CN113373505B - Single crystal furnace thermal field heat preservation cylinder and preparation method thereof - Google Patents
Single crystal furnace thermal field heat preservation cylinder and preparation method thereof Download PDFInfo
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- CN113373505B CN113373505B CN202110733046.4A CN202110733046A CN113373505B CN 113373505 B CN113373505 B CN 113373505B CN 202110733046 A CN202110733046 A CN 202110733046A CN 113373505 B CN113373505 B CN 113373505B
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- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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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
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- C30B29/06—Silicon
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Abstract
The invention discloses a thermal field heat-preserving cylinder of a single crystal furnace and a preparation method thereof, belonging to the technical field of thermal field materials for high temperature furnaces. The heat-preservation cylinder of the thermal field of the single crystal furnace is formed by combining six heat-preservation cylinder sheets, the heat-preservation cylinder sheets are combined through concave-convex grooves, the six heat-preservation cylinder sheets are divided into an A sheet and a B sheet, and the A sheet and the B sheet are respectively combined in a staggered mode at intervals; the preparation process of the A tablet comprises the following steps: superposing carbon fiber cloth and polyester aramid fiber mixed fiber, dipping the pre-immersion liquid, then spreading the pre-immersion liquid in a mould, performing hot-pressing curing and carbonizing; the preparation process of the B tablet comprises the following steps: impregnating carbon fiber cloth with resin, spreading in a mould, hot-pressing for curing, and carbonizing. The defects of easy deformation and difficult production in the whole manufacturing process are avoided, and meanwhile, the heat-insulating cylinder is easy to disassemble and assemble when being applied to a thermal field of a single crystal furnace, so that the inconvenience brought by carrying and applying the whole heat-insulating cylinder is avoided. And the combined heat-insulating cylinder has high mechanical and thermophysical properties, good dimensional stability and long service life.
Description
Technical Field
The invention belongs to the technical field of thermal field materials for high-temperature furnaces, and particularly relates to a thermal field heat-preserving cylinder of a single crystal furnace and a preparation method thereof.
Background
The high-temperature furnace is widely applied as indispensable equipment in the traditional industrial fields such as powder metallurgy, the new material and energy field and the national defense industry. The thermal field of the single crystal furnace contains an upper heat-preserving cylinder, a middle heat-preserving cylinder and a lower heat-preserving cylinder which are made of graphite or carbon-carbon composite materials; generally, in order to achieve better heat preservation effect, the heat preservation cylinder is placed in the curing heat preservation cylinder. At first, the heat preservation cylinder is made of graphite, so that the energy consumption and the production cost are high. The large-size graphite heat-insulating cylinder is high in processing cost, the source of the graphite ingot is single, the material can be replaced in order to reduce the cost, the carbon-carbon composite material becomes the preferred material due to the excellent physicochemical property, the heat-insulating cylinder produced by the carbon-carbon composite material is low in cost and convenient to process. For the small-sized heat preservation cylinder, an integral forming processing method is generally adopted: and paving the net and the woven cloth on a heat-insulating cylinder mould layer by layer, puncturing layer by using a puncturing needle of a puncturing cylinder machine, stopping puncturing when the number of layers reaches the required number of layers, and demoulding to obtain the heat-insulating cylinder preform. And after the inspection is qualified, a finished product of the heat-insulating cylinder is prepared by adopting vapor deposition.
Chinese patent application 201210230677.5 discloses a carbon/silicon carbide composite material heat-insulating cylinder with simple preparation process and silicon vapor erosion resistance and a preparation method thereof, which is characterized in that the carbon/silicon carbide composite material heat-insulating cylinder is prepared by carrying out alternate densification on pyrolytic carbon and silicon carbide or mixed densification on pyrolytic carbon and silicon carbide on a carbon fiber preform of the heat-insulating cylinder by adopting a chemical vapor infiltration method, and then machining and purifying the mixture, wherein the density of the carbon/silicon carbide composite material heat-insulating cylinder is 1.3g/cm 3 -2.5g/cm 3 Bending strength is more than or equal to 300MPa, and fracture toughness is more than or equal to 15 MPa.m 1/2 The invention can effectively inhibit the erosion of silicon vapor to the carbon fiber of the core part of the carbon/silicon carbide composite material, the bending strength of the prepared carbon/silicon carbide composite material is more than 300MPa and is 2-5 times of the carbon/carbon composite material, and the fracture toughness is more than or equal to 15 MPa.m 1/2 Compared with the carbon/carbon composite material, the silicon vapor corrosion resistance is improved by 5-10 times, the service life of the heat-insulating cylinder is greatly prolonged, and the higher strength is also beneficial to improving the safety of a thermal field.
