CN105525277A - Silicon carbide ceramic boat for plasma enhanced chemical vapor deposition and preparation method thereof - Google Patents
Silicon carbide ceramic boat for plasma enhanced chemical vapor deposition and preparation method thereof Download PDFInfo
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical 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
- C23C16/458—Chemical 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
- C23C16/4581—Chemical 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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
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Abstract
The invention provides a silicon carbide ceramic boat for plasma enhanced chemical vapor deposition. The silicon carbide ceramic boat comprises a silicon carbide ceramic boat body; the silicon carbide ceramic boat body is integrally molded by an U-shaped base, a first support frame arranged at the left top end of the base and a second support frame arranged at the right top end of the base; a first clamping groove is formed in the top of the first support frame; a second clamping groove is formed in the top of the second support frame; and the side wall of the base, the first support frame and the second support frame are all hollow structures. The invention further provides a method for preparing the silicon carbide ceramic boat for plasma enhanced chemical vapor deposition. The silicon carbide ceramic boat has such performances as low porosity, high strength, light mass, high oxidation resistance and high shock resistance, is not reacted with a silicon chip, and can be widely applied to the field of plasma enhanced chemical vapor deposition film plating.
Description
Technical field
The invention belongs to PECVD device technical field, be specifically related to a kind of plasma enhanced chemical vapor deposition silicon carbide ceramics boat and preparation method thereof.
Background technology
In recent years, along with the adjustment of national energy structure, sun power plays more and more important effect as a kind of clean reproducible energy in national economy, and wherein crystal silicon solar all has significant advantage from efficient energy conversion and output aspect.And as the indispensable link that solar silicon wafers is produced, PECVD (PlasmaEnhancedChemicalVaporDeposition, plasma enhanced chemical vapor deposition) plated film is the important procedure reducing silicon chip surface reflectivity, improve battery efficiency.Its ultimate principle utilizes additional highfield to make source of the gas molecule (NH
3and SiH
4) ionization, form the plasma body containing many high reactivity chemical groups, these plasma activated groups, after series of chemical, will form the Si of one deck suppression sunlight reflection at silicon chip surface
3n
4film, and then the photoelectric transformation efficiency improving cell piece.
At present, in order to improve plated film speed, graphite boat is usually adopted in Tubular PECVD device, to carry out batch deposition as silicon chip carrier.Traditional graphite boat is combined via the ceramic bar running through connection by the graphite flake that multi-disc is arranged vertically.But graphite boat used at present is but faced with the problem in two in PECVD coating process, the first causes the air flow method in PECVD boiler tube uneven due to the iris action of graphite boat, causes the Si deposited
3n
4thicknesses of layers and specific refractory power inequality, form aberration, and then affect Si wafer quality.Two to be graphite flakes with crystal silicon chip contact under the high temperature conditions chemical reaction can occur forms silicon carbide for it, certainly will reduce the quality of silicon chip.Therefore, for addressing these problems, just need a kind ofly do not react with silicon chip and the Novel silicon slice carrier of uniform stream can be ensured.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of plasma enhanced chemical vapor deposition silicon carbide ceramics boat.This silicon carbide ceramics boat has the performances such as porosity is low, high strength, lightweight, high antioxidant, high shock resistance, and it does not react with silicon chip, can be widely used in plasma enhanced chemical vapor deposition plated film field.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of plasma enhanced chemical vapor deposition silicon carbide ceramics boat, it is characterized in that, comprise silicon carbide ceramics boat body, described silicon carbide ceramics boat body is the pedestal of " U " shape by shape, the first bracing frame being arranged on the left top of described pedestal and the second bracing frame being arranged on the right top of described pedestal are made of one piece, the top of described first bracing frame offers multiple the first draw-in groove for plugging silicon chip, the top of described second bracing frame offers multiple the second draw-in groove for plugging silicon chip, described pedestal sidewall, first bracing frame and the second bracing frame are engraved structure.
Above-mentioned plasma enhanced chemical vapor deposition silicon carbide ceramics boat, is characterized in that, the shape of described first bracing frame and the second bracing frame is " L " shape, and described first bracing frame and the second bracing frame are parallel relative laying at the top of pedestal.
