CN105645397B - It is a kind of for hyperfine structure graphite of EDM and preparation method thereof - Google Patents
It is a kind of for hyperfine structure graphite of EDM and preparation method thereof Download PDFInfo
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- CN105645397B CN105645397B CN201610120488.0A CN201610120488A CN105645397B CN 105645397 B CN105645397 B CN 105645397B CN 201610120488 A CN201610120488 A CN 201610120488A CN 105645397 B CN105645397 B CN 105645397B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23H—WORKING OF METAL BY THE ACTION OF A HIGH CONCENTRATION OF ELECTRIC CURRENT ON A WORKPIECE USING AN ELECTRODE WHICH TAKES THE PLACE OF A TOOL; SUCH WORKING COMBINED WITH OTHER FORMS OF WORKING OF METAL
- B23H1/00—Electrical discharge machining, i.e. removing metal with a series of rapidly recurring electrical discharges between an electrode and a workpiece in the presence of a fluid dielectric
- B23H1/04—Electrodes specially adapted therefor or their manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23H—WORKING OF METAL BY THE ACTION OF A HIGH CONCENTRATION OF ELECTRIC CURRENT ON A WORKPIECE USING AN ELECTRODE WHICH TAKES THE PLACE OF A TOOL; SUCH WORKING COMBINED WITH OTHER FORMS OF WORKING OF METAL
- B23H1/00—Electrical discharge machining, i.e. removing metal with a series of rapidly recurring electrical discharges between an electrode and a workpiece in the presence of a fluid dielectric
- B23H1/04—Electrodes specially adapted therefor or their manufacture
- B23H1/06—Electrode material
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of hyperfine structure graphite for EDM, primary raw material is mesophase pitch carbon microspheres, pitch coke powder and binding agent modified coal tar pitch；Wherein the mass ratio of mesophase pitch carbon microspheres and pitch coke powder is 9:1~7:3；The additive amount of modified coal tar pitch accounts for the 6 ~ 16% of raw material gross mass.The preparation method of the present invention, step are as follows：Pitch coke and modified coal tar pitch progress kneading, film-making, crushing are first obtained into modified pitch coke piece powder；Modified pitch coke piece powder be uniformly mixed and then crushed with mesophase pitch carbon microspheres again, then the material after crushing is uniformly mixed and stood；The mixed material after standing is subjected to isostatic pressing again, green compact sample is obtained after demoulding；Roasting charing process, graphitization processing are carried out after green compact sample is stood again to get to hyperfine structure graphite.The present invention hyperfine structure graphite, fill up the ultra-fine grade in China, for EDM industries graphite products blank.
Description
Technical field
The present invention relates to graphite material fields more particularly to a kind of for hyperfine structure graphite of EDM and preparation method thereof.
Background technology
EDM（Electrical discharge machining）It is one of important process processed to labyrinth metal parts, it utilizes continuous moving
Electrode material to workpiece carry out pulse spark put, ablation metal, excision forming is usually used in the production of blanking die and mold.Mesh
The preceding electrode material for EDM industries has very much, mainly includes metal electrode and non-metal electrode.Metal electrode mainly includes
Associated materials such as copper, zinc, tungsten and alloy, but metal electrode there are problems that in produce reality, as copper electrode fusing point less than
1100 DEG C, coefficient of thermal expansion is big, loss is fast, and material process velocity is slow；Tungsten and alloy are expensive, processing difficulties, and electric conductivity is not
Enough ideals, operation strategies are very limited.Non-metal electrode is mainly graphite material, it shows metal and nonmetallic object simultaneously
Characteristic is managed, directly can become gaseous state from solid-state at high temperature, sublimation temperature is led up to 3600 DEG C or more, excellent conduction
Heat and processability, low thermal coefficient of expansion are cheap that graphite is enable to become fabulous electrode material.
