CN101797646B - Preparation method of high-strength charcoal/charcoal hot-pressing mould for vacuum hot-pressing furnace - Google Patents
Preparation method of high-strength charcoal/charcoal hot-pressing mould for vacuum hot-pressing furnace Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-strength charcoal/charcoal hot-pressing mould for a vacuum hot-pressing furnace, which is characterized in that a charcoal cloth to continuously and circularly wind a pseudo-three-dimensional structural preform which is acupunctured in the radial direction; the preform is compacted through chemical vapor immersion and resin pressure impregnation carbonization, and the preform is undertaken the high-temperature processing and mechanical processing after the compact process, so the charcoal/charcoal hot-pressing mould can be prepared. The charcoal/charcoal hot-pressing mould is compacted and prepared in the process method by adopting the charcoal cloth to continuously wind and acupuncture the preform and combining the chemical vapor immersion and resin pressure impregnation carbonization. Being applied to the aspects such as the powder metallurgy and ceramic hot-pressing mould to substitute the graphite mould, the thickness of the mould is greatly reduced, the charge batch of the product can be improved, and the production cost can be reduced; and the prepared mould has high tensile strength and strong hot vibration resistant capacity, and the service life can be greatly prolonged.
Description
Technical field
The invention belongs to powder metallurgy and Production of Ceramics hot pressing die technical field, be specifically related to the preparation method of a kind of vacuum hotpressing stove with high-strength carbon/charcoal hot pressing die.
Background technology
Heat pressing process is a kind of method of forming materials that mold pressing is combined with sintering, unidirectional or triaxial pressure are acted on powder compact or the bulky powder that is contained in graphite or other rigid die, at high temperature make powder produce the powder metallurgy densifying method of plastic deformation or creep, be usually used in preparing ceramic material such as silicon nitride, boron carbide etc., and the metal and alloy material such as the Ti-Al base alloy etc. that are difficult to sintering.
Vacuum hotpressing stove can move under vacuum condition or under the protective atmosphere, and is in the majority with vacuum condition.Because the needed pressure of hot pressing is less, the product densification, size is accurate, therefore is usually used in producing large parts and the very poor ceramic-metal combinations of agglutinating property such as hard alloy roll, top hammer.
Higher because of operating temperature, generally more than 1000 ℃, so heat pressing process requires that mold materials is high temperature resistant, higher-strength under the high temperature, and mould commonly used at present is a graphite material.The compressive strength of graphite is generally greater than 60MPa, shortcoming is that rupture strength, hot strength are low, rupture strength is about 35MPa, hot strength is about 20MPa, therefore the graphite jig design thickness is thicker, take space bigger in the hot pressing furnace, influenced production efficiency of products, and easily brittle fracture takes place.
Chinese patent CN1778490 discloses a kind of large-scale charcoal/charcoal hot pressing die former manufacture method, it be on the electrode graphite cylinder with unidirectional charcoal band resin pickup after uniform winding solidify, charing handles, all cut out or stay a small amount of former graphite post then, forming thickness is the thick cylinder of 20～50mm, makes the hot pressing die former.This method advantage is that technology is simple, and cost is low, and its weak point is: (1) density is lower, less than 1.5g/cm
3, bear the less 30MPa of being of pressure; (2) hoop twines but does not have radially needling fiber, belongs to two-dimensional structure, therefore layering takes place in manufacture process and use easily, break.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, the preparation method of a kind of vacuum hotpressing stove with high-strength carbon/charcoal hot pressing die is provided, charcoal/charcoal hot pressing die intensity height, long service life, the excellent performance of this method preparation, compare with the graphite material mould, make charcoal/charcoal hot pressing die thickness reduce 2/3rds.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of vacuum hotpressing stove preparation method of high-strength carbon/charcoal hot pressing die is characterized in that preparation process is:
