CN1778490A - Bed die of large thermal-pressure mould and its production thereof - Google Patents
Bed die of large thermal-pressure mould and its production thereof Download PDFInfo
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- CN1778490A CN1778490A CN 200510019593 CN200510019593A CN1778490A CN 1778490 A CN1778490 A CN 1778490A CN 200510019593 CN200510019593 CN 200510019593 CN 200510019593 A CN200510019593 A CN 200510019593A CN 1778490 A CN1778490 A CN 1778490A
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Abstract
A female die of large hot pressing die set is prepared from the ordinary electrode graphite and carbon-carbon composition through dipping the high-strength carbon fiber yarn or unidirectional narrow carbon fiber cloth in thermosetting resin, winding them on the surface of an electrode graphite column, heating for solidifying, high-temp carburizing to obtain resin carbon, and removing part or all of said graphite column.
Description
Technical field:
The present invention relates to graphite hot pressing die indispensable in the production technology of advanced materials such as hot pressed sintering special cermacis, ceramic matric composite, powder metallurgy product.
Background technology:
Hot pressed sintering is crucial a kind of in the advanced material sintering process such as special cermacis, ceramic matric composite, powder metallurgy product.The hot pressed sintering sample is the best a kind of technological measure of product properties in the various sintering processings, and the material of some specific use and device can only adopt the hot-pressing sintering technique manufacturing.
In the hot-pressing sintering technique, the hot pressed sintering furnace interior is put into whole system in the powder that is sintered moulding in advance or directly put into the mould that materials such as graphite are made without moulding in advance then.In the intensification sintering, promoting polishing head by the outer hydraulic piston of hot-pressed sintering furnace moves, produce very big mechanical pressure to being sintered sample, under the acting in conjunction of this pressure and high temperature, be sintered the powder contraction and sinter the compact block material sample consistent into mould cavity volume shape.As shown in Figure 1.Owing to have very big action of mechanical pressure, this technology can make the original material that is difficult to even can not sintering sinter compact block into, make sintered body have the highest performance.
Existing hot pressing die is generally made by graphite material.Because hot pressing will experience very high temperature, therefore require mold materials at high temperature still will keep higher intensity, especially in the high-temperature region more than 1000 ℃.Graphite material is more satisfactory hot pressing die material.More than 1600 ℃, graphite material is unique available hot pressing die material.
The graphite that can make hot pressing die belongs to high-strength graphite, and generally more than 60Mpa, rupture strength is more than 35Mpa for compressive resistance.Because its anti-folding (tension) intensity is lower, so the former of hot pressing die often thicker (generally greater than 40 millimeters, and big more its thickness of die size is thick more) reduces the danger that former splits in the hot pressing with this, the raising safety coefficient.But high-strength graphite preparation difficulty, price is very high, and diameter of rod is big more difficult more, and during actual the use, the high-strength graphite diameter of rod has obtained greater than 650 millimeters be difficult to.Therefore preparing hot pressing die former internal diameter with traditional graphite raw material almost is impossible greater than 500 millimeters, even create reluctantly, the probability that breaks in its use also is sizable.
As shown in Figure 1, in the hot pressing die use, the destructive power that former is subjected to mainly is the power that hot pressed samples outwards expands, when having liquid phase to occur in the sintering process, this destructive power is more obvious, even the axial compressive force (25～40Mpa) that will be subjected near sample.This expansive force acts on the tensile stress that just becomes on the former along hoop, in case this stress has surpassed the local fracture strength of former, just will cause the moment of former radially to split, and causes the accident.
Hot pressed sintering almost is irreplaceable as a kind of preparation technology in some field, but heat pressing process is owing to be Batch Process, and production efficiency is lower.Strengthen the hot pressing die size, the amount that improves every stove agglomerated material is to improve the effective way of heat pressing process production efficiency, also needs the large-size hot-press sintered ceramic product in aerospace and national defence field in addition, so needs large-sized hot pressing die in the practicality.
Carbon carbon composite is to be to strengthen body with the carbon fiber, with the class composite of carbon as matrix.The carbon carbon composite function admirable is widely used in fields such as Aeronautics and Astronautics, nuclear energy.The carbon carbon composite preparation method is a lot, mainly contains dipping, CVD (CVI) method, high pressure charring (PIC) and powder sintering.High performance carbon carbon composite complicated process of preparation, the cycle is long, and cost is quite high.Produce carbon carbon composite as infusion process, want woven carbon fiber fabric in advance, the technology that usually needs then to flood charing more repeatedly just can make highdensity carbon carbon composite.
