CN101240448A - Vacuum purifying furnace specially used for metal silicon/silicon dioxide and purifying method thereof - Google Patents
Vacuum purifying furnace specially used for metal silicon/silicon dioxide and purifying method thereof Download PDFInfo
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- CN101240448A CN101240448A CNA2007101965628A CN200710196562A CN101240448A CN 101240448 A CN101240448 A CN 101240448A CN A2007101965628 A CNA2007101965628 A CN A2007101965628A CN 200710196562 A CN200710196562 A CN 200710196562A CN 101240448 A CN101240448 A CN 101240448A
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Abstract
The invention provides a vacuum purifying furnace for silicon metal/silica, including an exinous crucible using for full of silicon metal/silica, and at least one temperature control heating system of control crucible temperature to heat the crucible, the vacuum purifying furnace can pull out the vacuum and fill into the inert gas or the oxygen, the temperature control system includes a plurality of heating elements on at least a portion of exine and a computer system of the same, a plurality of heating element along the direction of crucible are divided into several groups, each group of heating elements is controlled by computer system according to the first group of heating elements in the cooling and solidification process of first region are continued to heat around the peripheral part of the first region for the first group of heating elements in the head and melt in the crucible along this direction, the first region of the first group of heating elements. The invention also relates to a method of the vacuum purifying furnace for silicon metal/silica.
Description
Technical field
The present invention relates to the vacuum purifier apparatus, be particularly useful for the purifying of metal silicon/silicon dioxide, and corresponding purification process
Background technology
Chinese invention patent application 200610046525.4 discloses a kind of preparation method and device of high purity polycrystalline silicon, wherein in the vacuum chamber of preparation facilities, be provided with electromagnetic induction heater, crucible, directional freeze crucible and be placed in the directional freeze crucible outside holding furnace and drawing device, comprise the secondary purification process furnace of refining crucible, here, elder generation's melting solid silicon in crucible, then molten silicon is injected the directional freeze crucible, utilize the downward throwing of drawing device, realize directional freeze, remove impurity in the silicon, then purifying in secondary purification process furnace.The building block of above-mentioned preparation facilities is numerous, and needs drawing device to realize directional freeze and removal of impurities, complex structure, and increased equipment size.In addition, the operation of aforesaid method is many, complicated operation, running cost height.
Summary of the invention
Therefore, the purpose of this invention is to provide a kind of vacuum purifying furnace especially for the metal silicon/silicon dioxide, it does not need special drawing device, just can realize the directional freeze and the removal of impurities of fusion silicon/silicon dioxide simultaneously, and dwindled equipment size, structure is simpler.The present invention also will provide a kind of purification process of corresponding metal silicon/silicon dioxide, and its procedure of processing is few, and is simple to operate, and running cost is low.
For this reason, the invention provides a kind of vacuum purifying furnace that is used in particular for the metal silicon/silicon dioxide, comprise and be used for crucible splendid attire metal silicon/silicon dioxide and that have outer wall, and the heating crucible and heating system that comprise the temperature control system that is used to control crucible temperature at least, the vacuum purifying furnace can be evacuated and can fill rare gas element or oxygen, it is characterized in that, temperature control system comprises a plurality of heating members at least a portion that is arranged in this outer wall and the computer system that is connected with a plurality of heating members, described a plurality of heating member is divided into some groups along a direction of this crucible, computer system is controlled every group of heating member in such a way, for the fusion silicon/silicon dioxide of first group of heating member that on this direction, is positioned at the forefront and crucible, corresponding to the first area of first group of heating member, first group of heating member continues the peripheral part of heating first area in the cooled and solidified process of first area.
So, by computer system the heating power of first group of heating member is implemented control, can in the cooled and solidified process of first area, accurately regulate compensation in other words near the melted silicon/silicon-dioxide liquation periphery of heating member and away from the temperature head between the liquation center of heating member, and cool off above-mentioned periphery and center according to essentially identical cooling rate, thus one, impurity in the silicon/silicon dioxide is got rid of according to physics hot type impurity principle rear in the direction, and having avoided may be because of the high problem at the center of congealed solid enrichment impurity of core temperature.