(1) adopts alternately shop layer of charcoal cloth and short carbon fiber net tire, hoop twines continuously, adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, make cylindric accurate three-dimensional structure hot pressing die precast body, the density of cylindric accurate three-dimensional structure hot pressing die precast body is 0.30g/cm
3～0.70g/cm
3, the needling density in the described needling process is 20 pins/cm
2～45 pins/cm
2
(2) chemical gas-phase permeation compaction technology: with propylene or natural gas is raw material, under 850 ℃～1200 ℃ high temperature, after the cracking the cylindric accurate three-dimensional structure hot pressing die precast body in the step (1) is carried out chemical gas-phase permeation compaction and handle, make cylindric charcoal/charcoal hot pressing die base substrate;
(3) the furfural acetone resin dipping solidifies and the charing treatment process: the density 〉=1.0g/cm of the cylindric charcoal in step (2)/charcoal hot pressing die base substrate
3After, it is carried out curing of furfural acetone resin dipping and charing processing, impregnation pressure is 1.0MPa～3.0MPa, and solidification temperature is 160 ℃～220 ℃, and carbonization temperature is 800 ℃～1000 ℃;
(4) high-temperature processing technology: the density 〉=1.4g/cm of the cylindric charcoal/charcoal hot pressing die base substrate in the step (3) after curing of furfural acetone resin dipping and charing processing
3The time, it is carried out 1800 ℃～2500 ℃ high-temperature process;
(5) the cylindric charcoal after high-temperature process/charcoal hot pressing die base substrate in the step (4) is carried out furfural acetone resin dipping solidifies and charing is handled, make the density 〉=1.70g/cm of cylindric charcoal/charcoal hot pressing die base substrate
3Impregnation pressure is 1.0MPa～3.0MPa, and solidification temperature is 160 ℃～220 ℃, and carbonization temperature is 800 ℃～1000 ℃;
(6) the cylindric charcoal in the step (5)/charcoal hot pressing die base substrate is carried out 1800 ℃～2500 ℃ high-temperature process, make the hot strength 〉=150MPa of cylindric charcoal/charcoal hot pressing die base substrate;
(7) mechanical processing technique: the cylindric charcoal after high-temperature process/charcoal hot pressing die base substrate in the step (6) is machined, make cylindric high-strength carbon/charcoal hot pressing die of hot strength 〉=150MPa.
Charcoal cloth described in the above-mentioned steps (1) is 3K～12K plain weave charcoal cloth or twill charcoal cloth, and wherein K represents tow thousand radicals.
The surface roughness value of cylindric high-strength carbon/charcoal hot pressing die is no more than 6.4 μ m described in the above-mentioned steps (7).
The diameter of cylindric high-strength carbon/charcoal hot pressing die is 200mm～1300mm described in the above-mentioned steps (7), wall thickness 15mm～100mm, highly≤1000mm.
The present invention compared with prior art has the following advantages:
(1) adopt acupuncture 3～12K charcoal cloth and short carbon fiber net tire shop layer, hoop twines continuously and makes the three-dimensional structure precast body, because the hoop continuity of charcoal cloth has improved the hoop hot strength; Short carbon fiber net tire provides the silk source of acupuncture vertical fibers, has increased the content of vertical fibers, has improved the ability of precast body densification technique process and the anti-layering of goods use;
(2) adopt the high-temperature process that is higher than serviceability temperature, under the prerequisite that does not reduce charcoal/charcoal hot pressing die intensity, can improve thermal shock resistance and structural stability again.
(3) compare with graphite jig, it is nearly 2/3rds that charcoal/charcoal hot pressing die thickness reduces, and under the certain situation of furnace chamber size, uses charcoal/charcoal hot pressing die batch to improve greatly, improved production efficiency, reduces cost.
