CN113865357A - Production jig for artificial graphite film coiled material and process for producing artificial graphite film coiled material by using same - Google Patents
Production jig for artificial graphite film coiled material and process for producing artificial graphite film coiled material by using same Download PDFInfo
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- CN113865357A CN113865357A CN202111316744.0A CN202111316744A CN113865357A CN 113865357 A CN113865357 A CN 113865357A CN 202111316744 A CN202111316744 A CN 202111316744A CN 113865357 A CN113865357 A CN 113865357A
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- coiled material
- graphite film
- artificial graphite
- temperature
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- 239000000463 material Substances 0.000 title claims abstract description 59
- 229910021383 artificial graphite Inorganic materials 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000009423 ventilation Methods 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920001721 polyimide Polymers 0.000 claims abstract description 20
- 238000005087 graphitization Methods 0.000 claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 238000003723 Smelting Methods 0.000 claims abstract description 5
- 238000004804 winding Methods 0.000 claims abstract description 5
- 238000005096 rolling process Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000011800 void material Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 238000010304 firing Methods 0.000 abstract description 5
- 238000005520 cutting process Methods 0.000 abstract description 2
- 239000004642 Polyimide Substances 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a production jig for artificial graphite film coiled materials, which consists of a first cylinder and a second cylinder, wherein an inner cavity enclosed by the first cylinder and the second cylinder forms an accommodating cavity; the end faces of the first cylinder and the second cylinder are respectively provided with a bottom plate with a limiting nut, the first cylinder, the bottom plate of the first cylinder and the second cylinder are respectively provided with a ventilation circular hole, the first cylinder is provided with a limiting tip, and the second cylinder is provided with a limiting notch. The invention also discloses a process for producing the artificial graphite film coiled material by utilizing the jig, which comprises the following steps of 1) winding the polyimide film in the accommodating cavity; cutting a rectangular hole on the coiled material and placing the coiled material in the limit pin; 2) sending the smelting tool into a carbonization furnace for processing to obtain a carbon film coiled material; 3) extending the coiled material out of the outer ring of the smelting tool through the limiting notch, and then sending the coiled material into a graphitization furnace for processing to obtain a graphite film coiled material; 4) uncoiling and collecting; 5) and (5) rolling treatment. The holding cavity of the production jig can be fully utilized, and the apparent obvious defects can be greatly reduced by combining the auxiliary structure and firing the artificial graphite film by utilizing the holding cavity.
Description
Technical Field
The invention belongs to the technical field of graphite film preparation, and particularly relates to a production jig for an artificial graphite film coiled material and a process for producing the artificial graphite film coiled material by using the same.
Background
The high-thermal-conductivity artificial graphite film has excellent thermal conductivity and electrical conductivity, is commonly used for heat dissipation parts of semiconductor elements or other heating parts loaded in various electronic equipment such as computers, mobile phones and the like, and has very wide application prospect in the fields of microelectronic packaging and heat management in the integration field. In the preparation process of the high-thermal-conductivity artificial graphite film, the polyimide film is required to be loaded into a production jig for carbonization and graphitization. At present, two methods for manufacturing the high-thermal-conductivity artificial graphite film are mainly used, one method is a method for manufacturing the high-thermal-conductivity artificial graphite film sheet, and the polyimide film sheet is clamped between graphite papers and sequentially stacked in a sintering tool fixture for carbonization, graphitization and firing. This manufacturing method has a low space utilization rate and greatly affects the productivity. In addition, the polyimide film sheets at different positions are stressed by larger difference, so that the foaming thickness of the graphite film is uneven, and the product performance is influenced. The other method is a manufacturing method of the high-thermal-conductivity artificial graphite film coiled material, which comprises the steps of cutting the polyimide film into polyimide coiled materials with certain width and length, and then winding the polyimide coiled materials on a graphite cylinder of a production jig for carbonization and graphitization firing. Because the manufacturing method overcomes the defect of sheet firing, manufacturing enterprises have gradually transferred the manufacturing method of the high-thermal-conductivity artificial graphite film coiled material. However, there is still a certain disadvantage in the way of assembling the polyimide coil in the production jig. The polyimide coiled material is carbonized, graphitized and expanded in the containing cavity of the production jig, and is very easy to be limited by the volume of the containing cavity to cause the folding phenomenon, so that the appearance of the high-heat-conductivity artificial graphite film is not smooth. If the length of the polyimide coiled material is reduced, the problems can be solved, but the problems of insufficient space utilization rate and reduced production capacity exist. Therefore, it is necessary to design a production jig which can fully utilize the volume of the accommodating cavity and can burn the high-thermal-conductivity artificial graphite film without apparent defects.
