CN105884357B - It is a kind of for hot-forming graphite jig material and preparation method thereof - Google Patents

It is a kind of for hot-forming graphite jig material and preparation method thereof Download PDF

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CN105884357B
CN105884357B CN201610226522.2A CN201610226522A CN105884357B CN 105884357 B CN105884357 B CN 105884357B CN 201610226522 A CN201610226522 A CN 201610226522A CN 105884357 B CN105884357 B CN 105884357B
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preparation
rate
pitch
graphite
graphite jig
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CN105884357A (en
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杨程
刘金平
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Zhuzhou Changyu Carbon Co., Ltd
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HUNAN CHANGYU NEW CARBON MATERIALS CO Ltd
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Abstract

The invention discloses a kind of for hot-forming graphite jig material, and raw material includes mesophase pitch carbon microspheres, pitch and crystalline flake graphite, wherein the mass ratio of the mesophase pitch carbon microspheres and crystalline flake graphite is (19:1) ~ (7:3)；The additive amount of the pitch accounts for the 5% ~ 20% of total mass of raw material.The preparation method of graphite jig material of the invention, comprising the following steps: asphalt grout is made in pitch；By mesophase pitch carbon microspheres, crystalline flake graphite and asphalt grout, the kneading and roller rolls piece under conditions of vacuumizing, it is crushed after cooling, be added to the mixer mixing and successively carry out isostatic pressing after standing, roasting charing, is graphitized to get the graphite jig material is arrived.Of the invention not only reduces production cost for hot-forming graphite jig material and preparation method thereof, improves production efficiency, also energy saving, protects environment.

Description

It is a kind of for hot-forming graphite jig material and preparation method thereof
Technical field
The present invention relates to graphite jig fields more particularly to a kind of for hot-forming graphite jig material and its preparation Method.
Background technique
Graphite jig starts from phase earlier 1970s, along with geological prospecting, the probing and exploitation in mine, coal Exploration and exploitation, oil exploration and drilling well, the cutting of highway, especially granite and marble exploitation and cutting industry It grows rapidly, is increased considerably using the diamond alloy material of hot press forming technology and the demand of cemented carbide material, because The consumption of this graphite jig surges therewith, and the performance difference of graphite material directly influences hot-forming superhard material Quality.Hot-forming mode is generally divided into two kinds, resistance heating type and mid-frequency induction heating type.Hot-forming Superhard Drill Technique requirement: temperature close to 1000 DEG C, form hot pressing in 16 ~ 18MPa, 5 ~ 20min of heat-insulation pressure keeping under non-vacuum.? Under this condition, graphite mo(u)ld has consistency height, high mechanical strength, the porosity is small, antioxygenic property is good, degree of graphitization is high etc. is needed Feature.
Currently, the main raw material(s) of the production of domestic graphite jig is petroleum coke, pitch coke, natural or artificial graphite, drip Blueness, resin etc., by broken, kneading, roll film-making, second-time breakage, compression moulding, charing impregnation cycles, finally graphitization is made It is made the original idiosome of mold, then machined at hot pressing type graphite jig of different specifications and sizes.Using traditional former material Material and process conditions, which generally require, can just produce die blank for 8 ~ 10 months, and multiple charing impregnation technology not only expends largely The energy such as electric power, coal, while improving human cost, more aggravated the burden of environment, and longer fabrication cycle Increase uncertain risk cost.Also, domestic a large amount of graphite jig at present, is stressed by the charing dipping time of raising Pursue its high bulk density, high intensity and have ignored High Purity, hyperfine structure etc..And the graphite jig intensity of hyperfine structure Greatly, higher pressure when hot pressing can be resisted, convenient for forming the superhard material of higher performance；The light and compactness of finished surface are good After hot pressing workpiece is cooling, it can be conducive to demould；The graphite jig of High Purity has good inoxidizability, substantially reduces mold In impurity catalytic graphite oxidation at high temperature probability, mold can be improved in the excellent properties of comprehensive hyperfine structure and purifying Cycle-index improves hot pressing condition parameter, guarantees the preparation of superhard material.Therefore, the stone of a kind of High Purity, hyperfine structure is studied Black mold materials are also very necessary.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of for hot-forming graphite Mold materials and preparation method thereof.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
It is a kind of for hot-forming graphite jig material, raw material includes mesophase pitch carbon microspheres, pitch and scale Graphite, wherein the mass ratio of the mesophase pitch carbon microspheres and crystalline flake graphite is (19:1) ~ (7:3)；The addition of the pitch Amount accounts for the 5% ~ 20% of total mass of raw material.