According to the present invention, for other group heating member and the liquation at described first group of heating member rear, corresponding other zone with it, described other group heating member of described computer system control makes described other zone keep molten state in the cooled and solidified process of described first area.By this measure, the impurity of first area is entered in the zone of its below smoothly.In addition, after the cooled and solidified of first area, computer system can be controlled other group heating member that comes first group of heating member rear according to the mode identical with first group of heating member.Repeatedly temperature control is implemented in each zone of liquation in the manner described above by computer system, can make each regional impurity enter the zone at rear successively, definitely the say so bottom in zone, rear, and then can cut away the bottom after the complete cooled and solidified of liquation in crucible, promptly obtain the solid silicon/silicon dioxide of purifying.Certainly, can carry out above-mentioned purification process repeatedly, can obtain purity and reach solid silicon/silicon dioxide more than 99.9999%, wherein purifying silicon can be used as solar energy polycrystalline silicon.
In the present invention, heating member can be resistance, electric arc generation part or solenoid, preferred solenoid.And heating member is preferably to be arranged on the outer wall around mode.Here, crucible can be formed by highly purified quartz, silicon carbide or graphite.
In addition, the vacuum purifying furnace comprises liftable or the rotating bell jar that is used for airtight crucible.Preferably be provided with water-cooled tube on bell jar, water coolant can for example circulate in water-cooled tube by pump.
Temperature control system can also comprise temp sensor device, temp sensor device comprises a plurality of temperature sensors, a plurality of temperature sensors are configured in the zone described outer wall, corresponding to each group heating member according to mode one to one, are used to survey near the melt temperature described outer wall area.By a plurality of transmitters of corresponding configuration, can accurately grasp melt temperature, and then accurately control or regulate the heating power of corresponding heating member.Here, temperature sensor thermocouple meter preferably.Can certainly take the thermometric device of other form, as infrared thermometer.
Temp sensor device is connected with computer system, so that the data that take off data and this computer system are set compare.Like this, computer system can be through needing relatively determining whether heating or cooling.Here, computer system comprises many computers, and these computers are attached troops to a unit in many groups heating member with corresponded manner one by one.
On bell jar, be provided with tube stub that is used to vacuumize and the tube stub that is used for injecting inert gas.In addition, when the vacuum purifying silicon, adopt rare gas element, preferred nitrogen, preferably purity is 99.99999% nitrogen.Each regional speed of cooling of liquation is about 0.1 ℃/minute to 1 ℃/minute.Computer system is calculated the heating power of respectively organizing heating member in the differential mode.The vacuum purifying furnace can be evacuated to 0.5 millitorr.When vacuum purifying silicon-dioxide, in the vacuum purifying furnace, charge into oxygen.
According to one embodiment of present invention, described a plurality of heating members are arranged on the outer wall along the crucible vertical direction, definitely say to be arranged on the crucible perisporium, and at this moment, above-mentioned first group of heating member preferably that below coming on this vertical direction organized heating member.Perhaps, described a plurality of heating members are arranged on the crucible outer wall along the crucible horizontal direction, and definitely saying so is arranged on the roof and diapire of crucible, perhaps is arranged on the part of roof, diapire and perisporium.
Description of drawings
Below, describe embodiments of the invention in conjunction with the accompanying drawings in detail, wherein:
Fig. 1 represents that it is used for purified metal silicon according to vacuum purifying furnace of the present invention;
The concrete expression of Fig. 2 crucible shown in Figure 1.