With the demand of the thermal field of the single crystal furnace for the large-size heat preservation cylinder, how to well produce the large-size heat preservation cylinder becomes a great hotspot of research.
Chinese patent application 200810236547.6 discloses a method for preparing a carbon/carbon composite material cylinder for a high temperature furnace, which comprises the steps of dipping carbon fiber cloth into high temperature phenolic resin by a dipping machine to obtain a carbon fiber adhesive tape; controlling the winding tension of the carbon fiber adhesive tape through a tension controller, and pressurizing and curing the wound product after the product is wound; carbonizing the product; selectively performing densification according to the density of the carbonized product; according to the using conditions of the high-temperature furnace, performing high-temperature treatment on the product, and adjusting the comprehensive performance of the product; and finally, machining the product according to a drawing to obtain the carbon/carbon composite material cylindrical product for the high-temperature furnace. The invention is due to the adoption ofThe final density of the carbon/carbon composite material cylinder is more than or equal to 1.25g/cm 3 The plane tensile strength is high, the size is basically not limited, machining is not needed in the thickness direction, the cost performance advantage is excellent, the cost of the carbon/carbon cylindrical part for the high-temperature furnace can be obviously reduced, the process consistency is good, and the implementation performance is strong.
However, for the heat-insulating cylinder with larger size, the manufacturing difficulty is high, the heat-insulating cylinder with the whole large size is easy to deform during production, and the problem of unqualified size or difficult processing and forming exists in the subsequent quality inspection process of processing the heat-insulating cylinder into a finished product.
In view of the above, the applicant finds in experimental exploration that the heat preservation cylinder can be assembled together in a six-piece manner by a splicing method to form a complete large-size heat preservation cylinder. When the heat preservation cylinder is processed, each petal of the heat preservation cylinder is processed respectively, and the six petals are spliced together in an occlusion mode after each petal is processed and formed, so that the defects that the whole manufacturing process is easy to deform and difficult to produce are overcome, and meanwhile, the heat preservation cylinder is easy to disassemble and assemble when applied to a thermal field of a single crystal furnace, and inconvenience brought by carrying and application of the whole heat preservation cylinder is avoided.
Disclosure of Invention
The invention aims to provide a single crystal furnace thermal field heat preservation cylinder and a preparation method thereof, which avoid the defects of easy deformation and difficult production in the whole manufacturing process, are easy to disassemble and assemble when being applied to a single crystal furnace thermal field, and avoid the inconvenience caused by carrying and applying the whole heat preservation cylinder. And the combined heat-insulating cylinder has high mechanical and thermophysical properties, good dimensional stability and long service life.
In order to achieve the purpose, the technical scheme of the invention is as follows:
on one hand, the invention provides a thermal field heat preservation cylinder of a single crystal furnace, which is formed by combining six heat preservation cylinder pieces, wherein the heat preservation cylinder pieces are matched through concave-convex grooves, the six heat preservation cylinder pieces are divided into an A piece and a B piece, and the A piece and the B piece are respectively provided with three pieces which are alternately combined at intervals.
The preparation process of the A tablet comprises the following steps: superposing carbon fiber cloth and polyester aramid fiber mixed fiber, dipping the pre-immersion liquid, then spreading the pre-immersion liquid in a mould, performing hot-pressing curing and carbonizing;
the preparation process of the B tablet comprises the following steps: impregnating carbon fiber cloth with resin, spreading in a mould, hot-pressing for curing, and carbonizing.
By combining the heat-insulating cylinder sheets with different preparation processes, excellent performance can be achieved, meanwhile, the preparation cost is reduced to the greatest extent, and the preparation method is simplified.
Preferably, the heat preservation cylinder further comprises a circular ring buckle, and the circular ring buckle is fixed at the upper position and the lower position of the heat preservation cylinder respectively.