Above-mentioned graphite jig material, it is preferred that the softening point temperature of the pitch is 200 ~ 205 DEG C, the scale stone The purity of ink is 99% or more.
The inventive concept total as one, the present invention also provides a kind of preparation method of above-mentioned graphite jig material, packets Include following steps:
(1) asphalt grout is made in pitch；
(2) asphalt grout for obtaining mesophase pitch carbon microspheres, crystalline flake graphite and step (1), in the condition vacuumized Lower kneading and roller roll piece, crush after cooling, are added to the mixer mixing and stand；
(3) mixed material after step (2) is subjected to isostatic pressing, obtains green compact sample after demoulding；
(4) roasting charing process is carried out after standing the green compact sample that step (3) obtains；
(5) sample of step (4) roasting charing process is subjected to graphitization processing to get the graphite jig material is arrived.
Above-mentioned preparation method, it is preferred that the detailed process of the isostatic pressing in the step (3) are as follows: first will mixing Material is fitted into compacting and vacuumize process in mold, is re-fed into isostatic pressing machine and is risen to 7~10MPa/min rate of pressure rise 120~150MPa, 10~15min of pressure stabilizing, then with 15~20MPa/min pressure release rate pressure release to 70~90MPa, pressure stabilizing 5~ 10min；Finally with 10~15MPa/min pressure release rate pressure release to chamber pressure.
Above-mentioned preparation method, it is preferred that in the step (4), roasting charing process process segment is carried out, specific to walk Suddenly are as follows: (a) is first warming up to 300~302 DEG C with the heating rate of 8~10 DEG C/h；(b) again with the heating rate of 2.9~3.1 DEG C/h It is warming up to 450~452 DEG C；(c) 649~651 DEG C then 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 850~852 DEG C；(e) 1008 are warming up to the heating rate of 2.9~3.1 DEG C/h again~ 1012℃；(f) it is finally come out of the stove with the rate of temperature fall of 5 DEG C/h to 60 ~ 80 DEG C, natural cooling.Qualification rate is carbonized 90% or more.This The heating curve of the roasting charing process process of invention be by repeatedly testing, comprehensive analysis obtains, substantially reduce charcoal and melt The phenomenon that splitting guarantees product qualification rate.
Above-mentioned preparation method, it is preferred that in the step (5), graphitization uses medium acheson furnace, burner hearth Heating is stablized, fever is uniform.Graphited detailed process are as follows: be first uniformly heating to 1550~1850 DEG C, keep the temperature 2~5h, then It is even to stop power transmission when being warming up to 2680~2820 DEG C；Wherein in temperature-rise period, start to lead to when temperature reaches 2100 DEG C ~ 2150 DEG C Enter chlorine, continues to be passed through 10~12h of chlorine after stopping power-off, the rate that is passed through of chlorine is 12 ~ 15m3/h；Drop after stopping power transmission Warm rate is 2~6 DEG C/h.