Carbon fiber enhancement resin base composite material is to be to strengthen body with the carbon fiber, is the extraordinary advanced composite material of a class performance of matrix with the resin.According to the type of resin matrix, can divide carbon fiber-reinforced thermosetting resin and carbon fiber to strengthen thermoplastic resin.Being equipped with the carbon fiber-reinforced thermosetting resin composite materials with the winding legal system is a kind of special acquisition high-performance tube or jar shape device maturation method.
The winding method is convenient to improve the volume fraction of fiber in the composite because fiber is arranged substantially in the same way, helps giving full play to the high-strength performance of fortifying fibre most, but because it is vertical and the machine direction tensile strength is low, has limited it and used widely.
Summary of the invention:
The object of the present invention is to provide that a kind of technology is simple, lower-cost bed die of large thermal-pressure mould and preparation method thereof.
Technical scheme of the present invention is as follows:
1, bed die of large thermal-pressure mould: it is large scale, thin cylinder with the carbon carbon composite preparation.
2, the preparation method of bed die of large thermal-pressure mould: earlier to make inner core near the common graphite rod than minor diameter of the former internal diameter that will make, twine high-strength carbon fibre yarn or the carbon fiber thin layer arrowband that flooded thermosetting resins such as phenolic resins, epoxy resin, epoxy/resol in the above, as shown in Figure 2, be heating and curing after being wound into 15～50 millimeters thickness, make it to form carbon fiber-reinforced thermosetting polymer matrix composites shell.Then the bar that makes is put into carbonization, graphitizing furnace carries out carbonization, graphitization, make original carbon fiber-reinforced thermosetting polymer matrix composites become carbon fiber and strengthen the RESEARCH OF PYROCARBON material.And then all cut out or stay a small amount of former graphite post, forming thickness is the cylinder of 20～50 millimeters thick, utilizes common turning mode to be processed into the former of the hot pressing die that meets dimensional requirement then.Technological process as shown in Figure 3.
The carbon carbon composite function admirable is applied in aerospace, aviation and national defense industry.Carbon carbon composite can reach more than the 150Mpa in fortifying fibre direction tensile strength, and safe in utilization, brittle fracture can not take place, and will obtain extraordinary effect if therefore it is applied on the hot pressing die.
The carbon carbon composite for preparing in the technology of the present invention, the carbon fiber direction substantially all is that hoop is arranged, consider the bursting stress that former is subjected in the hot pressing, the carbon fiber that hoop is arranged just in time reinforcement the weak link of former, give full play to carbon carbon composite along the high characteristics of machine direction tensile strength, this helps realizing resisting expansive force in the hot pressing with thin thickness, realizes the thin-walled property of former.The inventive method can be prepared (diameter is greater than 300 millimeters), the thin-walled hot pressing die former of large diameter with lower cost.
Description of drawings:
Fig. 1 is a hot pressed sintering mould structure schematic diagram.
Fig. 2 is a mould structure schematic diagram of the present invention.
Fig. 3 is a mold production process FB(flow block) of the present invention.
Label declaration: 1 former, 2 hot pressed samples, 3 seaming chucks, 4 push-down heads, 5 graphite cores, 6 carbon fiber yarns or unidirectional braiding approach arrowband, 7 steeping vats, 8 carbon fiber spindles.
The specific embodiment:
The large scale of carbon carbon composite of the present invention preparation, its internal diameter of thin cylinder be greater than 200 millimeters, 15～40 millimeters of wall thickness.
Embodiment 1: 250 millimeters of preparation internal diameters, 20 millimeters of wall thickness, the former that length is 200 millimeters
1) intercepting 250 millimeters long, one section of the ordinary electrode graphite cylinder that diameter is 250 millimeters.With 30 millimeters through holes of above-mentioned graphite cylinder centre drill diameter, be used for installing turning cylinder.
2) above-mentioned graphite cylinder is installed on the hand rotating turret, makes it to rotate and can effectively brake with wind.
3) the high-strength carbon fibre spindle is fixed on another turning cylinder, carbon fibre thread is walked around the pulley of steeping vat inside, be fixed on the graphite cylinder one end outer rim with glue (502 glue and so on).Contain the B rank phenolic aldehyde acetone emulsion that modulates in the steeping vat.