Above-mentioned plasma enhanced chemical vapor deposition silicon carbide ceramics boat, is characterized in that, the bottom of described pedestal offers the locating slot for being fixed it.
In addition, present invention also offers a kind of method preparing above-mentioned plasma enhanced chemical vapor deposition silicon carbide ceramics boat, it is characterized in that, the method comprises the following steps:
Step one, carborundum powder and carbon dust to be mixed, obtain basic powder; In described basic powder, the mass percentage of carborundum powder is 70% ~ 90%, and surplus is carbon dust;
Step 2, by basic powder described in paraffin, oleic acid and step one in mass ratio (0.2 ~ 0.35): (0.005 ~ 0.03): 1 mixes, and obtains slurry;
Step 3, Fruit storage is carried out to described slurry, then injection forming is carried out to the slurry after Fruit storage, obtain blank;
Step 4, de-waxing process is carried out to blank described in step 3;
Step 5, the blank after de-waxing process in step 4 is placed in the crucible that silicon grain is housed, then vacuum sintering furnace is put into, be be incubated 20min ~ 60min under the condition of 1550 DEG C ~ 1600 DEG C to carry out siliconising sintering processes in temperature, obtain silicon carbide ceramics boat body; The quality of described silicon grain is 0.8 ~ 1.5 times of the blank quality after de-waxing process;
The method of step 6, employing Linear cut processes the first draw-in groove and the second draw-in groove on the boat of silicon carbide ceramics described in step 5 body, then adopt on the method for chemical vapour deposition silicon carbide ceramics boat body after dicing and prepare SiC coating, finally obtain plasma enhanced chemical vapor deposition silicon carbide ceramics boat.
Above-mentioned method, it is characterized in that, the detailed process of Fruit storage described in step 3 is: described slurry is placed in heating under vacuum reactor, it is 160 DEG C ~ 200 DEG C in temperature, stir speed (S.S.) is 50r/min ~ 400r/min, and vacuum tightness is degassed 20min ~ 60min under the condition of 0.001MPa ~ 0.01MPa.
Above-mentioned method, it is characterized in that, the number of times of the process of de-waxing described in step 4 is twice, the detailed process of twice de-waxing process is: imbed in aluminum oxide powder by described blank, then vacuum drying oven is placed in, 3h ~ 6h is incubated after being first warming up to 50 DEG C ~ 70 DEG C with the temperature rise rate of 2 DEG C/min ~ 5 DEG C/min, 2h ~ 6h is incubated after being warming up to 140 DEG C ~ 160 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min again, then heat up after 180 DEG C ~ 200 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min and be incubated 4h ~ 10h, finally cool to 25 DEG C of room temperatures with the furnace, obtain the blank after de-waxing process.。
Above-mentioned method, is characterized in that, blank described in step 4 is after completing first time de-waxing process, and the ethanolic soln being placed in resol floods 20min ~ 60min, carries out the process of second time de-waxing again after drying; The ethanolic soln of described resol is by resol and dehydrated alcohol in mass ratio (0.8 ~ 1): 1 mixes and forms.
Above-mentioned method, is characterized in that, the median size of silicon grain described in step 5 is 0.5mm ~ 5mm.
Above-mentioned method, is characterized in that, the detailed process of chemical vapour deposition described in step 5 is: the silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, argon gas is as diluent gas, be 200mL/min ~ 400mL/min at hydrogen flowing quantity, argon flow amount is 100mL/min ~ 150mL/min, temperature is deposit 3h ~ 12h under the condition of 1000 DEG C ~ 1200 DEG C, and silicon carbide ceramics boat body after dicing obtains SiC coating.