Embodiment
Fig. 1 represents that according to vacuum purifying furnace 1 of the present invention it especially uses physics hot type impurity principle to come the purified metal silicon/silicon dioxide, and wherein purified Pure Silicon Metal can be used as solar energy polycrystalline silicon.Vacuum purifying furnace 1 comprises crucible 2 and is used for the heating system 3 of crucible 2 that wherein the raw material silicon/silicon dioxide can be placed in the crucible 2 and by heating system 3 and be heated to fusion.Crucible 2 is preferably formed by highly purified quartz, silicon carbide or graphite, and preferably is placed in the closed environment.For this reason, a bell jar 4 can be set, be used for airtight cover cap on crucible.Bell jar 4 is liftable or rotating, so that move between closed position and open position at least.Be provided with water-cooled tube 5 on bell jar 4, water coolant circulates in water-cooled tube 5 by for example pump.On bell jar 4, also be provided with tube stub, its respectively be used for injecting inert gas such as nitrogen or be used to inject the pipeline of oxygen and vacuum pump 6 be housed so that the pipeline that vacuumizes links to each other, whereby, crucible 2 can be evacuated to for example 0.5 millitorr.In addition, can control the keying of the pipeline that is used for injecting inert gas or oxygen with electrovalve.
As depicted in figs. 1 and 2, crucible 2 has perisporium 2a and diapire 2b, and heating system 3 comprises temperature control system at least, and this temperature control system comprises a plurality of heating members 8 at least a portion that is arranged in perisporium 2a and the computer system 9 that is connected with heating member.Here, heating member 8 is divided into some groups of P1, P2, P3 along the short transverse of perisporium 2a ... Pn.Computer system 9 is controlled every group of heating member in such a way, promptly for the fused silicon/silicon dioxide of first group of P1 heating member below being positioned on the short transverse and crucible 2, corresponding to the first area of first group of P1 heating member, first group of heating member continues the peripheral part of heating first area in the cooled and solidified process of first area.In this case, for other group P2, the P3 that on short transverse, come first group of P1 heating member back ... Pn heating member and other corresponding with it zone, computer system 9 is other group of control P2, P3 so ... the Pn heating member makes other zone keep molten state in the cooled and solidified process of first area.Be provided with temp sensor device on the perisporium 2a of crucible, it is connected with this computer system, so that the data that take off data and this computer system are set compare.Temp sensor device comprises a plurality of temperature sensors, is the form of thermocouple meter 10 here.Described a plurality of temperature sensor is attached troops to a unit in many groups heating member with corresponded manner one by one.As shown in Figure 2, heating member 8 is solenoids, and it is arranged around whole perisporium.But, heating member 8 also can be that resistance or electric arc produce part.Be also contemplated that heating member 8 is only to center on the local mode layout of perisporium.Computer system can only have a computer, but also many computers can be arranged, and this moment, these computerized optimizations were attached troops to a unit in many groups heating member with corresponded manner one by one.Computer system is preferably calculated the heating power of respectively organizing heating member in the differential mode.
Certainly, computer system also can be after the cooled and solidified of first area be controlled at other group heating member that the height originating party upwards comes first group of heating member back according to the mode identical with first group of heating member, exactly, concerning second group of P2 heating member and corresponding with it second area, make second group of heating member in the cooled and solidified process of second area, continue the peripheral part of heating second area, after the second area cooled and solidified, make the 3rd group of P3 heating member in the cooled and solidified process in the 3rd zone, continue the peripheral part in heating the 3rd zone ..., thus up to the cooled and solidified that on short transverse, comes last zone.Subsequently, the bottom of the final area of enrichment impurity can be cut.