4) shake carbon fiber yarn that handle will soak glue and slowly closely be wrapped on the graphite cylinder with 5 kilograms tension force, 20 millimeters blank are respectively stayed at two ends.Blow the part that has wound with the electric heating hair-dryer and make wherein the acetone solvent volatilization while twining, the phenolic aldehyde emulsion becomes gel state, and primary solidification is progressively carried out this process and made winding layer thickness reach 20 millimeters.
5) will wind and take off, with the latex rubber bag splendid attire and vacuumize sealing through the graphite cylinder of primary solidification.Putting into drying baker solidified 6 hours for 150 ℃.Resin is fully solidified.
6) sample that is cured is put into vacuum sintering furnace, carbonization under nitrogen protection.Carbonization technique: per minute heats up 5 ℃ to 500 ℃; Per minute heats up 1 ℃ to 700 ℃ then; Per minute heats up 2 ℃ to 900 ℃ then;
Per minute heats up 5 ℃ to 2000 ℃; Cooling.
7) sample after the carbonization is taken out in sintering furnace, last outer circular end grinding machine is processed outer garden to 290 millimeters of diameters; Internal electrode graphite is dug up major part (240 millimeters of diameters), and finish turning went out conicity 1: 50 again, and the endoporus that minimum diameter is 245 millimeters is clipped the two ends transition portion.So obtain external diameter is 290 millimeters, and inside has 1: 50 tapering, and minimum diameter is 245 millimeters, long 200 millimeters former.
8) this former cooperates hot pressing to produce 132 * 200 * 60mm with other hot pressing die assemblies
3Base substrate, pressure 30Mpa uses 10 times, is not damaged.
Embodiment 2: the preparation wall thickness is 15 millimeters, 200 millimeters of internal diameters, long 100 millimeters cylinder
1. intercept one section ordinary electrode graphite cylinder,, be used for installing turning cylinder through hole of above-mentioned graphite cylinder centre drill;
2. above-mentioned graphite cylinder is installed on the hand rotating turret, makes it to rotate and can effectively brake with wind.
3. (have only the warp-wise carbon fiber, broadwise is fixed with sparse thin cotton to select the high-strength carbon fibre arrowband.This market, arrowband is on sale, be mainly used to the beam of the incompatible reinforcement bridge of epoxy gluing, building, post, and key structure such as shear wall).Narrow bag fabric width is less than 100 millimeters, and thickness is less than 0.5 millimeter.
4. narrow bag one end is fixed on the ready graphite post, can fixes, also can adopt other modes to fix with 502 glue; And the arrowband coiled be fixed on another turning cylinder, this turning cylinder has the device (this device is similar to bicycle brake device) that can regulate rotational resistance torque.The carbon fiber arrowband is wrapped on the glue-coated graphite post smearing one deck epoxide-resin glue (E44 adds amine curing agent) with scraper on the graphite post.The axle that the narrow bag of adjusting carbon fiber is coiled is gone up the moment of resistance, makes the narrow bag of carbon fiber tension force be controlled at 20 kilograms.After winding is enclosed near one, the unnecessary resin glue that also has is wiped off, used scraper blade coating one deck epoxide-resin glue above the carbon fiber arrowband that will twine then again with scraper, and then the rotation manual rocking handle, continue to twine the carbon fiber arrowband.Carry out said process so repeatedly, successively twine carbon fiber layer.
5. twine 20～30 layers according to 4 technology, 3～5 millimeter are thick, temporarily stop afterwards twining, and heating with hair dryer, winding layer makes it begin to solidify.Blow and used cold wind in 5～10 minutes behind the hot blast instead and blew 10 minutes, the purpose of blowing a cold wind over is to reduce temperature, slows down curing reaction speed.And then continue to twine by 4 technology.Carry out once cold and hot blowing after 20～30 layers of every windings, meet the requirements of size until twining gross thickness.Twine gross thickness in the present embodiment in 12 millimeter.
6. the carbon fiber arrowband is cut off, and then with scraper blade coating one deck epoxy glue.Notice that the container that holds epoxide-resin glue in the whole process will be placed on low temperature environment (below 10 ℃) in order to avoid the resin premature setting.
7. will wind and take off, with the latex rubber bag splendid attire and vacuumize sealing through the graphite cylinder of primary solidification.Putting into drying baker solidified 30 minutes～4 hours for 100～150 ℃.Resin is fully solidified.
8. the sample that is cured is put into vacuum sintering furnace, carbonization under nitrogen protection.Carbonization technique: per minute heats up 5 ℃ to 500 ℃; Per minute heats up 1 ℃ to 700 ℃ then; Per minute heats up 2 ℃ to 900 ℃ then; Per minute heats up 5 ℃ to 2000 ℃; Cooling.
