CN105525277B - Plasma enhanced chemical vapor deposition silicon carbide ceramics boat and preparation method thereof - Google Patents

Plasma enhanced chemical vapor deposition silicon carbide ceramics boat and preparation method thereof Download PDF

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CN105525277B
CN105525277B CN201510975417.4A CN201510975417A CN105525277B CN 105525277 B CN105525277 B CN 105525277B CN 201510975417 A CN201510975417 A CN 201510975417A CN 105525277 B CN105525277 B CN 105525277B
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silicon carbide
carbide ceramics
vapor deposition
chemical vapor
support frame
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CN105525277A (en
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杨万利
代丽娜
康文杰
张永辉
张旭辉
彭志刚
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Chaoma Science & Technology Co Ltd Xian
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Chaoma Science & Technology Co Ltd Xian
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4581Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber characterised by material of construction or surface finish of the means for supporting the substrate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • C04B35/65Reaction sintering of free metal- or free silicon-containing compositions
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32Carbides
    • C23C16/325Silicon carbide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422Carbon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes

Abstract

The invention provides a kind of plasma enhanced chemical vapor deposition silicon carbide ceramics boat, including silicon carbide ceramics boat body, the silicon carbide ceramics boat body is made of one piece by the second support frame for being shaped as the pedestal of " u "-shaped, being arranged on first support frame on the left top of the pedestal and being arranged on the right top of the pedestal, the first neck is offered at the top of first support frame, the second neck is offered at the top of second support frame, the pedestal side wall, the first support frame and the second support frame are engraved structure.Present invention also offers a kind of method for preparing above-mentioned plasma enhanced chemical vapor deposition silicon carbide ceramics boat.Silicon carbide ceramics boat of the present invention has the performances such as low porosity, high intensity, lightweight, high antioxidant, high shock resistance, and it does not react with silicon chip, can be widely used for plasma enhanced chemical vapor deposition plated film field.

Description

Plasma enhanced chemical vapor deposition silicon carbide ceramics boat and preparation method thereof
Technical field
The invention belongs to PECVD device technical field, and in particular to a kind of plasma enhanced chemical vapor deposition carbon SiClx ceramic boat and preparation method thereof.
Background technology
In recent years, with the adjustment of national energy structure, solar energy is as a kind of clean reproducible energy in national economy In play more and more important effect, wherein crystal silicon solar all has aobvious in terms of efficient energy conversion and yield The advantage of work.And as the indispensable link of solar silicon wafers production, PECVD (Plasma Enhanced Chemical Vapor Deposition, plasma enhanced chemical vapor deposition) plated film is to reduce silicon chip surface reflectivity, improve the weight of battery efficiency Want process.Its general principle is to make source of the gas molecule (NH using additional highfield3And SiH4) ionization, formed and contain many high activities The plasma of chemical group, these plasma activated groups will be formed after series of chemical in silicon chip surface One layer of Si for suppressing sunshine reflection3N4Film, and then improve the photoelectric transformation efficiency of cell piece.
At present, in order to improve plated film speed, generally use graphite boat is carried out as silicon chip carrier in Tubular PECVD device Batch deposition.Traditional graphite boat is to be combined by the graphite flake of multi-disc vertical arrangement via the ceramic bar through connection.So And presently used graphite boat is but faced with both sides problem in PECVD coating process, one is the resistance due to graphite boat Cause the air flow method in PECVD boiler tubes uneven every effect, cause the Si of deposition3N4Thicknesses of layers and refractive index are uneven, are formed Aberration, and then influence Si wafer quality.The second is graphite flake contacts under the high temperature conditions with crystal silicon chip can occur the shape that chemically reacts Into carborundum, the quality of silicon chip certainly will be reduced.Therefore, to solve these problems, it is necessary to a kind of not reacted with silicon chip and Ensure the uniform novel silicon slice carrier of air-flow.
The content of the invention
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of plasma increases Silicon carbide ceramics boat is used in extensive chemical vapour deposition.The silicon carbide ceramics boat have low porosity, high intensity, lightweight, high antioxidant, The performances such as high shock resistance, and it does not react with silicon chip, can be widely used for plasma enhanced chemical vapor deposition plated film field.
