CN112157929B - Hot-press forming and demoulding method for short fiber reinforced carbon/resin composite material - Google Patents
Hot-press forming and demoulding method for short fiber reinforced carbon/resin composite material Download PDFInfo
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- CN112157929B CN112157929B CN202011026835.6A CN202011026835A CN112157929B CN 112157929 B CN112157929 B CN 112157929B CN 202011026835 A CN202011026835 A CN 202011026835A CN 112157929 B CN112157929 B CN 112157929B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/44—Moulds or cores; Details thereof or accessories therefor with means for, or specially constructed to facilitate, the removal of articles, e.g. of undercut articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/44—Moulds or cores; Details thereof or accessories therefor with means for, or specially constructed to facilitate, the removal of articles, e.g. of undercut articles
- B29C33/48—Moulds or cores; Details thereof or accessories therefor with means for, or specially constructed to facilitate, the removal of articles, e.g. of undercut articles with means for collapsing or disassembling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
- B29C33/60—Releasing, lubricating or separating agents
Abstract
The invention discloses a hot-press molding and demolding method for short fiber reinforced carbon/resin composite materials, which comprises the following steps: (1) the hot-press forming demoulding is carried out by using a surface C, N co-cementation technology of the 65Mn partition plate, and the 65Mn partition plate is subjected to carbonitriding by adopting a method of dripping methanol and introducing ammonia gas; (2) the release agent for hot-press forming and demoulding comprises the specific components of 10-30% of flaky graphite powder, 20-40% of nano-scale cubic boron nitride powder and 30-50% of mixed powder of nano-scale zirconia powder, and polyethylene glycol is used as a binder. The invention has simple process and easily controlled process parameters, improves the finish, the hot-press-resistant embedding performance and the hot-press-resistant die bonding performance of the polished clapboard for hot-press molding, and obviously improves the surface quality and the production efficiency of the hot-press short fiber reinforced carbon/resin composite material.
Description
Technical Field
The invention relates to a carbon/carbon composite material and a preparation technology thereof, in particular to a hot-press molding and demolding method of a short fiber reinforced carbon/resin composite material.
Background
The carbon fiber reinforced carbon-based composite material has the characteristics of low density, high thermal conductivity, high specific strength, specific modulus, low thermal expansion coefficient, ablation resistance, thermal shock resistance and the like, and is widely applied to the technical fields of high-temperature and wear-resistant aerospace such as rocket nozzles, space shuttles and the like. At present, with the continuous promotion of research on carbon/carbon composite materials, the application range of the carbon/carbon composite materials is gradually expanded to various fields such as nuclear energy, chemical engineering, medical and civil materials. Due to its excellent properties, carbon/carbon composites are an ideal target for their wide application.
The production process of electrolytic manganese dioxide mainly adopts copper, graphite or carbon rods as cathodes, and the copper cathodes are easy to corrode and can be adsorbed into electrolytic products to influence the product quality. The graphite cathode and the carbon rod cathode are easy to break in the use process due to high brittleness of materials and need to be replaced continuously. And the graphite cathode and the carbon rod cathode can not be enlarged and can only be applied to the production of small electrolytic cells. The short fiber reinforced carbon/resin composite material can be prepared into large-size plates by compression molding. Then the high-strength and high-toughness carbon/carbon composite material is prepared through the processes of carbonization, graphitization, CVI and the like in sequence and is used as a cathode material for electrolytic manganese dioxide.
However, when the large-size short fiber reinforced carbon/resin composite material is molded, the resin is very easy to adhere to the surface of a mold, the demolding resistance is large after curing, and the surface quality of a blank body is influenced after demolding. The mould is in need constantly to go on polishing to upper and lower mould towards and bed die inner wall in the used repeatedly process, and long-term the use will influence the cooperation of mould.