9. the sample after the carbonization is taken out in sintering furnace, process inside and outside garden and end face, make the hot pressing die former at last with grinding machine, lathe; As: go up outer circular end grinding machine, process outer garden to 230 millimeters of diameters; Internal electrode graphite is dug up major part with lathe and, reprocess both ends of the surface, obtain 200 millimeters of internal diameters at last exquisite 200 millimeters of internal diameter finishing.230 millimeters of external diameters, long 100 millimeters carbon carbon cylinder.Changing the cylinder inner ring is the ordinary electrode graphite of 5 millimeters thick, and skin is the carbon carbon composite of 10 millimeters thick.
10. this former is cooperated with other hot pressing die assemblies, the inner 20 millimeters thick plasticine of placing, plus-pressure is 100 tons on 100 tons of forcing presses, calculates the about 30Mpa of its pressure, and this former does not damage.
Claims (5)
1, a kind of bed die of large thermal-pressure mould is characterized in that: it is large scale, thin cylinder with the carbon carbon composite preparation.
2, bed die of large thermal-pressure mould according to claim 1 is characterized in that: described large scale, its internal diameter of thin cylinder be greater than 200 millimeters, 15～50 millimeters of wall thickness.
3, the manufacture method of bed die of large thermal-pressure mould according to claim 1 and 2 is characterized in that: its processing step is as follows:
(1) make inner core with the common graphite rod than minor diameter of the approaching former internal diameter that will make earlier,
(2) twine high-strength carbon fibre yarn or the carbon fiber thin layer arrowband that flooded thermosetting resin in the above, be wound into 15～50 millimeters thickness,
(3) afterwards, be heating and curing, make it to form carbon fiber-reinforced thermosetting polymer matrix composites shell,
(4) bar that makes is put into carbonization, graphitizing furnace carries out carbonization, graphitization, make original carbon fiber-reinforced thermosetting polymer matrix composites become carbon fiber and strengthen the RESEARCH OF PYROCARBON material,
(5) and then all cut out or stay a small amount of former graphite post, forming thickness is the cylinder of 20～50 millimeters thick,
(6) utilize common turning mode to be processed into the former of the hot pressing die that meets dimensional requirement.
4, the manufacture method of bed die of large thermal-pressure mould according to claim 3 is characterized in that: described thermosetting resin is a kind of in phenolic resins or epoxy resin or the epoxy/resol.
5, the manufacture method of bed die of large thermal-pressure mould according to claim 4 is characterized in that: its concrete processing step is as follows:
(1) one section ordinary electrode graphite cylinder of intercepting with through hole of above-mentioned graphite cylinder centre drill, is used for installing turning cylinder; Above-mentioned graphite cylinder is installed on the hand rotating turret, makes it to rotate and can effectively brake with wind;
(2) select the high-strength carbon fibre arrowband, narrow bag fabric width is less than 100 millimeters, and thickness is less than 0.5 millimeter; Narrow bag one end is fixed on the ready graphite post, and the arrowband coiled is fixed on another turning cylinder, this turning cylinder has the device that can regulate rotational resistance torque;
(3) on the graphite post, smear one deck epoxide-resin glue, the carbon fiber arrowband is wrapped on the glue-coated graphite post with scraper; The axle that the narrow bag of adjusting carbon fiber is coiled is gone up the moment of resistance, makes the narrow bag of carbon fiber tension force be controlled at 20 kilograms; After winding is enclosed near one, the unnecessary resin glue that also has is wiped off, used scraper blade coating one deck epoxide-resin glue above the carbon fiber arrowband that will twine then again with scraper, and then the rotation manual rocking handle, continue to twine the carbon fiber arrowband.Carry out said process so repeatedly, successively twine carbon fiber layer;