In order to solve the above technical problems, the technical solution adopted by the present invention is:A kind of PECVD sinks Product uses silicon carbide ceramics boat, it is characterised in that including silicon carbide ceramics boat body, the silicon carbide ceramics boat body is by being shaped as " U " The pedestal of shape, the first support frame for being arranged on the left top of the pedestal and the second support frame one for being arranged on the right top of the pedestal It is body formed to form, multiple the first necks for being used to plug silicon chip, second support are offered at the top of first support frame Multiple the second necks for being used to plug silicon chip, the pedestal side wall, the first support frame and the second support frame are offered at the top of frame It is engraved structure.
Above-mentioned plasma enhanced chemical vapor deposition silicon carbide ceramics boat, it is characterised in that first support The shape of frame and the second support frame is " L " shape, and first support frame and the second support frame are in parallel phase at the top of pedestal To laying.
Above-mentioned plasma enhanced chemical vapor deposition silicon carbide ceramics boat, it is characterised in that the bottom of the pedestal Portion offers the locating slot for it to be fixed.
In addition, present invention also offers one kind to prepare above-mentioned plasma enhanced chemical vapor deposition silicon carbide ceramics boat Method, it is characterised in that this method comprises the following steps:
Step 1: carborundum powder and carbon dust are well mixed, basic powder is obtained;Carborundum powder in the basic powder Weight/mass percentage composition is 70%~90%, and surplus is carbon dust;
Step 2: by basic powder described in paraffin, oleic acid and step 1 (0.2~0.35) in mass ratio: (0.005~ 0.03): 1 is well mixed, obtains slurry;
Step 3: carrying out Fruit storage to the slurry, slip casting then is carried out to the slurry after Fruit storage Shaping, obtains blank;
Step 4: de-waxing processing is carried out to blank described in step 3;
Step 5: the blank after de-waxing processing in step 4 is placed in the crucible equipped with silicon grain, vacuum is then placed in 20min~60min is incubated in sintering furnace, under conditions of being 1550 DEG C~1600 DEG C in temperature and carries out siliconising sintering processes, is obtained Silicon carbide ceramics boat body;The quality of the silicon grain is 0.8~1.5 times of the blank quality after de-waxing processing;
Step 6: process the first neck and on silicon carbide ceramics boat body described in step 5 using the method for wire cutting Two draw-in groove, then using preparing SiC coatings on the method silicon carbide ceramics boat body after dicing of chemical vapor deposition, final To plasma enhanced chemical vapor deposition silicon carbide ceramics boat.
Above-mentioned method, it is characterised in that the detailed process of Fruit storage described in step 3 is:By the slurry It is placed in heating in vacuum reactor, is 160 DEG C~200 DEG C in temperature, stir speed (S.S.) is 50r/min~400r/min, vacuum For the 20min~60min that deaerated under conditions of 0.001MPa~0.01MPa.
Above-mentioned method, it is characterised in that de-waxing number of processing described in step 4 is twice, de-waxing is handled twice Detailed process is:By the blank be embedded to alumina powder in, be subsequently placed in vacuum drying chamber, first with 2 DEG C/min~5 DEG C/ Min heating rate is incubated 3h~6h after being warming up to 50 DEG C~70 DEG C, then is heated up with 5 DEG C/min~10 DEG C/min heating rate 2h~6h is incubated after to 140 DEG C~160 DEG C, is then heated up 180 DEG C~200 DEG C with 5 DEG C/min~10 DEG C/min heating rate 4h~10h is incubated afterwards, finally cools to 25 DEG C of room temperatures with the furnace, obtains the blank after de-waxing processing..
Above-mentioned method, it is characterised in that blank described in step 4 is placed in phenol after the processing of first time de-waxing is completed 20min~60min is impregnated in the ethanol solution of urea formaldehyde, second of de-waxing processing is carried out again after drying;The phenolic resin Ethanol solution is by phenolic resin and absolute ethyl alcohol (0.8~1) in mass ratio: 1 well mixed forms.
