CN104928757A - Quick purification method for thermal insulation system of PVT method carbonization silicon single crystal furnace - Google Patents
Quick purification method for thermal insulation system of PVT method carbonization silicon single crystal furnace Download PDFInfo
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- CN104928757A CN104928757A CN201510416752.0A CN201510416752A CN104928757A CN 104928757 A CN104928757 A CN 104928757A CN 201510416752 A CN201510416752 A CN 201510416752A CN 104928757 A CN104928757 A CN 104928757A
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Abstract
The invention relates to a quick purification method for a thermal insulation system of a PVT method carbonization silicon single crystal furnace. The quick purification method comprises the steps that firstly, vacuumizing processing is carried out on the thermal insulation system of the carbonization silicon furnace; secondly, the thermal insulation system of the carbonization silicon furnace is heated to raise the temperature; thirdly, after the preset temperature is reached, the temperature is maintained, and the system is continuously vacuumized; fourthly, when the pressure in the system reaches 1*10<-5>mbar and is stabilized, inert protection gas argon is slowly injected into the system at the gas feeding amount of 1 L/min for 10 minutes; fifthly, when the pressure in the system reaches the preset value of 400 mbar, the gas feeding amount is unchanged, sufficient inert gas is supplied, and the state is maintained for 30 min; sixthly, gas feeding is stopped, and the system is vacuumized for 1-2 hours; seventhly, the operation from the step four to the step six is repeated, the pressure is raised to be 900 mbar, cooling is started, and the purification work of the thermal insulation system is completed. The quick purification method has the advantages that the very high purification effect is achieved quickly, the impurity content of the nitrogen of carbonization silicon single crystals is obviously reduced, and the growth quality of the single crystals is greatly improved.
Description
Technical field
The present invention relates to a kind of PVT method single-crystal silicon carbide stove heat-insulation system, particularly a kind of method for quickly purifying of PVT method single-crystal silicon carbide stove heat-insulation system.
Background technology
At present, PVT method is the most ripe method of growing silicon carbide single crystal.In PVT method silicon carbide monocrystal growth process, usually adopt silicon carbide powder source to do raw material, its growing apparatus forms by plumbago crucible with at the heat-insulation system of crucible outer wrap.This heat-insulation system is made up of carbon felt, and its vesicular structure makes it have very strong gas sorption ability.When preparing high-purity silicon carbide monocrystalline, the nitrogen that in air, content is the highest is the impurity especially needing to avoid, and lagging material can inevitable ingress of air in the process of bought transportation, these nitrogen final will be incorporated in single-crystal silicon carbide, mixing of this involuntary impurity not only easily introduces defect in crystal, and add growing semi-insulated single-crystal silicon carbide difficulty.
Therefore, be ensure the high purity of carborundum crystals, just need the content reducing nitrogen as much as possible, in current silicon carbide monocrystal growth system, especially lagging material is one of significant source of impurity, and adsorption concentration when supplier all cannot ensure that it is stocked up.
Summary of the invention
In view of the problem of prior art, the invention provides a kind of method for quickly purifying of PVT method single-crystal silicon carbide stove heat-insulation system, achieve and the nitrogen in single-crystal silicon carbide stove heat-insulation system is discharged rapidly to greatest extent, thus obtain low nitrogen content, relatively highly purified single-crystal silicon carbide, concrete technical scheme is, a method for quickly purifying for PVT method single-crystal silicon carbide stove heat-insulation system, is characterized in that: concrete steps comprise
Step 1, described single crystal growing furnace heat-insulation system is placed in purifying furnace, carries out vacuumizing process, by vacuum extractor, the air in purifying furnace furnace chamber is tentatively taken out light;
Step 2, to single crystal growing furnace heat-insulation system heat temperature raising, open purifying furnace heating system, top temperature is presetting at 2400 ~ 2500 DEG C, and power is promoted to maximum value 10kW by the speed of 3kW per hour by zero;
Step 3, reach preset temperature after, maintain this temperature and continue system is vacuumized, can simultaneously by the nitrogen constantly discharged extract out go;
Step 4, continue to vacuumize after, stove furnace chamber internal pressure to be purified reaches 1 × 10
-5mbar also, after stablizing, slowly passes into inert protective gas, with 10 minutes, air input is at the uniform velocity risen to 1L/min from 0 in chamber;
Step 5, when purifying furnace furnace chamber internal pressure reaches preset value 400mbar, keep air input constant, maintain this state 30min, ensure sufficient rare gas element supply, the entrap bubble in heat-insulation system is fully replaced;
Step 6, stopping air inlet, vacuumize purifying furnace furnace chamber, continue 1-2h, fully discharged by the gas containing the nitrogen displaced from lagging material, oxygen in furnace chamber, total impurities amount in furnace chamber reduced;
Step 7, repeating step 4 to step 6 three times, successively reduce total impurities residual quantity in furnace chamber, promote purification effect further, be finally forced into 900mbar, starts cooling, complete heat-insulation system purification work.
Technique effect of the present invention is, reaches very high purification effect fast, and the nitrogen impurity content of semiconductor single crystal material obviously declines, and the growth quality of monocrystalline improves greatly.
Accompanying drawing explanation
Fig. 1 is schema of the present invention.
Embodiment
Illustrate below and method described in the embodiment of the present invention is further elaborated.
