CN105600786B - A kind of method of low power consumption, Fast back-projection algorithm SiC powders - Google Patents
A kind of method of low power consumption, Fast back-projection algorithm SiC powders Download PDFInfo
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- CN105600786B CN105600786B CN201610157371.XA CN201610157371A CN105600786B CN 105600786 B CN105600786 B CN 105600786B CN 201610157371 A CN201610157371 A CN 201610157371A CN 105600786 B CN105600786 B CN 105600786B
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Abstract
The present invention provides a kind of low power consumption, the method for Fast back-projection algorithm SiC powders, and this method is improved by Si powder ratio, SiO2Addition, prevent unnecessary C powder from existing, SiO2After reaction occurs, amount of heat produces, and as CO is released, promotes the reaction of Si+C powder with heat, promotes self- propagating, saved substantial amounts of electricity, carried out rapid reaction, using the pattern of compacting column block, reduces the reaction of powder and crucible wall.
Description
Technical field
The present invention relates to a kind of method of low power consumption, Fast back-projection algorithm SiC powders, belong to technical field of crystal growth.
Background technology
Carborundum represents as third generation semiconductor material with wide forbidden band, with energy gap is big, mobility is high, thermal conductivity is high
Etc. excellent electricity thermal characteristic, turn into the ideal material for making high frequency, high-power, high temperature resistant and radioresistance device.In device
In terms of development, carborundum blue-ray LED has been commercialized；The research and development of silicon carbide power device turn into novel power semiconductor
The main flow of research and development；In terms of High temperature semiconductor device, the carborundum JFET and silicon carbide device that are made using carbofrax material
Part can under 600 DEG C of high temperature under without any cooling heat radiation system normal work.Enter one with manufacturing silicon carbide semiconductor technology
Step development, the application of carbofrax material and device is more and more wide, in white-light illuminating, automotive circuit diagram, radar communication, petroleum drilling
Play vital effect in the fields such as well, Aero-Space, nuclear reactor system and military equipment.
Therefore, the SiC powders for SiC single crystal growth will reach high-purity, meet the requirement of stoichiometric proportion.But
The SiC powders of wide variety of self- propagating method and Acheson methods synthesis now, although wanting for industrial SiC powders can be met
Ask, but, can be to growing the electrical properties and crystal of crystal there is the problems such as impurity concentration is high, powder caking, remaining Si simple substance
Quality has a major impact.And although Purity of Coke Powder impurity content that organic synthesis method obtains is used in below 1ppm high-purity powder
Material, but subsequent processes are complicated, and micro mist collects difficult, unsuitable a large amount of production and applications.
Chinese patent literature 200810016665.6 discloses a kind of high-pure SiC power for semiconductor single-crystal growth
Artificial synthesis, this method is available for the high-pure SiC power of semiconductor single-crystal growth using secondary synthesis process
Material, but columbite process is more complicated, time-consuming, impurity can be artificially introduced in building-up process.
And for example, Chinese patent literature 201510253736.4 discloses a kind of side of low cost low temperature synthesizing silicon carbide powder
Method, although using single sintering method, overcome secondary synthesis complex procedures, time-consuming, is artificially introduced the shortcomings of impurity, reality
In, there is also following problem：
(1), due to one of graphite and reaction source, always introduced in synthetic reaction more as container using graphite crucible
Remaining carbon dust, cause to occur unnecessary carbon dust in the SiC powders of synthesis and also have other impurities.
(2) the 1420 degree of of fusing point of the synthesis temperature used more than Si powder.At high temperature, Si powder melts to form silica drop.In pine
In scattered Si powder and the mixture of C powder, silica drop can be affected by gravity and flow to crucible bottom, so as to be effectively synthesized SiC powders.
This reaction can cause the Si in SiC powders：C continues proportional imbalance, at the same grow to SiC single crystal introduce Si drops generation micro-pipe,
The defects of dislocation.
(3) SiC powders synthetic method is burning (CS) method, is directly to be synthesized Si powder and C powder at high temperature, mainly
Reaction equation is as follows：
Si(s)+C(s)→SiC(s)
Because this reaction is weak exothermic reaction, the heat reacted for guarantee needed for lasting progress needs continuous heating, meeting one
Determine the waste for causing electric power resource in degree.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of low power consumption, the method for Fast back-projection algorithm SiC powders.The present invention
Improved by Si powder ratio, SiO2Addition, adjust the ratio of Si powder and C powder, prevent the unnecessary C powder that graphite crucible introduces from depositing
.Add a certain proportion of SiO2With C powder react release amount of heat, these heats promote and accelerate Si+C powder self- propagating it is anti-
Should, save substantial amounts of electricity.Using the pattern of compacting column block, reduce the reaction of powder and crucible wall.
