CN103553711A - Composite coating carbon/carbon composite material crucible and preparation method thereof - Google Patents
Composite coating carbon/carbon composite material crucible and preparation method thereof Download PDFInfo
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- CN103553711A CN103553711A CN201310455254.8A CN201310455254A CN103553711A CN 103553711 A CN103553711 A CN 103553711A CN 201310455254 A CN201310455254 A CN 201310455254A CN 103553711 A CN103553711 A CN 103553711A
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Abstract
The invention discloses a composite coating carbon/carbon composite material crucible comprising a carbon/carbon composite material crucible, a silicon carbide coating adhered on the inner surface of the carbon/carbon composite material crucible, a silicon coating adhered on the silicon carbide coating, and a silicon nitride coating adhered on the silicon coating. Also, the invention discloses a preparation method of the composite coating carbon/carbon composite material crucible. According to the invention, silicon nitride is combined with the silicon carbide composite coating, such that corrosion of silicon-containing steam upon the inner profile of the carbon/carbon composite material crucible can be effectively inhibited, and crucible service life is greatly improved. With a chemical vapor reaction method, SiC coating in-situ production is achieved. Compared with a traditional SiC coating prepared with a CVD method, the bonding strength with the carbon/carbon substrate is higher. Also, excessive Si coating is produced on site, such that Si source is provided for the production of the silicon nitride coating. The silicon nitride coating produced with high-purity nitrogen has improved bonding strength, such that corrosion resistance of the crucible is further improved.
Description
Technical field
The invention belongs to high temperature furnace used thermal field component technical field, be specifically related to a kind of compound coating carbon/carbon composite material crucible and preparation method thereof.
Background technology
At present, monocrystalline silicon draw machines generally adopts Carbon Materials crucible (plumbago crucible or carbon/carbon composite material crucible) with crucible, and in pulling single crystal silicon process, (main component is SiO for silicon vapor and silicon-containing gas (SiO) and quartz crucible
2) all can with Carbon Materials generation chemical reaction, cause Carbon Materials crucible to be etched, until lost efficacy, therefore, the erosion that how effectively to suppress Carbon Materials is to improve the key technical problem of Carbon Materials pot life for monocrystalline silicon draw machines.
Utilize the charcoal of silicon carbide replacement matrix of carbon/carbon composite materials, can effectively improve the resistance to fouling of carbon/carbon composite; Patent 201110395843.2 adopts the mode of Polycarbosilane cracking to obtain silicon carbide substrate and prepare carbon silicon carbide crucible; Patent 201210230689.8 adopts chemical vapor infiltration method obtain silicon carbide substrate and prepare carbon/carbon/composite material of silicon carbide crucible.But silicon carbide in use still with silicon-containing gas and SiO
2there is chemical reaction, cause crucible to be etched.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and a kind of compound coating carbon/carbon composite material crucible is provided.This carbon/carbon composite material crucible utilizes silicon nitride combined silicon carbide compound coating, can effectively suppress, containing the erosion of silicon vapor to profile in carbon/carbon composite material crucible, to have increased substantially the work-ing life of crucible.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of compound coating carbon/carbon composite material crucible, it is characterized in that, comprise carbon/carbon composite material crucible, be attached to the coat of silicon carbide of carbon/carbon composite material crucible internal surface, be attached to the silicon coating on coat of silicon carbide and be attached to the silicon nitride coating on silicon coating.
Above-mentioned a kind of compound coating carbon/carbon composite material crucible, the thickness of described coat of silicon carbide is 100 μ m～300 μ m, and the thickness of described silicon coating is 10 μ m～20 μ m, and the thickness of described silicon nitride coating is 50 μ m～100 μ m.
In addition, the present invention also provides a kind of method of preparing above-mentioned compound coating carbon/carbon composite material crucible, it is characterized in that, the method comprises the following steps:
Step 1, by density, be 0.20g/cm
3～0.50g/cm
3charcoal fiber preform density to density be 1.30g/cm
3～1.65g/cm
3;
Step 2, the charcoal fiber preform after density in step 1 is carried out to mechanical workout, obtain carbon/carbon composite material crucible;
Step 3, carbon/carbon composite material crucible described in step 2 is placed in to graphitizing furnace, take HIGH-PURITY SILICON as raw material, adopt chemical vapor infiltration technique to generate coat of silicon carbide and silicon coating at carbon/carbon composite material crucible internal surface reaction in－situ; The quality purity of described HIGH-PURITY SILICON is more than 99.0%; The temperature of reaction of described chemical vapor infiltration technique is 1550 ℃～1950 ℃, and soaking time is 0.5h～6h;
Step 4, in graphitizing furnace described in step 3, pass into nitrogen, at carbon/carbon composite material crucible internal surface reaction in－situ, generate silicon nitride coating, furnace cooling, obtains compound coating carbon/carbon composite material crucible; The temperature of reaction of described in-situ chemical reaction is 900 ℃～1400 ℃, and soaking time is 0.5h～24h.
