentioned steps 4 is completed is placed in carbide furnace under 1500 DEG C of environment, anaerobic ring for the first time Weighing is taken out under border after carbonization treatment 6h, measures its bulk density；
6) step 4 is repeated, step 5 reaches 1.3g/cm until density of material3After terminate dipping/lytic cycle；
7) polycarbosilane precusor solution is prepared, and Polycarbosilane and acetone (analysis is pure) are prepared according to 0.5 mass ratio and gathered Carbon silane precursor solution is spare.
8) sample in above-mentioned steps 6 is impregnated in the polycarbosilane precusor solution of step 7 and carries out two by double-steeping Secondary dipping, impregnating autoclave are evacuated to 20KPa, and with 15 DEG C/h heating rate, after being warming up to 180 DEG C, it is public that sample applies pressure 5000 Jin, after keeping the temperature 5h, sample is taken out in cooling；
9) second pyrolysis；By above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, at carbonization Weighing is taken out after reason, measures its bulk density；
10) step 4) and step 5) are repeated until density of material reaches 1.8g/cm3After terminate double-steeping/lytic cycle；
11) mechanical process sets the resulting carbon/carbon fiber reinforced silicon carbide matrix composite of step 10) according to bearing frame final structure Meter (such as Fig. 1) is finely machined.
Embodiment 4
A kind of technique that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat, comprising the following steps:
1) prefabricated body formed, PAN (polypropylene cyanogen) carbon cloth and laminated cloth are subjected to laying according to mass ratio 2, then carry out Z To puncture, it is made with a thickness of 5mm, a length of 1200mm, width is the precast body plate of 1000mm；
2) precast body plate graphitization processing selects the precast body plate of corresponding size to be placed in high temperature according to preparation product specification In 2500 DEG C of graphitization processing 3h in furnace；
3) precursor solution is prepared, and phenolic resin is mixed with furane resins according to 10 mass ratio, hybrid resin is made Acetone soln；
4) it impregnates, the precursor solution that above-mentioned steps 3 prepare is placed in dipping pressure furnace, by prefabricated carbon fiber for the first time Body plate is embedded in resin, is evacuated to 40KPa, and with 15 DEG C/h heating rate, after being warming up to 300 DEG C, sample applies pressure 2000 Kilogram, heat preservation 30h obtains sample；
5) sample that the dipping of above-mentioned steps 4 is completed is placed in carbide furnace under 1800 DEG C of environment, under vacuum by carbonization cracking Weighing is taken out after carbonization treatment 10h, measures its bulk density；
6) step 4 is repeated, step 5 reaches 1.3g/cm until density of material3After terminate dipping/lytic cycle；
7) trichloromethyl silane precursor solution is prepared, by trichloromethyl silane and acetone (analysis is pure) according to 0.5 mass It is more spare than preparing trichloromethyl silane precursor solution；
8) double-steeping, by the sample in above-mentioned steps 6 be impregnated in the trichloromethyl silane precursor solution of step 7 into Row double-steeping, impregnating autoclave are evacuated to 20KPa, and with 15 DEG C/h heating rate, after being warming up to 160 DEG C, sample applies pressure 3000 kilograms, after keeping the temperature 7h, sample is taken out in cooling；
9) second pyrolysis；By above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, at carbonization Weighing is taken out after reason, measures its bulk density；Step 4) and step 5) are repeated until density of material reaches 1.68g/cm3After terminate Double-steeping/lytic cycle；
10) mechanical process sets the resulting carbon/carbon fiber reinforced silicon carbide matrix composite of step 10) according to bearing frame final structure Meter (such as Fig. 1) is finely machined.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (9)