Domestic market is many for the graphite electrode type of EDM industries, is divided into superfine grade by size（1 ~ 5 micron）、
Ultra-fine grade（6 ~ 10 microns）, fine-grade（11 ~ 20 microns）, middle grade（21 ~ 100 microns）.Granularity is thinner, and EDM machining accuracies are just
It is higher.Country's main preparation methods are with 15 ~ 20 microns of granularity at present（Fine-grade）Pitch coke or petroleum coke be aggregate, coal tar pitch
Or resin is bonding agent, and the technological processes such as piece, second-time breakage, molding, roasting impregnation cycles, graphitization are ground by kneading, roller
Prepare EDM graphite.At least need just have within 8 ~ 10 months ripe product using traditional raw material and process conditions, and making 6 ~
10 microns（Ultra-fine grade）Not only the period is longer, but also is also easy to be formed in roasting and graphitization temperature rise period for EDM graphitizations product
Crack leads to fault of construction, causes yield rate not high, and mainly due to ultra-fine grain product itself compactness height, internal stress is big,
The volatile matter generated with temperature raising is not easy to discharge outward from interiors of products, and the material of hot stage is from unordered Turbostratic
Carbon atom occurs and retakes the carbonization structure to form three-dimensional order, and is easy to cause the generation of minute crack；And dipping roasting repeatedly
Environmental pressure is further aggravated in burning, and the roasting number risk that excessively also larger production cracks increases production cost.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of for EDM industries, ultra-fine
Graphite of structure and preparation method thereof.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of hyperfine structure graphite for EDM, primary raw material are mesophase pitch carbon microspheres, pitch coke powder and bonding
Agent modified coal tar pitch（105 ~ 115 DEG C of softening point）；The mass ratio of wherein described mesophase pitch carbon microspheres and pitch coke powder is 9:1~
7:3；The additive amount of modified coal tar pitch accounts for the 6 ~ 16% of raw material gross mass.
The present invention also provides a kind of preparation methods of the hyperfine structure graphite for EDM, include the following steps：
（1）Pitch coke and modified coal tar pitch progress kneading, film-making, crushing are first obtained into modified pitch coke piece powder；Roller grinds piece
It can make aggregate and pitch Forced Mixing, improve pitch-coating intensity；
（2）By step（1）Obtained modified pitch coke piece powder and mesophase pitch carbon microspheres be uniformly mixed and then powder
It is broken, then the material after crushing is stood after mixing；It often adds a raw material or must pass through by primary crushing mixed
It closes, different material and different grain size is made to be uniformly dispersed；
（3）By step（2）Mixed material after standing carries out isostatic pressing, and green compact sample is obtained after demoulding；
（4）By step（3）Obtained green compact sample carries out roasting charing process after standing；
（5）By step（4）The sample of charing process carries out graphitization processing to get to the hyperfine structure graphite.
Above-mentioned preparation method, it is preferred that the step（4）In, roasting charing process process segment carries out, specific steps
For：（a）First 198~202 DEG C are warming up to the heating rate of 4.8~5.2 DEG C/h；（b）Again with the heating of 2.9~3.1 DEG C/h speed
Rate is warming up to 309~401 DEG C；（c）Then 649~651 DEG C are warming up to the heating rate of 1.4~1.6 DEG C/h；（d）Again with 1.9
The heating rate of~2.1 DEG C/h is warming up to 798~802 DEG C；（e）1008 are warming up to the heating rate of 4.8~5.2 DEG C/h again~
1012℃；（f）Finally come out of the stove, then natural cooling with the rate of temperature fall of 5 DEG C/h to 60 ~ 80 DEG C/h.Charing qualification rate is 92% at present
More than.
Above-mentioned preparation method, it is preferred that the step（5）In, graphitization uses medium acheson furnace, burner hearth
Heating is stablized, fever is uniform.The process of graphitization processing is specially that the sample after charing first is uniformly heating to 1550~1850
DEG C, 2~5h is kept the temperature, then be uniformly heating to 2680~2820 DEG C, being finally down to 90 DEG C with the rate of temperature fall of 0.2~0.6 DEG C/h goes out
Stove, natural cooling, you can obtain hyperfine structure graphite.Graphitization qualification rate reaches more than 96%.
