CN105884357A - Graphite die material for hot-press molding and preparation method of graphite die material - Google Patents

Graphite die material for hot-press molding and preparation method of graphite die material Download PDF

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CN105884357A
CN105884357A CN201610226522.2A CN201610226522A CN105884357A CN 105884357 A CN105884357 A CN 105884357A CN 201610226522 A CN201610226522 A CN 201610226522A CN 105884357 A CN105884357 A CN 105884357A
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preparation
graphite
warming
pitch
die material
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CN105884357B (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 graphite die material for hot-press molding. The graphite die material is prepared from raw materials including pitch mesocarbon microbeads, pitch and flake graphite, wherein the mass ratio of the pitch mesocarbon microbeads to the flake graphite is (19:1)-(7:3), and the additive amount of pitch accounts for 5%-20% the total mass of the raw materials. A preparation method of the graphite die material comprises the following steps; pitch grout is prepared from the pitch; the pitch mesocarbon microbeads, the flake graphite and the pitch grout are mixed, kneaded and rolled to form flakes under a vacuumized condition, cooled, crushed, added to a mixer to be mixed, left to stand and then sequentially subjected to isostatic pressure molding, carbonization through calcination and graphitization, and the graphite die material is obtained. According to the graphite die material for hot-press molding and the preparation method of the graphite die material, the production cost is reduced, the production efficiency is improved, energy is saved, and the environment is protected.

Description

A kind of for hot-forming graphite jig material and preparation method thereof
Technical field
The present invention relates to graphite jig field, particularly relate to a kind of for hot-forming graphite jig material and preparation method thereof.
Background technology
Graphite jig starts from phase earlier 1970s, along with geological prospecting, the probing in mine and exploitation, Coal Exploration and exploitation, oil exploration and drilling well, the cutting of highway, particularly granite and marble is exploited and the fast development of cutting industry, the diamond alloy material of hot press forming technology and the demand of Hardmetal materials is used to increase considerably, therefore the consumption of graphite jig surges therewith, and the performance difference of graphite material directly influences the quality of hot-forming superhard material.Hot-forming mode is generally divided into two kinds, resistance hot type and Frequency Induction Heating type.The technological requirement of hot-forming Superhard Drill: temperature close to 1000 DEG C, molding hot pressing at 16 ~ 18MPa, heat-insulation pressure keeping 5 ~ 20min under non-vacuum.With this understanding, consistency is high, mechanical strength is high, the porosity is little, antioxygenic property good, degree of graphitization high to need graphite mo(u)ld to have.
At present, the main raw material(s) of the making of domestic graphite jig is petroleum coke, pitch coke, natural or Delanium, Colophonium, resin etc., through broken, kneading, roll film-making, second-time breakage, the original idiosome that compressing, carbonization impregnation cycles, last graphitization are fabricated to mould, then the hot pressing type graphite jig of machined one-tenth different size size.Use traditional raw material and process conditions it is generally required to 8 ~ 10 months just can produce die blank, carbonization impregnation technology repeatedly not only expends substantial amounts of electric power, coal equal energy source, improve human cost simultaneously, more increase the weight of the burden of environment, and longer fabrication cycle has also increased uncertain risk cost.Further, current domestic substantial amounts of graphite jig, by the carbonization dipping number of times improved stress to pursue its high bulk density, high intensity and have ignored High Purity, hyperfine structure etc..And the graphite jig intensity of hyperfine structure is big, it is possible to higher pressure during opposing hot pressing, it is simple to the superhard material of molding higher performance；After the light of finished surface and the cooling of compactness good hot pressing workpiece, it is possible to be conducive to the demoulding；The graphite jig of High Purity has good non-oxidizability, the probability of the impurity being substantially reduced in mould at high temperature catalytic graphite oxidation, the excellent properties of comprehensive hyperfine structure and purification can improve the cycle-index of mould, improves hot pressing condition parameter, it is ensured that the preparation of superhard material.Therefore, study a kind of High Purity, the graphite jig material of hyperfine structure is also the most necessary.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, it is provided that a kind of for hot-forming graphite jig material and preparation method thereof.
For solving above-mentioned technical problem, the technical scheme that the present invention proposes is:
A kind of for hot-forming graphite jig material, its raw material includes that mesophase pitch carbon microspheres, Colophonium and crystalline flake graphite, the mass ratio of wherein said mesophase pitch carbon microspheres and crystalline flake graphite are (19:1) ~ (7:3)；The addition of described Colophonium accounts for the 5% ~ 20% of raw material gross mass.