Above-mentioned method, it is characterised in that the average grain diameter of silicon grain described in step 5 is 0.5mm~5mm.
Above-mentioned method, it is characterised in that the detailed process of chemical vapor deposition described in step 5 is:After cutting Silicon carbide ceramics boat body is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen is as carrier gas, argon gas conduct Diluent gas, it is 200mL/min~400mL/min in hydrogen flowing quantity, argon flow amount is 100mL/min~150mL/min, temperature To deposit 3h~12h under conditions of 1000 DEG C~1200 DEG C, SiC coatings are obtained on silicon carbide ceramics boat body after dicing.
The present invention has advantages below compared with prior art:
1st, PECVD silicon chips carrier of the present invention is silicon carbide ceramics boat, and it has high temperature resistant, high intensity and not anti-with silicon Characteristic should be waited, is the ideal material as silicon chip carrier;
2nd, the engraved structure design of silicon carbide ceramics boat of the present invention can be such that it is managed in PECVD with mitigation of gases barriering effect In formula cvd furnace, being uniformly distributed for air-flow can effectively ensure that;
3rd, silicon carbide ceramics boat of the present invention is compact-sized, can ensure more silicon chip insertions, significantly improve production efficiency;
4th, silicon carbide ceramics boat surface deposition of the present invention has fine and close SiC coatings, can effectively avoid gas absorption so that PECVD coated film deposition speed is fast, and coating quality is higher;
5th, silicon carbide ceramics boat of the present invention has the performances such as low porosity, high intensity, lightweight, high antioxidant, high shock resistance, And it does not react with silicon chip, can be widely used for plasma enhanced chemical vapor deposition plated film field.
The present invention is described in further detail with reference to the accompanying drawings and examples.
Brief description of the drawings
Fig. 1 is the structural representation of plasma enhanced chemical vapor deposition silicon carbide ceramics boat of the present invention.
Fig. 2 is the SEM photograph of the silicon carbide ceramics boat body of the embodiment of the present invention 2.
Fig. 3 is the SEM photograph of 2SiC coatings of the embodiment of the present invention.
Description of reference numerals:
1-1-pedestal;The support frames of 1-2-first;The support frames of 1-3-second;
1-4-locating slot;The necks of 2-1-first;The necks of 2-2-second.
Embodiment
The present invention relates to a kind of plasma enhanced chemical vapor deposition silicon carbide ceramics boat and preparation method thereof, its In, the structure of plasma enhanced chemical vapor deposition silicon carbide ceramics boat of the present invention is described by embodiment 1.
Embodiment 1
With reference to Fig. 1, the present embodiment plasma enhanced chemical vapor deposition includes silicon carbide ceramics with silicon carbide ceramics boat Boat body, the silicon carbide ceramics boat body is by be shaped as the pedestal 1-1 of " u "-shaped, be arranged on the left tops of pedestal 1-1 first Support 1-2 is made of one piece with the second support frame 1-3 for being arranged on the right tops of pedestal 1-1, the first support frame 1-2 Top offer and multiple be used to plug and offer multiple use at the top of the first neck 2-1, the second support frame 1-3 of silicon chip In the second neck 2-2 for plugging silicon chip, the pedestal 1-1 side walls, the first support frame 1-2 and the second support frame 1-3 are hollow out Structure.
As shown in figure 1, the first support frame 1-2 and the second support frame 1-3 shape are " L " shape, described first Support 1-2 and the second support frame 1-3 is at pedestal 1-1 top in parallel relative laying.
As shown in figure 1, the bottom of the pedestal 1-1 offers the locating slot 1-4 for it to be fixed.
With reference to Fig. 1, plasma enhanced chemical vapor deposition silicon carbide ceramics boat of the present invention will be in use, will wait to sink first Long-pending multiple silicon chips are plugged in the first neck 2-1 and the second neck 2-2, then will be inserted with the plasma enhancing of silicon chip Vapour deposition is learned to be pushed into plasma enhanced chemical vapor deposition equipment with silicon carbide ceramics boat, and will using locating slot 1-4 It is fixed, and is opened equipment afterwards and is carried out PECVD coating film treatments to silicon chip.