Disclosure of Invention
Aiming at the defects and problems in the prior art, the invention aims to provide a production jig for artificial graphite film coiled materials.
The invention is realized by the following technical scheme:
the invention provides a production jig for an artificial graphite film coiled material, which consists of a first cylinder and a second cylinder, wherein the second cylinder is sleeved on the periphery of the first cylinder, and an inner cavity formed by the first cylinder and the second cylinder forms an artificial graphite film coiled material accommodating cavity;
a bottom plate with a limiting nut I is arranged on one end face of the first cylinder, a plurality of uniformly distributed ventilation round holes I are arranged in the radial direction of the cylinder body of the first cylinder, a plurality of uniformly distributed ventilation round holes II are arranged on the bottom plate of the first cylinder, and a row of uniformly distributed limiting tips protruding outwards are arranged in the radial direction of the cylinder body of the first cylinder;
a bottom plate with a limit nut II is arranged on one end face of the second cylinder, a plurality of uniformly distributed ventilation circular holes III are arranged in the radial direction of the second cylinder body, and a limit notch is arranged in the radial direction of the second cylinder;
the limiting bolt is matched with the limiting nut I and the limiting nut II in a homogeneous phase mode, the two ends of the limiting bolt are combined with the limiting nut I and the limiting nut II respectively, the first cylinder is connected with the second cylinder, and the transverse moving distance of the first cylinder and the second cylinder is limited.
Furthermore, the ventilation round holes I and the ventilation round holes III are arranged in 4-8 rows, and the diameters of the ventilation round holes I and the ventilation round holes III are 2-5 mm.
Furthermore, the number of the ventilation round holes II is 4-8, and the diameter of the ventilation round holes II is 2-10 mm.
Furthermore, the number of the limit pins is 2-4, and the length of the limit pins is 5-10 mm.
Furthermore, the width of the limiting notch is 2-5 mm.
The invention also provides a process for producing artificial graphite film coiled materials by using the graphite film coiled material jig, which comprises the following steps:
1) assembling coiled materials: winding a polyimide film in an accommodating cavity defined by a first cylinder and a second cylinder, wherein the void ratio is 40% -90%; the polyimide film coiled material is cut out of a rectangular hole close to one end of the first cylinder and is arranged in the limit pin of the first cylinder.
2) Carbonizing: and (3) feeding the jig wound with the polyimide film in the step 1) into a carbonization furnace for carbonization treatment. Carbonizing at the following program temperature control under the condition that the vacuum degree of a furnace chamber is 1-50 Pa: raising the temperature to 480-500 ℃ at a heating rate of 1-6 ℃/min, and keeping the temperature for 0.5-1 h; raising the temperature to 600-700 ℃ at a heating rate of 0.5-2 ℃/min, and keeping the temperature for 0.5-1 h; raising the temperature to 1000-1400 ℃ at a heating rate of 0.5-4 ℃/min, and keeping the temperature for 0.5-1 h. Cooling to room temperature to obtain the carbon film coil.
3) Graphitization: one end of the carbon film coiled material prepared in the step 2) is close to the second cylinder and extends out of the outer ring of the smelting tool through a second cylinder limiting notch; sending the jig with the wound carbon film into a graphitization furnace for graphitization treatment; under the protection of flowing argon, the graphitization is carried out according to the following program temperature control: raising the temperature rise rate to 1000 ℃ at a speed of 20 ℃/min; raising the temperature rise rate to 1800-2000 ℃ at 4-6 ℃/min, and keeping the temperature for 0.5-1 h; the temperature rise rate is increased to 2700-2850 ℃ at the speed of 3-5 ℃/min, and the temperature is kept for 0.5-1 h. Cooling to room temperature to obtain the graphite film coiled material.
