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CN102557693B - Composite material for preparing crucible and application of composite material - Google Patents

Composite material for preparing crucible and application of composite material Download PDF

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Publication number
CN102557693B
CN102557693B CN 201210056374 CN201210056374A CN102557693B CN 102557693 B CN102557693 B CN 102557693B CN 201210056374 CN201210056374 CN 201210056374 CN 201210056374 A CN201210056374 A CN 201210056374A CN 102557693 B CN102557693 B CN 102557693B
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crucible
matrix material
quartz
composite material
organic dispersing
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CN102557693A (en
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倪道宏
吕铁铮
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Jiangsu Uonone Optoelectronics Technology Co., Ltd.
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JIANGSU UONONE OPTOELECTRONICS TECHNOLOGY Co Ltd
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Abstract

The invention provides a composite material for preparing a crucible. The composite material for preparing the crucible comprises quartz, an organic dispersing agent, a suspending agent and a nano material, wherein the mass percentage content of the quartz, the organic dispersing agent and the suspending agent is 90 to 99.9 percent; the mass ratio of the quartz to the organic dispersing agent to the suspending agent is (25-100):1:1; and the mass percentage content of the nano material is 0.1 to 10 percent. The invention also provides an application of the composite material. The crucible prepared by the composite material overcomes the defects of the traditional crucibles and has a good market application prospect.

