CN101724890A - Method for effectively controlling carbon content in single crystal silicon - Google Patents
Method for effectively controlling carbon content in single crystal silicon Download PDFInfo
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- CN101724890A CN101724890A CN200910175320A CN200910175320A CN101724890A CN 101724890 A CN101724890 A CN 101724890A CN 200910175320 A CN200910175320 A CN 200910175320A CN 200910175320 A CN200910175320 A CN 200910175320A CN 101724890 A CN101724890 A CN 101724890A
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- monocrystalline silicon
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 85
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 49
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005204 segregation Methods 0.000 claims description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 2
- 229920005591 polysilicon Polymers 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 description 10
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 238000002231 Czochralski process Methods 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a method for effectively controlling carbon content in single crystal silicon. The method uses raw materials with different carbon contents by reasonable collocation, and average carbon content in each furnace charge is reasonably calculated before controlling single crystal silicon, thus greatly improving utilization ratio of secondary material, effectively controlling carbon content in single crystal silicon, saving production cost and improving economic benefit.
Description
Technical Field
The invention relates to a method for controlling the quality of a process in production, in particular to a method for effectively controlling the carbon content in a process of preparing monocrystalline silicon by a Czochralski process.
Background
Dislocation-free monocrystalline silicon grown by the Czochralski method is a main material of large-scale integrated circuits at home and abroad at present. Because the single crystal silicon furnace used by the Czochralski method consists of a quartz crucible and a graphite thermal system, the prepared single crystal silicon usually comprises 1-50 multiplied by 1016atoms/cm3The concentration of the impurity carbon is usually about 1 to 2 orders of magnitude higher than that of phosphorus or boron which is an impurity doped by artificially controlling the conductivity type and the conductivity of the crystal, wherein the carbon concentration at the tail of the monocrystalline silicon is the highest. It is well known that the presence of carbon is detrimental to single crystal silicon and not beneficial. For example, the presence of carbon can affect the change in lattice parameter in a silicon single crystal, which in turn affects the resistivity of the single crystal silicon; high carbon content can compromise the lattice integrity of single crystal silicon, resulting in poor PN junction characteristics. With the increase of the carbon content, the degradation phenomenon of the semiconductor device is accelerated, the breakdown voltage is reduced, and the yield of the device is reduced.
The problem with carbon content has been a problem with semiconductor single crystal silicon and research has been initiated for a long time. However, with the continuous development of large-scale integrated circuits, the requirements on the purity and the crystalline integrity of monocrystalline silicon become more and more strict, and therefore the task of controlling the carbon content in monocrystalline silicon is more and more urgent.
Chinese patent publication No. CN 1824848A provides a method for controlling the carbon content of silicon single crystal by adjusting the flow rate of inert gas, in which the parameters influencing the flow rate of inert gas are numerous, so the operation flow is very complicated and difficult to control. In addition, the tail carbon concentration of the drawn monocrystalline silicon product is high, so that the parameter difference of the monocrystalline silicon is large, no rule is needed, and the monocrystalline silicon needs to be cut off, so that the phenomenon of serious waste of secondary materials is caused.
Disclosure of Invention
The invention aims to solve the technical problems that the utilization rate of the secondary material is low and the carbon content of the monocrystalline silicon is difficult to control at present by reasonably matching and using the raw materials with different carbon contents, thereby achieving the purposes of improving the utilization rate of the secondary material and effectively controlling the carbon content of the monocrystalline silicon to achieve the quality control standard.