The present invention compared with prior art has the following advantages:
1, PECVD silicon chip carrier of the present invention is silicon carbide ceramics boat, its there is high temperature resistant, high strength and not with the characteristics such as pasc reaction, be the ideal material as silicon chip carrier;
2, the engraved structure design of silicon carbide ceramics boat of the present invention can mitigation of gases barriering effect, makes it in PECVD tubular type cvd furnace, can effectively ensure being uniformly distributed of air-flow;
3, silicon carbide ceramics boat compact construction of the present invention, can ensure that more silicon chip inserts, significantly improve production efficiency;
4, silicon carbide ceramics boat surface deposition of the present invention has fine and close SiC coating, effectively can avoid gas adsorption, and make PECVD coated film deposition speed fast, coating quality is higher;
5, silicon carbide ceramics boat of the present invention has the performances such as porosity is low, high strength, lightweight, high antioxidant, high shock resistance, and it does not react with silicon chip, can be widely used in plasma enhanced chemical vapor deposition plated film field.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
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 photo of the embodiment of the present invention 2 silicon carbide ceramics boat body.
Fig. 3 is the SEM photo of embodiment of the present invention 2SiC coating.
Description of reference numerals:
1-1-pedestal; 1-2-the first bracing frame; 1-3-the second bracing frame;
1-4-locating slot; 2-1-the first draw-in groove; 2-2-the second draw-in groove.
Embodiment
The present invention relates to a kind of plasma enhanced chemical vapor deposition silicon carbide ceramics boat and preparation method thereof, wherein, the structure of plasma enhanced chemical vapor deposition silicon carbide ceramics boat of the present invention is described by embodiment 1.
Embodiment 1
Composition graphs 1, the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat comprises silicon carbide ceramics boat body, described silicon carbide ceramics boat body is the pedestal 1-1 of " U " shape by shape, the the first bracing frame 1-2 being arranged on the described left top of pedestal 1-1 and the second bracing frame 1-3 being arranged on the described right top of pedestal 1-1 is made of one piece, the top of described first bracing frame 1-2 offers multiple the first draw-in groove 2-1 for plugging silicon chip, the top of described second bracing frame 1-3 offers multiple the second draw-in groove 2-2 for plugging silicon chip, described pedestal 1-1 sidewall, first bracing frame 1-2 and the second bracing frame 1-3 is engraved structure.
As shown in Figure 1, the shape of described first bracing frame 1-2 and the second bracing frame 1-3 is " L " shape, and described first bracing frame 1-2 and the second bracing frame 1-3 are parallel relative laying at the top of pedestal 1-1.
As shown in Figure 1, the bottom of described pedestal 1-1 offers the locating slot 1-4 for being fixed it.
Composition graphs 1, when plasma enhanced chemical vapor deposition silicon carbide ceramics boat of the present invention uses, first multiple silicon chips to be deposited are plugged in the first draw-in groove 2-1 and the second draw-in groove 2-2, then the plasma enhanced chemical vapor deposition silicon carbide ceramics boat being inserted with silicon chip is pushed in plasma enhanced chemical vapor deposition equipment, and adopting locating slot 1-4 to be fixed, opening device carries out PECVD coating film treatment to silicon chip afterwards.
The preparation method of plasma enhanced chemical vapor deposition silicon carbide ceramics boat of the present invention is described by embodiment 2-6.
