CN103397389A - Production method of monocrystal rods - Google Patents
Production method of monocrystal rods Download PDFInfo
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- CN103397389A CN103397389A CN2013103270972A CN201310327097A CN103397389A CN 103397389 A CN103397389 A CN 103397389A CN 2013103270972 A CN2013103270972 A CN 2013103270972A CN 201310327097 A CN201310327097 A CN 201310327097A CN 103397389 A CN103397389 A CN 103397389A
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Abstract
The invention provides a production method of monocrystal rods. The production method comprises the following steps of S10, adding the first batch of silicon materials into a crucible, heating the crucible to melt the first batch of silicon materials, then, crystallizing the first batch of molten silicon materials to obtain a first monocrystal rod, and taking out the first monocrystal rod; and S20, adding a second batch of silicon materials into the crucible, heating the crucible to melt the second batch of silicon materials, and then, crystallizing the molten second batch of silicon materials to obtain a second monocrystal rod. By using the production method of monocrystal rods, provided by the invention, the utilization ratio of the crucible is increased, and furthermore, the production cost of the monocrystal rods is reduced.
Description
Technical field
The present invention relates to the single crystal rod production technical field, in particular to a kind of production method of single crystal rod.
Background technology
At present, the production process of single crystal rod is mainly: the solid silicon material is placed in crucible, and the crucible that then is contained with the solid silicon material is put into the working spaces of single crystal growing furnace, and realizes generating the process of single crystal rod at single crystal growing furnace.Single crystal growing furnace is divided into working spaces and concubine substantially, and concubine is positioned at the top of working spaces, and the sealing that arranges in single crystal growing furnace cuts off working spaces and concubine are separated.After a single crystal rod generates, crucible is taken out in single crystal growing furnace.Due to will be broken after crucible is from the high temperature cooling to normal temperature, that is to say, taking out in single crystal growing furnace after, crucible can't continue to be suitable for the crucible that therefore can only more renew and the production process that repeats above-mentioned single crystal rod.From the above, produce a single crystal rod and just need to consume a crucible.At present, the cost of crucible is also the part of single crystal rod production cost, therefore, reduces the quantity that consumes crucible and also just reduced the production cost of single crystal rod in the production process of single crystal rod.
At present, there is a kind of method of composite feeding-material can reduce the cost of crucible.Particularly, the crucible that is contained with the solid silicon material is put into single crystal growing furnace, when the temperature and pressure in the working spaces of the whole fusings of solid silicon material and single crystal growing furnace was stablized, the liquid level of liquid silicon material can be starkly lower than the aperture position of crucible.This is due to after crucible holds full solid silicon material, has gap between each solid silicon material, and after the solid silicon material was fused into liquid, the liquid level of liquid silicon material can be starkly lower than the aperture position of crucible.Then, the feeder that is contained with the solid silicon material is moved to working spaces from concubine, and by feeder to throwing in the solid silicon material in crucible, the solid silicon material of throwing in best in quality is can be with the liquid level of liquid silicon material concordant with the aperture position of crucible or slightly lower than the aperture position of crucible.Aforesaid method has increased the liquid silicon material that holds in crucible, that is to say, has increased and has promoted the silicon material that single crystal rod is used, and then increased the weight of the single crystal rod that promotes.Therefore, consumed the mass penalty of the single crystal rod that a crucible promotes, improved the rate of utilization of crucible, and then reduced the production cost of single crystal rod.
Summary of the invention
The present invention aims to provide and a kind ofly can improve the production method of crucible rate of utilization with the single crystal rod of the production cost that reduces single crystal rod.
To achieve these goals, the invention provides a kind of production method of single crystal rod, comprise the following steps: step S10: drop into first silicon material in crucible, heating crucible is to melt first silicon material, then make first silicon material crystallization after fusing to obtain first single crystal rod, and take out first single crystal rod, further comprising the steps of after step S10: step S20: drop into second batch silicon material in crucible, and heating crucible is with fusing second batch silicon material, then makes second batch silicon material crystallization after fusing to obtain second single crystal rod.
Further, to further comprising the steps in the step that drops into second batch silicon material in crucible: second batch silicon material is joined in feeder, then once or several times drop in crucible by feeder, when dropping into several times, have the timed interval between each the input.
