CN108048902B - 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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- CN108048902B CN108048902B CN201711033364.XA CN201711033364A CN108048902B CN 108048902 B CN108048902 B CN 108048902B CN 201711033364 A CN201711033364 A CN 201711033364A CN 108048902 B CN108048902 B CN 108048902B
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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
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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 equal static pressure high purity graphite piece, inner thermal insulating layer is the long fine hard felt of PAN base, phenolic resin glue is sprayed in interior insulation layer surface, multiple equal static pressure high purity graphite pieces are equidistantly fitted on inner thermal insulating layer surface spraying phenolic resin glue, and there are gaps for each equal static pressure high purity graphite piece equal static pressure high purity graphite piece adjacent thereto, the preparation process of insulating layer include the long fine hard felt of PAN base it is standby-dipping, spray phenolic resin glue-patch isostatic pressing formed graphite piece-carbonization-high temperature purification-machining.
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 technique
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.
Currently, polycrystalline ingot furnace thermal insulation material mainly weaves carbon felt made of bonding is sintered, heat preservation used using carbon fiber
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
The CO generated can be reacted with the ambient oxidation object of silicon and its grey branch volatilized is transported into silicon melt with inert gas
In, thus the oxidation that reduces the electric property of polysilicon chip, and can be volatilized during polycrystalline silicon ingot casting in polycrystalline ingot furnace
Object corrodes, to reduce thermal insulation property and service life, increases ingot casting power consumption.
Summary of the invention
The technical problem to be solved by the present invention is to, the shortcomings that overcoming the prior art, a kind of low impurity of high-purity is provided
Polycrystalline furnace thermal field insulating layer and its preparation process.
The technical solution that the present invention solves the above technical problem is: 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 equal static pressure high purity graphite piece, the inner thermal insulating layer is the long fine carbon felt of PAN base, in the inside holding
Phenolic resin glue is sprayed in layer surface, the multiple equal static pressure high purity graphite piece is equidistantly fitted in inner thermal insulating layer surface spraying phenolic aldehyde
On resin glue, and there are gap, the insulating layers for each equal static pressure high purity graphite piece equal static pressure high purity graphite piece adjacent thereto
Preparation process, specifically includes the following steps:
(1) the long fine hard felt of PAN base is standby
A. it is chopped: being cut into 4cm long using PAN base carbon fibre silk is isometric；
B. it combs: crossing carding machine and be combed into single fiber state, fiber in the fibre web of output is made from unidirectional array to be transformed into one
Determine the disordered arrangements of degree；
C. netting: cross folding is woven into 1cm thickness net tire；
D. needle pierces: plate needle thorn is three-dimensional in longitudinal entanglement, being allowed to be formed in the horizontal and vertical standard for having some strength
The long fine soft felt of PAN base is made in crossover network structure；
(2) it sprays resin glue: the long fine soft felt surface of 1cm thickness PAN base obtained being sprayed into phenolic resin glue, then 10 layers of cross
Vertical to be staggeredly superimposed impregnated phenolic resin glue together, hot-forming, hot pressing temperature is generally 160-165 DEG C, time 1.2-
Extra burr leftover pieces are eliminated in 1.5min, machining；
(3) it the static pressure high purity graphite piece such as patch: is equidistantly bonded and is paved on the surface of the long fine carbon felt spraying phenolic resin glue of PAN base
Equal static pressure high purity graphite piece, and each equal static pressure high purity graphite piece equal static pressure high purity graphite adjacent thereto during fitting
All there are gaps for piece；
(4) it is carbonized: being 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, decompose the resin after solidifying, polymerization reaction, temperature is then risen to 800-
1100 DEG C, 4-6h is kept the temperature, the volatile components such as hydrogen, oxygen is allowed to be detached from, pure carbon under residual；
(5) high temperature purification: step (4) are continued 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, purity is improved；
(6) be machined: temperature is cooled to room temperature, by being machined to required shape.
Of the invention further limits technical solution:
The specification of equal static pressure high purity graphite piece above-mentioned is 50mm × 50mm × 3mm (length × width × height), density >
1.85g/cm3。
There are the gaps 3-4mm for each equal static pressure high purity graphite piece above-mentioned equal static pressure high purity graphite piece adjacent thereto.