Technical scheme：
A kind of method of low power consumption, Fast back-projection algorithm SiC powders, including step are as follows：
(1) it is 1.03~1.08 by the molar ratio of Si powder and C powder:1 takes the other Si powder of semiconductor grade and C powder, Ran Houjia
Enter high-purity Si O2Powder；SiO2The addition of powder is Si powder and the 1-6% of C powder gross masses；
(2) powder in step (1) is uniformly mixed, suppressed by isostatic pressed, form cylindrical piece；
(3) cylindrical piece of powder pressing is placed in graphite crucible, be put into synthetic furnace；
(4) after extracting vacuum repeatedly, protective gas is passed through, and ensures that pressure 600-1000mbar is stable, is quickly heated up to
1200-1400 DEG C is reacted, and when monitoring air pressure fluctuating in reactor, stops heating, reaction is completed, and produces SiC powders.
Currently preferred, in step (1), the molar ratio of Si powder and C powder is 1.04~1.06:1, it is preferred that Si powder
Molar ratio with C powder is 1.05:1.
The present invention can be reacted by adjusting a small amount of unnecessary Si powder of powder ratio with graphite crucible wall, prevent unnecessary C
Powder introduces.
It is currently preferred, in step (1), SiO2The addition of powder is Si powder and the 3-5% of C powder gross masses.
Currently preferred, in step (2), the volume ratio of powder is optimized for 5 before and after compacting：1-3：1.
Currently preferred, step (2) cylindrical piece internal diameter is less than the diameter of reactor crucible, make cylindrical piece and sidewall of crucible it
Between formed 2-10mm gap.
After the material compacting of the present invention, fully contacted between powder, do not form space, prevent the Si that high temperature is formed from dropping in powder
Flowed in material.The cylindrical piece diameter of compacting is less than crucible, effectively reduces the reaction with graphite crucible side wall, prevents C powder from introducing.
Currently preferred, heating rate is more than or equal to 200 DEG C/h in step (3).
Preferably, heating rate is 300~500 DEG C/h in step (3).It is slow due to heating, easily cause Si powder to melt
Change.Using quick mode of heating, reach self- propagating temperature as early as possible.
The reaction of the present invention is as follows：SiO2+ 3C--SiC+2CO, this is a violent exothermic reaction, can be introduced substantial amounts of
Heat, so as to provide the heat of the self-propagating reaction of follow-up Si, C powder needs.Meanwhile rubbing for Si powder and C powder is have adjusted again
That ratio.SiO2+ C and Si+C reactions are a synergistic effects.In temperature more than 1200 DEG C, it is anti-that self- propagating occurs first
Should.Due to heating the heat with self-propagating reaction, SiO can be helped2With the reaction of carbon dust.SiO2Once triggering, this is one for reaction
Individual violent exothermic reaction, the heat that follow-up self- propagating needs can be provided completely.Therefore intermediate frequency power supply can be closed, saved significantly
About electricity.
It is currently preferred, in step (3), heated using intermediate frequency power supply.
Currently preferred, in step (3), described protective gas is argon gas.
The excellent results of the present invention：
1st, 1200 degree of low temperature starts to synthesize, and prevents silica drop from largely producing.
2、SiO2After reaction occurs, amount of heat produces.As CO is released, promote the reaction of Si+C powder with heat, promote
Enter self- propagating, save substantial amounts of electricity.
3rd, improved by Si powder ratio, SiO2Addition, prevent unnecessary C powder from existing.
4th, using the pattern of compacting column block, the reaction of powder and crucible wall is reduced.
Brief description of the drawings
Fig. 1 is the relation curve of the pressure and temperature reacted in the synthesis material course of reaction of the embodiment of the present invention 1.
Fig. 2 is the microphotograph that the embodiment of the present invention 1 obtains powder.
Embodiment
With reference to embodiment, the present invention will be further described, but not limited to this.
Embodiment 1：
A kind of method of low power consumption, Fast back-projection algorithm SiC powders, including step are as follows：
(1) it is 1.05 by the molar ratio of Si powder and C powder:1 takes the other Si powder of semiconductor grade and C powder, then adds high-purity
SiO2Powder；SiO2The addition of powder is the 5% of Si powder and C powder gross masses；
(2) powder in step (1) is uniformly mixed, suppressed by isostatic pressed, volume ratio 5：1, powder pressing into
Cylindrical piece；Cylindrical piece internal diameter is less than the diameter of reactor crucible, makes the gap that 5mm is formed between cylindrical piece and sidewall of crucible.
(3) cylindrical piece of powder pressing is placed in graphite crucible, be put into synthetic furnace；
(4) take out repeatedly and fill vacuum 6h, be passed through inert gas (argon gas), and ensure the stabilization of air pressure, pressure using mechanical pump
Control is after 600mbar, pressure stability, and when starting to quickly heat up to 1400 DEG C, 300 DEG C/h of heating rate, pressure rises
Volt, illustrates SiO2Reacted with C.Intermediate frequency power supply is closed, temperature continues for some time at 1250 DEG C, illustrates that self-propagating reaction is held
Continuous, reaction is completed, and produces SiC powders.