4) And (5) uncoiling and collecting.
5) And (5) rolling treatment.
Compared with the prior art, the invention has the beneficial effects that:
(1) the accommodating cavity of the production jig is formed by enclosing the first cylinder and the second cylinder, the accommodating cavity can be fully utilized, and meanwhile, the accommodating cavity is arranged by auxiliary structures such as a limiting pin, a ventilating round hole, a limiting notch and the like, and apparent defects can be greatly reduced by firing the artificial graphite film.
(2) The invention limits the transverse movement caused by the expansion or contraction of the inner ring end of the coiled material through the first cylinder limiting pin;
a sufficient transverse moving space is provided for the expansion of the outer ring end of the coiled material through the second cylinder limiting notch; the arrangement of the ventilation round holes is beneficial to the decomposition and exhaust of the polyimide coiled material.
(3) The production jig is adopted to prepare the artificial graphite film coiled material, the process is extremely simple, the operation is easy, the cost is low, and the production jig is suitable for industrial large-scale production.
Drawings
Fig. 1 is a cross-sectional view of the artificial graphite film coil production jig of the present invention.
Fig. 2 is a top view of the artificial graphite film coil production jig of the present invention.
FIG. 3 is a schematic front view of a first cylinder of the tool for manufacturing artificial graphite film coiled material according to the present invention.
FIG. 4 is a schematic top view of a first cylinder of the tool for manufacturing artificial graphite film coiled material according to the present invention.
FIG. 5 is a schematic front view of a second cylinder of the tool for manufacturing artificial graphite film coil according to the present invention.
FIG. 6 is a schematic top view of a second cylinder of the tool for manufacturing artificial graphite film coiled material according to the present invention.
Illustration of the drawings: : 100-a first cylinder; 101-a limit nut I; 102-vent circular hole I; 103-a ventilation circular hole II; 104-a limit pin; 105-a limit bolt; 200-a second cylinder; 201-limit nut II; 202-vent round hole III; 203-limit notch.
In the description of the present invention, the terms "radial", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, and integrally connected; can be mechanical connection and electrical connection; may be directly connected, indirectly connected through intervening agents, or may be interconnected between two elements. The specific meaning of the above terms in the present invention can be specifically understood by those of ordinary skill in the art.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, which are simplified schematic drawings and illustrate only the basic structure of the present invention, and therefore, only show the structures related to the present invention.
As shown in fig. 1-6, fig. 1 is a cross-sectional view of the artificial graphite film coil production jig of the present invention. Fig. 2 is a top view of the artificial graphite film coil production jig of the present invention. FIG. 3 is a schematic front view of a first cylinder of the tool for manufacturing artificial graphite film coiled material according to the present invention. FIG. 4 is a schematic top view of a first cylinder of the tool for manufacturing artificial graphite film coiled material according to the present invention. FIG. 5 is a schematic front view of a second cylinder of the tool for manufacturing artificial graphite film coil according to the present invention. FIG. 6 is a schematic top view of a second cylinder of the tool for manufacturing artificial graphite film coiled material according to the present invention.
A production jig for artificial graphite film coiled materials is composed of a first cylinder 100 and a second cylinder 200, wherein the second cylinder 200 is sleeved on the periphery of the first cylinder 100, and an inner cavity formed by the first cylinder 100 and the second cylinder 200 in a surrounding mode forms an artificial graphite film coiled material accommodating cavity.
A bottom plate with a limiting nut I101 is arranged on one end face of the first cylinder 100, 4-8 rows of uniformly distributed ventilation round holes I102 with the diameter of 2-5mm are arranged in the radial direction of the cylinder body of the first cylinder 100, 4-8 uniformly distributed ventilation round holes II 103 with the diameter of 2-10mm are arranged on the bottom plate of the first cylinder 100, and a row of 2-4 outwards-protruding and uniformly-distributed limiting tips 104 with the length of 5-10mm are arranged in the radial direction of the cylinder body of the first cylinder 100.