Above-mentioned method, the method for density described in step 1 is:
101, charcoal fiber preform is placed in to chemical vapor deposition stove, adopts carbon-source gas to carry out chemical vapor infiltration 1～2 time;
102, the charcoal fiber preform after chemical vapor infiltration in 101 is placed in to dipping stove and carries out acetone-furfural resin and/or resol pressure impregnation, be then placed in charring furnace charing;
103, repeat 102 until the density of charcoal fiber preform reaches 1.30g/cm
3～1.65g/cm
3.
Above-mentioned method, carbon-source gas described in 101 is propylene and/or Sweet natural gas, and carbon-source gas flow is 20L/min～100L/min, and the temperature of chemical vapor infiltration is 900 ℃～1100 ℃, and soaking time is 30h～60h.
Above-mentioned method, the pressure of pressure impregnation described in 102 is 1.0MPa～2.5MPa, the dwell time is 0.5h～5h.
Above-mentioned method, the temperature of charing described in 102 is 900 ℃～1000 ℃, soaking time is 2h～5h.
Above-mentioned method, the number of times repeating described in 103 is 1～3 time.
Above-mentioned method, the temperature of reaction of the technique of chemical vapor infiltration described in step 3 is 1750 ℃, soaking time is 3h.
The present invention compared with prior art has the following advantages:
1, the present invention utilizes silicon nitride combined silicon carbide compound coating, can effectively suppress, containing the erosion of silicon vapor to profile in carbon/carbon composite material crucible, to have increased substantially the work-ing life of crucible.
2, the present invention adopts chemical gas-phase reaction method original position to generate SiC coating, the relative standby SiC coating of traditional C VD legal system, higher with charcoal/carbon matrix bonding strength, original position generates the generation that excessive Si coating is silicon nitride coating simultaneously provides Si source, utilize the generated in-situ silicon nitride coating bonding strength of high pure nitrogen to improve, further improved the corrosion resistance of crucible.On the other hand, the generated in-situ SiC coating of chemical gas-phase reaction method in conjunction with the standby SiC coating of the relative CVD legal system of silicon nitride coating in conjunction with silicon nitride coating, owing to there is no corrosive gases source (as ammonia, trichloromethyl silane, hydrogen etc.), processing safety further improves, and has reduced production cost simultaneously.
3, single heat loss of compound coating carbon/carbon composite material crucible of the present invention is 0.04mm, and can reach 180 heats work-ing life.
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment
Embodiment 1
Step 1, according to crucible shape to be prepared and performance requriements, adopt ordinary method to utilize charcoal fiber, charcoal cloth and net tire to make density for 0.20g/cm
3charcoal fiber preform, by described charcoal fiber preform density to density, be then 1.30g/cm
3; The method of described density is:
101, charcoal fiber preform is placed in to chemical vapor deposition stove, adopt propylene (also can adopt the gas mixture of Sweet natural gas or propylene and Sweet natural gas) to carry out chemical vapor infiltration 2 times as carbon-source gas, the processing parameter of 2 chemical vapor infiltrations is: carbon-source gas flow is 20L/min, the temperature of chemical vapor infiltration is 900 ℃, and soaking time is 30h;
102, the charcoal fiber preform after 2 chemical vapor infiltrations in 101 is placed in to dipping stove and carries out acetone-furfural resin pressure impregnation (also can adopt resol pressure impregnation, or acetone-furfural resin and resol pressure impregnation), be then placed in charring furnace charing; The pressure of described pressure impregnation is 1.0MPa, and the dwell time is 0.5h; The temperature of described charing is 900 ℃, and soaking time is 2h;
103, repeat 102 once, obtaining density is 1.30g/cm
3charcoal fiber preform;
Step 2, to density described in 103, be 1.30g/cm
3charcoal fiber preform carry out mechanical workout, obtain carbon/carbon composite material crucible;
Step 3, carbon/carbon composite material crucible described in step 2 is placed in to graphitizing furnace, take HIGH-PURITY SILICON as raw material, adopt chemical vapor infiltration technique to generate coat of silicon carbide and silicon coating at carbon/carbon composite material crucible internal surface reaction in－situ; The quality purity of described HIGH-PURITY SILICON is 99.0%; The temperature of reaction of described chemical vapor infiltration technique is 1550 ℃, and soaking time is 0.5h;
Step 4, in graphitizing furnace described in step 3, pass into nitrogen, at carbon/carbon composite material crucible internal surface reaction in－situ, generate silicon nitride coating, furnace cooling, obtains compound coating carbon/carbon composite material crucible; The temperature of reaction of described in-situ chemical reaction is 900 ℃, and soaking time is 0.5h.