Preferably, in the preparation process of the A sheet, the length of the polyester-aramid mixed fiber is 1-5 mm.
Preferably, in the preparation process of the A sheet, in the polyester-aramid mixed fiber, the mass ratio of the polyester to the aramid is 3-8:1, and more preferably 4.5: 1.
Preferably, in the preparation process of the A sheet, the mass ratio of the carbon fiber cloth to the polyester aramid fiber mixed fiber is 3-10:2, and more preferably 5: 2.
Preferably, in the preparation process of the A sheet, the carbon fiber cloth and the polyester-aramid mixed fiber are overlapped, namely, one layer of polyester-aramid mixed fiber is paved every 1-3 layers of carbon fiber cloth are paved.
Preferably, in the preparation process of the A sheet, the pre-impregnation liquid consists of acetone, epoxy resin, coal tar pitch and nano-fibers. More preferably, in the pre-impregnation liquid, the mass ratio of the acetone to the epoxy resin to the coal pitch to the nanofibers is 15-30:1-8:1-8:1-5, and more preferably 20:4:4: 3.
Preferably, in the preparation process of the sheet A and the preparation process of the sheet B, the hot-pressing curing is as follows:
pressurizing to 1Kg/cm 2 Heating to 100-;
heating to 150 ℃ and 180 ℃ at a speed of 100 ℃/h, and keeping the temperature and the pressure for 90 minutes;
pressurizing 2Kg/cm 2 Heating to 200-;
regulating the pressure to 1Kg/cm 2 And cooling to below 75 ℃.
Preferably, in the preparation process of the sheet A and the preparation process of the sheet B, release paper is laid in advance in a mold.
Preferably, in the preparation process of the sheet a and the preparation process of the sheet B, the carbonization refers to:
the temperature of the carbonization furnace is raised to 180 ℃ at a heating rate of 100 ℃/h, then to 250 ℃ at a heating rate of 50 ℃/h, and then to 1000 ℃ at a heating rate of 500 ℃/h.
Preferably, in the preparation process of the B sheet, the resin is at least one selected from epoxy resin, phenolic resin and furan resin.
Preferably, the carbonization can be completed and the temperature can be kept for 1h at 2000 ℃.
In another aspect, the invention provides a method for preparing the thermal field heat preservation cylinder of the single crystal furnace, which comprises the following steps:
(1) preparation of a tablet: superposing carbon fiber cloth and polyester aramid fiber mixed fiber, dipping pre-immersion liquid, then spreading in a mould, hot-pressing for curing, and carbonizing;
(2) preparation of a B tablet: impregnating carbon fiber cloth with resin, flatly spreading in a mould, performing hot-pressing curing, and carbonizing;
(3) three A pieces and three B pieces are selected to be alternately combined into a cylinder shape.
Compared with the prior art, the invention has the beneficial effects that:
(1) the split type heat insulation barrel is manufactured in a split manufacturing mode, the defects that the whole manufacturing process is easy to deform and not easy to produce are overcome, the disassembly and the assembly are simple, and the inconvenience caused by carrying and application of the whole large heat insulation barrel is avoided.
(2) The combined heat-insulating cylinder has high mechanical and thermal properties, good stability and long service life.
(3) The combination of the heat preservation cylinder sheets with different performances is adopted, so that the cost is saved to the greatest extent while the optimal performance is kept.
Drawings
Fig. 1 is a schematic structural view of the heat preservation cylinder, wherein the heat preservation cylinder comprises a 1-circular buckle, a 2-A sheet and a 3-B sheet.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way. The following is merely an exemplary illustration of the scope of the invention as claimed, and various changes and modifications of the invention of the present application may be made by those skilled in the art based on the disclosure, which also fall within the scope of the invention as claimed.
The present invention will be further described below by way of specific examples. The various chemicals used in the examples of the present invention were obtained by conventional commercial routes unless otherwise specified.
In the embodiment described below, it is preferred that,
the carbon fiber cloth is polyacrylonitrile-based carbon fiber cloth;
the polyester-aramid mixed fiber is formed by mixing aramid fiber and polyester fiber, and the length range is 1-5 mm;
the nanofibers are microfibrillated cellulose (MFC);
the epoxy resin is Dow DER 671.
