CN106744919A - A kind of production technology of polycrystalline silicon base plate special graphite - Google Patents
A kind of production technology of polycrystalline silicon base plate special graphite Download PDFInfo
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- CN106744919A CN106744919A CN201710031000.1A CN201710031000A CN106744919A CN 106744919 A CN106744919 A CN 106744919A CN 201710031000 A CN201710031000 A CN 201710031000A CN 106744919 A CN106744919 A CN 106744919A
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention relates to a kind of production technology of polycrystalline silicon base plate special graphite, described production technology includes preparing raw material, mixed dehydration, pitch preparation, premix, rolled sheet, grinding, once pressing mold shaping, roasting, single-steeping, after baking, double-steeping, three roastings, three dippings, graphited steps, and the special graphite prepared by this kind of technique has the advantages that to lower the labour intensity of workman, improves product service life, reduces production cost.
Description
Technical field
The invention belongs to technical field of polysilicon production, more particularly to a kind of production work of polycrystalline silicon base plate special graphite
Skill.
Background technology
With industrial expansion, increasingly extensively, the field for setting foot in constantly expands the purposes of high purity graphite, for different
Industry characteristic, production sets extremely urgent with the graphite of single-minded purposes；For the client of downstream, them can be not only reduced
Production cost, improve the service life of product, and the labour intensity of workman can be reduced, reduce staff more
Frequency is changed, the demand with polysilicon increasingly increases, it is necessary to which exploitation one kind is specifically designed for polycrystalline silicon base plate special graphite.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, and provide a kind of strong with the work for lowering workman
Degree, raising product service life, the production technology of the polycrystalline silicon base plate special graphite of reduction production cost.
What the technical solution adopted by the present invention was realized in：A kind of production technology of polycrystalline silicon base plate special graphite, institute
The production technology stated comprises the following steps：
Step 1：Preparing raw material：Pitch coke, petroleum coke are crushed respectively by 5R pendulum type ring roll pulverizers, pitch coke, petroleum coke
Raw material particle size tails over 5%-10% by 325 mesh sieves；
Step 2：Mixed dehydration：Pitch coke, the petroleum coke particles that will be obtained in step 1 are 3 according to mass ratio：7 are added to stirring
Machine is well mixed, and then heats the mixture to 120-125 DEG C, and holding carries out thermal dehydration in 40 minutes；
Step 3：It is prepared by pitch：Stood by infusion from modified coal tar pitch and be not less than 100 hours, and by temperature control in 160-
Pitch is prepared at 165 DEG C；
Step 4：Premix：The compound that the pitch and step 2 prepared in optional step 3 are obtained, described compound and pitch
Mass ratio is 40%-41%, and compound and pitch such as to mixing in mixing plant will be controlled into mixing temperature at 173-178 DEG C,
Incorporation time is 60min；
Step 5：Rolled sheet：The mixture prepared in step 4 is put into plastics processing mill, flakiness is rolled by plastics processing mill,
The thickness of described thin slice is 2-2.5mm, will roll thin slice and is deposited 48 hours in the case of 50-60 DEG C of temperature；
Step 6：Grinding：Thin slice prepared by step 5 is put into 5R pendulum type ring roll pulverizers powder is obtained, and powder is passed through 200 mesh
Sieve, tails over no more than 20%-25%；
Step 7：Pressing mold is molded：The powder prepared in step 6 is encased in mould, the pressing mold density for making reaches 1.45-
1.46g/cm3, and place indoors no less than 48 hours；
Step 8：Once it is calcined：Mixture shove charge compressing in step 7 is calcined so that in-furnace temperature is rapidly achieved 350
DEG C, 5 DEG C for every eight hours of uniform intensification is then changed to, it is warming up to 520 DEG C and is kept for 24 hours, uniform intensification again rises for 27 DEG C for every eight hours
Temperature maintains close fire within 48 hours to 1250 DEG C in 1250 DEG C of stages of high temperature, and the mixture after roasting then is cooled down into 240 hours and stove
Interior temperature is come out of the stove when being less than 90 DEG C；
Step 9：Single-steeping：The impregnation mixture after being once calcined will be completed in medium temperature coal pitch, and with 50 DEG C -60 DEG C
The temperature rise speed of/h is heated to 300-500 degree, vacuumizes rear pressurize treatment, and single-steeping rate of body weight gain reaches 18-19%；
Step 10：After baking：By mixture shove charge after baking so that in-furnace temperature is rapidly achieved 350 DEG C, then it is changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 11：Double-steeping：The impregnation mixture after after baking will be completed in medium temperature coal pitch, and with 50 DEG C -60
DEG C/temperature rise speed of h is heated to 300-500 degree, vacuumizes rear pressurize treatment, single-steeping rate of body weight gain reaches 13-14%；
Step 12：Three roastings：By three roastings of mixture shove charge so that in-furnace temperature is rapidly achieved 350 DEG C, is then changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 13：Three dippings：The impregnation mixture after three roastings will be completed in medium temperature coal pitch, vacuumized at rear pressurize
Reason, single-steeping rate of body weight gain reaches 9-10%；
Step 14：Graphitization：The mixture that step 13 is obtained is put into acheson furnace, is that product temperature reaches 2800-
2900 DEG C so that mixture graphitization.
The temperature control of pressing mold shaping is at 25-30 DEG C in described step 7.
