CN108048902A - The polycrystalline furnace thermal field insulating layer and its preparation process of a kind of low impurity of high-purity - Google Patents
The polycrystalline furnace thermal field insulating layer and its preparation process of a kind of low impurity of high-purity Download PDFInfo
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- CN108048902A CN108048902A CN201711033364.XA CN201711033364A CN108048902A CN 108048902 A CN108048902 A CN 108048902A CN 201711033364 A CN201711033364 A CN 201711033364A CN 108048902 A CN108048902 A CN 108048902A
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- insulating layer
- temperature
- graphite piece
- high purity
- isostatic pressed
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The present invention is a kind of polycrystalline furnace thermal field insulating layer of the low impurity of high-purity, including inner thermal insulating layer and isostatic pressed high purity graphite piece, inner thermal insulating layer is the fine hard felt of PAN bases length, phenolic resin glue is sprayed in interior insulation layer surface, multiple isostatic pressed high purity graphite pieces are equidistantly fitted on inner thermal insulating layer surface spraying phenolic resin glue, and each isostatic pressed high purity graphite piece isostatic pressed high purity graphite piece adjacent thereto leaves gap, the preparation process of insulating layer include the fine hard felt of PAN bases length it is standby-dipping, spray phenolic resin glue-patch isostatic pressing formed graphite piece-carbonization-high temperature purification-mechanical processing.
Description
Technical field
The present invention relates to field of polycrystalline silicon ingot, the polycrystalline furnace thermal field insulating layer of the low impurity of specifically a kind of high-purity
And its preparation process.
Background technology
Carbon impurity is one of most important impurity in polycrystalline cast ingot, seriously affects the efficiency of solar cell, therefore, miscellaneous to carbon
The prediction and control of matter are to prepare the effective means of high-quality crystal silicon ingot casting, the main load that carbon impurity transports during polycrystalline cast ingot
Body is silicon melt and argon gas.
At present, the carbon felt that polycrystalline ingot furnace thermal insulation material is mainly formed using carbon fiber braiding bonding sintering, heat preservation used
Carbon felt thickness is generally 90mm, divides two layers and is fixed in steel construction cage, carbon felt density is low gap, during high temperature ingot casting
With the CO of the ambient oxidation object reaction generation of silicon and its grey branch volatilized silicon melt can be transported into inert gas
In, so as to reduce the electric property of polysilicon chip, and the oxidation that can be volatilized during polycrystalline silicon ingot casting in polycrystalline ingot furnace
Object corrodes, and so as to reduce heat-insulating property and service life, increases ingot casting power consumption.
The content of the invention
The shortcomings that technical problems to be solved by the invention are, overcome the prior art provides a kind of low impurity of high-purity
Polycrystalline furnace thermal field insulating layer and its preparation process.
The present invention solve more than technical problem technical solution be：The polycrystalline furnace thermal field for providing a kind of low impurity of high-purity is protected
Warm layer, including inner thermal insulating layer and isostatic pressed high purity graphite piece, the inner thermal insulating layer grows fine carbon felt for PAN bases, in the inside holding
Phenolic resin glue is sprayed in layer surface, the multiple isostatic pressed high purity graphite piece is equidistantly fitted in inner thermal insulating layer surface spraying phenolic aldehyde
On resin glue, and each isostatic pressed high purity graphite piece isostatic pressed high purity graphite piece adjacent thereto leaves gap, the insulating layer
Preparation process, specifically include following steps：
(1) the fine hard felt of PAN bases length is standby
A. it is chopped：4cm long is cut into using PAN base carbon fibre silks are isometric；
B. comb：It crosses carding machine and is combed into single fiber state, fiber in the fibre web of output is made to be transformed into one from unidirectional array
Determine the disordered arrangements of degree；
C. netting：Cross folding is woven into 1cm thickness net tires；
D. pin pierces：Tablet pin thorn is three-dimensional into longitudinal entanglement, being allowed to be formed in the horizontal and vertical standard for having some strength
The fine soft felt of PAN bases length is made in crossover network structure；
(2) resin glue is sprayed：1cm thickness PAN bases obtained are grown into fine soft felt surface spraying phenolic resin glue, then 10 layers of horizontal stroke
Vertical to be staggeredly superimposed impregnated phenolic resin glue together, hot-forming, hot pressing temperature is generally 160-165 DEG C, time 1.2-
1.5min, mechanical processing eliminate extra burr leftover pieces；
(3) isostatic pressed high purity graphite piece is pasted：The equidistant fitting in surface that fine carbon felt spraying phenolic resin glue is grown in PAN bases is paved with
Isostatic pressed high purity graphite piece, and each isostatic pressed high purity graphite piece isostatic pressed high purity graphite adjacent thereto during fitting
Piece all leaves gap；
(4) it is carbonized：It is put into what step (3) obtained into sintering furnace, under protecting under an inert gas, by given rate
Heating heating, temperature rise to 200-220 DEG C, are decomposed the resin after curing, polymerisation, then rise to temperature
800-1100 DEG C, 4-6h is kept the temperature, the volatile components such as hydrogen, oxygen is allowed to depart from, pure carbon under residual；
(5) high temperature purification：Step (4) is continued into 1900-2100 DEG C of heat temperature raising, soaking time 4-10h, according to density
Sintering temperature and time are controlled with thermal conductivity parameter；The impurity of material internal is excluded, improves purity；
(6) it is machined：Temperature is cooled to room temperature, by being machined to required shape.