The preparation method of plasma enhanced chemical vapor deposition silicon carbide ceramics boat of the present invention is entered by embodiment 2-6 Row description.
Embodiment 2
With reference to Fig. 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat includes Following steps:
Step 1: carborundum powder and carbon dust are well mixed, basic powder is obtained;Carborundum powder in the basic powder Weight/mass percentage composition is 80%, and surplus is carbon dust;
Step 2: basic powder in mass ratio 0.3: 0.01: 1 described in paraffin, oleic acid and step 1 is well mixed, obtain To slurry;
Step 3: carrying out Fruit storage to the slurry, slip casting then is carried out to the slurry after Fruit storage Shaping, obtains blank;The detailed process of the Fruit storage is:The slurry is placed in heating in vacuum reactor, Temperature is 180 DEG C, stir speed (S.S.) 200r/min, and vacuum is the 30min that deaerated under conditions of 0.005MPa;
Step 4: de-waxing processing is carried out to blank described in step 3;The de-waxing number of processing is twice, to arrange twice The detailed process of Lasaxing Oilfield is:By the blank be embedded to alumina powder in, be subsequently placed in vacuum drying chamber, first with 3 DEG C/ Min heating rate is incubated 4h after being warming up to 60 DEG C, then is warming up to 8 DEG C/min heating rate after 150 DEG C and is incubated 4h, then To be incubated 8h after 8 DEG C/min 190 DEG C of heating rate heating, alumina powder is removed after finally cooling to 25 DEG C of room temperatures with the furnace, is obtained Blank to after de-waxing processing;The blank is placed in the ethanol solution of phenolic resin after the processing of first time de-waxing is completed 40min is impregnated, second of de-waxing processing is carried out again after drying;The ethanol solution of the phenolic resin is by phenolic resin and anhydrous second Alcohol in mass ratio 0.9: 1 is well mixed to be formed;
Step 5: the blank after de-waxing processing in step 4 is placed in the crucible equipped with silicon grain, vacuum is then placed in 40min is incubated in sintering furnace, under conditions of being 1580 DEG C in temperature and carries out siliconising sintering processes, obtains silicon carbide ceramics boat body; The quality of the silicon grain is 1.2 times of the blank quality after de-waxing processing;The average grain diameter of the silicon grain is 3mm;
The SEM photograph of silicon carbide ceramics boat body described in the present embodiment is as shown in Fig. 2 the silicon carbide ceramics as shown in Figure 2 There is boat body low porosity, ceramic particle to be tightly combined, and impart the good mechanical behavior under high temperature of boat body.
Step 6: the first neck 2-1 is processed described in step 5 using the method for wire cutting on silicon carbide ceramics boat body With the second neck 2-2, then applied using preparing SiC on the method silicon carbide ceramics boat body after dicing of chemical vapor deposition Layer, finally gives plasma enhanced chemical vapor deposition silicon carbide ceramics boat;The detailed process of the chemical vapor deposition For:Silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen conduct Carrier gas, argon gas are 300mL/min in hydrogen flowing quantity, argon flow amount 120mL/min, temperature is 1100 DEG C as diluent gas Under conditions of deposit 8h.
The SEM photographs of SiC coatings described in the present embodiment is as shown in figure 3, the SiC coatings are compared with boat body more as shown in Figure 3 Densification, coating granule is uniformly regular, can avoid gas absorption, improves coating quality.
Plasma enhanced chemical vapor deposition manufactured in the present embodiment is shown in Table 1 with the performance data of silicon carbide ceramics boat.