Further, in step S20, second batch silicon material is divided and drops in crucible for three times by feeder.
Further, in step S20, the weight of throwing in for the first time and for the second time the silicon material in three inputs is all in the scope of 10KG to 15KG.
Further, drop into second batch silicon material in crucible before, the quality of first silicon material in crucible after remaining fusing is greater than 25KG.
Further, in step S20, the following steps operation is repeated one or many: second batch silicon material is joined in feeder and with second batch silicon material and puts in crucible.
further, step S20 is further comprising the steps: second batch silicon material is added in feeder and the operation that second batch silicon material is put into crucible is repeated once, the second batch silicon material of putting into for the first time the second batch silicon material of feeder and putting into for the second time feeder is all dropped into several times in crucible, has the timed interval between each the input, the impressions of putting into for the second time the second batch silicon material of feeder equates with the impressions of the second batch silicon material of putting into for the first time feeder, the weight of putting into for the second time each time input in the weight of each time input in the second batch silicon material of feeder and the second batch silicon material of putting into for the first time feeder is correspondent equal one by one, the interval time of putting into for the second time adjacent twice input in the interval time of adjacent twice input in the second batch silicon material of feeder and the second batch silicon material of putting into for the first time feeder is correspondent equal one by one.
Further, when dropping into second batch silicon material in crucible, the distance of the placement position of second batch silicon material and the silicon feed liquid face in crucible remains in predetermined scope.
Further, at second batch silicon material, drop in the process of crucible, the lowering speed by controlling crucible remains in predetermined scope with the placement position that realizes second batch silicon material and the distance of the silicon feed liquid face in crucible.
Further, also comprise following operation after obtaining second single crystal rod: repeating step S20 is to obtain many single crystal rod, wherein, first to before dropping into second batch silicon material in crucible, the quality of the remaining second batch silicon material in crucible is all greater than 25KG in each step S20 that repeats.
Apply technical scheme of the present invention, after producing first single crystal rod, in crucible, seldom, most of liquid-state silicon material exist with the form that sticks to the crucible inwall remaining liquid-state silicon material.Therefore, the space in crucible is larger, almost is equivalent to a crucible that does not hold the silicon material, can be very large to the weight of input second batch silicon material in crucible.Because the weight of the second batch silicon material that melts in crucible is very large, therefore, the quality of second single crystal rod of production can reach the weight that is approximately equal to first single crystal rod.As shown in the above, adopt the quality sum of the single crystal rod that method of the present invention produces larger, that is to say, the weight sum of applying the single crystal rod that same crucible produces is larger, therefore, the production method of the single crystal rod of the present embodiment has improved the rate of utilization of crucible, and then has reduced the production cost of single crystal rod.The production method of single crystal rod of the present invention has improved the rate of utilization of crucible, and then has reduced the production cost of single crystal rod.
Description of drawings
The Figure of description that forms the application's a part is used to provide a further understanding of the present invention, and illustrative examples of the present invention and explanation thereof are used for explaining the present invention, do not form improper restriction of the present invention.In the accompanying drawings:
Fig. 1 shows the schematic flow sheet according to the embodiment of the production method of single crystal rod of the present invention.
Embodiment
Need to prove, in the situation that do not conflict, embodiment and the feature in embodiment in the application can make up mutually.Describe below with reference to the accompanying drawings and in conjunction with the embodiments the present invention in detail.
As shown in Figure 1, the production method of the single crystal rod of the present embodiment comprises the following steps:
Step S10: to dropping into first silicon material in crucible, heating crucible to be to melt first silicon material, then makes first silicon material crystallization after fusing to obtain first single crystal rod, and takes out first single crystal rod.
Step S20: to dropping into second batch silicon material in crucible, and heating crucible is with fusing second batch silicon material, then makes second batch silicon material crystallization after fusing to obtain second single crystal rod.
The technical scheme of application the present embodiment, after producing first single crystal rod, in crucible, remaining liquid-state silicon material seldom, exists mainly with the form that sticks to the crucible inwall greatly.Therefore, the space in crucible is larger, almost is equivalent to a crucible that does not hold the silicon material, can be very large to the weight of input second batch silicon material in crucible.Because the weight of the second batch silicon material that melts in crucible is very large, therefore, the quality of second single crystal rod of production can reach the weight that is approximately equal to first single crystal rod.As shown in the above, the quality sum of the single crystal rod that the method for employing the present embodiment is produced is larger, that is to say, the weight sum of applying the single crystal rod that same crucible produces is larger, therefore, the production method of the single crystal rod of the present embodiment has improved the rate of utilization of crucible, and then has reduced the production cost of single crystal rod.