Above-mentioned preparation method, it is preferred that in the step (2), the detailed process of kneading are as follows: by granularity be 7~8 microns Mesophase pitch carbon microspheres be placed in vacuum kneader, with 120~140 DEG C of temperature open wide mixing 1~2h, then be added drip Green slurry vacuumizes simultaneously 1~2h of kneading, then is warming up to 220 ~ 240 DEG C of vacuum 1 ~ 2h of kneading, and wherein kneader forward rotational speed controls In 80~120r/min.
Above-mentioned preparation method, it is preferred that in the step (2), the granularity of mixed material is 9~10 microns after crushing, The volatile matter quality of mixed material accounts for 5wt% ~ 15wt% of mixed material quality；It is further preferred that the volatile matter of mixed material Quality accounts for 5wt% ~ 10wt% of entire mixed material quality.
Above-mentioned preparation method, it is preferred that in the step (2), the time of repose of mixed material is 3~5h；The step Suddenly the green compact sample time of repose in (4) is 24~48h.
Above-mentioned preparation method, it is preferred that in the step (1), the specific preparation process of asphalt grout are as follows: by pitch with Ethyl acetate is mixed according to the amount that mass ratio is (4:1) ~ (3:2), stirs 0.5 ~ 1h with the mixing speed of 80 ~ 120r/min.
The present invention does raw material using mesocarbon microspheres, not only has body contraction, aggregate itself also generates contraction, and contraction is got over Greatly, density increment is bigger, and compactness wants high after charing, it is possible to reduce the number of dipping and roasting.It is primary to carbonize later graphite again The density of change can achieve traditional dipping twice and roast charing three times or impregnate four charings graphited density again three times.
The present invention is due to using mesocarbon microspheres for the graphitization product of main aggregate, since overall shrinkage is bigger, It is particularly easy to crack in firing stage, inventor passes through research and raw material ratio many times, starches by hard pitch The mobility of material regulates and controls, and uniformity is dispersed in the case of a large number of experiments such as the mode of aggregate, repeatedly the adaptable charing of test and stone Inkization curve, the comprehensive charging curve obtained can guarantee to carbonize qualification rate, find out a whole set of finally and be suitble to prepare graphite The process conditions of mold original blank, charing and graphited qualification rate are more than 95%.
Compared with the prior art, the advantages of the present invention are as follows:
(1) present invention, using hard pitch as binder, is matched using mesophase pitch carbon microspheres as main raw material(s) using such Side does not need the circulation technology carbonize-impregnate, it is only necessary to which, by primary charing, primary graphitizing can be obtained by traditional material The density and intensity of material dipping, four carbonization products three times, process time can foreshorten to 3 ~ 5 months from original 8 ~ 10 months； Production cost is not only reduced, production efficiency is improved, it is also energy saving, protect environment.
(2) present invention disperses hard pitch using ethyl acetate for the first time, enhances mobility of the hard pitch in kneading, increases The ability of strong uniform cladding aggregate, improves cementability when forming and being heated evenly property when carbonizing, reduces after volatile matter is lost and produce Raw hole reduces material porosity.When vacuumizing simultaneously, 90% or more ethyl acetate can be recycled by condensing, circulation makes With economizing on resources.
(3) graphite jig of the invention passes through stringent purification process, and ash content is less than 10ppm, makes product hot-forming Impurity itself is reduced in technical process to the catalysis oxidation of mold body, greatly improves antioxygenic property.
(4) the mesophase pitch carbon microspheres of the invention using ultra-fine grain diameter are as main material, and body is shunk and self-constriction energy The compactness and intensity of material are enough greatly enhanced, oxidation resistance is improved, increases resistivity.
(5) preparation method of the invention is carbonized and is graphitized curve controlled by reasonable scientific matching, reasonable roasting, Make graphite products roasting and graphited qualification rate more than 95%, while enhancing product performance, effectively controls ultra-fine knot The graphite cost of structure.
(6) the raw material valence that the present invention uses is low to be easy to get, and property is stablized, and pre-treatment of raw material simple process is easy to operate, substantially The graphite jig haveing excellent performance can be completed by traditional equipment to prepare.