Embodiment 3
With reference to Fig. 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat includes Following steps:
Step 1: carborundum powder and carbon dust are well mixed, basic powder is obtained;Carborundum powder in the basic powder Weight/mass percentage composition is 90%, and surplus is carbon dust;
Step 2: basic powder in mass ratio 0.3: 0.01: 1 described in paraffin, oleic acid and step 1 is well mixed, obtain To slurry;
Step 3: carrying out Fruit storage to the slurry, slip casting then is carried out to the slurry after Fruit storage Shaping, obtains blank;The detailed process of the Fruit storage is:The slurry is placed in heating in vacuum reactor, Temperature is 200 DEG C, stir speed (S.S.) 400r/min, and vacuum is the 60min that deaerated under conditions of 0.01MPa;
Step 4: de-waxing processing is carried out to blank described in step 3;The de-waxing number of processing is twice, to arrange twice The detailed process of Lasaxing Oilfield is:By the blank be embedded to alumina powder in, be subsequently placed in vacuum drying chamber, first with 5 DEG C/ Min heating rate is incubated 3h after being warming up to 50 DEG C, then is warming up to 10 DEG C/min heating rate after 160 DEG C and is incubated 6h, so Heated up afterwards with 5 DEG C/min heating rate and be incubated 10h after 180 DEG C, alumina powder is removed after finally cooling to 25 DEG C of room temperatures with the furnace, Obtain the blank after de-waxing processing;The blank is placed in the ethanol solution of phenolic resin after the processing of first time de-waxing is completed Middle dipping 20min, second of de-waxing processing is carried out again after drying;The ethanol solution of the phenolic resin is by phenolic resin and anhydrous Ethanol in mass ratio 1: 1 is well mixed to be formed;
Step 5: the blank after de-waxing processing in step 4 is placed in the crucible equipped with silicon grain, vacuum is then placed in 30min is incubated in sintering furnace, under conditions of being 1550 DEG C in temperature and carries out siliconising sintering processes, obtains silicon carbide ceramics boat body; The quality of the silicon grain is 1.5 times of the blank quality after de-waxing processing;The average grain diameter of the silicon grain is 5mm;
Step 6: the first neck 2-1 is processed described in step 5 using the method for wire cutting on silicon carbide ceramics boat body With the second neck 2-2, then applied using preparing SiC on the method silicon carbide ceramics boat body after dicing of chemical vapor deposition Layer, finally gives plasma enhanced chemical vapor deposition silicon carbide ceramics boat;The detailed process of the chemical vapor deposition For:Silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen conduct Carrier gas, argon gas are 400mL/min in hydrogen flowing quantity, argon flow amount 150mL/min, temperature is 1200 DEG C as diluent gas Under conditions of deposit 3h.
Plasma enhanced chemical vapor deposition manufactured in the present embodiment is shown in Table 1 with the performance data of silicon carbide ceramics boat.
Embodiment 4
With reference to Fig. 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat includes Following steps:
Step 1: carborundum powder and carbon dust are well mixed, basic powder is obtained;Carborundum powder in the basic powder Weight/mass percentage composition is 70%, and surplus is carbon dust;
Step 2: basic powder in mass ratio 0.2: 0.005: 1 described in paraffin, oleic acid and step 1 is well mixed, Obtain slurry;
Step 3: carrying out Fruit storage to the slurry, slip casting then is carried out to the slurry after Fruit storage Shaping, obtains blank;The detailed process of the Fruit storage is:The slurry is placed in heating in vacuum reactor, Temperature is 160 DEG C, stir speed (S.S.) 50r/min, and vacuum is the 60min that deaerated under conditions of 0.001MPa;
Step 4: de-waxing processing is carried out to blank described in step 3;The de-waxing number of processing is twice, to arrange twice The detailed process of Lasaxing Oilfield is:By the blank be embedded to alumina powder in, be subsequently placed in vacuum drying chamber, first with 2 DEG C/ Min heating rate is incubated 3h after being warming up to 50 DEG C, then is warming up to 5 DEG C/min heating rate after 140 DEG C and is incubated 6h, then To be incubated 10h after 5 DEG C/min 180 DEG C of heating rate heating, alumina powder is removed after finally cooling to 25 DEG C of room temperatures with the furnace, is obtained Blank to after de-waxing processing;The blank is placed in the ethanol solution of phenolic resin after the processing of first time de-waxing is completed 20min is impregnated, second of de-waxing processing is carried out again after drying;The ethanol solution of the phenolic resin is by phenolic resin and anhydrous second Alcohol in mass ratio 0.8: 1 is well mixed to be formed;
Step 5: the blank after de-waxing processing in step 4 is placed in the crucible equipped with silicon grain, vacuum is then placed in 60min is incubated in sintering furnace, under conditions of being 1600 DEG C in temperature and carries out siliconising sintering processes, obtains silicon carbide ceramics boat body; The quality of the silicon grain is 0.8 times of the blank quality after de-waxing processing;The average grain diameter of the silicon grain is 0.5mm;
Step 6: the first neck 2-1 is processed described in step 5 using the method for wire cutting on silicon carbide ceramics boat body With the second neck 2-2, then applied using preparing SiC on the method silicon carbide ceramics boat body after dicing of chemical vapor deposition Layer, finally gives plasma enhanced chemical vapor deposition silicon carbide ceramics boat;The detailed process of the chemical vapor deposition For:Silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen conduct Carrier gas, argon gas are 200mL/min in hydrogen flowing quantity, argon flow amount 100mL/min, temperature is 1000 DEG C as diluent gas Under conditions of deposit 12h.