After testing, compound coating carbon/carbon composite material crucible prepared by the present embodiment, comprise carbon/carbon composite material crucible, the thickness that is attached to carbon/carbon composite material crucible internal surface is the coat of silicon carbide of 100 μ m, is attached to thickness on coat of silicon carbide and is the silicon coating of 10 μ m and the thickness that is attached on silicon coating is the silicon nitride coating of 50 μ m.
The present embodiment adopts chemical gas-phase reaction method original position to generate SiC coating, the relative standby SiC coating of traditional C VD legal system, higher with charcoal/carbon matrix bonding strength, original position generates the generation that excessive Si coating is silicon nitride coating simultaneously provides Si source, utilize the generated in-situ silicon nitride coating bonding strength of high pure nitrogen to improve, further improved the corrosion resistance of crucible; On the other hand, owing to there is no corrosive gases source (as ammonia, trichloromethyl silane, hydrogen etc.), processing safety further improves, and has reduced production cost simultaneously; The compound coating carbon/carbon composite material crucible of preparation utilizes silicon nitride combined silicon carbide compound coating, can effectively suppress, containing the erosion of silicon vapor to profile in carbon/carbon composite material crucible, to have increased substantially the work-ing life of crucible.
Embodiment 2
Step 1, according to crucible shape to be prepared and performance requriements, adopt ordinary method to utilize charcoal fiber, charcoal cloth and net tire to make density for 0.30g/cm
3charcoal fiber preform, by described charcoal fiber preform density to density, be then 1.45g/cm
3; The method of described density is:
101, charcoal fiber preform is placed in to chemical vapor deposition stove, adopt Sweet natural gas (also can adopt the gas mixture of propylene or propylene and Sweet natural gas) to carry out chemical vapor infiltration 1 time as carbon-source gas, the processing parameter of chemical vapor infiltration is: carbon-source gas flow is 60L/min, the temperature of chemical vapor infiltration is 1000 ℃, and soaking time is 40h;
102, the charcoal fiber preform after 2 chemical vapor infiltrations in 101 is placed in to dipping stove and carries out resol pressure impregnation (also can adopt acetone-furfural resin pressure impregnation, or acetone-furfural resin and resol pressure impregnation), be then placed in charring furnace charing; The pressure of described pressure impregnation is 1.5MPa, and the dwell time is 2.5h; The temperature of described charing is 950 ℃, and soaking time is 3h;
103, repeat, obtaining density is 1.45g/cm 102 twice
3charcoal fiber preform;
Step 2, to density described in 103, be 1.45g/cm
3charcoal fiber preform carry out mechanical workout, obtain carbon/carbon composite material crucible;
Step 3, carbon/carbon composite material crucible described in step 2 is placed in to graphitizing furnace, take HIGH-PURITY SILICON as raw material, adopt chemical vapor infiltration technique to generate coat of silicon carbide and silicon coating at carbon/carbon composite material crucible internal surface reaction in－situ; The quality purity of described HIGH-PURITY SILICON is 99.99%; The temperature of reaction of described chemical vapor infiltration technique is 1750 ℃, and soaking time is 3h;
Step 4, in graphitizing furnace described in step 3, pass into nitrogen, at carbon/carbon composite material crucible internal surface reaction in－situ, generate silicon nitride coating, furnace cooling, obtains compound coating carbon/carbon composite material crucible; The temperature of reaction of described in-situ chemical reaction is 1200 ℃, and soaking time is 10h.