Basic embodiment
1. Preparation of A tablets
(1) Carbon fiber cloth and polyester-aramid mixed fiber are overlapped, and one layer of polyester-aramid mixed fiber is paved every 2 layers of carbon fiber cloth, the mass ratio of polyester to aramid in the polyester-aramid mixed fiber is 4.5:1, and the mass ratio of the carbon fiber cloth to the polyester-aramid mixed fiber is 5:2, so that a mixed part 1 is obtained.
(2) Mixing acetone, epoxy resin, coal tar pitch and nano-fiber according to a ratio of 20:4:4:3, heating to 95 ℃, uniformly obtaining impregnation liquid, completely immersing the mixed piece in the impregnation liquid, wherein the mass ratio of the mixed piece to the impregnation liquid is 1:10, immersing for 30min at the temperature, and taking out to obtain a mixed piece 2.
(3) The mixed part 2 is flatly laid in a mould, hot-pressed and solidified, carbonized, cooled after heat preservation, and an A sheet is obtained;
the hot-pressing solidification is as follows:
pressurizing to 1Kg/cm 2 Heating to 110 ℃ at a speed of 100 ℃/h, preserving heat and maintaining pressure for 60 minutes;
heating to 160 ℃ at a speed of 100 ℃/h, preserving heat and maintaining pressure for 90 minutes;
pressurizing 2Kg/cm 2 Heating to 220 ℃ at a speed of 100 ℃/h, preserving heat and maintaining pressure for 60 minutes;
regulating the pressure to 1Kg/cm 2 And cooling to below 75 ℃.
Carbonizing into:
the temperature of the carbonization furnace is increased to 150 ℃ at the heating rate of 100 ℃/h, then is increased to 250 ℃ at the heating rate of 50 ℃/h, and then is increased to 1000 ℃ at the heating rate of 50 ℃/h.
Finally, the temperature is kept for 1h at 2000 ℃.
2. Preparation of B tablets
Impregnating the carbon fiber cloth with epoxy resin by a impregnator, flatly paving the carbon fiber cloth in a mould, performing hot-pressing solidification and carbonization according to the conditions in the preparation process of the A sheet, and cooling after heat preservation to obtain a B sheet;
3. preparation of heat-insulating cylinder
Cooling the sheets A and B, selecting three sheets A and three sheets B, fitting by using concave-convex grooves on the side surfaces, alternately combining into a cylinder shape, and fixing by using circular buckles respectively as shown in figure 1.
Preparation of A1-A5
The preparation of tablets A is carried out according to the basic examples, with only the parameters in the following table being changed:
table 1.
Preparation of A6-A7
The preparation of tablets A is carried out according to the basic examples, with only the parameters in the following table being changed:
TABLE 2 composition of pre-dip
| Parts by weight | A6 | A7 |
| Acetone (II) | 15 | 30 |
| |
1 | 8 |
| Coal tar pitch | 8 | 1 |
| Nano-fiber | 5 | 1 |
Examples 1 to 7
The combination was made in the following manner to prepare a heat-insulating cylinder.
Table 3.
| Combination mode | |
| Example 1 | A1-B |
| Example 2 | A2-B |
| Example 3 | A3-B |
| Example 4 | A4-B |
| Example 5 | A5-B |
| Example 6 | A6-B |
| Example 7 | A7-B |
Comparative example 1
The mold was changed to prepare an 8-piece heat-insulating cylinder, and the rest was the same as in example 1.
Comparative example 2
The mold was changed to prepare a 4-piece heat-insulating cylinder, and the rest was the same as in example 1.
Comparative example 3
Preparing the heat preservation cylinder by combining six B sheets.
Comparative example 4
The heat preservation cylinder is prepared by combining six sheets of A1 sheets.
Comparative example 5
Unlike example 1, a sheet a (A8) was prepared without adding the polyester-aramid hybrid fiber.
Comparative examples 6 to 7
Unlike example 1, a tablet was prepared with the following parameters varied.
Table 4.
Comparative examples 8 to 10
Unlike example 3, a tablet was prepared with the following parameters varied.
TABLE 5 composition of the Pre-infusion
Result testing
1. The physical parameters, mechanical properties, thermal properties, etc. of A1-13 and B were tested (handling temperature 2400 ℃ C.) (2500 ℃ C.), and the results are given in the following table:
table 6.