Plasma enhanced chemical vapor deposition manufactured in the present embodiment is shown in Table 1 with the performance data of silicon carbide ceramics boat.
Embodiment 5
With reference to Fig. 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat includes Following steps:
Step 1: carborundum powder and carbon dust are well mixed, basic powder is obtained;Carborundum powder in the basic powder Weight/mass percentage composition is 90%, and surplus is carbon dust;
Step 2: basic powder in mass ratio 0.35: 0.03: 1 described in paraffin, oleic acid and step 1 is well mixed, Obtain slurry;
Step 3: carrying out Fruit storage to the slurry, slip casting then is carried out to the slurry after Fruit storage Shaping, obtains blank;The detailed process of the Fruit storage is:The slurry is placed in heating in vacuum reactor, Temperature is 200 DEG C, stir speed (S.S.) 400r/min, and vacuum is the 20min that deaerated under conditions of 0.01MPa;
Step 4: de-waxing processing is carried out to blank described in step 3;The de-waxing number of processing is twice, to arrange twice The detailed process of Lasaxing Oilfield is:By the blank be embedded to alumina powder in, be subsequently placed in vacuum drying chamber, first with 2 DEG C/ Min heating rate is incubated 6h after being warming up to 50 DEG C, then is warming up to 5 DEG C/min heating rate after 140 DEG C and is incubated 2h, then To be incubated 4h after 5 DEG C/min 180 DEG C of heating rate heating, alumina powder is removed after finally cooling to 25 DEG C of room temperatures with the furnace, is obtained Blank to after de-waxing processing;The blank is placed in the ethanol solution of phenolic resin after the processing of first time de-waxing is completed 20min is impregnated, second of de-waxing processing is carried out again after drying;The ethanol solution of the phenolic resin is by phenolic resin and anhydrous second Alcohol in mass ratio 0.9: 1 is well mixed to be formed;
Step 5: the blank after de-waxing processing in step 4 is placed in the crucible equipped with silicon grain, vacuum is then placed in 20min is incubated in sintering furnace, under conditions of being 1550 DEG C in temperature and carries out siliconising sintering processes, obtains silicon carbide ceramics boat body; The quality of the silicon grain is 0.8 times of the blank quality after de-waxing processing;The average grain diameter of the silicon grain is 5mm;
Step 6: the first neck 2-1 is processed described in step 5 using the method for wire cutting on silicon carbide ceramics boat body With the second neck 2-2, then applied using preparing SiC on the method silicon carbide ceramics boat body after dicing of chemical vapor deposition Layer, finally gives plasma enhanced chemical vapor deposition silicon carbide ceramics boat;The detailed process of the chemical vapor deposition For:Silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen conduct Carrier gas, argon gas are 200mL/min in hydrogen flowing quantity, argon flow amount 150mL/min, temperature is 1000 DEG C as diluent gas Under conditions of deposit 3h.
Plasma enhanced chemical vapor deposition manufactured in the present embodiment is shown in Table 1 with the performance data of silicon carbide ceramics boat.