To sum up, the present invention overcomes traditional raw material (forging rear pitch coke and petroleum coke) occurs in roasting and graphitizing process The contraction (body contraction) of bulk sample, the contraction that almost pitch only around aggregate generates, the shrinking percentage very little of aggregate lack It falls into；Process time of the invention can foreshorten to 3 ~ 5 months from traditional 8 ~ 10 months；Production cost is not only reduced, production is improved Efficiency, it is also energy saving, protect environment.
Specific embodiment
To facilitate the understanding of 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 scope.
Except there is a special instruction, the various reagents used in the present invention, raw material be can commodity commercially or Person can the product as made from well known method.
Embodiment 1:
It is a kind of it is of the invention be used for hot-forming graphite jig material, primary raw material includes mesophase pitch carbon microspheres The crystalline flake graphite that (hereinafter referred to as: MCMB), hard pitch (softening point temperature is 202 DEG C) and purity are 99%；Wherein MCMB and squama Piece graphite mass ratio is 19:1；The additive amount of hard pitch is the 20% of total weight (hard pitch+MCMB+ crystalline flake graphite).
The preparation method for hot-forming graphite jig material of the present embodiment, comprising the following steps:
(1) the 10Kg hard pitch (softening point temperature is 202 DEG C) for sieving with 100 mesh sieve net is put into the acetic acid second of 2.5Kg In ester solution, hard pitch slurry is prepared with three leaf agitating paddle uniform stirring 0.5h, speed of agitator 80r/min；
(2) be with air-flow crushing to granularity by MCMB D50=8 micron MCMB, then put into 38KgMCMB and 2Kg scale For graphite into vacuum kneader, 120 DEG C are opened wide mixing 1h, stop heating, and the high temperature drip of 12.5Kg step (1) preparation is then added Green slurry closes cover, vacuumizes simultaneously kneading 1h, then be warming up to 240 DEG C of kneading 1h, kneader forward rotational speed is controlled in 80r/ min；
(3) roll shaft pelleter is added in the thickener obtained after step (2) kneading while hot, passes through four film-making (roll surface temperatures 210 DEG C, revolving speed 30r/min), air-cooled be cooled to room temperature of obtained sheet stock is crushed to D50=25 micron, is subsequently placed in V-type mixing 1h(revolving speed 100r/min is tentatively mixed in machine) after, by mixed material progress air-flow crushing to D50=9 micron, then put into V-type The revolving speed 200r/min of 3h(batch mixer is mixed in batch mixer), 4h is stood after blanking, uniformly mixed material is obtained, mixes at this time The quality of volatile matter accounts for the 11.3wt% of mixture total mass in material；
(4) mixed material after step (3) is slowly put into φ 166mm nitrile rubber mold, counterweight vibration compacting, 15min is vacuumized, equal pressing equipment is put into after glue sealing, 150MPa, pressure stabilizing are first risen to the rate of pressure rise of 10MPa/min 10min；Again with 15MPa/min pressure release rate pressure release to 90MPa, pressure stabilizing 10min；Finally extremely with the pressure release of 5MPa/min pressure release rate Chamber pressure, demoulding, obtains regular cylindrical type green compact sample after demoulding, be placed in room temperature environment and stand 48h；
(5) green compact sample that step (4) obtains is fitted into stainless steel crucible, filling up granularity is that 0.5mm is below artificial Graphite powder, ram-jolt, sample are greater than 80mm apart from sidewall of crucible, are greater than 220mm apart from crucible top, start to carry out roasting carbonization process: (a) 300 DEG C first are warming up to the heating rate of 6.5 DEG C/h；(b) 400 DEG C are warming up to the heating rate of 4.5 DEG C/h again；(c) so 700 DEG C are warming up to afterwards with the heating rate of 1.5 DEG C/h；(d) 850 DEG C are warming up to the heating rate of 2 DEG C/h again；(e) again with 2.5 DEG C/heating rate of h is warming up to 1100 DEG C；(f) it is finally cooled to room temperature with the rate of temperature fall of 5 DEG C/h, obtains charing sample, charcoal Change 90% or more qualification rate；
(6) sample after step (5) charing is placed in medium acheson furnace and is uniformly heating to 1850 DEG C, heat preservation 5h, then 2100 DEG C are uniformly heating to, start with 15m3The rate of/h is passed through chlorine, when temperature rises to 2820 DEG C, stops power transmission, Chlorine continue convey 10h, be finally down to 90 DEG C with the rate of temperature fall of 5 DEG C/h and come out of the stove, natural cooling, can be obtained hyperfine structure, High-intensitive, high-densit, High Purity, low-ash graphite jig original blank, graphitization qualification rate reach 98% or more.