Step 1, process is vacuumized to described silicon carbide furnace heat-insulation system, by vacuum extractor, the air in silicon carbide furnace heat-insulation system is taken out light;
Step 2, to silicon carbide furnace heat-insulation system heat temperature raising, open heating system, top temperature is presetting at 2400 DEG C, and power is promoted to maximum value 10kW by the speed of 3kW per hour by zero;
Step 3, reach preset temperature after, maintain this temperature and continue system is vacuumized, can simultaneously by the nitrogen constantly discharged extract out go; Because in the above-mentioned treating processes heated up to single-crystal silicon carbide stove heat-insulation system, nitrogen in lagging material can constantly discharge, so need constantly to carry out vacuumizing process, at any time the nitrogen discharged is extracted out and go, thus effectively remove to be adsorbed on the nitrogen existed in single-crystal silicon carbide stove heat-insulation system; And continue the vacuum-treat of certain hour after stabilizing the temperature, contribute to heat-insulation system of being discharged by the gas discharged as much as possible;
Step 4, continue to vacuumize after, stove furnace chamber internal pressure to be purified reaches 1 × 10
-5mbar also, after stablizing, slowly passes into inert protective gas, with 10 minutes, air input is at the uniform velocity risen to 1L/min from 0 in chamber;
Step 5, when purifying furnace furnace chamber internal pressure reaches preset value 400mbar, keep air input constant, maintain this state 30min, ensure sufficient rare gas element supply, the entrap bubble in heat-insulation system is fully replaced;
Step 6, stopping air inlet, vacuumize purifying furnace furnace chamber, continue 1-2h, fully discharged by the gas containing the nitrogen displaced from lagging material, oxygen in furnace chamber, total impurities amount in furnace chamber reduced;
Step 7, repeating step 4 to step 6 three times, successively reduce total impurities residual quantity in furnace chamber, promote purification effect further, be finally forced into 900mbar, starts cooling, complete heat-insulation system purification work.
Principle, hot conditions can destroy the impurity such as nitrogen rely exist some physics, chemical bond, it is made to discharge rapidly at short notice, repeatedly gas washing then can displace the entrap bubble of lagging material inside absorption more fully, reduce total impurities residual quantity to the full extent, therefore, under whole heat-insulation system being maintained the processing condition of a relatively-high temperature, and combine repeatedly gas washing, can purifying heat-insulation system to the full extent.
Claims (1)
1. a method for quickly purifying for PVT method single-crystal silicon carbide stove heat-insulation system, is characterized in that: concrete steps comprise,
Step 1, described single crystal growing furnace heat-insulation system is placed in purifying furnace, carries out vacuumizing process, by vacuum extractor, the air in purifying furnace furnace chamber is tentatively taken out light;
Step 2, to single crystal growing furnace heat-insulation system heat temperature raising, open purifying furnace heating system, top temperature is presetting at 2400 ~ 2500 DEG C, and power is promoted to maximum value 10kW by the speed of 3kW per hour by zero;
Step 3, reach preset temperature after, maintain this temperature and continue system is vacuumized, can simultaneously by the nitrogen constantly discharged extract out go;
Step 4, continue to vacuumize after, stove furnace chamber internal pressure to be purified reaches 1 × 10
-5mbar also, after stablizing, slowly passes into inert protective gas, with 10 minutes, air input is at the uniform velocity risen to 1L/min from 0 in chamber;
Step 5, when purifying furnace furnace chamber internal pressure reaches preset value 400mbar, keep air input constant, maintain this state 30min, ensure sufficient rare gas element supply, the entrap bubble in heat-insulation system is fully replaced;
Step 6, stopping air inlet, vacuumize purifying furnace furnace chamber, continue 1-2h, fully discharged by the gas containing the nitrogen displaced from lagging material, oxygen in furnace chamber, total impurities amount in furnace chamber reduced;
Step 7, repeating step 4 to step 6 three times, successively reduce total impurities residual quantity in furnace chamber, promote purification effect further, be finally forced into 900mbar, starts cooling, complete heat-insulation system purification work.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105463573A (en) * | 2015-12-22 | 2016-04-06 | 中国电子科技集团公司第二研究所 | Method for reducing silicon carbide crystal impurities and obtaining high-purity semi-insulating silicon carbide crystal |
| CN105821471A (en) * | 2016-05-10 | 2016-08-03 | 山东大学 | Preparation method of low-stress and high-purity semi-insulating SiC single crystal |
| CN108118394A (en) * | 2017-12-28 | 2018-06-05 | 河北同光晶体有限公司 | A kind of method of nitrogen impurity content in reduction single-crystal silicon carbide |
| CN111663176A (en) * | 2020-06-18 | 2020-09-15 | 眉山博雅新材料有限公司 | Crystal growth method and device |
| CN113061988A (en) * | 2021-03-10 | 2021-07-02 | 中国恩菲工程技术有限公司 | Silicon core preparation method and silicon core preparation equipment |
| CN113550009A (en) * | 2021-07-27 | 2021-10-26 | 河北天达晶阳半导体技术股份有限公司 | Method and device for growing high-purity silicon carbide single crystal |
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| CN105463573A (en) * | 2015-12-22 | 2016-04-06 | 中国电子科技集团公司第二研究所 | Method for reducing silicon carbide crystal impurities and obtaining high-purity semi-insulating silicon carbide crystal |
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| CN113061988A (en) * | 2021-03-10 | 2021-07-02 | 中国恩菲工程技术有限公司 | Silicon core preparation method and silicon core preparation equipment |
| CN113550009A (en) * | 2021-07-27 | 2021-10-26 | 河北天达晶阳半导体技术股份有限公司 | Method and device for growing high-purity silicon carbide single crystal |
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