Above-mentioned preparation method, it is preferred that the step（3）In, the process of isostatic pressing is：First mixture is packed into
Compacting and vacuumize process, are re-fed into isostatic pressing machine in mold, first rise to 150MPa, voltage stabilizing with 7~10MPa/min rates
3~5min, then with 12~15MPa/min pressure release rate pressure releases to 70~90MPa, 3~5min of voltage stabilizing；Again with 8~10MPa/min
The pressure release of pressure release rate is to 20~40MPa, 2~5min of voltage stabilizing；Finally with 8~10MPa/min pressure release rate pressure releases to chamber pressure.
Above-mentioned preparation method, it is preferred that the step（1）In, the detailed process of kneading is：It is 4.2~5.9 by granularity
The pitch coke powder of micron is placed in vacuum kneader, and 120~160 DEG C are opened wide 1~2h of mixing, then add in 160~190 DEG C of moltens
State, softening point be 105~115 DEG C of modified coal tar pitch, close cover, vacuumize and 1~2h of kneading, wherein kneader rotating
Speed control is controlled in 80~100r/min, kneading temperature at 170~190 DEG C.
Above-mentioned preparation method, it is preferred that the step（2）In, it is 9~10 that the mixture that finally obtains, which is crushed to granularity,
Micron, the volatile matter quality of mixture account for 8wt% ~ 20wt% of entire mixture quality, the volatile matter quality of preferred mixture
Account for 8wt% ~ 15wt% of entire mixture quality.
Above-mentioned preparation method, it is preferred that the step（2）The time of repose of middle mixture is 3~5h；The step
（4）In green compact sample time of repose be 24~48h.
The present invention does raw material using mesocarbon microspheres, not only there is body contraction, and aggregate also generates contraction in itself, and contraction is got over
Greatly, density increment is bigger.Density graphited again can reach traditional two roasting of a leaching or two leachings, three roasting again after primary roasting
Graphited density.And graphitization product of the mesocarbon microspheres for aggregate is used, since overall shrinkage is bigger, roasting
Stage is particularly easy to crack.Inventor gropes to test with raw material induration property by experiment many times, studies and makes
Determined the present invention preparation method during good roasting and Graphitizing Furnace Rise Temprature Process Curve, make total pass rate reach 80% with
On.Overcome traditional raw material（Forge rear pitch coke and petroleum coke）With technique manufacturing process, occur in roasting and graphitizing process
The contraction of bulk sample（Body is shunk）, almost the contraction of the pitch generation only around aggregate, the shrinking percentage very little of aggregate lack
It falls into.
Compared with prior art, the advantage of the invention is that：
（1）The present invention, using modified coal tar pitch as binding agent, is adopted using mesophase pitch carbon microspheres and pitch coke as main raw material(s)
The circulation technology roast-impregnate is not needed to such formula, it is only necessary to once be roasted, primary graphitizing can obtain
Impregnating the density and intensity of roasted product three times twice to traditional material, the process time can foreshorten to 3 from original 8 ~ 10 months ~
5 months；Production cost is not only reduced, improves production efficiency, also energy saving, environmental protection.
（2）The preparation method of the present invention is by rational scientific matching, and rational roasting is carbonized and graphitization curve controlled,
Graphite products roasting and graphited qualification rate is made while enhancing product performance, effectively to control ultra-fine knot more than 92%
The graphite cost of structure.
（3）Raw material valency that the present invention uses is low to be easy to get, and property is stablized, and pre-treatment of raw material is simple for process easy to operate, substantially
The hyperfine structure graphite haveing excellent performance can be completed by traditional equipment to prepare.
（4）Hyperfine structure graphite made of the preparation method of the present invention, fills up the ultra-fine grade in China, the stone for EDM industries
The blank of graphite product.