Above-mentioned graphite jig material, it is preferred that the softening point temperature of described Colophonium is 200 ~ 205 DEG C, and the purity of described crystalline flake graphite is more than 99%.
As a total inventive concept, the present invention also provides for the preparation method of a kind of above-mentioned graphite jig material, comprises the following steps:
(1) Colophonium is made asphalt grout；
(2) asphalt grout mesophase pitch carbon microspheres, crystalline flake graphite and step (1) obtained, under conditions of evacuation, kneading roller roll sheet, pulverize after cooling, add in mixer batch mixing and stand；
(3) mixed material after step (2) is carried out isostatic pressing, after the demoulding, obtain green compact sample；
(4) green compact sample step (3) obtained carries out roasting carbonization process after standing；
(5) sample that step (4) roasting carbonization processes is carried out graphitization processing, i.e. obtain described graphite jig material.
Above-mentioned preparation method, preferably, the detailed process of the isostatic pressing in described step (3) is: mixed material first loads compacting evacuation in mould and processes, it is re-fed in isostatic pressing machine rising to 120～150MPa voltage stabilizings 10～15min with 7～10MPa/min rate of pressure rise, again with 15～20MPa/min pressure release speed pressure releases to 70～90MPa, voltage stabilizing 5～10min；Finally with 10～15MPa/min pressure release speed pressure releases to chamber pressure.
Above-mentioned preparation method, it is preferred that in described step (4), roasting carbonization processing procedure segmentation is carried out, and it concretely comprises the following steps: (a) is first warming up to 300～302 DEG C with the heating rate of 8～10 DEG C/h；B () is warming up to 450～452 DEG C with the heating rate of 2.9～3.1 DEG C/h again；C () is then warming up to 649～651 DEG C with the heating rate of 1.4～1.6 DEG C/h；D () is warming up to 850～852 DEG C with the heating rate of 1.9～2.1 DEG C/h again；E () is warming up to 1008～1012 DEG C with the heating rate of 2.9～3.1 DEG C/h again；F () is finally come out of the stove to 60 ~ 80 DEG C with the rate of temperature fall of 5 DEG C/h, natural cooling.Carbonization qualification rate is more than 90%.The heating curve of the roasting carbonization processing procedure of the present invention draws through repeatedly test, comprehensive analysis, is substantially reduced the phenomenon of carbonization cracking, it is ensured that conforming product rate.
Above-mentioned preparation method, it is preferred that in described step (5), graphitization uses medium acheson furnace, and burner hearth intensification is stable, heating is uniform.Graphited detailed process is: be first uniformly heating to 1550～1850 DEG C, is incubated 2～5h, then is uniformly heating to when 2680～2820 DEG C stop power transmission；Wherein in temperature-rise period, starting to be passed through chlorine when temperature reaches 2100 DEG C ~ 2150 DEG C, continue to be passed through chlorine 10～12h after stopping power-off, the speed that is passed through of chlorine is 12 ~ 15m3/h；Stopping the rate of temperature fall after power transmission is 2～6 DEG C/h.
Above-mentioned preparation method, preferably, in described step (2), the detailed process of kneading is: be placed in vacuum kneader by the mesophase pitch carbon microspheres that granularity is 7～8 microns, open wide mixing 1～2h with the temperature of 120～140 DEG C, be subsequently adding asphalt grout, evacuation kneading 1～2h, being warming up to 220 ~ 240 DEG C of vacuum kneading 1 ~ 2h again, wherein kneader forward rotational speed controls 80～120r/min.
Above-mentioned preparation method, it is preferred that in described step (2), after pulverizing, the granularity of mixed material is 9～10 microns, and the volatile matter quality of mixed material accounts for the 5wt% ~ 15wt% of mixed material quality；It is further preferred that the volatile matter quality of mixed material accounts for the 5wt% ~ 10wt% of whole mixed material quality.
Above-mentioned preparation method, it is preferred that in described step (2), the time of repose of mixed material is 3～5h；Green compact sample time of repose in described step (4) is 24～48h.
Above-mentioned preparation method, preferably, in described step (1), the concrete preparation process of asphalt grout is: mixed according to the amount that mass ratio is (4:1) ~ (3:2) with ethyl acetate by Colophonium, stirs 0.5 ~ 1h with the mixing speed of 80 ~ 120r/min.