After testing, compound coating carbon/carbon composite material crucible prepared by the present embodiment, comprise carbon/carbon composite material crucible, the thickness that is attached to carbon/carbon composite material crucible internal surface is the coat of silicon carbide of 200 μ m, is attached to thickness on coat of silicon carbide and is the silicon coating of 15 μ m and the thickness that is attached on silicon coating is the silicon nitride coating of 70 μ m.
The present embodiment adopts chemical gas-phase reaction method original position to generate SiC coating, the relative standby SiC coating of traditional C VD legal system, higher with charcoal/carbon matrix bonding strength, original position generates the generation that excessive Si coating is silicon nitride coating simultaneously provides Si source, utilize the generated in-situ silicon nitride coating bonding strength of high pure nitrogen to improve, further improved the corrosion resistance of crucible; On the other hand, owing to there is no corrosive gases source (as ammonia, trichloromethyl silane, hydrogen etc.), processing safety further improves, and has reduced production cost simultaneously; The compound coating carbon/carbon composite material crucible of preparation utilizes silicon nitride combined silicon carbide compound coating, can effectively suppress, containing the erosion of silicon vapor to profile in carbon/carbon composite material crucible, to have increased substantially the work-ing life of crucible.
Embodiment 3
Step 1, according to crucible shape to be prepared and performance requriements, adopt ordinary method to utilize charcoal fiber, charcoal cloth and net tire to make density for 0.50g/cm
3charcoal fiber preform, by described charcoal fiber preform density to density, be then 1.65g/cm
3; The method of described density is:
101, charcoal fiber preform is placed in to chemical vapor deposition stove, the propylene that employing volume ratio is 1: 1 and the gas mixture (also can adopt propylene or Sweet natural gas) of Sweet natural gas carry out chemical vapor infiltration 2 times as carbon-source gas, the processing parameter of 2 chemical vapor infiltrations is: carbon-source gas flow is 100L/min, the temperature of chemical vapor infiltration is 1100 ℃, and soaking time is 60h;
102, the charcoal fiber preform after 2 chemical vapor infiltrations in 101 is placed in to dipping stove and carries out acetone-furfural resin and resol (mass ratio 1: 1) pressure impregnation (also can adopt acetone-furfural resin pressure impregnation or resol pressure impregnation), be then placed in charring furnace charing; The pressure of described pressure impregnation is 2.5MPa, and the dwell time is 5h; The temperature of described charing is 1000 ℃, and soaking time is 5h;
103, repeat 102 3 times, obtaining density is 1.65g/cm
3charcoal fiber preform;
Step 2, to density described in 103, be 1.65g/cm
3charcoal fiber preform carry out mechanical workout, obtain carbon/carbon composite material crucible;
Step 3, carbon/carbon composite material crucible described in step 2 is placed in to graphitizing furnace, take HIGH-PURITY SILICON as raw material, adopt chemical vapor infiltration technique to generate coat of silicon carbide and silicon coating at carbon/carbon composite material crucible internal surface reaction in－situ; The quality purity of described HIGH-PURITY SILICON is 99.5%; The temperature of reaction of described chemical vapor infiltration technique is 1950 ℃, and soaking time is 6h;
Step 4, in graphitizing furnace described in step 3, pass into nitrogen, at carbon/carbon composite material crucible internal surface reaction in－situ, generate silicon nitride coating, furnace cooling, obtains compound coating carbon/carbon composite material crucible; The temperature of reaction of described in-situ chemical reaction is 1400 ℃, and soaking time is 24h.
After testing, compound coating carbon/carbon composite material crucible prepared by the present embodiment, comprise carbon/carbon composite material crucible, the thickness that is attached to carbon/carbon composite material crucible internal surface is the coat of silicon carbide of 300 μ m, is attached to thickness on coat of silicon carbide and is the silicon coating of 20 μ m and the thickness that is attached on silicon coating is the silicon nitride coating of 100 μ m.
The present embodiment adopts chemical gas-phase reaction method original position to generate SiC coating, the relative standby SiC coating of traditional C VD legal system, higher with charcoal/carbon matrix bonding strength, original position generates the generation that excessive Si coating is silicon nitride coating simultaneously provides Si source, utilize the generated in-situ silicon nitride coating bonding strength of high pure nitrogen to improve, further improved the corrosion resistance of crucible; On the other hand, owing to there is no corrosive gases source (as ammonia, trichloromethyl silane, hydrogen etc.), processing safety further improves, and has reduced production cost simultaneously; The compound coating carbon/carbon composite material crucible of preparation utilizes silicon nitride combined silicon carbide compound coating, can effectively suppress, containing the erosion of silicon vapor to profile in carbon/carbon composite material crucible, to have increased substantially the work-ing life of crucible.