The working process of vacuum purifying furnace of the present invention is as follows:
Under the situation of purifying silicon, the raw silicon of desiring purifying is inserted in the crucible 2, cover bell jar 4, by connecting vacuum extractor at corresponding tube stub place, be evacuated to 0.5 millitorr, and come injecting inert gas such as nitrogen by on the respective tube joint, inserting the rare gas element source of supply.Subsequently, begin to heat crucible 2 by heating system 3.When crucible 2 is warming up to the silicon fusing point more than 1415 ℃ the time, silicon is melt into liquid.At this moment, continue to heat and stop half an hour at 1500 ℃.Afterwards, from first area, utilize temperature control system to control the cooling of crucible 2 corresponding to first group of heating member.For this reason, computer system is first group of heating member of control so, that is, make its peripheral part that in the cooled and solidified process of first area, continues the heating first area, make the peripheral part of first area and the approaching basically identical in other words of cooling rate of centre portions thus.At this moment, preferably be about 0.1 ℃/minute to 1 ℃/minute cooling rate, thus with the past second area that comes the rear of first area along short transverse of the impurity vertical row in the molten silicon.In the cooled and solidified process of first area, keep the zone at its rear to be on the silicon fusing point, make the silicon in the rear area keep liquid.Behind the crystallisation by cooling of first area, second area is for example just since 1450 ℃ of coolings, and up to crystallisation by cooling, carry out the temperature control of second area according to the mode identical with the first area this moment, definitely say, make second group of heating member continue the peripheral part of heating second area.By that analogy, to the last the zone is cooled and solidifies.At this moment, the impurity of the silicon body in the crucible 2 is effectively drained into the bottom of final area.After complete cooled and solidified, take out the silicon solid, the part of impurity promptly is rich in the bottom of cutting away final area, has obtained the silicon of purifying.
Above process can repeated multiple times, be about in purifying operation next time, drop into crucible as raw material through the silicon solid of last purifying, and repeat above-mentioned purification process, and can obtain purity at last and reach silicon more than 99.9999%, it can be used as solar energy polycrystalline silicon.
Why adopt above-mentioned purification treating method to be because in the prior art, conventional cooling is closeall heating member, for example, closes the power supply that is used for described heating member.Thus one, for example in the first area, can reduce by 10 to 15 ℃ at the temperature per minute of peripheral part, and the cooling rate of the temperature of centre portions will be slowly many.The result, be cooled to when (promptly being lower than the silicon fusing point) below 1415 ℃ at peripheral part, the temperature of centre portions can exceed tens of degrees centigrade (about 1455 ℃), and imports lower zone in this temperature distribution mode, causes the temperature difference of interior centre portions of lower zone and peripheral part bigger.Therefore, according to physics hot type impurity principle, the impurity in the silicon is drained into centre portions from peripheral part, and the purity of centre portions is the poorest, and the purity of peripheral part is best, and the purity variation is concentrically ringed form, and the result is difficult for obtaining the silicon of purifying.
In contrast to this, vacuum purifying furnace of present method and correlation method are by its peripheral part of compensation heating in the cooled and solidified process of respective regions, make the temperature and the cooling rate of centre portions and peripheral part be tending towards approaching, avoid producing impurity thus from the phenomenon of periphery to the center enrichment.And, compared with the 99.9% silicon purity that the past pickling is purified, under utilization method of the present invention and vacuum purifying furnace situation, can obtain purity and reach 99.9999% silicon body silicon purifying 2 times.In addition, vacuum purifying furnace of the present invention and purification process compared with prior art are more suitable for producing in enormous quantities, and equipment cost is lower, and device structure has also become simple, and the advantage aspect energy-conservation and environmental protection is very obvious.
Vacuum purifying furnace of the present invention also can be used to purifying silicon-dioxide, at this moment, charges into oxygen in the vacuum purifying furnace, rather than rare gas element, and Heating temperature is higher than the fusing point (about 1700 ℃) of silicon-dioxide.Condition when other working conditions and vacuum purifying furnace purifying silicon is basic identical.
It is to be noted,, also can expect horizontal crucible although crucible illustrated in figures 1 and 2 is vertical.Horizontal crucible has roof, diapire and perisporium, offers charging bole in roof, and a plurality of heating members such as solenoid are for example to be arranged on roof, diapire and the part perisporium of crucible around mode.Here, described a plurality of heating member along continuous straight runs are divided into a plurality of groups, at this moment, cooled and solidified can with from left to right or sequencing from right to left carry out.