The average grain diameter of graphite jig material manufactured in the present embodiment is 9 μm, bulk density 1.92g/cm3, pressure resistance Degree is 125.6MPa, flexural strength 69.8Mpa, 20.1 μ Ω m of resistivity, Shore hardness 56, the porosity 12%, ash content 7 Ppm, product qualified rate is 89% or more；Wherein, using GB/T 24528-2009 test stone bulk density；Compressive resistance According to GB/T 1431-2009 standard testing；Resistivity is tested according to GB/T 1410-2006；Shore hardness is according to GB/T 4341-2001 standard testing；The porosity is tested according to GB/T 6155-2008 examination criteria；Ash content is according to GB/T 9345.1- 2008.Entire graphite jig material production cycle is 5 months.
Embodiment 2:
It is a kind of it is of the invention be used for hot-forming graphite jig material, primary raw material includes mesophase pitch carbon microspheres (hereinafter referred to as: MCMB), hard pitch (softening point temperature is 202 DEG C) and High Purity crystalline flake graphite (purity 99%)；Wherein MCMB and High Purity crystalline flake graphite mass ratio are 9:1；The additive amount of hard pitch is total weight (hard pitch+MCMB+ High Purity Crystalline flake graphite) 10%.
The preparation method for hot-forming graphite jig material of the present embodiment, comprising the following steps:
(1) the 10Kg hard pitch (softening point temperature is 202 DEG C) for sieving with 100 mesh sieve net is put into the acetic acid second of 2.5Kg In ester solution, hard pitch slurry is prepared with three leaf agitating paddle uniform stirring 20min, speed of agitator 100r/min；
(2) be with air-flow crushing to granularity by MCMB D50=8 micron MCMB, then put into 81KgMCMB and 9Kg it is high-purity Change crystalline flake graphite into vacuum kneader, 110 DEG C are opened wide mixing 1h, stop heating, and 12.5Kg step (1) preparation is then added Hard pitch slurry closes cover, vacuumizes simultaneously kneading 1.5h, then be warming up to 250 DEG C of kneading 0.5h, kneader forward rotational speed control System is in 50r/min；
(3) roll shaft pelleter is added in the thickener obtained after step (2) kneading while hot, passes through four film-making (roll surface temperatures 230 DEG C, revolving speed 20r/min), air-cooled be cooled to room temperature of obtained sheet stock is crushed to D50=25 micron, is subsequently placed in V-type mixing 2h(revolving speed 100r/min is tentatively mixed in machine) after, by mixed material progress air-flow crushing to D50=9 micron, then put into V-type The revolving speed 200r/min of 3h(batch mixer is mixed in batch mixer), 4h is stood after blanking, uniformly mixed material is obtained, mixes at this time The quality of volatile matter accounts for the 8.67wt% of mixture total mass in material；