The present invention uses MCMB to do raw material, and the most only body shrinks, and aggregate itself also produces contraction, shrinks the biggest, and density increment is the biggest, and after carbonization, compactness wants height, it is possible to reduce dipping and the number of times of roasting.After carbonization, the most graphited density can reach traditional three roasting carbonizations of twice dipping or four the most graphited density of carbonization of three dippings.
Due to the fact that the graphitization goods using MCMB to be main aggregate, owing to overall shrinkage is bigger, it is particularly easy to crack at firing stage, inventor is by research many times and raw material ratio, regulated and controled by the mobility of hard pitch slurry, in the case of the lot of experiments such as the mode of uniformity dispersion aggregate, repeatedly test the carbonization adapted and graphitization curve, the charging curve comprehensively drawn, carbonization qualification rate can ensured, finally a whole set of process conditions being suitable for preparing graphite jig original blank are found out, carbonization and graphited qualification rate are all more than 95%.
Compared with prior art, it is an advantage of the current invention that:
(1) present invention is with mesophase pitch carbon microspheres as main raw material(s), with hard pitch as binding agent, this kind of formula is used to be made without the circulation technology of carbonization-dipping, have only to through a carbonization, primary graphitizing can be obtained by three dippings of traditional material, the density of four carbonization products and intensity, and the process time can foreshorten to 3 ~ 5 months from original 8 ~ 10 months；Not only reduce production cost, improve production efficiency, also save the energy, protect environment.
(2) present invention uses ethyl acetate to disperse hard pitch first, strengthen hard pitch mobility in kneading, strengthen the ability being uniformly coated with aggregate, being heated evenly property when cementability and carbonization when improving molding, reduce the hole produced after volatile matter runs off, reduce material porosity.Simultaneously during evacuation, the ethyl acetate of more than 90% can be reclaimed by condensation, recycle, economize on resources.
(3) graphite jig of the present invention is less than 10ppm through strict purification process, ash, makes product reduce impurity own during hot press forming technology and aoxidizes the catalysis of mould itself, is greatly improved antioxygenic property.
(4) the mesophase pitch carbon microspheres using ultra-fine grain diameter of the present invention can be greatly enhanced compactness and the intensity of material as main material, body contraction and self-constriction, improve oxidation resistance, increase resistivity.
(5) preparation method of the present invention passes through rational scientific matching, reasonably roasting carbonization and graphitization curve controlled, make graphite products roasting and graphited qualification rate all more than 95%, while enhancing product performance, effectively control the graphite cost of hyperfine structure.
(6) the raw material valency that the present invention uses low is easy to get, stable in properties, and pre-treatment of raw material technique is simple to operation, substantially can complete the graphite jig of excellent performance by legacy equipment and prepare.
To sum up, instant invention overcomes tradition raw material (forging rear pitch coke and petroleum coke) in the contraction (body contractions) of roasting and graphitizing process generation bulk sample, the most only contraction of the Colophonium generation around aggregate, the defect that the shrinkage factor of aggregate is the least；The process time of the present invention can foreshorten to 3 ~ 5 months from traditional 8 ~ 10 months；Not only reduce production cost, improve production efficiency, also save the energy, protect environment.
Detailed description of the invention
For the ease of understanding the present invention, below in conjunction with preferred embodiment, the present invention is made more comprehensively, describes meticulously, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical term used hereinafter is generally understood that with those skilled in the art is identical.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to limit the scope of the invention.
Except there being special instruction, the various reagent used in the present invention, raw material are can commodity commercially or can be by the prepared product of known method.
Embodiment 1 :
A kind of present invention for hot-forming graphite jig material, its primary raw material includes that mesophase pitch carbon microspheres (hereinafter referred to as: MCMB), hard pitch (softening point temperature is 202 DEG C) and purity are the crystalline flake graphite of 99%；Wherein MCMB and crystalline flake graphite mass ratio are 19:1；The addition of hard pitch is the 20% of gross weight (hard pitch+MCMB+ crystalline flake graphite).