Specific embodiment
For the ease of understanding the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Except there is a special instruction, the various reagents used in the present invention, raw material be can be commercially commodity or
Person can pass through product made from well known method.
Embodiment 1：
A kind of hyperfine structure graphite for EDM of the present invention, primary raw material are mesophase pitch carbon microspheres（Following letter
Claim：MCMB）, pitch coke powder and binding agent modified coal tar pitch（115 DEG C of softening point）；Wherein mesophase pitch carbon microspheres（MCMB）And drip
Green coke powder mass ratio is 9：1；The additive amount of modified coal tar pitch is total weight（Modified coal tar pitch+pitch coke powder+mesocarbon microspheres）
6.25%。
The preparation method of the hyperfine structure graphite of the present embodiment, includes the following steps：
（1）First by the pitch coke pitch coke powder that air-flow crushing to granularity is D50=5 micron, 30Kg pitch cokes are then put into
In powder to vacuum kneader, 150 DEG C are opened wide mixing 1h, add the modified coal tar pitch (softening point of the molten condition of about 170 DEG C of 20Kg
It is 115 DEG C), cover is closed, vacuumizes simultaneously kneading 2h, it is 180 DEG C to ensure the temperature in kneading process, the positive and negative rotating speed control of kneader
System is in 100r/min.
（2）By step（1）The thickener obtained after kneading adds in roll shaft pelleter while hot, by four film-makings, by what is obtained
Sheet stock is air-cooled to be down to room temperature；170 DEG C of roll surface temperature wherein in tableting processes, rotating speed 30r/min.
（3）By step（2）Obtained tablet be crushed to D50=22 micron modified pitch coke piece powder and 270Kg D50=
20 microns of MCMB（Pitch coke powder and MCMB ratios are 1: 9）It puts into V-type batch mixer together and tentatively mixes 2h, batch mixer
Rotating speed 100r/min.
（4）By step（3）Mixed material carries out air-flow crushing to D50=10 micron, then puts into V-type batch mixer and mix
3h is closed, the rotating speed 200r/min of batch mixer stands 4h after blanking, the quality of volatile matter accounts for mixture gross mass in mixture at this time
8.4wt%.
（5）Again by step（4）The material of middle mixing is slowly put into φ 166mm nitrile rubber molds, is compacted and is taken out true
20min is managed in vacancy, and isostatic pressing machine is put into after glue sealing, first rises to 150M pa, voltage stabilizing with the rate of pressure rise of 10MPa/min
5min；Again with 15MPa/min pressure release rate pressure releases to 90MPa, voltage stabilizing 5 minutes；Again with the pressure release of 10MPa/min pressure release rates extremely
30MPa, voltage stabilizing 2min；Finally with 10MPa/min pressure release rate pressure releases to chamber pressure, demoulding obtains regular cylindrical type after demoulding
Green compact sample is placed in room temperature environment and stands for 24 hours.
（6）Green compact sample is packed into stainless steel crucible, fills up the quartz sand that granularity is below 1mm, ram-jolt, sample is apart from earthenware
Crucible wall is more than 100mm, is more than 300mm apart from crucible top.Proceed by roasting carbonization process：（a）First with the heating rate of 5 DEG C/h
It is warming up to 200 DEG C；（b）Again 400 DEG C are warming up to the heating rate of 3 DEG C/h；（c）Then it is heated up with the heating rate of 1.5 DEG C/h
To 650 DEG C；（d）Again 800 DEG C are warming up to the heating rate of 2 DEG C/h；（e）Again 1100 DEG C are warming up to the heating rate of 5 DEG C/h；
（f）Finally with the rate of temperature fall of 5 DEG C/h to being cooled to room temperature, charing sample is obtained.