The further of the present invention limits technical solution：
The specification of foregoing isostatic pressed high purity graphite piece is 50mm × 50mm × 3mm (length × width × height), density ＞
1.85g/cm3。
Foregoing each isostatic pressed high purity graphite piece isostatic pressed high purity graphite piece adjacent thereto leaves 3-4mm gaps.
Hot pressing temperature is 163 DEG C in foregoing step (2), time 1.3min.
In foregoing step (4) carbonisation, under protecting under an inert gas, heat up and heat by given rate, temperature
900 DEG C are heated to, the volatile components such as hydrogen, oxygen is allowed to depart from, pure carbon under residual.
The sintering temperature of foregoing step (5) high temperature purification is 2000 DEG C, time 8h.
The beneficial effects of the invention are as follows：
Inner thermal insulating layer of the present invention is the fine hard felt of PAN bases length, and thermal conductivity factor is low, high insulating effect is light-weight, hot conditions
Lower performance is stablized, and during the fine hard felt of PAN bases length is standby, tablet pin thorn is allowed to be formed in horizontal and vertical into longitudinal entanglement
To the quasi- three dimensional intersection network structure for having some strength, so in even pore distribution, easily compact formed, higher face
The features such as intensity being cut with layer；
The fine hard felt of PAN bases obtained length is placed in resin sol solution by the present invention to be impregnated, and then carries out drying sintering, main
Fine carbon felt carbon fiber establishment is grown because of PAN bases, is loose, impregnating resin glue, be then sintered, such resin glue is carbon containing
The elements such as hydrogen-oxygen, in inert gas after high temperature, hydrogen and oxygen etc. can vapor away remaining carbon, toughen up, and have certain strong
Degree；
For the present invention in carbonisation, first temperature is first heated to certain temperature, and the resin after curing is made to be decomposed, polymerize
Reaction has certain cementability, while the carbon decomposed in resin is filled in the gap of carbon felt, improves its intensity and heat preservation is imitated
Then temperature is risen to 900 DEG C by fruit again, the volatile components such as hydrogen, nitrogen, oxygen is allowed to depart from, pure carbon under residual；
The present invention is during high temperature ingot casting, and graphite flake and silicon-containing gas react and one layer of inertia carbon of uniform deposition on it
SiClx layer, and then isolate insulation quilt reaction, stop the volatilization of impurity ash content, reach clean effect.
Description of the drawings
Fig. 1 is common thermal field ingot casting carbon content with solid fraction relational graph；
Fig. 2 is the clean thermal field ingot casting carbon content of the present invention with solid fraction relational graph.
Specific embodiment
Embodiment 1
It is high including inner thermal insulating layer and isostatic pressed the present embodiment provides a kind of polycrystalline furnace thermal field insulating layer of the low impurity of high-purity
Pure graphite flake, wherein, inner thermal insulating layer grows fine carbon felt for PAN bases, and isostatic pressed high purity graphite piece specification is 50mm × 50mm × 3mm
(length × width × height), density 1.92g/cm3, phenolic resin glue, multiple high-purity stones of isostatic pressed are sprayed in interior insulation layer surface
Ink sheet is equidistantly fitted on inner thermal insulating layer surface spraying phenolic resin glue, and each isostatic pressed high purity graphite piece it is adjacent thereto etc.