As shown in Figure 1, in the present embodiment, to further comprising the steps in the step that drops into second batch silicon material in crucible: second batch silicon material is joined in feeder, then by feeder, drop in crucible several times, have the timed interval between each the input.The second batch silicon material gradation that joins in feeder is put in crucible, can be reduced the time that the second batch silicon material in above-mentioned feeder melts fully.Particularly, when throwing in for the N time (N is the integer greater than 1), the fusing of part second batch silicon material may be arranged in crucible, solid-state second batch silicon material is more easily fusing in liquid second batch silicon material, even when throwing in for the N time, the solid-state second batch silicon material in crucible is all less than fusing, but the heat of the absorption of the solid-state second batch silicon material in crucible is many, still can transfer heat to the second batch silicon material of the N time input, the time of having accelerated equally second batch silicon material melt-through.Like this, not only saved the time, and can save the electric energy that heating unit consumes, saved cost.Certainly,, as feasible embodiment, also can all drop in crucible in feeder, second batch silicon material is disposable.
In the step S20 of the present embodiment, second batch silicon material is divided and drops in crucible for three times from feeder.Consider the environment of working spaces of single crystal growing furnace and the composite factor of the silicon material quality that existing feeder can carry, the contriver is by specifically testing discovery, and it is more reasonable that the second batch silicon material that feeder is carried is divided into three inputs.
In the present embodiment, the weight of throwing in for the first time of the second batch silicon material in the above-mentioned feeder of step S20 is 13 with the weight of throwing in for the second time, certainly, also can select between 10 to 15KG.At present, the maximum bearing capacity of feeder is the 35KG left and right, and the weight of the weight of throwing in for the first time and input for the second time all in 10 to 15KG scope, is all rendered to the quality of feeder excess silicon material in crucible.Aforesaid way can further reduce the fusing time of second batch silicon material in step S20.Adopt aforesaid way to throw in through experiment showed,, it is about 40 minutes that the second batch silicon material of 35KG melts the needed time fully.If directly with disposable the rendering in crucible of second batch silicon material of 35KG, it is about 70 minutes that second batch silicon material melts the needed time fully, when there is no first silicon material of remaining liquid in crucible, directly with disposable the rendering in crucible of second batch silicon material of 35KG, it is about 5 to 6 hours that second batch silicon material melts the needed time fully.
In the present embodiment, drop into second batch silicon material in crucible before, the quality of first silicon material in crucible after remaining fusing is greater than 25KG.Due to residue first silicon material more than 25KG in crucible, second batch silicon material and liquid first silicon material mix mutually have been accelerated second batch silicon material and has all melted, and has saved the time that second batch silicon material melts.In crucible, the weight of first silicon material of remaining liquid can record by the weighing device that is arranged on crucible bottom.
In the present embodiment, the working spaces of single crystal growing furnace carries out step S20 under the following conditions, and the power range of heating unit is 85 to 95KW.The contriver found through experiments the condition saves energy to greatest extent of the working spaces of above-mentioned single crystal growing furnace.
In the step S20 of the present embodiment, the following steps operation is repeated once: second batch silicon material is joined feeder and second batch silicon material is put in crucible.By aforesaid operations, can throw in more second batch silicon material in crucible, and then the heavier single crystal rod of the quality of production, further reduce production costs.In addition, in repeating second batch silicon material to be joined feeder and second batch silicon material put into the operation of crucible, liquid second batch silicon material in crucible is many, accelerated the burn-off rate of second batch silicon material in crucible that above-mentioned repetition adds to feeder, saved the production time, and then enhanced productivity.Certainly, above-mentioned steps also can repeatedly, can increase the weight of the second batch silicon material that melts in crucible like this.