Hot pressing temperature is 163 DEG C in aforementioned step (2), time 1.3min.
In aforementioned step (4) carbonisation, under protecting under an inert gas, heats up and heat by given rate, temperature
900 DEG C are heated to, the volatile components such as hydrogen, oxygen is allowed to be detached from, pure carbon under residual.
The sintering temperature of aforementioned step (5) high temperature purification is 2000 DEG C, time 8h.
The beneficial effects of the present invention are:
Inner thermal insulating layer of the present invention is the long fine hard felt of PAN base, and thermal coefficient is low, the good light-weight, hot conditions of heat insulation effect
Lower performance is stablized, and during the hard felt of the long fibre of PAN base is standby, plate needle thorn is lateral and vertical in longitudinal entanglement, being allowed to be formed in
The quasi- three dimensional intersection network structure of Xiang Junyou some strength has in this way in even pore distribution, easily compact formed, higher face
The features such as cutting intensity with layer；
The long fine hard felt of PAN base obtained is placed in resin sol solution by the present invention to be impregnated, and drying sintering is then carried out, main
Will because of the long fine carbon felt carbon fiber establishment of PAN base, be it 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 solidifying is made to be decomposed, be 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 effect
Then temperature is risen to 900 DEG C again by fruit, the volatile components such as hydrogen, nitrogen, oxygen is allowed to be detached from, pure carbon under residual；
For the present invention during high temperature ingot casting, graphite flake is reacted with silicon-containing gas and one layer of inertia carbon of uniform deposition on it
SiClx layer, and then insulation quilt reaction is isolated, stop the volatilization of impurity ash content, reaches clean effect.
Detailed description of the invention
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
The present embodiment provides a kind of polycrystalline furnace thermal field insulating layers of the low impurity of high-purity, including inner thermal insulating layer and equal static pressure height
Pure graphite flake, wherein inner thermal insulating layer is the long fine carbon felt of PAN base, and waiting static pressure high purity graphite piece specification is 50mm × 50mm × 3mm
(length × width × height), density 1.92g/cm3, phenolic resin glue, multiple equal high-purity stones of static pressure are sprayed in interior insulation layer surface
Ink sheet is equidistantly fitted on inner thermal insulating layer surface spraying phenolic resin glue, and each equal static pressure high purity graphite piece it is adjacent thereto etc.
Static pressure high purity graphite piece is there are the gap 3mm, the preparation process of the insulating layer, specifically includes the following steps:
(1) the long fine carbon felt preparation of PAN base
A. it is chopped: being cut into 4cm long using PAN base carbon fibre silk is isometric；
B. it combs: crossing carding machine and be combed into single fiber state, fiber in the fibre web of output is made from unidirectional array to be transformed into one
Determine the disordered arrangements of degree；
C. netting: cross folding is woven into 1cm thickness net tire；
D. needle pierces: plate needle thorn is three-dimensional in longitudinal entanglement, being allowed to be formed in the horizontal and vertical standard for having some strength
The long fine carbon felt of PAN base is made in crossover network structure；
(2) the long fine soft felt surface of 1cm thickness PAN base obtained is sprayed into phenolic resin glue, then 10 layers of transverse and longitudinal are staggeredly superimposed
Impregnated phenolic resin glue together, hot-forming, hot pressing temperature is generally 163 DEG C, time 1.3min, and it is extra that machining is eliminated
Burr leftover pieces；
(3) it the static pressure high purity graphite piece such as patch: is equidistantly bonded and is paved on the surface of the long fine carbon felt spraying phenolic resin glue of PAN base
Equal static pressure high purity graphite piece, and each equal static pressure high purity graphite piece equal static pressure high purity graphite adjacent thereto during fitting
All there are the gaps 3mm for piece；
(4) it is carbonized: being 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, decompose the resin after solidifying, polymerization reaction, and temperature is then risen to 900 DEG C, protect
Warm 5h allows the volatile components such as hydrogen, nitrogen, oxygen to be detached from, pure carbon under residual；
(6) high temperature purification: continuing heat temperature raising for step (4), and temperature rises to 2000 DEG C, time 8h, excludes in material
The impurity in portion improves purity；
(7) be 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 in clean thermal field during brilliant ingot casting, the carbon content of ingot casting is substantially reduced；
As seen from Table 1, the length of the normal heat undesirable removal of minority carrier life time off field is greater than few sub- longevity under clean thermal field
The length of undesirable removal is ordered, and clean thermal field is made 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 embodiments.It is all to use equivalent substitution or equivalent transformation shape
At technical solution, fall within the scope of protection required by the present invention.