Description

Matrix material of a kind of spare-crucible and uses thereof
Technical field
The present invention relates to a kind of matrix material, particularly a kind of matrix material of spare-crucible.
Background technology
In the photovoltaic generation industry, along with the continuous development of crystal silicon solar photovoltaic industry, maturation, whole cost constantly reduces, and the silicon chip price of industrial chain upper end in the falling of the rational faculty, has also caused the continuous compression of silicon substrate manufacturer profit margin simultaneously gradually.Improve the substrate quality, cutting down finished cost becomes the problem of pendulum in face of all solar silicon wafers manufacturers, is solidified because cost is low, and output is big by the polycrystalline typing that heat-exchanging method grows up, and has become the mainstream technology that silicon chip is produced.As its name suggests, in the directional freeze process of polycrystalline ingot casting, silicon melt is melted quartz crucible and loads, and after crystal growth began, heat was derived from crucible bottom, form vertical thermograde, thereby the directional freeze of melt began from the bottom up.Yet, quartz crucible is the poor conductor of heat, and because of quartz crucible be injection forming to cause the density pattern be not uniformity, therefore, the thermal properties of crucible bottom and sidepiece can't accurately be controlled, in most cases the thermal conductive property of crucible bottom and sidepiece is because thickness is approaching, its thermal conductive property is approaching substantially, and it solidifies the inside edge that at first occurs in crucible in the long brilliant primary stage, becomes the growth of certain inclined-plane then to inside, forming an interface that is similar to W, is not directional freeze truly.
In order to realize that vertical orientation solidifies to the full extent, need the bottom of crucible and sidepiece to have different thermal conductivities, namely require the crucible bottom thermal conductivity greater than its sidepiece thermal conductivity specifically, thereby make that the hot-fluid that produces in the crystal growing process can vertical conduction.Appolon solar has designed a kind of novel crucible structure, makes its bottom be very different with sidepiece thermal conductivity tool, and its bottom is made up of transparent crystal quartz glass, and its sidepiece then adopts normal nontransparent fused quartz.Although this scheme has reached design effect, it adopts two kinds of different quartz materials, has increased the crucible production cost, and has reduced the success ratio of producing.
Therefore, need the searching additive method badly, guaranteeing that crucible produces on the basis of power, improve the thermal conductivity of crucible.
Summary of the invention
In order to address the above problem, the invention provides a kind of matrix material of new spare-crucible.
At first, the invention provides a kind of matrix material of spare-crucible, it comprises quartz, organic dispersing agent, suspension agent and nano material, the quality percentage composition of quartz, organic dispersing agent and suspension agent is 10~99.9%, the mass ratio of quartz, organic dispersing agent and suspension agent is 25~100: 1: 1, the quality percentage composition of nano material was 0.1~10%.
Wherein, described quartz is glass sand.
Wherein, described organic dispersing agent is the polyacrylamide material.
Wherein, described suspension agent is mineral oil.
Wherein, described nano material is carbon nanotube.
Wherein, the mass ratio of described quartz material, organic dispersing agent and suspension agent is 99: 1: 1.
Wherein, the quality percentage composition of nano material is 0.5%.
The present invention also provides the purposes of aforementioned matrix material in spare-crucible.
The invention provides the Composite Preparation quartz crucible can regulate its thermal conductivity, both can improve heating efficiency, can improve the radiating efficiency of crucible bottom again, greatly improved the directional solidification effect of silicon melt, thereby improve the weight of silicon crystal growth, reduce the cost of crystalline silicon photovoltaic generating.
Obviously, according to foregoing of the present invention, according to ordinary skill knowledge and the customary means of this area, not breaking away under the above-mentioned basic fundamental thought of the present invention prerequisite, can also make modification, replacement or the change of other various ways.
The embodiment of form is described in further detail foregoing of the present invention again by the following examples.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following example.All technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Embodiment
Embodiment 1 usefulness Composite Preparation crucible provided by the invention
1, preparation method
(1) preparation of matrix material
Get glass sand (purity of quartz sand is 99.99%), polyacrylamide material, mineral oil, mix at 25: 1: 1 with mass ratio, get quartzy slurry, add carbon nanotube again, mixing, the weight percent 99.9% of quartzy slurry, the weight percent of carbon nanotube is 0.1%, namely gets matrix material of the present invention.
(2) preparation of crucible
Secondary grouting: get quartzy slurry and the matrix material of step (1) preparation, matrix material is injected mould in advance, fill up the crucible die bottom, the height that the quartzy slurry that reinjects, slurry are filled into crucible die to be needed gets final product.This kind grouting mode can realize that the thermal conductivity of crucible bottom is higher than the thermal conductivity of sidepiece.
Perhaps, once grouting: get the matrix material of step (1) preparation, matrix material is injected mould, the height that being filled into crucible die needs gets final product.
Embodiment 2 usefulness Composite Preparation crucible provided by the invention
1, preparation method
(1) preparation of matrix material
Get glass sand (purity of quartz sand is 99.99%), polyacrylamide material, mineral oil, mix at 99: 1: 1 with mass ratio, get quartzy slurry, add carbon nanotube again, mixing, the weight percent 99.5% of quartzy slurry, the weight percent of carbon nanotube is 0.5%, namely gets matrix material of the present invention.
(2) preparation of crucible
Secondary grouting: get quartzy slurry and the matrix material of step (1) preparation, matrix material is injected mould in advance, fill up the crucible die bottom, the height that the quartzy slurry that reinjects, slurry are filled into crucible die to be needed gets final product.This kind grouting mode can realize that the thermal conductivity of crucible bottom is higher than the thermal conductivity of sidepiece.
Perhaps, once grouting: get the matrix material of step (1) preparation, matrix material is injected mould, the height that being filled into crucible die needs gets final product.
Embodiment 3 usefulness Composite Preparation crucible provided by the invention
1, preparation method
(1) preparation of matrix material
Get glass sand (purity of quartz sand is 99.99%), polyacrylamide material, mineral oil, mix at 100: 1: 1 with mass ratio, get quartzy slurry, add carbon nanotube again, mixing, the weight percent 90% of quartzy slurry, the weight percent of carbon nanotube is 10%, namely gets matrix material of the present invention.
(2) preparation of crucible
Secondary grouting: get quartzy slurry and the matrix material of step (1) preparation, matrix material is injected mould in advance, fill up the crucible die bottom, the height that the quartzy slurry that reinjects, slurry are filled into crucible die to be needed gets final product.This kind grouting mode can realize that the thermal conductivity of crucible bottom is higher than the thermal conductivity of sidepiece.
Perhaps, once grouting: get the matrix material of step (1) preparation, matrix material is injected mould, the height that being filled into crucible die needs gets final product.
After using the crucible moulding of Composite Preparation of the present invention, its thermal conductivity can be greatly improved, in the polycrystalline silicon ingot casting process, can shorten the thawing time of polysilicon greatly, can also realize that with the crucible that the secondary grouting mode prepares the vertical orientation of silicon ingot solidifies.
In order to further specify beneficial effect of the present invention, now provide following experiment:
Crucible thickness is generally 880 * 880 millimeters, it highly is the 420-480 millimeter, under so big size, be difficult to carry out the measurement of thermal conductivity, but the thermal conductivity difference of crucible, be equipped with under the situation of identical silicon material, it is also different that the silicon material melts the required time fully, therefore, can melt the thermal conductivity of speed and whole technology required time judgement crucibles according to the silicon material.
1, experimental technique
(1) gets the not matrix material of quartzy slurry, embodiment 1 and embodiment 2 preparations of carbon nanotubes, the crucible of preparation same model;
(2) the silicon material of adding identical weight in three kinds of crucibles of step (1) preparation early, heating power is identical, detects the thawing time of silicon material.
2, experimental result
Detected result is as shown in table 1:
The thermal conductivity detected result of the different crucibles of table 1
Figure BDA0000141020450000041
As can be seen from Table 1, the group two that adds carbon nanotube, group three and organize four and compare with the group one that does not add carbon nanotube, silicon material thawing time and whole process time obviously shorten, when content of carbon nanotubes 10% when following, silicon material thawing time and whole process time shorten along with the increase of content of carbon nanotubes, wherein, content of carbon nanotubes is 0.1% and 0.5% o'clock, it is remarkable that silicon material thawing time and whole process time shorten amplitude, but when the content of carbon nanotube increases to 10%, it is not obvious that silicon material thawing time and whole process time shorten amplitude, and particularly content of carbon nanotubes increases at 30% o'clock, and crucible can't moulding.
Experimental results show that, in the matrix material of the present invention, when content of carbon nanotubes 10% when following, thermal conductivity improves with the increase of content of carbon nanotubes, but it changes with content of carbon nanotubes is not linear, when content of carbon nanotubes approached or reaches 10%, thermal conductivity and content of carbon nanotubes were suitable 0.5% o'clock thermal conductivity.When content of carbon nanotubes surpasses 10%, reach at 30% o'clock, crucible namely can't moulding.
In actual applications, because of carbon nanotube price height, take into account thermal conductivity and the production cost of crucible, the content of carbon nanotube is preferably 0.5% in the matrix material of the present invention.
To sum up, matrix material provided by the invention can improve the thermal conductivity of crucible, can also realize that with the crucible that the secondary grouting mode prepares the vertical orientation of silicon ingot solidifies, the crucible of Composite Preparation of the present invention is used for the thawing time that polycrystalline silicon ingot casting can shorten polysilicon greatly, reduce production costs significantly, have favorable industrial application prospect.