in the present embodiment, step S20 is further comprising the steps: second batch silicon material is added in feeder and the operation that second batch silicon material is put into crucible is repeated once, the second batch silicon material of putting into for the first time the second batch silicon material of feeder and putting into for the second time feeder is all dropped into several times in crucible, has the timed interval between each the input, the impressions of putting into for the second time the second batch silicon material of feeder equates with the impressions of the second batch silicon material of putting into for the first time feeder, the weight of putting into for the second time each time input in the weight of each time input in the second batch silicon material of feeder and the second batch silicon material of putting into for the first time feeder is correspondent equal one by one, the interval time of putting into for the second time adjacent twice input in the interval time of adjacent twice input in the second batch silicon material of feeder and the second batch silicon material of putting into for the first time feeder is correspondent equal one by one.Prove by experiment, the above-mentioned impressions of putting into for the second time the second batch silicon material of feeder is three times, the weight of throwing in for the first time is 10 to 15KG with the weight of throwing in for the second time, the quality of feeder excess silicon material is all rendered in crucible, altogether thrown in the required fusing time of 35KG second batch silicon material about 20 minutes in crucible.If the above-mentioned disposable interior required fusing time of crucible of rendering to of 35KG second batch silicon material of feeder of putting into for the second time is about 35 minutes.
In order to prevent that when throwing in second batch silicon material in crucible, the liquid-state silicon material of crucible splashes to outside crucible, therefore, the placement position of silicon material (namely feeder) the silicon feed liquid face in close crucible of should try one's best.But because the temperature of liquid-state silicon material in crucible is very high, feeder, near the silicon feed liquid face in crucible, can cause the feeder fusing, causes and can't produce.To sum up, through the contriver, test discovery, while dropping into second batch silicon material in crucible, the distance of the placement position of silicon material and the silicon feed liquid face in crucible remains in 160 to 250mm pre-determined range.Proof, neither can splash to outside crucible by the liquid-state silicon material in above-mentioned scope by experiment, also can not make the feeder fusing.
In the present embodiment, at second batch silicon material, drop in the process of crucible, the lowering speed by controlling crucible remains in predetermined scope with the placement position that realizes second batch silicon material and the distance of the silicon feed liquid face in crucible.Particularly, input speed is 65KG/min to 75KG/min and crucible uniform descent, and dropping speed of the crucible is 290mm/min to 310mm/min, and wherein, while stopping throwing in, crucible stops descending.When being in repeatedly the timed interval between input, crucible temporarily stops descending.Aforesaid way can safe and reliablely must realize that the distance of the placement position of silicon material and the silicon feed liquid face in crucible remains in 160 to 250mm scope.The calculating of input speed is determined by be connected weighing device and timing register with feeder.In addition, input speed is 65KG/min to 75KG/min under the prerequisite that guarantees comparatively fast to make second batch silicon material to melt fully, reduces the total time of throwing in.
In the present embodiment, also comprise following operation after obtaining second single crystal rod: repeating step S20 is to obtain many single crystal rod, wherein, first to before dropping into second batch silicon material in crucible, the quality of the remaining second batch silicon material in crucible is all greater than 25KG in each step S20 that repeats.Aforesaid way, realize the repeatedly recycling of crucible, the duration of service of further having improved crucible, reduced the production cost of manufacture order crystal bar.
Preferably,, in order further to improve the rate of utilization of crucible, reduce production costs.Step S10 in, drop into first certain silicon material after first silicon material fusing in crucible so that in crucible the liquid level of liquid-state silicon material rise, increase the quality that produces first single crystal rod.
As follows according to the application's preferred embodiment:
Step S10 is same as the previously described embodiments, before carry out step 20, and the liquid-state silicon material of residue 25KG in crucible.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. the production method of a single crystal rod comprises the following steps:
Step S10:, to dropping into first silicon material in crucible, heat described crucible to melt described first silicon material, then make described first silicon material crystallization after fusing to obtain first single crystal rod, and take out described first single crystal rod,
It is characterized in that, further comprising the steps of after step S10:
Step S20: to dropping into second batch silicon material in described crucible, and heat described crucible to melt described second batch silicon material, then make described second batch silicon material crystallization after fusing to obtain second single crystal rod.
2. the production method of single crystal rod according to claim 1, is characterized in that, and is further comprising the steps in described step to dropping into second batch silicon material in described crucible:
Described second batch silicon material is joined in feeder, then by described feeder, once or several times drop in described crucible, when dropping into several times, have the timed interval between each the input.
3. the production method of single crystal rod according to claim 2, is characterized in that, in described step S20, described second batch silicon material divided and drops in described crucible for three times by described feeder.