Utilization vacuum purifying furnace according to the present invention comes the method for purified metal silicon/silicon dioxide to comprise: insert silicon raw material/silica material in crucible; Under the situation that vacuumizes and fill rare gas element or oxygen, utilize the heating system that has the temperature control system of controlling crucible temperature this crucible to be heated to more than the fusing point of silicon/silicon dioxide; Utilize the computer system of this temperature control system, control being arranged in some groups of heating members on the crucible outer wall, that separate along a direction of crucible in such a way, for first group of heating member that on this direction, is positioned at the forefront and crucible inner melt, corresponding to the first area of first group of heating member, first group of heating member continues the peripheral part of heating first area in the cooled and solidified process of first area.
Certainly, vacuum purifying furnace of the present invention is not limited to the purifying silicon/silicon dioxide, and those of ordinary skills can expect using it for the purifying of other material fully.
Claims (22)
1. vacuum purifying furnace that is particularly useful for the metal silicon/silicon dioxide, comprise and be used for crucible splendid attire metal silicon/silicon dioxide and that have outer wall, and heat this crucible and comprise the heating system of the temperature control system that is used to control crucible temperature at least, this vacuum purifying furnace can be evacuated and can be filled with rare gas element or oxygen, it is characterized in that, this temperature control system comprises a plurality of heating members at least a portion that is arranged in this crucible outer wall and the computer system that is connected with described a plurality of heating members, described a plurality of heating member is along being divided into some groups on the direction of described crucible, this computer system is controlled every group of heating member in such a way, for the first group of heating member that on this direction, is positioned at the forefront and this crucible inner melt, corresponding to the first area of this first group of heating member, this first group of heating member continues the peripheral part of this first area of heating in the cooled and solidified process of this first area.
2. vacuum purifying furnace according to claim 1, it is characterized in that, for other group heating member and fused silicon/silicon dioxide of described first group of heating member back, corresponding other zone with it, described other group heating member of described computer system control makes described other zone keep molten state in the cooled and solidified process of described first area.
3. vacuum purifying furnace according to claim 2 is characterized in that, after the cooled and solidified of described first area, described computer system is controlled other group heating member that comes after described first group of heating member according to the mode identical with first group of heating member.
4. according to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that described heating member is resistance, electric arc generation part or solenoid.
5, vacuum purifying furnace according to claim 4 is characterized in that, described heating member is to arrange around mode.
6, according to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that described crucible is formed by highly purified quartz, silicon carbide or graphite.
7, vacuum purifying furnace according to claim 1 and 2 is characterized in that, described vacuum purifying furnace comprise be used for airtight this crucible, liftable or rotating bell jar.
8, vacuum purifying furnace according to claim 7 is characterized in that, is provided with water-cooled tube on described bell jar, and water coolant can circulate in this water-cooled tube.
9, vacuum purifying furnace according to claim 1, it is characterized in that, described temperature control system also comprises temp sensor device, described temp sensor device comprises a plurality of temperature sensors, described a plurality of temperature sensor is configured in the zone described outer wall, corresponding to each group heating member according to mode one to one, is used to survey near the temperature of the liquation described outer wall area.
10, vacuum purifying furnace according to claim 9 is characterized in that, described temperature sensor is the thermocouple meter.
11, according to Claim 8 or 9 described vacuum purifying furnaces, it is characterized in that described temp sensor device is connected with this computer system, so that the data that take off data and this computer system are set compare.
12, according to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that described computer system comprises many computers, described many computers are attached troops to a unit in described some groups of heating members with corresponded manner one by one.
13, vacuum purifying furnace according to claim 7 is characterized in that, is provided with tube stub that is used to vacuumize and the tube stub that is used for injecting inert gas or oxygen on described bell jar.
14, according to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that described rare gas element is a nitrogen.
According to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that 15, each regional speed of cooling of fused silicon/silicon dioxide is about 0.1 ℃/minute to 1 ℃/minute.
16, according to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that described computer system is calculated the heating power of respectively organizing heating member in the differential mode.
17, according to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that, described direction is the vertical direction of this crucible, described outer wall comprises perisporium and diapire at least, described a plurality of heating member is arranged on the described perisporium, and described first group of heating member be in the described some groups of heating members, that group heating member below coming on this vertical direction.