The preparation method for hot-forming graphite jig material of the present embodiment, comprises the following steps:
(1) 10Kg is crossed in the ethyl acetate solution that the hard pitch (softening point temperature is 202 DEG C) of 100 eye mesh screens puts into 2.5Kg, with SANYE stirring paddle uniform stirring 0.5h, speed of agitator 80r/min, prepare hard pitch slurry；
(2) by MCMB that MCMB comminution by gas stream to granularity is D50=8 micron, then 38KgMCMB and 2Kg crystalline flake graphite is put into in vacuum kneader, 120 DEG C are opened wide mixing 1h, stop heating, it is subsequently adding hard pitch slurry prepared by 12.5Kg step (1), closes cover, evacuation kneading 1h, being warming up to 240 DEG C of kneadings 1h again, kneader forward rotational speed controls at 80r/min；
(3) thickener obtained after step (2) kneading is added roll shaft pelleter while hot, by four film-makings (roll surface temperature 210 DEG C, rotating speed 30r/min), by air-cooled for the sheet stock obtained be down to room temperature after be crushed to D50=25 micron, it is subsequently placed in V-type batch mixer preliminary mixing 1h(rotating speed 100r/min) after, the material of mixing is carried out comminution by gas stream to D50=9 micron, put into the rotating speed 200r/min mixing 3h(batch mixer in V-type batch mixer again), 4h is stood after blanking, the material being uniformly mixed, now in compound, the quality of volatile matter accounts for the 11.3wt% of compound gross mass；
(4) mixed material after step (3) is slowly put in φ 166mm nitrile rubber mould, counterweight vibrations compacting, evacuation 15min, put into equal pressing equipment, first rise to 150MPa, voltage stabilizing 10min with the rate of pressure rise of 10MPa/min after glue sealing；Again with 15MPa/min pressure release speed pressure release to 90MPa, voltage stabilizing 10min；Finally with 5MPa/min pressure release speed pressure release to chamber pressure, the demoulding, after the demoulding, obtain regular column type green compact sample, be placed in room temperature environment and stand 48h；
(5) green compact sample step (4) obtained loads in stainless steel crucible, fill up the graphous graphite powder that granularity is below 0.5mm, ram-jolt, sample distance sidewall of crucible is more than 80mm, distance crucible top, more than 220mm, proceeds by roasting carbonization process: (a) is first warming up to 300 DEG C with the heating rate of 6.5 DEG C/h；B () is warming up to 400 DEG C with the heating rate of 4.5 DEG C/h again；C () is then warming up to 700 DEG C with the heating rate of 1.5 DEG C/h；D () is warming up to 850 DEG C with the heating rate of 2 DEG C/h again；E () is warming up to 1100 DEG C with the heating rate of 2.5 DEG C/h again；F () is finally cooled to room temperature with the rate of temperature fall of 5 DEG C/h, obtain carbonization sample, carbonization qualification rate more than 90%；
(6) sample after step (5) carbonization is placed in medium acheson furnace it is uniformly heating to 1850 DEG C, be incubated 5h, then be uniformly heating to 2100 DEG C, start with 15m3/h Speed be passed through chlorine, when temperature rises to 2820 DEG C, stop power transmission, chlorine continues conveying 10h, finally it is down to 90 DEG C with the rate of temperature fall of 5 DEG C/h come out of the stove, natural cooling, i.e. can get hyperfine structure, high intensity, high densification, High Purity, low-ash graphite jig original blank, and graphitization qualification rate reaches more than 98%.
The mean diameter of graphite jig material prepared by the present embodiment is 9 μm, and bulk density is 1.92g/cm3, comprcssive strength is 125.6MPa, and rupture strength is 69.8Mpa, resistivity 20.1 μ Ω m, and Shore hardness is 56, the porosity 12%, and ash 7 ppm, product qualified rate is more than 89%；Wherein, GB/T 24528-2009 touchstone bulk density is used；Compressive resistance is 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 is according to GB/T 9345.1-2008.Whole graphite jig material production cycle is 5 months.
Embodiment 2 :
A kind of present invention for hot-forming graphite jig material, its 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 is 99%)；Wherein MCMB and High Purity crystalline flake graphite mass ratio are 9:1；The addition of hard pitch is the 10% of gross weight (hard pitch+MCMB+ High Purity crystalline flake graphite).