Claims (1)

1. the matrix material of a spare-crucible, it is characterized in that: it comprises quartz, organic dispersing agent, suspension agent and nano material, the quality percentage composition of quartz, organic dispersing agent and suspension agent is 10 ~ 99.9%, the mass ratio of quartz, organic dispersing agent and suspension agent is 25 ~ 100:1:1, and the quality percentage composition of nano material is 0.1 ~ 10%; Described nano material is carbon nanotube.
2, matrix material according to claim 1 is characterized in that: described quartz is glass sand.
3, matrix material according to claim 1 is characterized in that: described organic dispersing agent is the polyacrylamide material.
4, matrix material according to claim 1 is characterized in that: described suspension agent is mineral oil.
5, matrix material according to claim 1 is characterized in that: the mass ratio of described quartz material, organic dispersing agent and suspension agent is 99:1:1.
6, matrix material according to claim 1 is characterized in that: the quality percentage composition of nano material is 0.5%.
7, the purposes of any described matrix material of claim 1-6 in spare-crucible.
CN 201210056374 2012-03-06 2012-03-06 Composite material for preparing crucible and application of composite material Expired - Fee Related CN102557693B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105088340A (en) * 2015-09-06 2015-11-25 江苏协鑫硅材料科技发展有限公司 Crucible and preparation method thereof
CN106966711B (en) * 2016-01-14 2019-09-03 杭州大和江东新材料科技有限公司 A method of improving quartz sand slurry suspension
CN107986769B (en) * 2017-12-13 2021-06-15 苏州浩焱精密模具有限公司 Preparation method of quartz crucible mold

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1522230A (en) * 2001-03-08 2004-08-18 赫罗伊斯石英玻璃股份有限两合公司 Method of producing a quartz glass crucible
CN1789204A (en) * 2004-12-17 2006-06-21 德国贝格有限公司 Herbst bremer goldschlaegerei

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19541372A1 (en) * 1994-11-15 1996-05-23 Gen Electric Mfg. quartz crucible for Czochralski semiconductor crystals

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1522230A (en) * 2001-03-08 2004-08-18 赫罗伊斯石英玻璃股份有限两合公司 Method of producing a quartz glass crucible
CN1789204A (en) * 2004-12-17 2006-06-21 德国贝格有限公司 Herbst bremer goldschlaegerei

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