4. the production method of single crystal rod according to claim 3, is characterized in that, in described step S20, the weight of throwing in for the first time and for the second time the silicon material in described three inputs is all in the scope of 10KG to 15KG.
5. the production method of single crystal rod according to claim 1, is characterized in that, drop into second batch silicon material in described crucible before, the quality of described first silicon material in described crucible after remaining fusing is greater than 25KG.
6. the production method of single crystal rod according to claim 2, is characterized in that, in described step S20, the following steps operation repeated one or many:
Described second batch silicon material is joined in described feeder and with described second batch silicon material and puts in described crucible.
7. the production method of single crystal rod according to claim 6, is characterized in that, described step S20 is further comprising the steps:
add described second batch silicon material in described feeder and the operation that described second batch silicon material is put into described crucible repeats once, the second batch silicon material of putting into for the first time the second batch silicon material of feeder and putting into for the second time feeder is all dropped into several times in described crucible, has the timed interval between each the input, the described impressions of putting into for the second time the second batch silicon material of feeder equates with the impressions of the second batch silicon material of putting into for the first time feeder, the weight of each time input correspondent equal one by one in the weight of each time input and the described second batch silicon material of putting into for the first time feeder in the described second batch silicon material of putting into for the second time feeder, in the described second batch silicon material of putting into for the second time feeder in the interval time of adjacent twice input and the described second batch silicon material of putting into for the first time feeder the interval time of adjacent twice input correspondent equal one by one.
8. the production method of the described single crystal rod of any one according to claim 1 to 7, it is characterized in that, when dropping into described second batch silicon material in described crucible, the distance of the placement position of described second batch silicon material and the silicon feed liquid face in described crucible remains in predetermined scope.
9. the production method of single crystal rod according to claim 8, it is characterized in that, drop in the process of crucible at described second batch silicon material, the lowering speed by controlling crucible remains in predetermined scope with the placement position that realizes second batch silicon material and the distance of the silicon feed liquid face in described crucible.
10. the production method of the described single crystal rod of any one according to claim 1 to 7, is characterized in that, also comprises following operation after obtaining described second single crystal rod:
Repeating said steps S20 to be to obtain many single crystal rod, and wherein, first to before dropping into described second batch silicon material in described crucible, the quality of the remaining second batch silicon material in described crucible is all greater than 25KG in each described step S20 that repeats.
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| CN201310327097.2A CN103397389B (en) | 2013-07-30 | 2013-07-30 | The production method of monocrystal rod |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585838A (en) * | 2001-11-15 | 2005-02-23 | Memc电子材料有限公司 | Intermittent feeding technique for increasing the melting rate of polycrystalline silicon |
| CN1696355A (en) * | 2004-05-11 | 2005-11-16 | 上海卡姆丹克半导体有限公司 | Technical method for drawing silicon single-crystal |
| EP2267188A1 (en) * | 2008-04-25 | 2010-12-29 | SUMCO Corporation | Single-crystal growth apparatus and raw-material supply method |
| CN102345157A (en) * | 2011-10-09 | 2012-02-08 | 内蒙古中环光伏材料有限公司 | Continuous re-feeding production method of solar-grade Czochralski silicon |
| CN103074681A (en) * | 2013-02-17 | 2013-05-01 | 英利集团有限公司 | Secondary feeding method |
-
2013
- 2013-07-30 CN CN201310327097.2A patent/CN103397389B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585838A (en) * | 2001-11-15 | 2005-02-23 | Memc电子材料有限公司 | Intermittent feeding technique for increasing the melting rate of polycrystalline silicon |
| CN1696355A (en) * | 2004-05-11 | 2005-11-16 | 上海卡姆丹克半导体有限公司 | Technical method for drawing silicon single-crystal |
| EP2267188A1 (en) * | 2008-04-25 | 2010-12-29 | SUMCO Corporation | Single-crystal growth apparatus and raw-material supply method |
| CN102345157A (en) * | 2011-10-09 | 2012-02-08 | 内蒙古中环光伏材料有限公司 | Continuous re-feeding production method of solar-grade Czochralski silicon |
| CN103074681A (en) * | 2013-02-17 | 2013-05-01 | 英利集团有限公司 | Secondary feeding method |
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