（7）Charing sample is fitted into acheson furnace and is uniformly heating to 1700 DEG C, keeps the temperature 2h, then be uniformly heating to
2800 DEG C, 90 DEG C/h is finally cooled to get to hyperfine structure graphite with 0.5 DEG C/h.
The present embodiment hyperfine structure graphite is by test：Its average grain diameter is 10 μm, bulk density 1.72g/cm3, resist
Compressive Strength is 68.6MPa, and flexural strength 32.1Mpa, 17.1 μ Ω m of resistivity, product qualified rate is more than 92%.Entire production
The product production cycle is 5 months.
Embodiment 2：
The technical process of the present embodiment is same as Example 1, and the difference lies in steps（3）In obtained MCMB and pitch
The grain size of coke powder is 9 microns, and the two mixing quality ratio is 8:2, volatile matter content accounts for mixture gross mass in mixture
9.1wt%.Final finished qualification rate is 88%.By graphite performance detection, average grain diameter is 9.5 microns；Bulk density is
1.74g/cm3, resistance to compression 71.1Mpa, anti-folding 32.9Mpa, 17.0 μ Ω m of resistivity.The present embodiment sample process-cycle is 5
Month.
Embodiment 3：
The technical process of the present embodiment is same as Example 2, and the mass ratio the difference lies in MCMB and pitch coke powder is
7:3, volatile matter content accounts for the 10wt% of mixture gross mass in mixture.Final sample qualification rate is more than 85%.By graphitization
Detection, average grain diameter are 9.9 microns；Bulk density is 1.77g/cm3, resistance to compression 79.5Mpa, anti-folding 41.5Mpa, resistivity
15.2μΩ·m.The present embodiment sample process-cycle is 5 months.
Claims (5)
- A kind of 1. preparation method of hyperfine structure graphite for EDM, which is characterized in that the hyperfine structure stone for EDM The primary raw material of ink is mesophase pitch carbon microspheres, pitch coke powder and binding agent modified coal tar pitch；Wherein described mesophase pitch charcoal The mass ratio of microballoon and pitch coke powder is 9:1~7:3；The additive amount of modified coal tar pitch accounts for the 6 ~ 16% of raw material gross mass；It is described to be used for The preparation method of the hyperfine structure graphite of EDM includes the following steps：（1）Pitch coke powder and modified coal tar pitch progress kneading, film-making, crushing are first obtained into modified pitch coke piece powder；（2）By step（1）Obtained modified pitch coke piece powder and mesophase pitch carbon microspheres be uniformly mixed and then are crushed, then Material after crushing is uniformly mixed and stood；（3）By step（2）Mixed material after standing carries out isostatic pressing, and green compact sample is obtained after demoulding；（4）By step（3）Obtained green compact sample carries out roasting charing process after standing；Roast charing process process segment into Row, the specific steps are：（a）First 198~202 DEG C are warming up to the heating rate of 4.8~5.2 DEG C/h；（b）Again with 2.9~3.1 DEG C/heating rate of h is warming up to 309~401 DEG C；（c）Then 649~651 are warming up to the heating rate of 1.4~1.6 DEG C/h ℃；（d）Again 798~802 DEG C are warming up to the heating rate of 1.9~2.1 DEG C/h；（e）Again with the heating of 4.8~5.2 DEG C/h speed Rate is warming up to 1008~1012 DEG C；（f）Finally come out of the stove, then natural cooling to 60~80 DEG C with the rate of temperature fall of 5 DEG C/h；（5）By step（4）The sample of charing process carries out graphitization processing to get to the hyperfine structure graphite；At graphitization The process of reason is specially that the sample after charing first is uniformly heating to 1550~1850 DEG C, keeps the temperature 2~5h, then be uniformly heating to 2680~2820 DEG C, finally 90 DEG C are down to the rate of temperature fall of 0.2~0.6 DEG C/h and come out of the stove, natural cooling, you can obtain ultra-fine knot Structure graphite.