A bottom plate with a limit nut II 201 is arranged on one end face of the second cylinder 200, 4-8 rows of uniformly distributed ventilation round holes III202 with the diameter of 2-5mm are arranged in the radial direction of the cylinder body of the second cylinder 200, and a limit notch 203 with the width of 2-5mm is arranged in the radial direction of the second cylinder 200.
In a specific implementation, when the second cylinder 200 is sleeved on the periphery of the first cylinder 100, the position of the limiting nut I101 corresponds to that of the limiting nut II 201, and the through fastening hole is formed between the limiting nut I101 and the limiting nut II 201.
The invention is also provided with a limit bolt 105 matched with the limit nut I101 and the limit nut II 201, and the two ends of the limit bolt 105 are respectively combined with the limit nut I101 and the limit nut II 201, namely the limit bolt 105 is inserted into the fastening hole and screwed and fixed, so that the bottom plates of the first cylinder 100 and the second cylinder 200 are fixedly connected, the first cylinder 100 and the second cylinder 200 are fastened and connected, and the transverse moving distance of the first cylinder 100 and the second cylinder 200 is limited.
A process for producing artificial graphite film coiled materials by utilizing the production jig comprises the following steps:
1) assembling coiled materials: winding a polyimide film in an accommodating cavity surrounded by the first cylinder 100 and the second cylinder 200, wherein the void ratio is 50%; the polyimide film roll is cut out of a rectangular hole near one end of the first cylinder 100 and placed in the stop pin 104 of the first cylinder 100.
2) Carbonizing: and (3) feeding the jig wound with the polyimide film in the step 1) into a carbonization furnace for carbonization treatment. Carbonizing at the following program temperature control under the condition that the vacuum degree of a furnace chamber is 1-50 Pa: heating to 500 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 0.5 h; heating to 650 ℃ at the heating rate of 1 ℃/min, and keeping the temperature for 1 h; raising the temperature to 1200 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 0.5 h. Cooling to room temperature to obtain the carbon film coil.
3) Graphitization: and (3) extending one end of the carbon film coiled material prepared in the step 2) close to the second cylinder 200 to the outer ring of the smelting tool through a limiting gap of the second cylinder 200. And feeding the jig with the wound carbon film into a graphitization furnace for graphitization treatment. Under the protection of flowing argon, the graphitization is carried out according to the following program temperature control: raising the temperature rise rate to 1000 ℃ at a speed of 20 ℃/min; raising the temperature rise rate to 2000 ℃ at the speed of 6 ℃/min, and keeping the temperature for 0.5 h; the temperature rise rate of 3 ℃/min is increased to 2800 ℃, and the temperature is preserved for 0.5 h. Cooling to room temperature to obtain the graphite film coiled material.
4) And (5) uncoiling and collecting.
5) And (5) rolling treatment.
By adopting the production jig of the artificial graphite film and the process for producing the artificial graphite film coiled material by using the production jig, the production yield of the graphite film coiled material reaches 95 percent, and the apparent defect is avoided.
The foregoing merely represents preferred embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. The utility model provides a production smelting tool of artifical graphite membrane coiled material which characterized in that: the production jig comprises a first cylinder (100) and a second cylinder (200), wherein the second cylinder (200) is sleeved on the periphery of the first cylinder (100), and an inner cavity surrounded by the first cylinder (100) and the second cylinder (200) forms an artificial graphite film coiled material accommodating cavity;
a bottom plate with a limiting nut I (101) is arranged on one end face of the first cylinder (100), a plurality of uniformly distributed ventilation round holes I (102) are arranged in the radial direction of the cylinder body of the first cylinder (100), a plurality of uniformly distributed ventilation round holes II (103) are arranged on the bottom plate of the first cylinder (100), and a row of uniformly distributed limiting tips (104) protruding outwards are arranged in the radial direction of the cylinder body of the first cylinder (100);
a bottom plate with a limit nut II (201) is arranged on one end face of the second cylinder (200), a plurality of uniformly distributed ventilation circular holes III (202) are arranged in the radial direction of the cylinder body of the second cylinder (200), and limit notches (203) are arranged in the radial direction of the second cylinder (200);
the first cylinder (100) and the second cylinder (200) are connected through the limiting bolt (105) which is matched with the limiting nut I (101) and the limiting nut II (201) respectively and the two ends of the limiting bolt (105) are combined with the limiting nut I (101) and the limiting nut II (201).