In order to solve the technical problems, the technical scheme adopted by the invention is to provide a method for effectively controlling the total carbon content in a monocrystalline silicon raw material, which comprises the following steps:
1) the carbon content C of each raw material used was measured and well documentediAccurately measuring the weight M of each raw materiali；
2) According to the formula C ═ C1×M1+C2×M2+C3×M3… …) x 0.07/rho M to make the carbon content less than 10 x 1016atoms/cm3；
Wherein: c is the carbon content of the raw materials1、C2、C3… … carbon content, M, of each raw material1、M2、M3… … are for different carbon contents C1、C2、C3… …, the segregation coefficient is 0.07, the rho is the density of silicon, and M is the total amount of the prepared raw materials;
3) putting the prepared raw materials into a monocrystalline silicon furnace, and heating and melting to pull up monocrystalline silicon;
4) measuring the carbon content of the top, middle and tail ends of the pulled monocrystalline silicon to obtain a monocrystalline silicon with a carbon content of more than 10 × 1016atoms/cm3The portion (A) is cut off and used as a raw material for pulling the single crystal silicon next time.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: by reasonably matching and using raw materials with different carbon contents, drawingThe average carbon content of raw materials in each furnace is reasonably calculated before the monocrystalline silicon, so that the carbon content of the prepared raw materials is controlled within an allowable range, the carbon content of the drawn monocrystalline silicon is effectively controlled, and the utilization rate of secondary materials is greatly improved. The carbon content of the drawing can be less than 5 x 10 in the production16atoms/cm3The silicon single crystal is improved from 47.40 percent of the original total number to 92.39 percent, and about 140Kg of silicon single crystal can be ensured to have carbon content of more than 10 multiplied by 10 per month16atoms/cm3Reduced to carbon content < 10X 1016atoms/cm3The quality of the drawn monocrystalline silicon is improved, the production cost is saved, and the economic benefit is improved.
Drawings
FIG. 1 is a graph of the carbon content distribution of single crystal silicon after the method of the present invention;
FIG. 2 is a graph of the carbon content of single crystal silicon prior to use of the method of the present invention;
wherein,
representing the number, - ●, representing the proportion of the total number.
Detailed Description
As can be seen from FIGS. 1 and 2, the yield of the drawn single crystal silicon is significantly improved by using the method for effectively controlling the carbon content in the single crystal silicon provided by the invention, and the drawn carbon content is less than 5 × 1016atoms/cm3The single crystal silicon is improved from 47.40 percent of the original total number to 92.39 percent, and the carbon content is more than 30 multiplied by 1016atoms/cm3The silicon single crystal is reduced from 25.00 percent of the original total growing number to 0.31 percent of the total growing number. The carbon content of the drawing is 5 x 1016atoms/cm3～10×1016atoms/cm3，10×1016atoms/cm3～20×1016atoms/cm3，20×1016atoms/cm3～30×1016atoms/cm3The number of the single crystal silicon in the range is reduced from 8.80%, 7.30% and 11.70% to 4.83%, 2.16% and 0.31%, respectively, based on the original total number of the single crystal silicon. Therefore, the method provided by the invention has strong practicability and creates high economic benefit.
The present invention will be described in further detail with reference to specific embodiments.
The method for effectively controlling the carbon content in the monocrystalline silicon comprises the following steps:
1) the carbon content C of each raw material used was measured and well documentediAccurately measuring the weight M of each raw materiali(ii) a They can be classified according to the carbon content of the raw material, and are preferably classified into three categories: the carbon content of the A-type raw material is less than or equal to 10 multiplied by 1016atoms/cm3，10×1016atoms/cm3The carbon content of < B raw material is less than or equal to 30 multiplied by 1016atoms/cm3C-based raw material with carbon content of more than 30X 1016atoms/cm3。
2) According to the formula C ═ C1×M1+C2×M2+C3×M3… …) x 0.07/rho M to make the carbon content less than 10 x 1016atoms/cm3；
Wherein: c is the carbon content of the raw materials1、C2、C3… … carbon content, M, of each raw material1、M2、M3… … are for different carbon contents C1、C2、C3… …, the segregation coefficient is 0.07, the rho is the density of silicon, and M is the total amount of the prepared raw materials;
3) putting the prepared raw materials into a monocrystalline silicon furnace, and heating and melting to pull up monocrystalline silicon;
4) measuring the carbon content of the top, middle and tail ends of the pulled monocrystalline silicon to obtain a monocrystalline silicon with a carbon content of more than 10 × 1016atoms/cm3The portion (A) is cut off and used as a raw material for pulling the single crystal silicon next time.