2. The heat-insulating cylinders prepared in the examples and the comparative examples were used on a single-crystal silicon stretching furnace, and the number of times of use was recorded until problems of surface deformation, peeling, cracking, corrosion, and the like occurred.
Table 7.
In conclusion, the heat-insulating cylinder has the advantages that the high performance and the low cost are realized through the improvement and optimization of the preparation process, the raw materials and the combination mode, the service life is greatly prolonged compared with the heat-insulating cylinder prepared from common materials, the defect of the performance of the B sheet is relieved under the combined action of the A sheet and the B sheet by using the six-section staggered combination mode, the highest durability and the lowest cost are realized, the split combination is convenient, and the transportation and the maintenance are more convenient.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The single crystal furnace thermal field heat preservation cylinder is characterized by being formed by combining six heat preservation cylinder pieces, wherein the heat preservation cylinder pieces are matched through concave-convex grooves, the six heat preservation cylinder pieces are divided into an A piece and a B piece, and the A piece and the B piece are respectively combined in a staggered mode at intervals;
the preparation process of the A tablet comprises the following steps: superposing carbon fiber cloth and polyester aramid fiber mixed fiber, dipping pre-immersion liquid, then spreading in a mould, hot-pressing for curing, and carbonizing;
the preparation process of the B tablet comprises the following steps: impregnating carbon fiber cloth with resin, spreading in a mould, hot-pressing for curing, and carbonizing.
2. The single crystal furnace thermal field heat preservation cylinder of claim 1, further comprising a circular ring buckle, which is fixed at the upper and lower positions of the heat preservation cylinder respectively.
3. The single crystal furnace thermal field heat preservation cylinder according to claim 1, wherein in the preparation process of the A sheet, the length of the polyester-aramid fiber mixed fiber is 1-5 mm.
4. The single crystal furnace thermal field heat preservation cylinder according to claim 1, characterized in that in the polyester-aramid mixed fiber, the mass ratio of the polyester to the aramid is 3-8: 1.
5. The single crystal furnace thermal field heat preservation cylinder according to claim 1, wherein in the preparation process of the A sheet, the mass ratio of the carbon fiber cloth to the polyester aramid fiber mixed fiber is 3-10: 2.
6. The single crystal furnace thermal field heat preservation cylinder according to claim 1, characterized in that in the preparation process of the A sheet, the carbon fiber cloth and the polyester aramid fiber mixed fiber are overlapped, namely, one layer of polyester aramid fiber mixed fiber is paved every 1-3 layers of carbon fiber cloth.
7. The single crystal furnace thermal field heat preservation cylinder according to claim 1, wherein in the A sheet preparation process, the pre-immersion liquid is composed of acetone, epoxy resin, coal tar pitch and nano fibers.
8. The single crystal furnace thermal field heat preservation cylinder according to claim 7, wherein in the A sheet preparation process, the mass ratio of acetone, epoxy resin, coal pitch and nano fibers in the pre-immersion liquid is 15-30:1-8:1-8: 1-5.
9. The single crystal furnace thermal field heat preservation cylinder according to claim 1, wherein in the A sheet preparation process and the B sheet preparation process, the hot-pressing solidification is as follows:
pressurizing to 1Kg/cm 2 Heating to 100-;
heating to 150 ℃ and 180 ℃ at a speed of 100 ℃/h, and keeping the temperature and the pressure for 90 minutes;
pressurizing 2Kg/cm 2 Heating to 200-;
regulating the pressure to 1Kg/cm 2 And cooling to below 75 ℃.
10. The preparation method of the single crystal furnace thermal field heat preservation cylinder of any one of claims 1 to 9 is characterized by comprising the following steps:
(1) preparation of a tablet: superposing carbon fiber cloth and polyester aramid fiber mixed fiber, dipping the pre-immersion liquid, then spreading the pre-immersion liquid in a mould, performing hot-pressing curing and carbonizing;
(2) preparation of a B tablet: impregnating carbon fiber cloth with resin, spreading in a mold, performing hot-pressing curing, and carbonizing;
(3) three A pieces and three B pieces are selected to be alternately combined into a cylinder shape.
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