Embodiment 2
Composition graphs 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat comprises the following steps:
Step one, carborundum powder and carbon dust to be mixed, obtain basic powder; In described basic powder, the mass percentage of carborundum powder is 80%, and surplus is carbon dust;
Step 2, basic powder described in paraffin, oleic acid and step one to be mixed in mass ratio at 0.3: 0.01: 1, obtain slurry;
Step 3, Fruit storage is carried out to described slurry, then injection forming is carried out to the slurry after Fruit storage, obtain blank; The detailed process of described Fruit storage is: described slurry is placed in heating under vacuum reactor, is 180 DEG C in temperature, and stir speed (S.S.) is 200r/min, and vacuum tightness is degassed 30min under the condition of 0.005MPa;
Step 4, de-waxing process is carried out to blank described in step 3; The number of times of described de-waxing process is twice, the detailed process of twice de-waxing process is: imbed in aluminum oxide powder by described blank, then vacuum drying oven is placed in, 4h is incubated after being first warming up to 60 DEG C with the temperature rise rate of 3 DEG C/min, 4h is incubated after being warming up to 150 DEG C with the temperature rise rate of 8 DEG C/min again, then heat up after 190 DEG C with the temperature rise rate of 8 DEG C/min and be incubated 8h, remove aluminum oxide powder after finally cooling to 25 DEG C of room temperatures with the furnace, obtain the blank after de-waxing process; Described blank is after completing first time de-waxing process, and the ethanolic soln being placed in resol floods 40min, carries out the process of second time de-waxing again after drying; The ethanolic soln of described resol in mass ratio by resol and dehydrated alcohol is mixed forms at 0.9: 1;
Step 5, the blank after de-waxing process in step 4 is placed in the crucible that silicon grain is housed, then puts into vacuum sintering furnace, be incubated 40min under the condition of 1580 DEG C to carry out siliconising sintering processes in temperature, obtain silicon carbide ceramics boat body; The quality of described silicon grain is 1.2 times of the blank quality after de-waxing process; The median size of described silicon grain is 3mm;
As shown in Figure 2, described silicon carbide ceramics boat body has low porosity to the SEM photo of silicon carbide ceramics boat body described in the present embodiment as shown in Figure 2, ceramic particle combines closely, imparts the mechanical behavior under high temperature that boat body is good.
The method of step 6, employing Linear cut processes the first draw-in groove 2-1 and the second draw-in groove 2-2 on the boat of silicon carbide ceramics described in step 5 body, then adopt on the method for chemical vapour deposition silicon carbide ceramics boat body after dicing and prepare SiC coating, finally obtain plasma enhanced chemical vapor deposition silicon carbide ceramics boat; The detailed process of described chemical vapour deposition is: the silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 300mL/min at hydrogen flowing quantity, and argon flow amount is 120mL/min, and temperature is deposit 8h under the condition of 1100 DEG C.
As shown in Figure 3, comparatively boat body is more fine and close for described SiC coating as shown in Figure 3, and coating particles is evenly regular, can avoid gas adsorption for the SEM photo of SiC coating described in the present embodiment, improves coating quality.
The performance data of plasma enhanced chemical vapor deposition silicon carbide ceramics boat prepared by the present embodiment is in table 1.
Embodiment 3
Composition graphs 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat comprises the following steps:
Step one, carborundum powder and carbon dust to be mixed, obtain basic powder; In described basic powder, the mass percentage of carborundum powder is 90%, and surplus is carbon dust;
Step 2, basic powder described in paraffin, oleic acid and step one to be mixed in mass ratio at 0.3: 0.01: 1, obtain slurry;
Step 3, Fruit storage is carried out to described slurry, then injection forming is carried out to the slurry after Fruit storage, obtain blank; The detailed process of described Fruit storage is: described slurry is placed in heating under vacuum reactor, is 200 DEG C in temperature, and stir speed (S.S.) is 400r/min, and vacuum tightness is degassed 60min under the condition of 0.01MPa;
Step 4, de-waxing process is carried out to blank described in step 3; The number of times of described de-waxing process is twice, the detailed process of twice de-waxing process is: imbed in aluminum oxide powder by described blank, then vacuum drying oven is placed in, 3h is incubated after being first warming up to 50 DEG C with the temperature rise rate of 5 DEG C/min, 6h is incubated after being warming up to 160 DEG C with the temperature rise rate of 10 DEG C/min again, then heat up after 180 DEG C with the temperature rise rate of 5 DEG C/min and be incubated 10h, remove aluminum oxide powder after finally cooling to 25 DEG C of room temperatures with the furnace, obtain the blank after de-waxing process; Described blank is after completing first time de-waxing process, and the ethanolic soln being placed in resol floods 20min, carries out the process of second time de-waxing again after drying; The ethanolic soln of described resol in mass ratio by resol and dehydrated alcohol is mixed forms at 1: 1;
Step 5, the blank after de-waxing process in step 4 is placed in the crucible that silicon grain is housed, then puts into vacuum sintering furnace, be incubated 30min under the condition of 1550 DEG C to carry out siliconising sintering processes in temperature, obtain silicon carbide ceramics boat body; The quality of described silicon grain is 1.5 times of the blank quality after de-waxing process; The median size of described silicon grain is 5mm;
The method of step 6, employing Linear cut processes the first draw-in groove 2-1 and the second draw-in groove 2-2 on the boat of silicon carbide ceramics described in step 5 body, then adopt on the method for chemical vapour deposition silicon carbide ceramics boat body after dicing and prepare SiC coating, finally obtain plasma enhanced chemical vapor deposition silicon carbide ceramics boat; The detailed process of described chemical vapour deposition is: the silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 400mL/min at hydrogen flowing quantity, and argon flow amount is 150mL/min, and temperature is deposit 3h under the condition of 1200 DEG C.