(4) mixed material after step (3) is slowly put into φ 166mm nitrile rubber mold, counterweight vibration compacting, 20min is vacuumized, equal pressing equipment is put into after glue sealing, 150MPa, pressure stabilizing are first risen to the rate of pressure rise of 10MPa/min 8min；Again with 15MPa/min pressure release rate pressure release to 90MPa, pressure stabilizing 18min；Finally extremely with the pressure release of 5MPa/min pressure release rate Chamber pressure, demoulding, obtains regular cylindrical type green compact sample after demoulding, be placed in room temperature environment and stand for 24 hours；
(5) green compact sample that step (4) obtains is fitted into stainless steel crucible, filling up granularity is that 0.5mm is below artificial Graphite powder, ram-jolt, sample are greater than 80mm apart from sidewall of crucible, are greater than 220mm apart from crucible top, start to carry out roasting carbonization process: (a) 300 DEG C first are warming up to the heating rate of 6.5 DEG C/h；(b) 400 DEG C are warming up to the heating rate of 4.5 DEG C/h again；(c) so 700 DEG C are warming up to afterwards with the heating rate of 1.5 DEG C/h；(d) 800 DEG C are warming up to the heating rate of 2 DEG C/h again；(e) again with 2.5 DEG C/heating rate of h is warming up to 1100 DEG C；(f) finally with the rate of temperature fall of 5 DEG C/h to being cooled to room temperature, charing sample is obtained, Carbonize 85% or more qualification rate；
(6) sample after step (5) charing is placed in medium acheson furnace and is uniformly heating to 1850 DEG C, heat preservation 5h, then 2100 DEG C are uniformly heating to, start with 15m3The rate of/h is passed through chlorine, when temperature rises to 2820 DEG C, stops power transmission, Chlorine continue convey 10h, be finally down to 90 DEG C with the rate of temperature fall of 5 DEG C/h and come out of the stove, natural cooling, can be obtained hyperfine structure, High-intensitive, high-densit, High Purity, low-ash graphite jig original blank, graphitization qualification rate reach 98% or more.
The average grain diameter of graphite jig material manufactured in the present embodiment is 9 μm, bulk density 1.90g/cm3, pressure resistance Degree is 115.6MPa, flexural strength 62.8MPa, 19.1 μ Ω m of resistivity, Shore hardness 54, the porosity 14%, ash content 7 Ppm, product qualified rate is 84% or more；Wherein, using GB/T 24528-2009 test stone bulk density；Compressive resistance According to GB/T 1431-2009 standard testing；Resistivity is tested according to GB/T 1410-2006；Shore hardness is according to GB/T 4341-2001 standard testing；The porosity is tested according to GB/T 6155-2008 examination criteria；Ash content is according to GB/T 9345.1- 2008.Entire graphite jig material production cycle is 5 months.
Embodiment 3:
It is a kind of it is of the invention be used for hot-forming graphite jig material, primary raw material includes mesophase pitch carbon microspheres (hereinafter referred to as: MCMB), hard pitch (softening point temperature is 202 DEG C) and High Purity crystalline flake graphite (purity 99%)；Wherein MCMB and High Purity crystalline flake graphite mass ratio are 17:3；The additive amount of hard pitch is that (hard pitch+MCMB+ is high-purity for total weight Change crystalline flake graphite) 10%.