Static pressure high purity graphite piece leaves 3mm gaps, and the preparation process of the insulating layer specifically includes following steps：
(1) prepared by the fine carbon felt of PAN bases length
A. it is chopped：4cm long is cut into using PAN base carbon fibre silks are isometric；
B. comb：It crosses carding machine and is combed into single fiber state, fiber in the fibre web of output is made to be transformed into one from unidirectional array
Determine the disordered arrangements of degree；
C. netting：Cross folding is woven into 1cm thickness net tires；
D. pin pierces：Tablet pin thorn is three-dimensional into longitudinal entanglement, being allowed to be formed in the horizontal and vertical standard for having some strength
The fine carbon felt of PAN bases length is made in crossover network structure；
(2) by the fine soft felt surface spraying phenolic resin glue of 1cm thickness PAN bases obtained length, then 10 layers of transverse and longitudinal staggeredly superposition
Impregnated phenolic resin glue together, hot-forming, hot pressing temperature is generally 163 DEG C, time 1.3min, and it is extra that mechanical processing eliminates
Burr leftover pieces；
(3) isostatic pressed high purity graphite piece is pasted：The equidistant fitting in surface that fine carbon felt spraying phenolic resin glue is grown in PAN bases is paved with
Isostatic pressed high purity graphite piece, and each isostatic pressed high purity graphite piece isostatic pressed high purity graphite adjacent thereto during fitting
Piece all leaves 3mm gaps；
(4) it is carbonized：It is put into what step (3) obtained into sintering furnace, under protecting under an inert gas, by given rate
Heating heating, temperature rise to 210 DEG C, are decomposed the resin after curing, polymerisation, and temperature then is risen to 900 DEG C, protect
Warm 5h allows the volatile components such as hydrogen, nitrogen, oxygen to depart from, pure carbon under residual；
(6) high temperature purification：Step (4) is continued into heat temperature raising, temperature rises to 2000 DEG C, time 8h, excludes in material
The impurity in portion improves purity；
(7) it is machined：Temperature is cooled to room temperature, by being machined to required shape.
Table 1
Insulating layer manufactured in the present embodiment is added it can be seen from Figure of description 1 and Figure of description 2 so that more
It is substantially reduced during brilliant ingot casting in clean thermal field, the carbon content of ingot casting；
As seen from Table 1, the length of the normal heat undesirable removal of minority carrier life time off field is more than few sub- longevity under clean thermal field
The length of undesirable removal is ordered, and clean thermal field is caused integrally to lack the service life of son also above normal thermal field.
In addition to the implementation, the present invention can also have other embodiment.It is all to use equivalent substitution or equivalent transformation shape
Into technical solution, all fall within the present invention claims protection domain.
Claims (6)
1. a kind of polycrystalline furnace thermal field insulating layer of the low impurity of high-purity, special including inner thermal insulating layer and isostatic pressed high purity graphite piece
Sign is：The inner thermal insulating layer is the fine hard felt of PAN bases length, and phenolic resin glue is sprayed on the inner thermal insulating layer surface, described more
A isostatic pressed high purity graphite piece is equidistantly fitted on inner thermal insulating layer surface spraying phenolic resin glue, and each isostatic pressed high purity graphite
Piece isostatic pressed high purity graphite piece adjacent thereto leaves gap, and the preparation process of the insulating layer specifically includes following steps：
（1）The fine hard felt of PAN bases length is standby
A. it is chopped：4cm long is cut into using PAN base carbon fibre silks are isometric；
B. comb：It crosses carding machine and is combed into single fiber state, fiber in the fibre web of output is made to be transformed into certain journey from unidirectional array
The disordered arrangements of degree；
C. netting：Cross folding is woven into 1cm thickness net tires；
D. pin pierces：Tablet pin thorn is allowed to be formed in the horizontal and vertical quasi- three dimensional intersection for having some strength into longitudinal entanglement
The fine soft felt of PAN bases length is made in network structure；
（2）Spray resin glue：By the fine soft felt surface spraying phenolic resin glue of 1cm thickness PAN bases obtained length, then 10 layers of transverse and longitudinals friendship
Mistake is superimposed impregnated phenolic resin glue together, and hot-forming, hot pressing temperature is generally 160-165 DEG C, time 1.2-1.5min, machine
Tool processing eliminates extra burr leftover pieces；
（3）Paste isostatic pressed high purity graphite piece：PAN bases grow fine carbon felt spraying phenolic resin glue surface equidistantly fitting be paved with etc. it is quiet
Press high purity graphite piece, and each isostatic pressed high purity graphite piece isostatic pressed high purity graphite piece adjacent thereto during fitting
Leave gap；
（4）Carbonization：By step（3）What is obtained is put into sintering furnace, under protecting under an inert gas, heats up by given rate
Heating, temperature rise to 200-220 DEG C, are decomposed the resin after curing, polymerisation, temperature then is risen to 800-1100
DEG C, 4-6h is kept the temperature, the volatile components such as hydrogen, oxygen is allowed to depart from, pure carbon under residual；
（5）High temperature purification：By step（4）Continue 1900-2100 DEG C of heat temperature raising, soaking time 4-10h according to density and is led
Heating rate parameter controls sintering temperature and time；The impurity of material internal is excluded, improves purity；
（6）Mechanical processing：Temperature is cooled to room temperature, by being machined to required shape.