Embodiment 6
With reference to Fig. 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat includes Following steps:
Step 1: carborundum powder and carbon dust are well mixed, basic powder is obtained;Carborundum powder in the basic powder Weight/mass percentage composition is 90%, and surplus is carbon dust;
Step 2: basic powder in mass ratio 0.2: 0.03: 1 described in paraffin, oleic acid and step 1 is well mixed, obtain To slurry;
Step 3: carrying out Fruit storage to the slurry, slip casting then is carried out to the slurry after Fruit storage Shaping, obtains blank;The detailed process of the Fruit storage is:The slurry is placed in heating in vacuum reactor, Temperature is 200 DEG C, stir speed (S.S.) 50r/min, and vacuum is the 20min that deaerated under conditions of 0.001MPa;
Step 4: de-waxing processing is carried out to blank described in step 3;The de-waxing number of processing is twice, to arrange twice The detailed process of Lasaxing Oilfield is:By the blank be embedded to alumina powder in, be subsequently placed in vacuum drying chamber, first with 5 DEG C/ Min heating rate is incubated 3h after being warming up to 50 DEG C, then is warming up to 5 DEG C/min heating rate after 140 DEG C and is incubated 2h, then To be incubated 10h after 10 DEG C/min 200 DEG C of heating rate heating, alumina powder is removed after finally cooling to 25 DEG C of room temperatures with the furnace, Obtain the blank after de-waxing processing;The blank is placed in the ethanol solution of phenolic resin after the processing of first time de-waxing is completed Middle dipping 20min, second of de-waxing processing is carried out again after drying;The ethanol solution of the phenolic resin is by phenolic resin and anhydrous Ethanol in mass ratio 0.9: 1 is well mixed to be formed;
Step 5: the blank after de-waxing processing in step 4 is placed in the crucible equipped with silicon grain, vacuum is then placed in 20min is incubated in sintering furnace, under conditions of being 1550 DEG C in temperature and carries out siliconising sintering processes, obtains silicon carbide ceramics boat body; The quality of the silicon grain is 1.5 times of the blank quality after de-waxing processing;The average grain diameter of the silicon grain is 5mm;
Step 6: the first neck 2-1 is processed described in step 5 using the method for wire cutting on silicon carbide ceramics boat body With the second neck 2-2, then applied using preparing SiC on the method silicon carbide ceramics boat body after dicing of chemical vapor deposition Layer, finally gives plasma enhanced chemical vapor deposition silicon carbide ceramics boat;The detailed process of the chemical vapor deposition For:Silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen conduct Carrier gas, argon gas are 400mL/min in hydrogen flowing quantity, argon flow amount 150mL/min, temperature is 1200 DEG C as diluent gas Under conditions of deposit 12h.
Plasma enhanced chemical vapor deposition manufactured in the present embodiment is shown in Table 1 with the performance data of silicon carbide ceramics boat.
Table 1 plasma enhanced chemical vapor deposition of the present invention silicon carbide ceramics boat performance data
As shown in Table 1, the silicon carbide ceramics boat body that prepared by the present invention has low porosity, high intensity, lightweight, high antioxygen The performances such as property, high shock resistance;And material does not react with silicon chip in itself, can be widely used for plasma enhanced chemical vapor deposition Plated film field.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to invention skill Any simple modification, change and equivalence change that art is substantially made to above example, still fall within technical solution of the present invention Protection domain in.

Claims (9)

1. a kind of plasma enhanced chemical vapor deposition silicon carbide ceramics boat, it is characterised in that including silicon carbide ceramics boat Body, the silicon carbide ceramics boat body is by being shaped as the pedestal (1-1) of " u "-shaped, being arranged on the first of the pedestal (1-1) left top Support frame (1-2) and it is arranged on second support frame (1-3) on the pedestal (1-1) right top and is made of one piece, described first Multiple the first necks (2-1) for being used to plug silicon chip are offered at the top of support frame (1-2), second support frame (1-3) Top offer it is multiple be used to plugging the second necks (2-2) of silicon chip, pedestal (1-1) side wall, the first support frame (1-2) and Second support frame (1-3) is engraved structure.