Claims (6)
1. a kind of polycrystalline furnace thermal field insulating layer of the low impurity of high-purity, including inner thermal insulating layer and equal static pressure high purity graphite piece, special
Sign is: the inner thermal insulating layer is the long fine hard felt of PAN base, and phenolic resin glue is sprayed on the inner thermal insulating layer surface, described more
A equal static pressure high purity graphite piece is equidistantly fitted in inner thermal insulating layer surface and sprays on phenolic resin glue, and each equal static pressure high purity graphite
Piece equal static pressure high purity graphite piece adjacent thereto is there are gap, the preparation process of the insulating layer, specifically includes the following steps:
(1) the long fine hard felt of PAN base is standby
A. it is chopped: being cut into 4cm long using PAN base carbon fibre silk is isometric；
B. it combs: crossing carding machine and be combed into single fiber state, fiber in the fibre web of output is made from unidirectional array to be transformed into certain journey
The disordered arrangements of degree；
C. netting: cross folding is woven into 1cm thickness net tire；
D. needle pierces: plate needle thorn is in longitudinal entanglement, being allowed to be formed in the horizontal and vertical quasi- three dimensional intersection for having some strength
The long fine soft felt of PAN base is made in network structure；
(2) it sprays resin glue: the long fine soft felt surface of 1cm thickness PAN base obtained being sprayed into phenolic resin glue, then 10 layers of transverse and longitudinal are handed over
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
Extra burr leftover pieces are eliminated in tool processing；
(3) the static pressure high purity graphite piece such as patch: the surface of the long fine carbon felt spraying phenolic resin glue of PAN base be equidistantly bonded be paved with etc. it is quiet
High purity graphite piece is pressed, and each equal static pressure high purity graphite piece equal static pressure high purity graphite piece adjacent thereto during fitting
There are gaps；
(4) it is carbonized: being put into what step (3) obtained into sintering furnace, under protecting under an inert gas, heat up by given rate
Heating, temperature rise to 200-220 DEG C, decompose the resin after solidifying, polymerization reaction, temperature is then risen to 800-1100
DEG C, 4-6h is kept the temperature, the volatile components such as hydrogen, oxygen is allowed to be detached from, pure carbon under residual；
(5) high temperature purification: step (4) are continued 1900-2100 DEG C of heat temperature raising, soaking time 4-10h, according to density and are led
Heating rate parameter controls sintering temperature and time；The impurity of material internal is excluded, purity is improved；
(6) be machined: 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 equal static pressure
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: described each etc.
There are the gaps 3-4mm for static pressure high purity graphite piece equal static pressure high purity graphite piece adjacent thereto.
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) hot pressing temperature is generally 163 DEG C in, 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) it in carbonisation, under protecting under an inert gas, heats up and heats by given rate, temperature rises to 210 DEG C, after making solidification
Resin decomposed, polymerization reaction, then temperature is heated to 900 DEG C, keeps the temperature 5h, allows the volatile components such as hydrogen, oxygen to be detached 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) sintering temperature of high temperature purification is 2000 DEG C, time 8h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100567217C (en) * | 2006-12-06 | 2009-12-09 | 湖南南方搏云新材料有限责任公司 | The high purity cured charcoal felt silicon crystal growth oven manufacture method |
| CN101445376B (en) * | 2008-12-31 | 2011-06-15 | 西安超码科技有限公司 | Method for preparing high temperature furnace used carbon/carbon composite material cylinders |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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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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