The performance data of plasma enhanced chemical vapor deposition silicon carbide ceramics boat prepared by the present embodiment is in table 1.
Embodiment 4
Composition graphs 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat comprises the following steps:
Step one, carborundum powder and carbon dust to be mixed, obtain basic powder; In described basic powder, the mass percentage of carborundum powder is 70%, and surplus is carbon dust;
Step 2, basic powder described in paraffin, oleic acid and step one to be mixed in mass ratio at 0.2: 0.005: 1, obtain slurry;
Step 3, Fruit storage is carried out to described slurry, then injection forming is carried out to the slurry after Fruit storage, obtain blank; The detailed process of described Fruit storage is: described slurry is placed in heating under vacuum reactor, is 160 DEG C in temperature, and stir speed (S.S.) is 50r/min, and vacuum tightness is degassed 60min under the condition of 0.001MPa;
Step 4, de-waxing process is carried out to blank described in step 3; The number of times of described de-waxing process is twice, the detailed process of twice de-waxing process is: imbed in aluminum oxide powder by described blank, then vacuum drying oven is placed in, 3h is incubated after being first warming up to 50 DEG C with the temperature rise rate of 2 DEG C/min, 6h is incubated after being warming up to 140 DEG C with the temperature rise rate of 5 DEG C/min again, then heat up after 180 DEG C with the temperature rise rate of 5 DEG C/min and be incubated 10h, remove aluminum oxide powder after finally cooling to 25 DEG C of room temperatures with the furnace, obtain the blank after de-waxing process; Described blank is after completing first time de-waxing process, and the ethanolic soln being placed in resol floods 20min, carries out the process of second time de-waxing again after drying; The ethanolic soln of described resol in mass ratio by resol and dehydrated alcohol is mixed forms at 0.8: 1;
Step 5, the blank after de-waxing process in step 4 is placed in the crucible that silicon grain is housed, then puts into vacuum sintering furnace, be incubated 60min under the condition of 1600 DEG C to carry out siliconising sintering processes in temperature, obtain silicon carbide ceramics boat body; The quality of described silicon grain is 0.8 times of the blank quality after de-waxing process; The median size of described silicon grain is 0.5mm;
The method of step 6, employing Linear cut processes the first draw-in groove 2-1 and the second draw-in groove 2-2 on the boat of silicon carbide ceramics described in step 5 body, then adopt on the method for chemical vapour deposition silicon carbide ceramics boat body after dicing and prepare SiC coating, finally obtain plasma enhanced chemical vapor deposition silicon carbide ceramics boat; The detailed process of described chemical vapour deposition is: the silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 200mL/min at hydrogen flowing quantity, and argon flow amount is 100mL/min, and temperature is deposit 12h under the condition of 1000 DEG C.
The performance data of plasma enhanced chemical vapor deposition silicon carbide ceramics boat prepared by the present embodiment is in table 1.