Disclosure of Invention
The invention aims to solve the technical problem of providing a demoulding method for hot-press forming of short fiber reinforced carbon/resin composite materials aiming at the defects of the demoulding technology. The 65Mn partition plate subjected to surface treatment is added between the blank and the upper punch and the lower punch, so that the blank is prevented from being directly contacted with the upper punch and the lower punch, and meanwhile, the 65Mn partition plate subjected to surface treatment has higher hardness, so that the 65Mn partition plate has excellent hot-press-resistant embedding performance and has better surface finish after polishing. Besides, a release agent is used on the inner wall of the female die and the contact surface of the 65Mn partition plate and the blank, so that the hot-press resistant adhesive film performance of the female die and the partition plate is improved.
The technical scheme adopted by the invention is as follows:
a hot-press moulding demoulding method for short-fibre reinforced carbon/resin composite material includes such steps as adding surficially treated 65Mn partition between blank and upper and lower punches and demoulding agent on the internal surface of female mould and the contact surface between 65Mn partition and blank.
Further, the 65Mn separator is subjected to surface treatment by a carbonitriding (C, N) method, and specifically comprises the following steps:
(a) dripping methanol into the well type furnace at the speed of 70-100 drops/min, introducing ammonia gas at the speed of 300-500L/h, controlling the temperature to be 820-840 ℃ and the time to be 2-3 h;
(b) and after carbonitriding, carrying out oil cooling to room temperature, quenching and medium-temperature tempering, wherein the quenching temperature is 800-850 ℃, keeping the temperature for 15-25 min, then carrying out oil cooling to the room temperature, and tempering at 400-450 ℃ for 1.5-2.5 h.
Further, the release agent comprises the following components in percentage by mass: 10 to 30 percent of flaky graphite powder, 20 to 40 percent of nano-scale cubic boron nitride powder and 30 to 50 percent of nano-scale zirconia powder, and polyethylene glycol is used as a binder.
Further, the preparation method of the release agent comprises the following steps: (A) respectively weighing mixed powder of 10-30% of flaky graphite powder, 20-40% of nano-scale cubic boron nitride powder and 30-50% of nano-scale zirconia powder according to mass percentage;
(B) mixing the weighed powder with a V-shaped mixed material for 3-5h to prepare uniform mixed powder;
(C) mixing polyethylene glycol and alcohol according to the proportion of 1: preparing a solution according to a volume ratio of 3-5;
(D) mixing the mixed powder in the step (B) with the solution in the step (C) according to the ratio of 1: 1.5-3, and preparing slurry;
(E) and (D) drying the slurry in the step (D) in an oven for 3-5 hours to obtain the release agent.
The invention has the beneficial effects that:
(1) by adopting the method, the finish degree of the 65Mn clapboard for hot press molding after grinding and polishing and the hot press pressing resistance inlaying performance are obviously improved, so that the 65Mn clapboard and the die have excellent hot press pressing resistance and die sticking resistance. The hot-press forming efficiency and the surface quality of the hot-press green body are greatly improved.
(2) The use of the specific release agent can obviously reduce the release resistance, so that the release is easy, and the surface quality of the demoulded blank is not influenced.
Drawings
FIG. 1 is a 65Mn partition carbonitrided layer metallographic composed of carbonitrided martensite, retained austenite and a small amount of carbonitrides.
FIG. 2 is a metallographic phase of a transition layer between carbonitrided layer and 65Mn, consisting of high carbon martensite containing carbon and nitrogen, ferrite and retained austenite.
FIG. 3 shows the metallographic phase of the core of a 65Mn separator consisting of ferrite and a small amount of low-carbon martensite.
Fig. 4 shows the mold release effect of the hot-pressed billet without using a mold release agent, and cracks are generated in the mold release process due to hot-pressing mold sticking.
FIG. 5 shows the hot-pressed billet mold release effect after the use of the mold release agent, and the generation of mold release cracks is avoided due to the excellent hot-press mold adhesion effect of the mold release agent.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
A short fiber reinforced carbon/resin composite material hot-press molding demoulding method comprises (1) adding a 65Mn partition plate with surface treatment between a blank and upper and lower punches during hot-press molding and (2) using a demoulding agent on the inner wall of a female die and the contact surface of the 65Mn partition plate and the blank;
the 65Mn partition plate is subjected to surface treatment by adopting a carbonitriding (C, N) method, and specifically comprises the following steps:
(a) dripping methanol into the well type furnace at the speed of 80 drops/min, introducing ammonia gas at the speed of 350L/h, and controlling the temperature to be about 830 ℃ and the time to be 3 h;
(b) and after carbonitriding, carrying out oil cooling to room temperature, quenching and medium-temperature tempering, wherein the quenching temperature is 830 ℃, keeping the temperature for 20min, carrying out oil cooling to the room temperature, and tempering for 2h at 430 ℃.