- 2. preparation method as described in claim 1, which is characterized in that the step（3）In, the process of isostatic pressing is： Mixture is first fitted into compacting and vacuumize process in mold, is re-fed into isostatic pressing machine, first in 7~10MPa/min rates 150MPa, 3~5min of voltage stabilizing are risen to, then with 12~15MPa/min pressure release rate pressure releases to 70~90MPa, 3~5min of voltage stabilizing； Again with 8~10MPa/min pressure release rate pressure releases to 20~40MPa, 2~5min of voltage stabilizing；Finally with 8~10MPa/min pressure releases speed Rate pressure release is to chamber pressure.
- 3. preparation method as described in claim 1, which is characterized in that the step（1）In, the detailed process of kneading is：It will The pitch coke powder that granularity is 4.2~5.9 microns is placed in vacuum kneader, and 120~160 DEG C are opened wide 1~2h of mixing, are then added in 160~190 DEG C of molten conditions, modified coal tar pitch that softening point is 105~115 DEG C, close cover, vacuumize and 1~2h of kneading, In 80~100r/min, kneading temperature is controlled at 170~190 DEG C for the wherein positive and negative rotating speed control of kneader.
- 4. preparation method as described in claim 1, which is characterized in that the step（2）In, the mixture finally obtained crushes It it is 9~10 microns to granularity, the volatile matter quality of mixture accounts for 8wt% ~ 20wt% of entire mixture quality.
- 5. preparation method as described in claim 1, which is characterized in that the step（2）The time of repose of middle mixture for 3~ 5h；The step（4）In green compact sample time of repose be 24~48h.
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| CN106220178B (en) * | 2016-07-20 | 2020-01-10 | 湖南长宇科技发展有限公司 | Graphite material for heat exchanger and preparation method thereof |
| CN107903064A (en) * | 2017-12-21 | 2018-04-13 | 天津锦美碳材科技发展有限公司 | A kind of preparation method of hyperfine structure graphite for electrical discharge machining |
| CN108640682B (en) * | 2018-04-28 | 2021-04-23 | 深圳市赛普戴蒙德科技有限公司 | Graphite plate and manufacturing method thereof |
| CN109319775B (en) * | 2018-11-19 | 2020-10-02 | 成都炭素有限责任公司 | Preparation method of short-process high-density high-strength isotropic graphite |
| CN111925212B (en) * | 2020-07-03 | 2023-04-11 | 韶关赛普超硬材料科技有限公司 | Preparation method and application of special carbon material for electric spark machining |
| CN112441835A (en) * | 2020-12-04 | 2021-03-05 | 拓米(成都)应用技术研究院有限公司 | High-strength high-density carbon material and preparation method and application thereof |
| CN115609940B (en) * | 2022-12-20 | 2023-04-07 | 石家庄中正碳素有限公司 | Production process of graphite crucible |
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| CN102910912A (en) * | 2012-07-25 | 2013-02-06 | 天津市贝特瑞新能源科技有限公司 | High-hardness isostatic graphite and preparation method thereof |
| TWI455879B (en) * | 2012-08-09 | 2014-10-11 | China Steel Corp | Isotropic graphite material and method of producing the same |
| CN102898142B (en) * | 2012-09-04 | 2014-11-26 | 天津锦美碳材科技发展有限公司 | Preparation method for die graphite material used for electrical discharge machining |
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Address after: 410600 Xinkang Road, Yutan Town, Ningxiang County, Changsha City, Hunan Province (Huaxia Small and Medium-sized Enterprise Park) Patentee after: HUNAN CHANGYU SCIENCE AND TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: 410600 Xinkang Road, Yutan Town, Ningxiang County, Changsha City, Hunan Province (Huaxia Small and Medium-sized Enterprise Park) Patentee before: HUNAN CHANGYU NEW CARBON MATERIALS Co.,Ltd. |
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Denomination of invention: An Ultrafine Graphite for EDM and Its Preparation Method Effective date of registration: 20220928 Granted publication date: 20180629 Pledgee: Ningxiang sub branch of Bank of Changsha Co.,Ltd. Pledgor: HUNAN CHANGYU SCIENCE AND TECHNOLOGY DEVELOPMENT Co.,Ltd. Registration number: Y2022980016842 |