The following specific production control processes can be summarized:
testing the carbon content of the raw material by Nykuri 5700 infrared spectrometer, and testing the carbon content of the drawn monocrystalline silicon secondary material (namely the end cone body, the tail cone body and the carbon content of the monocrystalline silicon rod are more than 10 multiplied by 10)16atoms/cm3Silicon single crystal rod) and other raw materials (such as polysilicon) to establish a corresponding carbon content database, record the carbon content of each raw material in detail and classify the raw materials, wherein the preferred classification mode is divided into three types: the A-type raw material is less than or equal to 10 multiplied by 1016atoms/cm3，10×1016atoms/cm3Less than or equal to 30 multiplied by 10 of B raw material16atoms/cm3C-type raw material > 30X 1016atoms/cm3. And strictly recording carbon content data during testing, corrosion and rechecking procedures. Finally, when dosing, according to the formula C ═ C (C)1×M1+C2×M2+C3×M3… …). times.0.07/. rho.M, such that the calculated carbon content C meets the requirements for drawing a single crystal silicon product, Ci(i ═ 1, 2, 3 … …) is the carbon content of each raw material used, MiIs the weight of each raw material that is accurately measured. If not, the raw material with different carbon content can be replaced or other raw materials with carbon content increased until the calculated carbon content falls within the range required for pulling the single crystal silicon. The calculated carbon content value should be as small as possible in relation to the given desired value, since part of the carbon will also enter the monocrystalline silicon crystal during the actual drawing process due to oxidation of the thermal field elements in the monocrystalline silicon furnace.
And placing the prepared raw materials into a crucible and placing the crucible into a furnace, melting the raw materials at high temperature, and then placing seed crystals into the crucible to start to draw the monocrystalline silicon. Testing the carbon content of the top, middle and tail ends of the drawn monocrystalline silicon by using a Nile 5700 infrared spectrometer after the drawing is finished, and mainly testing the carbon content of the tail part of the monocrystalline silicon to ensure that the carbon content is more than 10 multiplied by 10 because the carbon is mainly deposited on the tail part of the drawn monocrystalline silicon16atoms/cm3Is partially cut off and recordedThe carbon content is good for use as a raw material for pulling the single crystal silicon next time. The top and tail of the drawn silicon single crystal rod are both conical bodies, and the part cannot be used as a finished product, so the part needs to be cut off, listed as a secondary monocrystalline silicon material and used as a raw material for drawing the monocrystalline silicon next time.
Claims (4)
1. A method for effectively controlling the carbon content in monocrystalline silicon is characterized by comprising the following steps:
1) the carbon content C of each raw material used was measured and well documentediAccurately measuring the weight M of each raw materiali；
2) According to the formula C ═ C1×M1+C2×M2+C3×M3… …) x 0.07/rho M to make the carbon content less than 10 x 1016atoms/cm3；
Wherein: c is aCarbon content of the ingredients, C1、C2、C3… … carbon content, M, of each raw material1、M2、M3… … are for different carbon contents C1、C2、C3… …, the segregation coefficient is 0.07, the rho is the density of silicon, and M is the total amount of the prepared raw materials;
3) putting the prepared raw materials into a monocrystalline silicon furnace, and heating and melting to pull up monocrystalline silicon;
4) measuring the carbon content of the top, middle and tail ends of the pulled monocrystalline silicon to obtain a monocrystalline silicon with a carbon content of more than 10 × 1016atoms/cm3The portion (A) is cut off and used as a raw material for pulling the single crystal silicon next time.
2. The method of claim 1, wherein the starting materials comprise: polysilicon or a sub-charge or a combination of both.
3. Method for efficiently controlling the carbon content in single crystal silicon according to claim 1, characterized in that the raw materials are classified before batching according to their carbon content, preferably into three categories: the carbon content of the A-type raw material is less than or equal to 10 multiplied by 1016atoms/cm3，10×1016atoms/cm3The carbon content of < B raw material is less than or equal to 30 multiplied by 1016atoms/cm3C-based raw material with carbon content of more than 30X 1016atoms/cm3；
4. The method for effectively controlling the carbon content in single crystal silicon according to claim 1, wherein the instrument used for measuring the carbon content is a Nidok 5700 infrared spectrometer.
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| CN200910175320A CN101724890A (en) | 2009-12-14 | 2009-12-14 | Method for effectively controlling carbon content in single crystal silicon |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
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Application publication date: 20100609 |