Twine 20～30 layers according to above-mentioned technology, 3～5 millimeter are thick, temporarily stop afterwards twining, and heating with hair dryer, winding layer makes it begin to solidify; Blow and used cold wind in 5～10 minutes behind the hot blast instead and blew 10 minutes, the purpose of blowing a cold wind over is to reduce temperature, slows down curing reaction speed; And then by above-mentioned technology continuation winding; Carry out once cold and hot blowing after 20～30 layers of every windings, meet the requirements of size until twining gross thickness;
The carbon fiber arrowband is cut off, and then with scraper blade coating one deck epoxy glue;
(4) will wind and take off, with the latex rubber bag splendid attire and vacuumize sealing through the graphite cylinder of primary solidification; Put into drying baker and solidified 30 minutes～4 hours for 100～150 ℃, resin is fully solidified;
(5) sample that is cured is put into vacuum sintering furnace, carbonization under nitrogen protection; Carbonization technique: per minute heats up 5 ℃ to 500 ℃; Per minute heats up 1 ℃ to 700 ℃ then; Per minute heats up 2 ℃ to 900 ℃ then; Per minute heats up 5 ℃ to 2000 ℃, cooling;
(6) sample after the carbonization is taken out in sintering furnace, processes inside and outside garden and end face, make the hot pressing die former at last with grinding machine, lathe.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102528037A (en) * | 2011-12-30 | 2012-07-04 | 宁波江丰电子材料有限公司 | Sintering mold and manufacturing method thereof |
| CN101911827B (en) * | 2008-07-17 | 2013-09-11 | Jc科技有限公司 | Carbon heating element and production method thereof |
| CN104943245A (en) * | 2015-05-26 | 2015-09-30 | 南通山剑石墨设备有限公司 | Carbon fiber wound graphite cylinder and machining process thereof |
| CN105252830A (en) * | 2015-09-17 | 2016-01-20 | 南通山剑石墨设备有限公司 | Graphite cylinder |
| CN105299049A (en) * | 2015-04-24 | 2016-02-03 | 侯玉杰 | Carbon fiber-wound graphite bearing |
| CN106832750A (en) * | 2016-07-01 | 2017-06-13 | 宜兴市凯诚模具有限公司 | A kind of carbon fibre moulding and preparation method thereof |
| CN110526730A (en) * | 2019-09-12 | 2019-12-03 | 北京动力机械研究所 | A kind of reinforced graphite heating element structure and preparation method thereof |
| TWI701215B (en) * | 2019-05-21 | 2020-08-11 | 日商杰富意化學股份有限公司 | Method for manufacturing negative-electrode material for li-ion secondary cell |
| CN113416087A (en) * | 2021-07-20 | 2021-09-21 | 西安美兰德新材料有限责任公司 | Preparation method of high-strength combined carbon/carbon hot-pressing mold |
| CN113847805A (en) * | 2021-09-28 | 2021-12-28 | 山东交通学院 | Ultra-high temperature sintering furnace |
| CN113956060A (en) * | 2021-12-03 | 2022-01-21 | 福州赛瑞特新材料技术开发有限公司 | Carbon-carbon composite material ring for hot-pressing sintering and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101911827B (en) * | 2008-07-17 | 2013-09-11 | Jc科技有限公司 | Carbon heating element and production method thereof |
| 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 |
| CN102528037A (en) * | 2011-12-30 | 2012-07-04 | 宁波江丰电子材料有限公司 | Sintering mold and manufacturing method thereof |
| CN105299049A (en) * | 2015-04-24 | 2016-02-03 | 侯玉杰 | Carbon fiber-wound graphite bearing |
| CN104943245A (en) * | 2015-05-26 | 2015-09-30 | 南通山剑石墨设备有限公司 | Carbon fiber wound graphite cylinder and machining process thereof |
| CN105252830A (en) * | 2015-09-17 | 2016-01-20 | 南通山剑石墨设备有限公司 | Graphite cylinder |
| CN106832750A (en) * | 2016-07-01 | 2017-06-13 | 宜兴市凯诚模具有限公司 | A kind of carbon fibre moulding and preparation method thereof |
| TWI701215B (en) * | 2019-05-21 | 2020-08-11 | 日商杰富意化學股份有限公司 | Method for manufacturing negative-electrode material for li-ion secondary cell |
| CN110526730A (en) * | 2019-09-12 | 2019-12-03 | 北京动力机械研究所 | A kind of reinforced graphite heating element structure and preparation method thereof |
| CN113416087A (en) * | 2021-07-20 | 2021-09-21 | 西安美兰德新材料有限责任公司 | Preparation method of high-strength combined carbon/carbon hot-pressing mold |
| CN113416087B (en) * | 2021-07-20 | 2022-06-28 | 西安美兰德新材料有限责任公司 | Preparation method of high-strength combined carbon/carbon hot-pressing mold |
| CN113847805A (en) * | 2021-09-28 | 2021-12-28 | 山东交通学院 | Ultra-high temperature sintering furnace |
| CN113956060A (en) * | 2021-12-03 | 2022-01-21 | 福州赛瑞特新材料技术开发有限公司 | Carbon-carbon composite material ring for hot-pressing sintering and preparation method thereof |
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