Mixture test resistance rate after the graphitization that described step 14 is obtained, it is desirable in 12-13 μ Ω m.
Beneficial effects of the present invention：A kind of production technology of polycrystalline silicon base plate special graphite of the present invention, specifically designed for polycrystalline
Silicon base plate is processed with graphite, with strong points, and the special of special 1100X1100X250mm is processed using rational production technology
With graphite, the specialized degree of production is high, reduces the labour intensity of workman, reduces workman's replacement frequency, considerably reduces life
Produce cost, it is adaptable to large-scale production.
Specific embodiment
Embodiment 1
A kind of production technology of polycrystalline silicon base plate special graphite, described production technology comprises the following steps：
Step 1：Preparing raw material：Pitch coke, petroleum coke are crushed respectively by 5R pendulum type ring roll pulverizers, pitch coke, petroleum coke
Raw material particle size tails over 5% by 325 mesh sieves；
Step 2：Mixed dehydration：Pitch coke, the petroleum coke particles that will be obtained in step 1 are 3 according to mass ratio：7 are added to stirring
Machine is well mixed, and then heats the mixture to 120 DEG C, and holding carries out thermal dehydration in 40 minutes；
Step 3：It is prepared by pitch：100 hours are stood by infusion from modified coal tar pitch, and temperature control is made at 160 DEG C
Standby pitch；
Step 4：Premix：The compound that the pitch and step 2 prepared in optional step 3 are obtained, described compound and pitch
Mass ratio is 40%, will such as to mixing in mixing plant by compound and pitch, and control mixing temperature is in 173 DEG C, incorporation time
It is 60min；
Step 5：Rolled sheet：The mixture prepared in step 4 is put into plastics processing mill, flakiness is rolled by plastics processing mill,
The thickness of described thin slice is 2mm, will roll thin slice and is deposited in the case of temperature 50 C 48 hours；
Step 6：Grinding：Thin slice prepared by step 5 is put into 5R pendulum type ring roll pulverizers powder is obtained, and powder is passed through 200 mesh
Sieve, tails over no more than 20%；
Step 7：Pressing mold is molded：The powder prepared in step 6 is encased in mould, the pressing mold density for making reaches 1.45g/
Cm3, and place 48 hours indoors；
Step 8：Once it is calcined：Mixture shove charge compressing in step 7 is calcined so that in-furnace temperature is rapidly achieved 350
DEG C, 5 DEG C for every eight hours of uniform intensification is then changed to, it is warming up to 520 DEG C and is kept for 24 hours, uniform intensification again rises for 27 DEG C for every eight hours
Temperature maintains close fire within 48 hours to 1250 DEG C in 1250 DEG C of stages of high temperature, and the mixture after roasting then is cooled down into 240 hours and stove
Interior temperature is come out of the stove when being less than 90 DEG C；
Step 9：Single-steeping：The impregnation mixture after being once calcined will be completed in medium temperature coal pitch, and with 50 DEG C/h's
Temperature rise speed is heated to 300 degree, vacuumizes rear pressurize treatment, and single-steeping rate of body weight gain reaches 18%；
Step 10：After baking：By mixture shove charge after baking so that in-furnace temperature is rapidly achieved 350 DEG C, then it is changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 11：Double-steeping：The impregnation mixture after after baking will be completed in medium temperature coal pitch, and with 50 DEG C/h's
Temperature rise speed is heated to 300 degree, vacuumizes rear pressurize treatment, and single-steeping rate of body weight gain reaches 13%；
Step 12：Three roastings：By three roastings of mixture shove charge so that in-furnace temperature is rapidly achieved 350 DEG C, is then changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 13：Three dippings：The impregnation mixture after three roastings will be completed in medium temperature coal pitch, vacuumized at rear pressurize
Reason, single-steeping rate of body weight gain reaches 9%；
Step 14：Graphitization：The mixture that step 13 is obtained is put into acheson furnace, is that product temperature reaches 2800 DEG C,
So that mixture graphitization.
The temperature control of pressing mold shaping is at 25 DEG C in described step 7.