18, according to claim 1 or 2 or 3 described vacuum purifying furnaces, it is characterized in that described direction is the horizontal direction of this crucible, described outer wall comprises roof, diapire and perisporium, and described a plurality of heating members are arranged on described roof and the diapire at least.
19, vacuum purifying furnace according to claim 17 is characterized in that, the last zone that comes on described vertical direction of fused silicon/silicon dioxide is cut off the bottom after cooled and solidified.
20, vacuum purifying furnace according to claim 18 is characterized in that, the last zone that comes on described horizontal direction of fused silicon/silicon dioxide is cut off the bottom after cooled and solidified.
According to claim 19 or 20 described vacuum purifying furnaces, it is characterized in that 21, described vacuum purifying furnace can carry out purifying to same silicon material or earth silicon material repeatedly.
22, a kind of method of utilizing as each described vacuum purifying furnace purified metal silicon/silicon dioxide in the claim 1 to 21, this method comprises:
In crucible, insert silicon raw material/silica material;
Under the situation that vacuumizes and fill rare gas element or oxygen, utilize the heating system that has the temperature control system of controlling crucible temperature this crucible to be heated to more than the fusing point of silicon/silicon dioxide;
Utilize the computer system of this temperature control system, control being arranged in some groups of heating members on the crucible outer wall, that separate along a direction of crucible in such a way, for first group of heating member that on this direction, is positioned at the forefront and crucible inner melt, corresponding to the first area of this first group of heating member, this first group of heating member continues the peripheral part of this first area of heating in the cooled and solidified process of this first area.
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| CNA2007101965628A CN101240448A (en) | 2007-11-29 | 2007-11-29 | Vacuum purifying furnace specially used for metal silicon/silicon dioxide and purifying method thereof |
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| CNA2007101965628A CN101240448A (en) | 2007-11-29 | 2007-11-29 | Vacuum purifying furnace specially used for metal silicon/silicon dioxide and purifying method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775642A (en) * | 2010-03-04 | 2010-07-14 | 北京中联阳光科技有限公司 | Combined resistance heater and energy-saving heat field design for polycrystalline silicon ingot or purifying furnace |
| CN102492980A (en) * | 2011-12-16 | 2012-06-13 | 国电宁夏太阳能有限公司 | Method and device for preparing silicon cores for polycrystalline silicon deposition |
| WO2015100984A1 (en) * | 2013-12-31 | 2015-07-09 | 深圳市华星光电技术有限公司 | Coating machine crucible device |
| CN104928757A (en) * | 2015-07-16 | 2015-09-23 | 中国电子科技集团公司第四十六研究所 | Quick purification method for thermal insulation system of PVT method carbonization silicon single crystal furnace |
| CN108025917A (en) * | 2015-08-07 | 2018-05-11 | 派洛珍尼西斯加拿大公司 | The method that silica produces high purity silicon |
-
2007
- 2007-11-29 CN CNA2007101965628A patent/CN101240448A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775642A (en) * | 2010-03-04 | 2010-07-14 | 北京中联阳光科技有限公司 | Combined resistance heater and energy-saving heat field design for polycrystalline silicon ingot or purifying furnace |
| CN102492980A (en) * | 2011-12-16 | 2012-06-13 | 国电宁夏太阳能有限公司 | Method and device for preparing silicon cores for polycrystalline silicon deposition |
| CN102492980B (en) * | 2011-12-16 | 2014-07-23 | 国电宁夏太阳能有限公司 | Method and device for preparing silicon cores for polycrystalline silicon deposition |
| WO2015100984A1 (en) * | 2013-12-31 | 2015-07-09 | 深圳市华星光电技术有限公司 | Coating machine crucible device |
| CN104928757A (en) * | 2015-07-16 | 2015-09-23 | 中国电子科技集团公司第四十六研究所 | Quick purification method for thermal insulation system of PVT method carbonization silicon single crystal furnace |
| CN108025917A (en) * | 2015-08-07 | 2018-05-11 | 派洛珍尼西斯加拿大公司 | The method that silica produces high purity silicon |
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