The release agent comprises the following components in percentage by mass: the preparation method comprises the following steps of mixing 20% of scaly graphite powder, 30% of nano-scale cubic boron nitride powder and 50% of nano-scale zirconia powder, and adopting polyethylene glycol as a binder, wherein the preparation method specifically comprises the following steps:
(A) respectively weighing mixed powder of 20% of flaky graphite powder, 30% of nano-scale cubic boron nitride powder and 50% of nano-scale zirconia powder according to mass percentage;
(B) mixing the weighed powder for 4 hours by adopting a V-shaped mixed material to prepare uniform mixed powder;
(C) mixing polyethylene glycol and alcohol according to the proportion of 1: 4 to prepare a solution;
(D) mixing the mixed powder in the step (B) with the solution in the step (C) according to the ratio of 1: 2 to prepare slurry;
(E) and (D) drying the slurry in the oven for 4 hours to obtain the release agent.
Example 2
A short fiber reinforced carbon/resin composite material hot-press molding demoulding method comprises (1) adding a 65Mn partition plate with surface treatment between a blank and upper and lower punches during hot-press molding and (2) using a demoulding agent on the inner wall of a female die and the contact surface of the 65Mn partition plate and the blank;
the 65Mn partition plate is subjected to surface treatment by adopting a carbonitriding (C, N) method, and specifically comprises the following steps:
(a) dripping methanol into the well type furnace at the speed of 100 drops/min, introducing ammonia gas at the speed of 500L/h, and controlling the temperature to be about 830 ℃ and the time to be 2 h;
(b) and after carbonitriding, carrying out oil cooling to room temperature, quenching and medium-temperature tempering, wherein the quenching temperature is 830 ℃, keeping the temperature for 20min, carrying out oil cooling to the room temperature, and tempering for 2h at 430 ℃.
The release agent comprises the following components in percentage by mass: the preparation method comprises the following steps of mixing 30% of scaly graphite powder, 40% of nano-scale cubic boron nitride powder and 30% of nano-scale zirconia powder, and adopting polyethylene glycol as a binder, wherein the preparation method specifically comprises the following steps:
(A) respectively weighing mixed powder of 30% of flaky graphite powder, 40% of nano-scale cubic boron nitride powder and 30% of nano-scale zirconia powder according to the mass percentage;
(B) mixing the weighed powder for 4 hours by adopting a V-shaped mixed material to prepare uniform mixed powder;
(C) mixing polyethylene glycol and alcohol according to the proportion of 1: 5 to prepare a solution;
(D) mixing the mixed powder in the step (B) with the solution in the step (C) according to the ratio of 1: 3, mixing the raw materials in a mass ratio to prepare slurry;
(E) and (D) drying the slurry in the oven for 4 hours to obtain the release agent.
Example 1 the surface quality of the plate before and after the use of the release agent is shown in fig. 4 (without the use of the release agent) and fig. 5 (with the use of the release agent). As can be seen from FIGS. 4 and 5, the use of the mold release agent can improve the hot-press-resistant adhesion of the material, and avoid the cracks generated by hot-press mold adhesion during the mold release process, so that the surface quality of the hot-pressed blank is obviously improved. The results of example 2 are substantially identical to those of example 1.