Beneficial effects of the present invention：A kind of production technology of polycrystalline silicon base plate special graphite of the present invention, specifically designed for polycrystalline
Silicon base plate is processed with graphite, with strong points, and the special of special 1100X1100X250mm is processed using rational production technology
With graphite, the specialized degree of production is high, reduces the labour intensity of workman, reduces workman's replacement frequency, considerably reduces life
Produce cost, it is adaptable to large-scale production.
Embodiment 2
A kind of production technology of polycrystalline silicon base plate special graphite, described production technology comprises the following steps：
Step 1：Preparing raw material：Pitch coke, petroleum coke are crushed respectively by 5R pendulum type ring roll pulverizers, pitch coke, petroleum coke
Raw material particle size tails over 10% by 325 mesh sieves；
Step 2：Mixed dehydration：Pitch coke, the petroleum coke particles that will be obtained in step 1 are 3 according to mass ratio：7 are added to stirring
Machine is well mixed, and then heats the mixture to 125 DEG C, and holding carries out thermal dehydration in 40 minutes；
Step 3：It is prepared by pitch：120 hours are stood by infusion from modified coal tar pitch, and temperature control is made at 165 DEG C
Standby pitch；
Step 4：Premix：The compound that the pitch and step 2 prepared in optional step 3 are obtained, described compound and pitch
Mass ratio is 41%, will such as to mixing in mixing plant by compound and pitch, and control mixing temperature is in 178 DEG C, incorporation time
It is 60min；
Step 5：Rolled sheet：The mixture prepared in step 4 is put into plastics processing mill, flakiness is rolled by plastics processing mill,
The thickness of described thin slice is 2.5mm, will roll thin slice and is deposited in the case of temperature 60 C 48 hours；
Step 6：Grinding：Thin slice prepared by step 5 is put into 5R pendulum type ring roll pulverizers powder is obtained, and powder is passed through 200 mesh
Sieve, tails over no more than 25%；
Step 7：Pressing mold is molded：The powder prepared in step 6 is encased in mould, the pressing mold density for making reaches 1.46g/
Cm3, and place 50 hours indoors；
Step 8：Once it is calcined：Mixture shove charge compressing in step 7 is calcined so that in-furnace temperature is rapidly achieved 350
DEG C, 5 DEG C for every eight hours of uniform intensification is then changed to, it is warming up to 520 DEG C and is kept for 24 hours, uniform intensification again rises for 27 DEG C for every eight hours
Temperature maintains close fire within 48 hours to 1250 DEG C in 1250 DEG C of stages of high temperature, and the mixture after roasting then is cooled down into 240 hours and stove
Interior temperature is come out of the stove when being less than 90 DEG C；
Step 9：Single-steeping：The impregnation mixture after being once calcined will be completed in medium temperature coal pitch, and with 60 DEG C/h's
Temperature rise speed is heated to 500 degree, vacuumizes rear pressurize treatment, and single-steeping rate of body weight gain reaches 19%；
Step 10：After baking：By mixture shove charge after baking so that in-furnace temperature is rapidly achieved 350 DEG C, then it is changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 11：Double-steeping：The impregnation mixture after after baking will be completed in medium temperature coal pitch, and with 60 DEG C/h
Temperature rise speed be heated to 500 degree, vacuumize rear pressurize treatment, single-steeping rate of body weight gain reaches 14%；
Step 12：Three roastings：By three roastings of mixture shove charge so that in-furnace temperature is rapidly achieved 350 DEG C, is then changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 13：Three dippings：The impregnation mixture after three roastings will be completed in medium temperature coal pitch, vacuumized at rear pressurize
Reason, single-steeping rate of body weight gain reaches 10%；
Step 14：Graphitization：The mixture that step 13 is obtained is put into acheson furnace, is that product temperature reaches 2900 DEG C,
So that mixture graphitization.
The temperature control of pressing mold shaping is at 25-30 DEG C in described step 7.
Beneficial effects of the present invention：A kind of production technology of polycrystalline silicon base plate special graphite of the present invention, specifically designed for polycrystalline
Silicon base plate is processed with graphite, with strong points, and the special of special 1100X1100X250mm is processed using rational production technology
With graphite, the specialized degree of production is high, reduces the labour intensity of workman, reduces workman's replacement frequency, considerably reduces life
Produce cost, it is adaptable to large-scale production.