Embodiment 5
Composition graphs 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat comprises the following steps:
Step one, carborundum powder and carbon dust to be mixed, obtain basic powder; In described basic powder, the mass percentage of carborundum powder is 90%, and surplus is carbon dust;
Step 2, basic powder described in paraffin, oleic acid and step one to be mixed in mass ratio at 0.35: 0.03: 1, obtain slurry;
Step 3, Fruit storage is carried out to described slurry, then injection forming is carried out to the slurry after Fruit storage, obtain blank; The detailed process of described Fruit storage is: described slurry is placed in heating under vacuum reactor, is 200 DEG C in temperature, and stir speed (S.S.) is 400r/min, and vacuum tightness is degassed 20min under the condition of 0.01MPa;
Step 4, de-waxing process is carried out to blank described in step 3; The number of times of described de-waxing process is twice, the detailed process of twice de-waxing process is: imbed in aluminum oxide powder by described blank, then vacuum drying oven is placed in, 6h is incubated after being first warming up to 50 DEG C with the temperature rise rate of 2 DEG C/min, 2h is incubated after being warming up to 140 DEG C with the temperature rise rate of 5 DEG C/min again, then heat up after 180 DEG C with the temperature rise rate of 5 DEG C/min and be incubated 4h, remove aluminum oxide powder after finally cooling to 25 DEG C of room temperatures with the furnace, obtain the blank after de-waxing process; Described blank is after completing first time de-waxing process, and the ethanolic soln being placed in resol floods 20min, carries out the process of second time de-waxing again after drying; The ethanolic soln of described resol in mass ratio by resol and dehydrated alcohol is mixed forms at 0.9: 1;
Step 5, the blank after de-waxing process in step 4 is placed in the crucible that silicon grain is housed, then puts into vacuum sintering furnace, be incubated 20min under the condition of 1550 DEG C to carry out siliconising sintering processes in temperature, obtain silicon carbide ceramics boat body; The quality of described silicon grain is 0.8 times of the blank quality after de-waxing process; The median size of described silicon grain is 5mm;
The method of step 6, employing Linear cut processes the first draw-in groove 2-1 and the second draw-in groove 2-2 on the boat of silicon carbide ceramics described in step 5 body, then adopt on the method for chemical vapour deposition silicon carbide ceramics boat body after dicing and prepare SiC coating, finally obtain plasma enhanced chemical vapor deposition silicon carbide ceramics boat; The detailed process of described chemical vapour deposition is: the silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 200mL/min at hydrogen flowing quantity, and argon flow amount is 150mL/min, and temperature is deposit 3h under the condition of 1000 DEG C.
The performance data of plasma enhanced chemical vapor deposition silicon carbide ceramics boat prepared by the present embodiment is in table 1.
Embodiment 6
Composition graphs 1, the preparation method of the present embodiment plasma enhanced chemical vapor deposition silicon carbide ceramics boat comprises the following steps:
Step one, carborundum powder and carbon dust to be mixed, obtain basic powder; In described basic powder, the mass percentage of carborundum powder is 90%, and surplus is carbon dust;
Step 2, basic powder described in paraffin, oleic acid and step one to be mixed in mass ratio at 0.2: 0.03: 1, obtain slurry;
Step 3, Fruit storage is carried out to described slurry, then injection forming is carried out to the slurry after Fruit storage, obtain blank; The detailed process of described Fruit storage is: described slurry is placed in heating under vacuum reactor, is 200 DEG C in temperature, and stir speed (S.S.) is 50r/min, and vacuum tightness is degassed 20min under the condition of 0.001MPa;
Step 4, de-waxing process is carried out to blank described in step 3; The number of times of described de-waxing process is twice, the detailed process of twice de-waxing process is: imbed in aluminum oxide powder by described blank, then vacuum drying oven is placed in, 3h is incubated after being first warming up to 50 DEG C with the temperature rise rate of 5 DEG C/min, 2h is incubated after being warming up to 140 DEG C with the temperature rise rate of 5 DEG C/min again, then heat up after 200 DEG C with the temperature rise rate of 10 DEG C/min and be incubated 10h, remove aluminum oxide powder after finally cooling to 25 DEG C of room temperatures with the furnace, obtain the blank after de-waxing process; Described blank is after completing first time de-waxing process, and the ethanolic soln being placed in resol floods 20min, carries out the process of second time de-waxing again after drying; The ethanolic soln of described resol in mass ratio by resol and dehydrated alcohol is mixed forms at 0.9: 1;
Step 5, the blank after de-waxing process in step 4 is placed in the crucible that silicon grain is housed, then puts into vacuum sintering furnace, be incubated 20min under the condition of 1550 DEG C to carry out siliconising sintering processes in temperature, obtain silicon carbide ceramics boat body; The quality of described silicon grain is 1.5 times of the blank quality after de-waxing process; The median size of described silicon grain is 5mm;
The method of step 6, employing Linear cut processes the first draw-in groove 2-1 and the second draw-in groove 2-2 on the boat of silicon carbide ceramics described in step 5 body, then adopt on the method for chemical vapour deposition silicon carbide ceramics boat body after dicing and prepare SiC coating, finally obtain plasma enhanced chemical vapor deposition silicon carbide ceramics boat; The detailed process of described chemical vapour deposition is: the silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, and argon gas, as diluent gas, is 400mL/min at hydrogen flowing quantity, and argon flow amount is 150mL/min, and temperature is deposit 12h under the condition of 1200 DEG C.