The relation curve of pressure and temperature is as shown in Figure 1 in synthesis material course of reaction in the present embodiment step (4).By Fig. 1
Understand, pressure rises and falls, and illustrates SiO2Reacted with C.Intermediate frequency power supply is closed, temperature continues for some time at 1250 DEG C,
Illustrate that self-propagating reaction continues.
SiC powders microphotograph that the present embodiment obtains as shown in Fig. 2 by Fig. 2 it can be seen that without carbon dust, only
Granular SiC powder.
Embodiment 2：
A kind of method of low power consumption, Fast back-projection algorithm SiC powders, including step are as follows：
(1) it is 1.06 by the molar ratio of Si powder and C powder:1 takes the other Si powder of semiconductor grade and C powder, then adds high-purity
SiO2Powder；SiO2The addition of powder is the 6% of Si powder and C powder gross masses；
(2) powder in step (1) is uniformly mixed, suppressed by isostatic pressed, volume ratio 4：1, powder pressing into
Cylindrical piece；Cylindrical piece internal diameter is less than the diameter of reactor crucible, makes the gap that 2mm is formed between cylindrical piece and sidewall of crucible.
(3) cylindrical piece of powder pressing is placed in graphite crucible, be put into synthetic furnace；
(4) after vacuumizing repeatedly, protective gas argon gas is passed through, and ensures the stabilization of air pressure using mechanical pump, quick heating
Reacted to 1200 DEG C, 500 DEG C/h of heating rate, the fluctuating of air pressure is seen by monitoring window, illustrates SiO2Reaction hair
It is raw, intermediate frequency power supply is closed, reaction is completed, and produces SiC powders.
Claims (7)
1. a kind of method of low power consumption, Fast back-projection algorithm SiC powders, including step are as follows：
(1) it is 1.04~1.06 by the molar ratio of Si powder and C powder:1 takes the other Si powder of semiconductor grade and C powder, then adds high
Pure SiO2Powder；SiO2The addition of powder is Si powder and the 3-5% of C powder gross masses；
(2) powder in step (1) is uniformly mixed, suppressed by isostatic pressed, form cylindrical piece；
(3) cylindrical piece is placed in vacuum, cylindrical piece internal diameter is less than the diameter of reactor crucible, makes between cylindrical piece and sidewall of crucible
Form 2-10mm gap；Protective gas is passed through, and ensures stable gas pressure, 1200-1400 DEG C is quickly heated up to and is reacted, is supervised
When controlling air pressure fluctuating in reactor, stop heating, reaction is completed, and produces SiC powders.
2. the method for low power consumption according to claim 1, Fast back-projection algorithm SiC powders, it is characterised in that in step (1), Si
The molar ratio of powder and C powder is 1.05:1.
3. the method for low power consumption according to claim 1, Fast back-projection algorithm SiC powders, it is characterised in that in step (2), pressure
The volume ratio of powder is 5 before and after system：1-3：1.
4. the method for low power consumption according to claim 1, Fast back-projection algorithm SiC powders, it is characterised in that risen in step (3)
Warm speed is more than or equal to 200 DEG C/h.
5. the method for low power consumption according to claim 1, Fast back-projection algorithm SiC powders, it is characterised in that risen in step (3)
Warm speed is 300~500 DEG C/h.
6. the method for low power consumption according to claim 1, Fast back-projection algorithm SiC powders, it is characterised in that in step (3), adopt
Heated with intermediate frequency power supply.
7. the method for low power consumption according to claim 1, Fast back-projection algorithm SiC powders, it is characterised in that in step (3), institute
The protective gas stated is argon gas.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU177312C (en) * | 1988-07-12 | 1994-09-30 | Институт структурной макрокинетики РАН | Process for preparing silicon carbide |
| CN102874810A (en) * | 2012-10-26 | 2013-01-16 | 浙江理工大学 | Preparation method of beta-SiC nano powder |
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2016
- 2016-03-18 CN CN201610157371.XA patent/CN105600786B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU177312C (en) * | 1988-07-12 | 1994-09-30 | Институт структурной макрокинетики РАН | Process for preparing silicon carbide |
| CN102874810A (en) * | 2012-10-26 | 2013-01-16 | 浙江理工大学 | Preparation method of beta-SiC nano powder |
Non-Patent Citations (1)
| Title |
|---|
| 化学气相反应制备碳化硅纳米线;赵建国等;《功能材料》;20071231;第38卷;第2部分实验以及第3.2 部分碳化硅纳米线的生长机理 * |
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Effective date of registration: 20190321 Address after: 511458 Nansha District, Guangzhou City, Guangdong Province, No. 7 Nanjiang Second Road, Zhujiang Street, self-compiled 2 buildings and 2 floors Patentee after: Guangzhou Nansha Wafer Semiconductor Technology Co., Ltd. Address before: No. 27, mountain Dana Road, Ji'nan City, Shandong, Shandong Patentee before: Shandong University |
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