2. plasma enhanced chemical vapor deposition according to claim 1 silicon carbide ceramics boat, it is characterised in that institute The shape for stating the first support frame (1-2) and the second support frame (1-3) is " L " shape, first support frame (1-2) and second Support (1-3) is at the top of pedestal (1-1) in parallel relative laying.
3. plasma enhanced chemical vapor deposition according to claim 1 silicon carbide ceramics boat, it is characterised in that institute The bottom for stating pedestal (1-1) offers locating slot (1-4) for it to be fixed.
4. a kind of method for preparing plasma enhanced chemical vapor deposition silicon carbide ceramics boat as claimed in claim 1, its It is characterised by, this method comprises the following steps:
Step 1: carborundum powder and carbon dust are well mixed, basic powder is obtained;The quality of carborundum powder in the basic powder Percentage composition is 70%~90%, and surplus is carbon dust;
Step 2: by basic powder described in paraffin, oleic acid and step 1 (0.2~0.35) in mass ratio: (0.005~0.03) : 1 is well mixed, obtains slurry;
Step 3: carrying out Fruit storage to slurry described in step 2, then the slurry after Fruit storage is carried out Injection forming, obtain blank;
Step 4: de-waxing processing is carried out to blank described in step 3;
Step 5: the blank after de-waxing processing in step 4 is placed in the crucible equipped with silicon grain, vacuum-sintering is then placed in 20min~60min is incubated in stove, under conditions of being 1550 DEG C~1600 DEG C in temperature and carries out siliconising sintering processes, is carbonized Silicon ceramic boat body;The quality of the silicon grain is 0.8~1.5 times of the blank quality after de-waxing processing;
Step 6: processed using the method for wire cutting on silicon carbide ceramics boat body described in step 5 the first neck (2-1) and Second neck (2-2), then applied using preparing SiC on the method silicon carbide ceramics boat body after dicing of chemical vapor deposition Layer, finally gives plasma enhanced chemical vapor deposition silicon carbide ceramics boat.
5. according to the method for claim 4, it is characterised in that the detailed process of Fruit storage described in step 3 For:The slurry is placed in heating in vacuum reactor, temperature be 160 DEG C~200 DEG C, stir speed (S.S.) be 50r/min~ 400r/min, degassing 20min~60min under conditions of vacuum is 0.001MPa~0.01MPa.
6. according to the method for claim 4, it is characterised in that de-waxing number of processing described in step 4 is twice two The detailed process of secondary de-waxing processing is:The blank is embedded in alumina powder, is subsequently placed in vacuum drying chamber, first with 2 DEG C/min~5 DEG C/min heating rate is incubated 3h~6h after being warming up to 50 DEG C~70 DEG C, then with 5 DEG C/min~10 DEG C/min's Heating rate is incubated 2h~6h after being warming up to 140 DEG C~160 DEG C, is then heated up with 5 DEG C/min~10 DEG C/min heating rate 4h~10h is incubated after 180 DEG C~200 DEG C, finally cools to 25 DEG C with the furnace, obtains the blank after de-waxing processing.
7. according to the method for claim 6, it is characterised in that blank described in step 4 completes the processing of first time de-waxing Afterwards, dipping 20min~60min in the ethanol solution of phenolic resin is placed in, second of de-waxing processing is carried out again after drying;It is described The ethanol solution of phenolic resin is by phenolic resin and absolute ethyl alcohol (0.8~1) in mass ratio: 1 well mixed forms.
8. according to the method for claim 4, it is characterised in that the average grain diameter of silicon grain described in step 5 is 0.5mm ~5mm.
9. according to the method for claim 4, it is characterised in that the detailed process of chemical vapor deposition described in step 5 For:Silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, using CH3SiCl3As raw material, hydrogen conduct Carrier gas, argon gas are 200mL/min~400mL/min in hydrogen flowing quantity as diluent gas, argon flow amount be 100mL/min~ 150mL/min, temperature deposits 3h~12h under conditions of being 1000 DEG C~1200 DEG C, on silicon carbide ceramics boat body after dicing Obtain SiC coatings.
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