The performance data of plasma enhanced chemical vapor deposition silicon carbide ceramics boat prepared by the present embodiment is in table 1.
Table 1 plasma enhanced chemical vapor deposition silicon carbide ceramics of the present invention boat performance data
As shown in Table 1, the silicon carbide ceramics boat body that prepared by the present invention has the performances such as porosity is low, high strength, lightweight, high antioxidant, high shock resistance; And material itself does not react with silicon chip, plasma enhanced chemical vapor deposition plated film field can be widely used in.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (9)
1. a plasma enhanced chemical vapor deposition silicon carbide ceramics boat, it is characterized in that, comprise silicon carbide ceramics boat body, described silicon carbide ceramics boat body is the pedestal (1-1) of " U " shape by shape, the first bracing frame (1-2) being arranged on described pedestal (1-1) left top and the second bracing frame (1-3) being arranged on described pedestal (1-1) right top are made of one piece, the top of described first bracing frame (1-2) offers multiple the first draw-in groove (2-1) for plugging silicon chip, the top of described second bracing frame (1-3) offers multiple the second draw-in groove (2-2) for plugging silicon chip, described pedestal (1-1) sidewall, first bracing frame (1-2) and the second bracing frame (1-3) are engraved structure.
2. plasma enhanced chemical vapor deposition silicon carbide ceramics boat according to claim 1, it is characterized in that, the shape of described first bracing frame (1-2) and the second bracing frame (1-3) is " L " shape, and described first bracing frame (1-2) and the second bracing frame (1-3) are parallel relative laying at the top of pedestal (1-1).
3. plasma enhanced chemical vapor deposition silicon carbide ceramics boat according to claim 1, is characterized in that, the bottom of described pedestal (1-1) offers the locating slot (1-4) for being fixed it.
4. prepare a method for plasma enhanced chemical vapor deposition silicon carbide ceramics boat as claimed in claim 1, it is characterized in that, the method comprises the following steps:
Step one, carborundum powder and carbon dust to be mixed, obtain basic powder; In described basic powder, the mass percentage of carborundum powder is 70% ~ 90%, and surplus is carbon dust;
Step 2, by basic powder described in paraffin, oleic acid and step one in mass ratio (0.2 ~ 0.35): (0.005 ~ 0.03): 1 mixes, and obtains slurry;
Step 3, Fruit storage is carried out to slurry described in step 2, then injection forming is carried out to the slurry after Fruit storage, obtain blank;
Step 4, de-waxing process is carried out to blank described in step 3;
Step 5, the blank after de-waxing process in step 4 is placed in the crucible that silicon grain is housed, then vacuum sintering furnace is put into, be be incubated 20min ~ 60min under the condition of 1550 DEG C ~ 1600 DEG C to carry out siliconising sintering processes in temperature, obtain silicon carbide ceramics boat body; The quality of described silicon grain is 0.8 ~ 1.5 times of the blank quality after de-waxing process;
The method of step 6, employing Linear cut processes the first draw-in groove (2-1) and the second draw-in groove (2-2) on the boat of silicon carbide ceramics described in step 5 body, then adopt on the method for chemical vapour deposition silicon carbide ceramics boat body after dicing and prepare SiC coating, finally obtain plasma enhanced chemical vapor deposition silicon carbide ceramics boat.