(4) charcoal/charcoal hot pressing die density is big, and intensity and thermal shock resistance are higher, and is not fragile in the use, the service life of energy significant prolongation hot pressing die.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
The preparation method of high-strength carbon/charcoal hot pressing die of a kind of vacuum hotpressing stove as shown in Figure 1, preparation process is:
(1) adopts alternately shop layer of charcoal cloth and short carbon fiber net tire, hoop twines continuously, adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, make cylindric accurate three-dimensional structure hot pressing die precast body, the density of cylindric accurate three-dimensional structure hot pressing die precast body is 0.30g/cm
3～0.70g/cm
3, the needling density in the described needling process is 20 pins/cm
2～45 pins/cm
2, described charcoal cloth is 3K～12K plain weave charcoal cloth or twill charcoal cloth, wherein K represents tow thousand radicals;
(2) chemical gas-phase permeation compaction technology: in chemical vapor deposition stove, with propylene or natural gas is raw material, under 850 ℃～1200 ℃ high temperature, after the cracking the cylindric accurate three-dimensional structure hot pressing die precast body in the step (1) is carried out chemical gas-phase permeation compaction and handle, make cylindric charcoal/charcoal hot pressing die base substrate;
(3) the furfural acetone resin dipping solidifies and the charing treatment process: the density 〉=1.0g/cm of the cylindric charcoal in step (2)/charcoal hot pressing die base substrate
3After, in impregnating autoclave, it is carried out the furfural acetone resin dipping and solidify, in retort, it is carried out charing and handle, impregnation pressure is 1.0MPa～3.0MPa, and solidification temperature is 160 ℃～220 ℃, and carbonization temperature is 800 ℃～1000 ℃;
(4) high-temperature processing technology: the density 〉=1.4g/cm of the cylindric charcoal/charcoal hot pressing die base substrate in the step (3) after curing of furfural acetone resin dipping and charing processing
3The time, in the graphitizable high temperature stove, it is carried out 1800 ℃～2500 ℃ high-temperature process;
(5) the cylindric charcoal after high-temperature process/charcoal hot pressing die base substrate in the step (4) is carried out furfural acetone resin dipping solidifies and charing is handled, make the density 〉=1.70g/cm of cylindric charcoal/charcoal hot pressing die base substrate
3Impregnation pressure is 1.0MPa～3.0MPa, and solidification temperature is 160 ℃～220 ℃, and carbonization temperature is 800 ℃～1000 ℃;
(6) the cylindric charcoal in the step (5)/charcoal hot pressing die base substrate is carried out 1800 ℃～2500 ℃ high-temperature process in the graphitizable high temperature stove, make the hot strength 〉=150MPa of cylindric charcoal/charcoal hot pressing die base substrate;
(7) mechanical processing technique: the cylindric charcoal after high-temperature process/charcoal hot pressing die base substrate in the step (6) is machined, make cylindric high-strength carbon/charcoal hot pressing die of hot strength 〉=150MPa, its surface roughness value is no more than 6.4 μ m, diameter is 200mm～1300mm, wall thickness 15mm～100mm, highly≤1000mm.
Embodiment 1
(1) adopt alternately shop layer of 3K twill charcoal cloth and short carbon fiber net tire, hoop twines continuously, adopts needling process to introduce fortifying fibre in vertical charcoal cloth direction, makes cylindric accurate three-dimensional structure hot pressing die precast body, and its density is 0.30g/cm
3, the needling density in the needling process is 20 pins～30 pins/cm
2Adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, prevent manufacture process, make layering and cracking in the process;
(2) chemical vapor infiltration technology: in chemical vapor deposition stove, with the propylene is raw material, after cracking under 850 ℃ of temperature, cylindric accurate three-dimensional structure hot pressing die precast body is carried out gas-phase permeation compaction handled for two cycles, make cylindric charcoal/charcoal hot pressing die base substrate;
(3) the furfural acetone resin dipping solidifies and the charing processing: charcoal/charcoal hot pressing die blank density 〉=1.0g/cm
3The time, in impregnating autoclave, carrying out the furfural acetone resin impregnation process, impregnation pressure 1.0MPa carries out 160 ℃ of curing behind the dipping 4h, carries out 800 ℃ of charings and handle in retort;
(4) high-temperature process: as charcoal/charcoal hot pressing die blank density 〉=1.4g/cm
3The time, in the graphitizable high temperature stove, carry out 2300 ℃ of high-temperature process, purpose is carried out perforate to material, is beneficial to the later stage densification;
(5) repeating step (3) is to the density 〉=1.70g/cm of cylindric charcoal/charcoal hot pressing die base substrate
3
(6) repeating step (4) carries out high-temperature process, and the high-temperature process temperature is 2300 ℃;
(7) machining: to the cylindric charcoal/charcoal hot pressing die base substrate machined into after the process high-temperature process in the step (6), make cylindric high-strength carbon/charcoal hot pressing die of hot strength 〉=150MPa, its surface roughness value is no more than 6.4 μ m.
Vacuum hotpressing stove in the above-mentioned steps (7) is of a size of diameter 200mm with high-strength carbon/charcoal hot pressing die, height 500mm, thickness 15mm.