The preparation method for hot-forming graphite jig material of the present embodiment, comprising the following steps:
(1) the 10Kg hard pitch (softening point temperature is 202 DEG C) for sieving with 100 mesh sieve net is put into the acetic acid second of 2.5Kg In ester solution, hard pitch slurry is prepared with three leaf agitating paddle uniform stirring 15min, speed of agitator 120r/min；
(2) be with air-flow crushing to granularity by MCMB D50=8 micron MCMB, then put into 76.5KgMCMB and 13.5Kg For High Purity crystalline flake graphite into vacuum kneader, 110 DEG C are opened wide mixing 1h, stop heating, and 12.5Kg step (1) system is then added Standby hard pitch slurry closes cover, vacuumizes simultaneously kneading 1.5h, then be warming up to 250 DEG C of kneading 0.5h, kneader forward direction turns Speed control is in 50r/min；
(3) roll shaft pelleter is added in the thickener obtained after step (2) kneading while hot, passes through four film-making (roll surface temperatures 230 DEG C, revolving speed 20r/min), air-cooled be cooled to room temperature of obtained sheet stock is crushed to D50=25 micron, is subsequently placed in V-type mixing 1h(revolving speed 100r/min is tentatively mixed in machine) after, by mixed material progress air-flow crushing to D50=9 micron, then put into V-type The revolving speed 200r/min of 2h(batch mixer is mixed in batch mixer), 4h is stood after blanking, uniformly mixed material is obtained, mixes at this time The quality of volatile matter accounts for the 8.35wt% of mixture total mass in material；
(4) mixed material after step (3) is slowly put into φ 166mm nitrile rubber mold, counterweight vibration compacting, 20min is vacuumized, equal pressing equipment is put into after glue sealing, 150MPa, pressure stabilizing are first risen to the rate of pressure rise of 10MPa/min 8min；Again with 15MPa/min pressure release rate pressure release to 90MPa, pressure stabilizing 18min；Finally extremely with the pressure release of 5MPa/min pressure release rate Chamber pressure, demoulding, obtains regular cylindrical type green compact sample after demoulding, be placed in room temperature environment and stand for 24 hours；
(5) green compact sample that step (4) obtains is fitted into stainless steel crucible, filling up granularity is that 0.5mm is below artificial Graphite powder, ram-jolt, sample are greater than 80mm apart from sidewall of crucible, are greater than 220mm apart from crucible top, start to carry out roasting carbonization process: (a) 300 DEG C first are warming up to the heating rate of 6.5 DEG C/h；(b) 400 DEG C are warming up to the heating rate of 4.5 DEG C/h again；(c) so 700 DEG C are warming up to afterwards with the heating rate of 1.5 DEG C/h；(d) 850 DEG C are warming up to the heating rate of 2 DEG C/h again；(e) again with 2.5 DEG C/heating rate of h is warming up to 1100 DEG C；(f) finally with the rate of temperature fall of 5 DEG C/h to being cooled to room temperature, charing sample is obtained, Carbonize 88% or more qualification rate；
(6) sample after step (5) charing is placed in medium acheson furnace and is uniformly heating to 1850 DEG C, heat preservation 5h, then 2100 DEG C are uniformly heating to, start with 15m3The rate of/h is passed through chlorine, when temperature rises to 2820 DEG C, stops power transmission, Chlorine continue convey 10h, be finally down to 90 DEG C with the rate of temperature fall of 5 DEG C/h and come out of the stove, natural cooling, can be obtained hyperfine structure, High-intensitive, high-densit, High Purity, low-ash graphite jig original blank, graphitization qualification rate reach 98% or more.
Its average grain diameter of graphite jig material manufactured in the present embodiment is 9 μm, bulk density 1.89g/cm3, resistance to compression Intensity is 102.2MPa, flexural strength 60.1MPa, 18.5 μ Ω m of resistivity, Shore hardness 55, the porosity 15%, ash content 7.5 ppm, product qualified rate is 84% or more；Wherein, using GB/T 24528-2009 test stone bulk density；Pressure resistance Intensity is according to GB/T 1431-2009 standard testing；Resistivity is tested according to GB/T 1410-2006；Shore hardness according to GB/T 4341-2001 standard testing；The porosity is tested according to GB/T 6155-2008 examination criteria；Ash content is according to GB/T 9345.1-2008.Entire graphite jig material production cycle is 5 months.