Claims (3)
1. a kind of production technology of polycrystalline silicon base plate special graphite, it is characterised in that：Described production technology comprises the following steps：
Step 1：Preparing raw material：Pitch coke, petroleum coke are crushed respectively by 5R pendulum type ring roll pulverizers, pitch coke, petroleum coke
Raw material particle size tails over 5%-10% by 325 mesh sieves；
Step 2：Mixed dehydration：Pitch coke, the petroleum coke particles that will be obtained in step 1 are 3 according to mass ratio：7 are added to stirring
Machine is well mixed, and then heats the mixture to 120-125 DEG C, and holding carries out thermal dehydration in 40 minutes；
Step 3：It is prepared by pitch：Stood by infusion from modified coal tar pitch and be not less than 100 hours, and by temperature control in 160-
Pitch is prepared at 165 DEG C；
Step 4：Premix：The compound that the pitch and step 2 prepared in optional step 3 are obtained, described compound and pitch
Mass ratio is 40%-41%, and compound and pitch such as to mixing in mixing plant will be controlled into mixing temperature at 173-178 DEG C,
Incorporation time is 60min；
Step 5：Rolled sheet：The mixture prepared in step 4 is put into plastics processing mill, flakiness is rolled by plastics processing mill,
The thickness of described thin slice is 2-2.5mm, will roll thin slice and is deposited 48 hours in the case of 50-60 DEG C of temperature；
Step 6：Grinding：Thin slice prepared by step 5 is put into 5R pendulum type ring roll pulverizers powder is obtained, and powder is passed through 200 mesh
Sieve, tails over no more than 20%-25%；
Step 7：Pressing mold is molded：The powder prepared in step 6 is encased in mould, the pressing mold density for making reaches 1.45-
1.46g/cm3, and place indoors no less than 48 hours；
Step 8：Once it is calcined：Mixture shove charge compressing in step 7 is calcined so that in-furnace temperature is rapidly achieved 350
DEG C, 5 DEG C for every eight hours of uniform intensification is then changed to, it is warming up to 520 DEG C and is kept for 24 hours, uniform intensification again rises for 27 DEG C for every eight hours
Temperature maintains close fire within 48 hours to 1250 DEG C in 1250 DEG C of stages of high temperature, and the mixture after roasting then is cooled down into 240 hours and stove
Interior temperature is come out of the stove when being less than 90 DEG C；
Step 9：Single-steeping：The impregnation mixture after being once calcined will be completed in medium temperature coal pitch, and with 50 DEG C -60 DEG C
The temperature rise speed of/h is heated to 300-500 degree, vacuumizes rear pressurize treatment, and single-steeping rate of body weight gain reaches 18-19%；
Step 10：After baking：By mixture shove charge after baking so that in-furnace temperature is rapidly achieved 350 DEG C, then it is changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 11：Double-steeping：The impregnation mixture after after baking will be completed in medium temperature coal pitch, and with 50 DEG C -60
DEG C/temperature rise speed of h is heated to 300-500 degree, vacuumizes rear pressurize treatment, single-steeping rate of body weight gain reaches 13-14%；
Step 12：Three roastings：By three roastings of mixture shove charge so that in-furnace temperature is rapidly achieved 350 DEG C, is then changed to
5 DEG C for every eight hours of even intensification, is warming up to 520 DEG C and is kept for 24 hours, and uniform intensification again is warming up to 1250 DEG C for 27 DEG C for every eight hours,
1250 DEG C of stages of high temperature maintain 48 hours to close fire, then cool down the mixture after roasting 240 hours and in-furnace temperature is less than 90
DEG C when come out of the stove；
Step 13：Three dippings：The impregnation mixture after three roastings will be completed in medium temperature coal pitch, vacuumized at rear pressurize
Reason, single-steeping rate of body weight gain reaches 9-10%；
Step 14：Graphitization：The mixture that step 13 is obtained is put into acheson furnace, is that product temperature reaches 2800-
2900 DEG C so that mixture graphitization.
2. a kind of production technology of polycrystalline silicon base plate special graphite as claimed in claim 1, it is characterised in that：Described step
The temperature control of pressing mold shaping is at 25-30 DEG C in 7.
3. a kind of production technology of polycrystalline silicon base plate special graphite as claimed in claim 1, it is characterised in that：Described step
Mixture test resistance rate after 14 graphitizations for obtaining, it is desirable in 12-13 μ Ω m.
Priority Applications (1)
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| CN201710031000.1A CN106744919A (en) | 2017-01-17 | 2017-01-17 | A kind of production technology of polycrystalline silicon base plate special graphite |
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Cited By (2)
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| CN110294479A (en) * | 2019-07-23 | 2019-10-01 | 中国恩菲工程技术有限公司 | The preparation facilities of carbon-silicon composite material |
| CN114031405A (en) * | 2021-10-27 | 2022-02-11 | 宝丰县五星石墨有限公司 | Manufacturing process and application of cold isostatic pressing graphite |
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| CN114031405A (en) * | 2021-10-27 | 2022-02-11 | 宝丰县五星石墨有限公司 | Manufacturing process and application of cold isostatic pressing graphite |
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Application publication date: 20170531 |
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| RJ01 | Rejection of invention patent application after publication |