Embodiment 2
(1) adopt alternately shop layer of 6K plain weave charcoal cloth and short carbon fiber net tire, hoop twines continuously, adopts needling process to introduce fortifying fibre in vertical charcoal cloth direction, makes cylindric three-dimensional structure hot pressing die precast body, and its density is 0.50g/cm
3, the needling density in the needling process is 30 pins～40 pins/cm
2Adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, prevent layering and cracking in manufacture process, the use;
(2) chemical vapor infiltration technology: in chemical vapor deposition stove, be raw material, after cracking under 940 ℃ of temperature, cylindric three-dimensional structure hot pressing die precast body carried out gas-phase permeation compaction handled for two cycles, make cylindric charcoal/charcoal hot pressing die base substrate with the propylene;
(3) the furfural acetone resin dipping solidifies and the charing processing: cylindric charcoal/charcoal hot pressing die blank density 〉=1.0g/cm
3The time, in impregnating autoclave, carrying out the furfural acetone resin impregnation process, impregnation pressure 2.0MPa carries out 190 ℃ of curing behind the dipping 4h, carries out 900 ℃ of charings and handle in retort;
(4) high-temperature process: repeating step (3), as its density 〉=1.4g/cm
3The time, in the graphitizable high temperature stove, carry out 2500 ℃ of high-temperature process, purpose is carried out perforate to material, is beneficial to the later stage densification;
(5) repeating step (3) is to the density 〉=1.70g/cm of cylindric charcoal/charcoal hot pressing die base substrate
3
(6) repeating step (4) carries out high-temperature process, and the high-temperature process temperature is 2300 ℃;
(7) machining: to the cylindric charcoal after high-temperature process in the step (6)/charcoal hot pressing die base substrate machined into, make cylindric high-strength carbon/charcoal hot pressing die of hot strength 〉=150MPa, its surface roughness value is no more than 6.4 μ m.
Vacuum hotpressing stove in the above-mentioned steps (7) is of a size of diameter 500mm with high-strength carbon/charcoal hot pressing die, height 800mm, thickness 50mm.
Embodiment 3
(1) adopt alternately shop layer of 12K plain weave charcoal cloth and short carbon fiber net tire, hoop twines continuously, adopts needling process to introduce fortifying fibre in vertical charcoal cloth direction, makes cylindric three-dimensional structure hot pressing die precast body, and its density is 0.70g/cm
3, the needling density in the needling process is 40-45 pin/cm
2Adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, prevent layering and cracking in manufacture process, the use;
(2) chemical vapor infiltration technology: in chemical vapor deposition stove, with the natural gas is raw material, after cracking under 1200 ℃ of temperature, cylindric three-dimensional structure hot pressing die precast body is carried out gas-phase permeation compaction handled for two cycles, make cylindric charcoal/charcoal hot pressing die base substrate;
(3) the furfural acetone resin dipping solidifies and the charing processing: cylindric charcoal/charcoal hot pressing die blank density 〉=1.0g/cm
3The time, in impregnating autoclave, carrying out the furfural acetone resin impregnation process, impregnation pressure 3.0MPa carries out 220 ℃ of curing behind the dipping 4h, carries out 1000 ℃ of charings and handle in retort;
(4) high-temperature process: repeating step (3), as cylindric charcoal/charcoal hot pressing die blank density 〉=1.4g/cm
3The time, in the graphitizable high temperature stove, carry out 2000 ℃ of high-temperature process, purpose is carried out perforate to material, is beneficial to the later stage densification;
(5) repeating step (3) is to the density 〉=1.70g/cm of cylindric charcoal/charcoal hot pressing die base substrate
3
(6) repeating step (4) carries out high-temperature process, and the high-temperature process temperature is 1800 ℃;
(7) machining: to the cylindric charcoal after high-temperature process in the step (6)/charcoal hot pressing die base substrate machined into, make cylindric high-strength carbon/charcoal hot pressing die of hot strength 〉=150MPa, its surface roughness value is no more than 6.4 μ m.
Vacuum hotpressing stove in the above-mentioned steps (7) is of a size of diameter 1300mm with high-strength carbon/charcoal hot pressing die, height 1000mm, thickness 100mm.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, everyly any simple modification that above embodiment did, change and equivalence changed, all still belong in the protection domain of technical solution of the present invention according to the technology of the present invention essence.