Claims (6)

1. a kind of preparation method for hot-forming graphite jig material, which is characterized in that the graphite jig material Raw material includes mesophase pitch carbon microspheres, pitch and crystalline flake graphite, wherein the mesophase pitch carbon microspheres and crystalline flake graphite Mass ratio is (19:1)~(7:3)；The additive amount of the pitch accounts for the 5%~20% of total mass of raw material；The mesophase pitch The granularity of carbon microspheres is 7~8 microns；The preparation method of the graphite jig the following steps are included:
(1) pitch and ethyl acetate are mixed and made into asphalt grout；
(2) asphalt grout for obtaining mesophase pitch carbon microspheres, crystalline flake graphite and step (1) is mixed under conditions of vacuumizing It pinches and roller rolls piece, crushed after cooling, be added to the mixer mixing and stand；
(3) mixed material after step (2) is subjected to isostatic pressing, obtains green compact sample after demoulding；The tool of isostatic pressing Body process are as follows: mixed material is first fitted into compacting and vacuumize process in mold, is re-fed into isostatic pressing machine with 7~10MPa/ Min rate of pressure rise rises to 120~150MPa, 10~15min of pressure stabilizing, then with 15~20MPa/min pressure release rate pressure release to 70~ 90MPa, 5~10min of pressure stabilizing；Finally with 10~15MPa/min pressure release rate pressure release to chamber pressure；
(4) roasting charing process is carried out after standing the green compact sample that step (3) obtains；Roast charing process process segment into Row, the specific steps are that: (a) 300~302 DEG C first are warming up to the heating rate of 8~10 DEG C/h；(b) again with 2.9~3.1 DEG C/ The heating rate of h is warming up to 450~452 DEG C；(c) 649~651 DEG C then are warming up to the heating rate of 1.4~1.6 DEG C/h； (d) 850~852 DEG C are warming up to the heating rate of 1.9~2.1 DEG C/h again；(e) again with the heating rate liter of 2.9~3.1 DEG C/h Temperature is to 1008~1012 DEG C；(f) it is finally come out of the stove with the rate of temperature fall of 5 DEG C/h to 60~80 DEG C, natural cooling；
(5) sample of step (4) roasting charing process is graphitized to get the graphite jig material is arrived；It is graphited Detailed process are as follows: be first uniformly heating to 1550~1850 DEG C, keep the temperature 2~5h, then be uniformly heating to stopping at 2680~2820 DEG C Power transmission；Wherein in temperature-rise period, starts to be passed through chlorine when temperature reaches 2100 DEG C~2150 DEG C, continue to be passed through after stopping power-off The rate that is passed through of 10~12h of chlorine, chlorine are 12~15m3/h；Rate of temperature fall after stopping power transmission is 2~6 DEG C/h.
2. preparation method as described in claim 1, which is characterized in that the softening point temperature of the pitch is 200~205 DEG C, The purity of the crystalline flake graphite is 99% or more.
3. preparation method as described in claim 1, which is characterized in that in the step (2), the detailed process of kneading are as follows: will The mesophase pitch carbon microspheres and crystalline flake graphite that granularity is 7~8 microns are placed in vacuum kneader, with 120~140 DEG C of temperature 1~2h of mixing is opened wide, asphalt grout is then added, vacuumizes simultaneously 1~2h of kneading, then be warming up to 220~240 DEG C of vacuum kneadings 1 ~2h, wherein the control of kneader forward rotational speed is in 80~120r/min.
4. preparation method as described in claim 1, which is characterized in that in the step (2), the granularity of mixed material after crushing It is 9~10 microns, the volatile matter quality of mixed material accounts for 5wt%~15wt% of mixed material quality.
5. preparation method as described in claim 1, which is characterized in that the mixed material time of repose in the step (2) is 3 ~5h；Green compact sample time of repose in the step (4) is 24~48h.
6. preparation method as described in claim 1, which is characterized in that in the step (1), asphalt grout was specifically prepared Journey are as follows: mix pitch, according to the amount that mass ratio is (4:1)~(3:2) with ethyl acetate with the stirring speed of 80~120r/min 0.5~1h of degree stirring.
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