2. The production tool of the artificial graphite film coiled material according to claim 1, characterized in that: the ventilation round holes I (102) and the ventilation round holes III (202) are arranged in 4-8 rows, and the diameters of the ventilation round holes I and the ventilation round holes III are 2-5 mm.
3. The production tool of the artificial graphite film coiled material according to claim 1, characterized in that: the number of the ventilation round holes II (103) is 4-8, and the diameter of the ventilation round holes II is 2-10 mm.
4. The production tool of the artificial graphite film coiled material according to claim 1, characterized in that: the number of the limit pins (104) is 2-4, and the length of the limit pins is 5-10 mm.
5. The production tool of the artificial graphite film coiled material according to claim 1, characterized in that: the width of the limiting notch (203) is 2-5 mm.
6. A process for producing artificial graphite film coiled materials by using the production jig as claimed in any one of claims 1 to 5, which is characterized by comprising the following steps:
1) assembling coiled materials: winding a polyimide film in an accommodating cavity defined by a first cylinder (100) and a second cylinder (200), wherein the void ratio is 40% -90%; one end of the polyimide film coiled material close to the first cylinder (100) is cut into a rectangular hole and is arranged in a limit pin (104) of the first cylinder (100);
2) carbonizing: sending the jig wound with the polyimide film in the step 1) into a carbonization furnace for carbonization treatment, controlling the temperature under the condition that the vacuum degree of the furnace chamber is 1-50Pa for carbonization, and cooling to room temperature to obtain a carbon film coiled material;
3) graphitization: one end of the carbon film coiled material prepared in the step 2) close to the second cylinder (200) extends out of the outer ring of the jig through a limiting notch (203) of the second cylinder (200), the jig wound with the carbon film is sent into a graphitization furnace for graphitization treatment, the temperature is controlled under the protection of flowing argon for graphitization, and the graphite film coiled material is obtained after cooling to room temperature;
4) uncoiling and collecting;
5) and (5) rolling treatment.
7. The process for producing an artificial graphite film coil according to claim 6, wherein the temperature control in step 2) is performed according to the following procedure: raising the temperature to 480-500 ℃ at a heating rate of 1-6 ℃/min, and keeping the temperature for 0.5-1 h; raising the temperature to 600-700 ℃ at a heating rate of 0.5-2 ℃/min, and keeping the temperature for 0.5-1 h; raising the temperature to 1000-1400 ℃ at a heating rate of 0.5-4 ℃/min, and keeping the temperature for 0.5-1 h.
8. The process for producing an artificial graphite film coil according to claim 6, wherein the temperature control in step 3) is performed according to the following procedure: : raising the temperature rise rate to 1000 ℃ at a speed of 20 ℃/min; raising the temperature rise rate to 1800-2000 ℃ at 4-6 ℃/min, and keeping the temperature for 0.5-1 h; the temperature rise rate is increased to 2700-2850 ℃ at the speed of 3-5 ℃/min, and the temperature is kept for 0.5-1 h.
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|---|---|---|---|
| CN202111316744.0A CN113865357B (en) | 2021-11-08 | 2021-11-08 | Production jig for artificial graphite film coiled material and process for producing artificial graphite film coiled material by using production jig |
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|---|---|---|---|
| CN202111316744.0A CN113865357B (en) | 2021-11-08 | 2021-11-08 | Production jig for artificial graphite film coiled material and process for producing artificial graphite film coiled material by using production jig |
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| JP2021067409A (en) * | 2019-10-24 | 2021-04-30 | 柴田 勝美 | Heating treatment device |
| CN216205345U (en) * | 2021-11-08 | 2022-04-05 | 江西昌大高新能源材料技术有限公司 | Production smelting tool for artificial graphite film coiled material |
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