Claims (3)
1. a vacuum hotpressing stove is characterized in that preparation process is with the preparation method of high-strength carbon/charcoal hot pressing die:
(1) adopts alternately shop layer of charcoal cloth and short carbon fiber net tire, hoop twines continuously, adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, make cylindric accurate three-dimensional structure hot pressing die precast body, the density of cylindric accurate three-dimensional structure hot pressing die precast body is 0.30g/cm
3～0.70g/cm
3, the needling density in the described needling process is 20 pins/cm
2～45 pins/cm
2Described charcoal cloth is 3K～12K plain weave charcoal cloth or twill charcoal cloth, and wherein K represents tow thousand radicals;
(2) chemical gas-phase permeation compaction technology: with propylene or natural gas is raw material, under 850 ℃～1200 ℃ high temperature, after the cracking the cylindric accurate three-dimensional structure hot pressing die precast body in the step (1) is carried out chemical gas-phase permeation compaction and handle, make cylindric charcoal/charcoal hot pressing die base substrate;
(3) the furfural acetone resin dipping solidifies and the charing treatment process: the density 〉=1.0g/cm of the cylindric charcoal in step (2)/charcoal hot pressing die base substrate
3After, it is carried out curing of furfural acetone resin dipping and charing processing, impregnation pressure is 1.0MPa～3.0MPa, and solidification temperature is 160 ℃～220 ℃, and carbonization temperature is 800 ℃～1000 ℃;
(4) high-temperature processing technology: the density 〉=1.4g/cm of the cylindric charcoal/charcoal hot pressing die base substrate in the step (3) after curing of furfural acetone resin dipping and charing processing
3The time, it is carried out 1800 ℃～2500 ℃ high-temperature process;
(5) the cylindric charcoal after high-temperature process/charcoal hot pressing die base substrate in the step (4) is carried out furfural acetone resin dipping solidifies and charing is handled, make the density 〉=1.70g/cm of cylindric charcoal/charcoal hot pressing die base substrate
3Impregnation pressure is 1.0MPa～3.0MPa, and solidification temperature is 160 ℃～220 ℃, and carbonization temperature is 800 ℃～1000 ℃;
(6) the cylindric charcoal in the step (5)/charcoal hot pressing die base substrate is carried out 1800 ℃～2500 ℃ high-temperature process, make the hot strength 〉=150MPa of cylindric charcoal/charcoal hot pressing die base substrate;
(7) mechanical processing technique: the cylindric charcoal after high-temperature process/charcoal hot pressing die base substrate in the step (6) is machined, make cylindric high-strength carbon/charcoal hot pressing die of hot strength 〉=150MPa.
2. according to the preparation method of the described a kind of vacuum hotpressing stove of claim 1, it is characterized in that the surface roughness value of cylindric high-strength carbon/charcoal hot pressing die is no more than 6.4 μ m described in the step (7) with high-strength carbon/charcoal hot pressing die.
3. according to the preparation method of the described a kind of vacuum hotpressing stove of claim 1 with high-strength carbon/charcoal hot pressing die, it is characterized in that, the diameter of cylindric high-strength carbon/charcoal hot pressing die is 200mm～1300mm described in the step (7), wall thickness 15mm～100mm, highly≤1000mm.
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| CN102060555A (en) * | 2010-11-24 | 2011-05-18 | 西安超码科技有限公司 | Method for manufacturing high-strength carbon/carbon hot-press die |
| CN104418604A (en) * | 2013-08-21 | 2015-03-18 | 甘肃郝氏炭纤维有限公司 | Tubular-type carbon/carbon composite material quickly preparing method |
| CN114853495A (en) * | 2022-04-21 | 2022-08-05 | 西安超码科技有限公司 | Preparation method of carbon/carbon hot pressing mold for high-pressure hot pressing sintering furnace |
| CN115823151B (en) * | 2023-02-15 | 2023-06-20 | 西安超码科技有限公司 | Sandwich-structured carbon/ceramic brake disc |
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| US20060027792A1 (en) * | 2004-07-28 | 2006-02-09 | Butcher Jonah V | Carbon composite near-net-shape molded part and method of making |
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