2. the polycrystalline furnace thermal field insulating layer of the low impurity of high-purity according to claim 1, it is characterised in that：The isostatic pressed
The specification of high purity graphite piece is 50mm × 50mm × 3mm（Length × width × height）, density ＞ 1.85g/cm3。
3. the polycrystalline furnace thermal field insulating layer of the low impurity of high-purity according to claim 1, it is characterised in that：It is described each etc.
Static pressure high purity graphite piece isostatic pressed high purity graphite piece adjacent thereto leaves 3-4mm gaps.
4. the polycrystalline furnace thermal field insulating layer of the low impurity of high-purity according to claim 1, it is characterised in that：The step
（2）Middle hot pressing temperature is generally 163 DEG C, time 1.3min.
5. the polycrystalline furnace thermal field insulating layer of the low impurity of high-purity according to claim 1, it is characterised in that：The step
（4）In carbonisation, under protecting under an inert gas, heat up and heat by given rate, temperature rises to 210 DEG C, after making curing
Resin decomposed, polymerisation, then temperature be heated to 900 DEG C, keep the temperature 5h, the volatile components such as hydrogen, oxygen allowed to depart from, residual
Under pure carbon.
6. the polycrystalline furnace thermal field insulating layer of the low impurity of high-purity according to claim 1, it is characterised in that：The step
（5）The sintering temperature of high temperature purification is 2000 DEG C, time 8h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711033364.XA CN108048902B (en) | 2017-10-30 | 2017-10-30 | The polycrystalline furnace thermal field insulating layer and its preparation process of a kind of low impurity of high-purity |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711033364.XA CN108048902B (en) | 2017-10-30 | 2017-10-30 | The polycrystalline furnace thermal field insulating layer and its preparation process of a kind of low impurity of high-purity |
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| CN108048902A true CN108048902A (en) | 2018-05-18 |
| CN108048902B CN108048902B (en) | 2019-10-29 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994972A (en) * | 2006-12-06 | 2007-07-11 | 湖南南方搏云新材料有限责任公司 | Production method of high purity cured charcoal felt silicon crystal growth oven |
| CN101445376A (en) * | 2008-12-31 | 2009-06-03 | 西安超码科技有限公司 | Method for preparing high temperature furnace used carbon/carbon composite material cylinders |
| CN101571351A (en) * | 2008-05-01 | 2009-11-04 | 揖斐电株式会社 | Crucible holding member and method for producing the same |
| CN102408254A (en) * | 2011-11-10 | 2012-04-11 | 石金精密科技（深圳）有限公司 | Carbon fiber hard felt surface treatment method and carbon fiber hard felt |
| CN203513825U (en) * | 2013-08-30 | 2014-04-02 | 宁夏隆基硅材料有限公司 | Main heat preservation cylinder used in single crystal furnace |
-
2017
- 2017-10-30 CN CN201711033364.XA patent/CN108048902B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994972A (en) * | 2006-12-06 | 2007-07-11 | 湖南南方搏云新材料有限责任公司 | Production method of high purity cured charcoal felt silicon crystal growth oven |
| CN101571351A (en) * | 2008-05-01 | 2009-11-04 | 揖斐电株式会社 | Crucible holding member and method for producing the same |
| CN101445376A (en) * | 2008-12-31 | 2009-06-03 | 西安超码科技有限公司 | Method for preparing high temperature furnace used carbon/carbon composite material cylinders |
| CN102408254A (en) * | 2011-11-10 | 2012-04-11 | 石金精密科技（深圳）有限公司 | Carbon fiber hard felt surface treatment method and carbon fiber hard felt |
| CN203513825U (en) * | 2013-08-30 | 2014-04-02 | 宁夏隆基硅材料有限公司 | Main heat preservation cylinder used in single crystal furnace |
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| CN108048902B (en) | 2019-10-29 |
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Effective date of registration: 20190919 Address after: 014010 No. 1 Tuoye Road, Kundulun District, Baotou City, Inner Mongolia Autonomous Region Applicant after: Baotou Meike Silicon Energy Co., Ltd. Address before: 212200 Jiangsu city of Zhenjiang province Yangzhong Youfang Town New Material Industrial Park Applicant before: Zhenjiang Huantai Silicon Technology Co., Ltd. |
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