1. a kind of technique that precursor dipping/cracking process prepares carbon/carbon compound material PECVD boat, which is characterized in that including following Step:
1) prefabricated body formed, polypropylene cyanogen carbon cloth and laminated cloth are subjected to laying according to mass ratio, then carry out Z-direction puncture, system Obtain precast body plate；
2) by the precast body plate graphitization processing；
3) precursor solution is prepared, and phenolic resin, furane resins is mixed according to certain mass ratio, acetone is made in hybrid resin Or ethanol solution is spare；
4) it impregnates for the first time, the precursor solution is placed in dipping hot pressing furnace, the precast body plate is embedded in the pioneer It in liquid solution, vacuumizes, is kept the temperature after being warming up to specific temperature, apply certain pressure to precast body, certain time takes out to obtain sample；
5) cracking for the first time, by above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, after carbonization treatment Weighing is taken out, its bulk density is measured；
6) step 4) and step 5) are repeated until density of material reaches 1.2g/cm3Terminate to impregnate/lytic cycle for the first time after above；
7) siliceous precursor solution is prepared；
8) double-steeping, by above-mentioned steps 6) in sample obtained be impregnated in the siliceous precursor solution of step 7 carry out it is secondary Dipping；
9) second pyrolysis；By above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under oxygen-free environment, after carbonization treatment Weighing is taken out, its bulk density is measured；
10) step 4) and step 5) are repeated until density of material reaches 1.6g/cm3Terminate double-steeping/lytic cycle after above；
11) mechanical process, by the resulting carbon/carbon fiber reinforced silicon carbide matrix composite of step 10) according to bearing frame final structure design into The fine machining of row.
2. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, which is characterized in that the step 1) In, the mass ratio of the polypropylene cyanogen carbon cloth and laminated cloth is 1~4, and precast body plate thickness obtained is 5~30mm, a length of 1200~2000mm, width are 500~2000mm.
3. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, it is characterised in that；The step 2) In, the precast body plate is placed in high temperature furnace in 2200 DEG C~2600 DEG C 2~5h of graphitization processing.
4. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, which is characterized in that the step 3) Described in phenolic resin, furane resins mixed according to 0.1~10 mass ratio, 50% or more acetone or alcohol is made in hybrid resin Solution for standby.
5. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, which is characterized in that the step 4) In, it is evacuated to 1~50KPa, with 10~30 DEG C/h heating rate, after being warming up to 250~400 DEG C, sample applies pressure 1000 ~5000 kilograms, 5~50h of heat preservation obtains sample.
6. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, which is characterized in that the step 5) In, by above-mentioned steps 4) sample completed of dipping is placed in carbide furnace under 1200~1800 DEG C of environment of vacuum environment, at carbonization Weighing is taken out after managing 2~10h, measures its bulk density.
7. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, which is characterized in that the step 7) In, Polycarbosilane or trichloromethyl silane and acetone are prepared into the siliceous precursor solution according to 0.05~0.5 mass ratio.
8. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, which is characterized in that the step 8) In, it is evacuated to 1~50KPa, with 10~30 DEG C/h heating rate, after being warming up to 150~400 DEG C, sample applies pressure 1000 ~10000 kilograms, after keeping the temperature 3~10h, sample is taken out in cooling.
9. the technique according to claim 1 for preparing carbon/carbon compound material PECVD boat, which is characterized in that the step 9) The carbide furnace of middle carbonization is warming up to 1000 DEG C~1300 DEG C with the heating rate of 30~50 DEG C/h, keeps the temperature 2~10h.
CN201811527766.XA 2018-12-13 2018-12-13 A kind of precursor dipping/cracking process prepares the preparation process of carbon/carbon compound material PECVD boat Pending CN109503187A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811527766.XA CN109503187A (en) 2018-12-13 2018-12-13 A kind of precursor dipping/cracking process prepares the preparation process of carbon/carbon compound material PECVD boat

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811527766.XA CN109503187A (en) 2018-12-13 2018-12-13 A kind of precursor dipping/cracking process prepares the preparation process of carbon/carbon compound material PECVD boat

Publications (1)

Publication Number Publication Date
CN109503187A true CN109503187A (en) 2019-03-22

Family

ID=65752401

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811527766.XA Pending CN109503187A (en) 2018-12-13 2018-12-13 A kind of precursor dipping/cracking process prepares the preparation process of carbon/carbon compound material PECVD boat

Country Status (1)