Claims (1)
1. A short fiber reinforced carbon/resin composite material hot-press molding demoulding method is characterized by comprising the steps of (1) adding a 65Mn partition plate subjected to surface treatment between a blank body and upper and lower punches during hot-press molding and (2) using a demoulding agent on the inner wall of a female die and the contact surface of the 65Mn partition plate and the blank body;
the 65Mn partition plate is subjected to surface treatment by adopting a carbonitriding method, and the method specifically comprises the following steps:
(a) dripping methanol into the well type furnace at the speed of 70-100 drops/min, introducing ammonia gas at the speed of 300-500L/h, controlling the temperature to be 820-840 ℃ and the time to be 2-3 h;
(b) after carbonitriding, carrying out oil cooling to room temperature, quenching and medium-temperature tempering, wherein the quenching temperature is 800-850 ℃, keeping the temperature for 15-25 min, then carrying out oil cooling to the room temperature, and tempering at 400-450 ℃ for 1.5-2.5 h;
the release agent comprises the following components in percentage by mass: 10 to 30 percent of flaky graphite powder, 20 to 40 percent of nano-scale cubic boron nitride powder and 30 to 50 percent of nano-scale zirconia powder, and polyethylene glycol is used as a binder;
the preparation method of the release agent comprises the following steps:
(A) respectively weighing mixed powder of 10-30% of flaky graphite powder, 20-40% of nano-scale cubic boron nitride powder and 30-50% of nano-scale zirconia powder according to mass percentage;
(B) mixing the weighed powder with a V-shaped mixed material for 3-5h to prepare uniform mixed powder;
(C) mixing polyethylene glycol and alcohol according to the proportion of 1: preparing a solution according to a volume ratio of 3-5;
(D) mixing the mixed powder in the step (B) with the solution in the step (C) according to the ratio of 1: 1.5-3, and preparing slurry;
(E) and (D) drying the slurry in the step (D) in an oven for 3-5 hours to obtain the release agent.
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| CN202011026835.6A CN112157929B (en) | 2020-09-25 | 2020-09-25 | Hot-press forming and demoulding method for short fiber reinforced carbon/resin composite material |
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| CN202011026835.6A CN112157929B (en) | 2020-09-25 | 2020-09-25 | Hot-press forming and demoulding method for short fiber reinforced carbon/resin composite material |
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| CN112157929B true CN112157929B (en) | 2022-07-08 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101027250A (en) * | 2004-08-16 | 2007-08-29 | 弗罗蒂尔碳元素公司 | Article for film formation, method for film formation, and release agent |
| CN102277581A (en) * | 2011-08-11 | 2011-12-14 | 眉山恒升机械装备有限公司 | Heat treatment process of low-carbon alloy material |
| CN102925903A (en) * | 2012-09-27 | 2013-02-13 | 厦门真冈热处理有限公司 | Heat treatment method for die-casting die |
| CN103568447A (en) * | 2013-09-12 | 2014-02-12 | 中国工程物理研究院化工材料研究所 | Lamination forming device and method for preparing thermoset polymer based composite material by using same |
| CN108749033A (en) * | 2018-08-14 | 2018-11-06 | 北京航天新风机械设备有限责任公司 | A kind of precast body reinforcing plate class universal vacuum mould closing mould |
| EP3533579A1 (en) * | 2016-10-31 | 2019-09-04 | 3M Innovative Properties Company | Three-dimensionally shaped thermally conductive molded body, and manufacturing method thereof |
-
2020
- 2020-09-25 CN CN202011026835.6A patent/CN112157929B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101027250A (en) * | 2004-08-16 | 2007-08-29 | 弗罗蒂尔碳元素公司 | Article for film formation, method for film formation, and release agent |
| CN102277581A (en) * | 2011-08-11 | 2011-12-14 | 眉山恒升机械装备有限公司 | Heat treatment process of low-carbon alloy material |
| CN102925903A (en) * | 2012-09-27 | 2013-02-13 | 厦门真冈热处理有限公司 | Heat treatment method for die-casting die |
| CN103568447A (en) * | 2013-09-12 | 2014-02-12 | 中国工程物理研究院化工材料研究所 | Lamination forming device and method for preparing thermoset polymer based composite material by using same |
| EP3533579A1 (en) * | 2016-10-31 | 2019-09-04 | 3M Innovative Properties Company | Three-dimensionally shaped thermally conductive molded body, and manufacturing method thereof |
| CN108749033A (en) * | 2018-08-14 | 2018-11-06 | 北京航天新风机械设备有限责任公司 | A kind of precast body reinforcing plate class universal vacuum mould closing mould |
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