Compare the work-ing life to the work-ing life of compound coating carbon/carbon composite material crucible of the present invention and conventional crucible, the results are shown in following table:
The contrast of table 1 differing materials pot life
| Material | Single heat loss (mm) | Work-ing life (heat) |
| Plumbago crucible | 0.2 | 40 |
| Charcoal/charcoal crucible | 0.1 | 80 |
| Crucible of the present invention | 0.04 | 180 |
As can be seen from Table 1, in use, single heat loss obviously reduces compound coating carbon/carbon composite material crucible of the present invention, and obviously extend the work-ing life of crucible.
The above; it is only preferred embodiment of the present invention; not the present invention is done to any restriction, every any simple modification of above embodiment being done according to invention technical spirit, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.
Claims (9)
1. a compound coating carbon/carbon composite material crucible, it is characterized in that, comprise carbon/carbon composite material crucible, be attached to the coat of silicon carbide of carbon/carbon composite material crucible internal surface, be attached to the silicon coating on coat of silicon carbide and be attached to the silicon nitride coating on silicon coating.
2. a kind of compound coating carbon/carbon composite material crucible according to claim 1, it is characterized in that, the thickness of described coat of silicon carbide is 100 μ m～300 μ m, and the thickness of described silicon coating is 10 μ m～20 μ m, and the thickness of described silicon nitride coating is 50 μ m～100 μ m.
3. prepare a method for compound coating carbon/carbon composite material crucible as claimed in claim 1 or 2, it is characterized in that, the method comprises the following steps:
Step 1, by density, be 0.20g/cm
3～0.50g/cm
3charcoal fiber preform density to density be 1.30g/cm
3～1.65g/cm
3;
Step 2, the charcoal fiber preform after density in step 1 is carried out to mechanical workout, obtain carbon/carbon composite material crucible;
Step 3, carbon/carbon composite material crucible described in step 2 is placed in to graphitizing furnace, take HIGH-PURITY SILICON as raw material, adopt chemical vapor infiltration technique to generate coat of silicon carbide and silicon coating at carbon/carbon composite material crucible internal surface reaction in－situ; The quality purity of described HIGH-PURITY SILICON is more than 99.0%; The temperature of reaction of described chemical vapor infiltration technique is 1550 ℃～1950 ℃, and soaking time is 0.5h～6h;
Step 4, in graphitizing furnace described in step 3, pass into nitrogen, at carbon/carbon composite material crucible internal surface reaction in－situ, generate silicon nitride coating, furnace cooling, obtains compound coating carbon/carbon composite material crucible; The temperature of reaction of described in-situ chemical reaction is 900 ℃～1400 ℃, and soaking time is 0.5h～24h.
4. method according to claim 3, is characterized in that, the method for density described in step 1 is:
101, charcoal fiber preform is placed in to chemical vapor deposition stove, adopts carbon-source gas to carry out chemical vapor infiltration 1～2 time;
102, the charcoal fiber preform after chemical vapor infiltration in 101 is placed in to dipping stove and carries out acetone-furfural resin and/or resol pressure impregnation, be then placed in charring furnace charing;
103, repeat 102 until the density of charcoal fiber preform reaches 1.30g/cm
3～1.65g/cm
3.
5. method according to claim 4, is characterized in that, carbon-source gas described in 101 is propylene and/or Sweet natural gas, and carbon-source gas flow is 20L/min～100L/min, and the temperature of chemical vapor infiltration is 900 ℃～1100 ℃, and soaking time is 30h～60h.
6. method according to claim 4, is characterized in that, the pressure of pressure impregnation described in 102 is 1.0MPa～2.5MPa, and the dwell time is 0.5h～5h.
7. method according to claim 4, is characterized in that, the temperature of charing described in 102 is 900 ℃～1000 ℃, and soaking time is 2h～5h.
8. method according to claim 4, is characterized in that, the number of times repeating described in 103 is 1～3 time.
9. method according to claim 3, is characterized in that, the temperature of reaction of the technique of chemical vapor infiltration described in step 3 is 1750 ℃, and soaking time is 3h.
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