Country Link
CN (1) CN109503187A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1547992A1 (en) * 2003-12-18 2005-06-29 Deutsches Zentrum für Luft- und Raumfahrt e.V. Process for producing a fibre reinforced composite material and the fibre reinforced composite material
CN103553692A (en) * 2013-09-27 2014-02-05 西安超码科技有限公司 Carbon/silicon carbide composite material crucible preparation method
CN104355648A (en) * 2014-10-22 2015-02-18 重庆市旭星化工有限公司 Preparation method of carbon fiber composite
CN105060913A (en) * 2015-08-13 2015-11-18 中国科学院光电技术研究所 Preparation method of C/C-SiC (carbon fiber reinforced carbon-silicon carbide) composite with low CTE (coefficient of thermal expansion)
CN105483621A (en) * 2016-01-28 2016-04-13 福州赛瑞特新材料技术开发有限公司 Combined type graphite electrode-ceramic evaporator boat
CN107790167A (en) * 2017-10-26 2018-03-13 江苏大学 A kind of difunctional classifying porous composite of adsorption photochemical catalysis and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1547992A1 (en) * 2003-12-18 2005-06-29 Deutsches Zentrum für Luft- und Raumfahrt e.V. Process for producing a fibre reinforced composite material and the fibre reinforced composite material
CN103553692A (en) * 2013-09-27 2014-02-05 西安超码科技有限公司 Carbon/silicon carbide composite material crucible preparation method
CN104355648A (en) * 2014-10-22 2015-02-18 重庆市旭星化工有限公司 Preparation method of carbon fiber composite
CN105060913A (en) * 2015-08-13 2015-11-18 中国科学院光电技术研究所 Preparation method of C/C-SiC (carbon fiber reinforced carbon-silicon carbide) composite with low CTE (coefficient of thermal expansion)
CN105483621A (en) * 2016-01-28 2016-04-13 福州赛瑞特新材料技术开发有限公司 Combined type graphite electrode-ceramic evaporator boat
CN107790167A (en) * 2017-10-26 2018-03-13 江苏大学 A kind of difunctional classifying porous composite of adsorption photochemical catalysis and preparation method thereof

Similar Documents

Publication Publication Date Title
WO2022142475A1 (en) N-type high-efficiency solar cell and preparation method for
CN101661971B (en) Method for preparing light absorption layer of CuInSe2 (CIS) based thin film solar cell
CN102299206B (en) Heterojunction solar cell and manufacturing method thereof
CN101866991A (en) Preparation method of amorphous silicon/crystalline silicon heterojunction solar battery
CN101431127B (en) Production method of flexible amorphous silicon thin-film solar cell
CN110534591A (en) A kind of antimony selenide thin-film solar cells and preparation method
CN101789466A (en) Method for manufacturing solar battery
CN110416356A (en) A kind of preparation method of antimony selenide thin-film solar cells
CN112725892A (en) Method for improving bonding quality of silicon carbide seed crystal
CN106904986B (en) Manufacturing method of high-performance composite carbon fiber insulation board
CN112687753B (en) HJT solar cell TCO film, preparation method thereof and cell containing film
CN206685356U (en) A kind of graphite frame for board-like PECVD device
CN109503187A (en) A kind of precursor dipping/cracking process prepares the preparation process of carbon/carbon compound material PECVD boat
CN102254799B (en) Method for preparing AZO antireflective film of solar cell
CN112430116A (en) Preparation method of carbon/carbon composite material PECVD bearing frame
CN102817004B (en) Method for preparing nanometer silicon film through intermediate-frequency magnetron sputtering process, and its special device
CN104201250A (en) All Al-back surface field emitter N-type single crystal cell manufacturing method
CN105977318A (en) Sodium-doped CIGS (copper indium gallium selenide) film based on composite substrate and preparation method thereof
CN206814841U (en) The graphite carrying plate structure of above and below board-like PECVD plated film equipment integratings
CN101710568B (en) Method for inducing crystallization of amorphous silicon thin film by use of nickel acetate solution
CN109437954A (en) A kind of preparation method of carbon/carbon compound material PECVD bearing frame
CN109518149A (en) Along the preparation method of the antimony selenide optoelectronic film of<002>direction preferential growth
CN109385602A (en) A kind of novel uniform surface shape deposition evaporation coating device and method
CN105448707A (en) Method for preparing polycrystalline silicon thin film by using ceramic substrate
CN101295749B (en) Powder metallurgy metallic silicon solar battery underlay producing technique

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190322

WD01 Invention patent application deemed withdrawn after publication