5. method according to claim 4, it is characterized in that, the detailed process of Fruit storage described in step 3 is: described slurry is placed in heating under vacuum reactor, it is 160 DEG C ~ 200 DEG C in temperature, stir speed (S.S.) is 50r/min ~ 400r/min, and vacuum tightness is degassed 20min ~ 60min under the condition of 0.001MPa ~ 0.01MPa.
6. method according to claim 4, it is characterized in that, the number of times of the process of de-waxing described in step 4 is twice, the detailed process of twice de-waxing process is: imbed in aluminum oxide powder by described blank, then vacuum drying oven is placed in, 3h ~ 6h is incubated after being first warming up to 50 DEG C ~ 70 DEG C with the temperature rise rate of 2 DEG C/min ~ 5 DEG C/min, 2h ~ 6h is incubated after being warming up to 140 DEG C ~ 160 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min again, then heat up after 180 DEG C ~ 200 DEG C with the temperature rise rate of 5 DEG C/min ~ 10 DEG C/min and be incubated 4h ~ 10h, finally cool to 25 DEG C of room temperatures with the furnace, obtain the blank after de-waxing process.
7. method according to claim 6, is characterized in that, blank described in step 4 is after completing first time de-waxing process, and the ethanolic soln being placed in resol floods 20min ~ 60min, carries out the process of second time de-waxing again after drying; The ethanolic soln of described resol is by resol and dehydrated alcohol in mass ratio (0.8 ~ 1): 1 mixes and forms.
8. method according to claim 4, is characterized in that, the median size of silicon grain described in step 5 is 0.5mm ~ 5mm.
9. method according to claim 4, is characterized in that, the detailed process of chemical vapour deposition described in step 5 is: the silicon carbide ceramics boat body after cutting is placed in chemical vapor deposition stove, adopts CH
3siCl
3as raw material, hydrogen is as carrier gas, argon gas is as diluent gas, be 200mL/min ~ 400mL/min at hydrogen flowing quantity, argon flow amount is 100mL/min ~ 150mL/min, temperature is deposit 3h ~ 12h under the condition of 1000 DEG C ~ 1200 DEG C, and silicon carbide ceramics boat body after dicing obtains SiC coating.
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| CN111892419A (en) * | 2020-08-03 | 2020-11-06 | 福赛特(唐山)新材料有限公司 | High-shock-resistance silicon carbide boat and preparation method thereof |
| CN114395797A (en) * | 2021-11-26 | 2022-04-26 | 华灿光电(苏州）有限公司 | Growth method and growth equipment of high-resistance silicon epitaxial wafer |
| CN114409407A (en) * | 2022-02-15 | 2022-04-29 | 陕西固勤材料技术有限公司 | Method for purifying and improving silicon carbide content of semiconductor cantilever paddle product |
| CN116393845A (en) * | 2023-06-08 | 2023-07-07 | 山东华美新材料科技股份有限公司 | Silicon carbide ceramic wafer boat cutting equipment |
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| CN202322983U (en) * | 2011-11-10 | 2012-07-11 | 山东鹏程特种陶瓷有限公司 | U-shaped conductive ceramic evaporation boat |
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| CN111892419A (en) * | 2020-08-03 | 2020-11-06 | 福赛特(唐山)新材料有限公司 | High-shock-resistance silicon carbide boat and preparation method thereof |
| CN114395797A (en) * | 2021-11-26 | 2022-04-26 | 华灿光电(苏州）有限公司 | Growth method and growth equipment of high-resistance silicon epitaxial wafer |
| CN114409407A (en) * | 2022-02-15 | 2022-04-29 | 陕西固勤材料技术有限公司 | Method for purifying and improving silicon carbide content of semiconductor cantilever paddle product |
| CN116393845A (en) * | 2023-06-08 | 2023-07-07 | 山东华美新材料科技股份有限公司 | Silicon carbide ceramic wafer boat cutting equipment |
| CN116393845B (en) * | 2023-06-08 | 2023-08-15 | 山东华美新材料科技股份有限公司 | Silicon carbide ceramic wafer boat cutting equipment |
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