The preparation method for hot-forming graphite jig material of the present embodiment, comprises the following steps:
(1) 10Kg is crossed in the ethyl acetate solution that the hard pitch (softening point temperature is 202 DEG C) of 100 eye mesh screens puts into 2.5Kg, with SANYE stirring paddle uniform stirring 20min, speed of agitator 100r/min, prepare hard pitch slurry；
(2) by MCMB that MCMB comminution by gas stream to granularity is D50=8 micron, then 81KgMCMB and 9Kg High Purity crystalline flake graphite is put into in vacuum kneader, 110 DEG C are opened wide mixing 1h, stop heating, it is subsequently adding hard pitch slurry prepared by 12.5Kg step (1), closes cover, evacuation kneading 1.5h, being warming up to 250 DEG C of kneadings 0.5h again, kneader forward rotational speed controls at 50r/min；
(3) thickener obtained after step (2) kneading is added roll shaft pelleter while hot, by four film-makings (roll surface temperature 230 DEG C, rotating speed 20r/min), by air-cooled for the sheet stock obtained be down to room temperature after be crushed to D50=25 micron, it is subsequently placed in V-type batch mixer preliminary mixing 2h(rotating speed 100r/min) after, the material of mixing is carried out comminution by gas stream to D50=9 micron, put into the rotating speed 200r/min mixing 3h(batch mixer in V-type batch mixer again), 4h is stood after blanking, the material being uniformly mixed, now in compound, the quality of volatile matter accounts for the 8.67wt% of compound gross mass；
(4) mixed material after step (3) is slowly put in φ 166mm nitrile rubber mould, counterweight vibrations compacting, evacuation 20min, put into equal pressing equipment, first rise to 150MPa, voltage stabilizing 8min with the rate of pressure rise of 10MPa/min after glue sealing；Again with 15MPa/min pressure release speed pressure release to 90MPa, voltage stabilizing 18min；Finally with 5MPa/min pressure release speed pressure release to chamber pressure, the demoulding, after the demoulding, obtain regular column type green compact sample, be placed in room temperature environment and stand 24h；
(5) green compact sample step (4) obtained loads in stainless steel crucible, fill up the graphous graphite powder that granularity is below 0.5mm, ram-jolt, sample distance sidewall of crucible is more than 80mm, distance crucible top, more than 220mm, proceeds by roasting carbonization process: (a) is first warming up to 300 DEG C with the heating rate of 6.5 DEG C/h；B () is warming up to 400 DEG C with the heating rate of 4.5 DEG C/h again；C () is then warming up to 700 DEG C with the heating rate of 1.5 DEG C/h；D () is warming up to 800 DEG C with the heating rate of 2 DEG C/h again；E () is warming up to 1100 DEG C with the heating rate of 2.5 DEG C/h again；(f) finally with the rate of temperature fall of 5 DEG C/h to being cooled to room temperature, obtain carbonization sample, carbonization qualification rate more than 85%；
(6) sample after step (5) carbonization is placed in medium acheson furnace it is uniformly heating to 1850 DEG C, be incubated 5h, then be uniformly heating to 2100 DEG C, start with 15m3/h Speed be passed through chlorine, when temperature rises to 2820 DEG C, stop power transmission, chlorine continues conveying 10h, finally it is down to 90 DEG C with the rate of temperature fall of 5 DEG C/h come out of the stove, natural cooling, i.e. can get hyperfine structure, high intensity, high densification, High Purity, low-ash graphite jig original blank, and graphitization qualification rate reaches more than 98%.
The mean diameter of graphite jig material prepared by the present embodiment is 9 μm, and bulk density is 1.90g/cm3, comprcssive strength is 115.6MPa, and rupture strength is 62.8MPa, resistivity 19.1 μ Ω m, and Shore hardness is 54, the porosity 14%, and ash 7 ppm, product qualified rate is more than 84%；Wherein, GB/T 24528-2009 touchstone bulk density is used；Compressive resistance is 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 is according to GB/T 9345.1-2008.Whole graphite jig material production cycle is 5 months.
Embodiment 3 :
A kind of present invention for hot-forming graphite jig material, its 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 is 99%)；Wherein MCMB and High Purity crystalline flake graphite mass ratio are 17:3；The addition of hard pitch is the 10% of gross weight (hard pitch+MCMB+ High Purity crystalline flake graphite).
The preparation method for hot-forming graphite jig material of the present embodiment, comprises the following steps:
(1) 10Kg is crossed in the ethyl acetate solution that the hard pitch (softening point temperature is 202 DEG C) of 100 eye mesh screens puts into 2.5Kg, with SANYE stirring paddle uniform stirring 15min, speed of agitator 120r/min, prepare hard pitch slurry；
(2) by MCMB that MCMB comminution by gas stream to granularity is D50=8 micron, then 76.5KgMCMB and 13.5Kg High Purity crystalline flake graphite is put into in vacuum kneader, 110 DEG C are opened wide mixing 1h, stop heating, it is subsequently adding hard pitch slurry prepared by 12.5Kg step (1), closes cover, evacuation kneading 1.5h, being warming up to 250 DEG C of kneadings 0.5h again, kneader forward rotational speed controls at 50r/min；
(3) thickener obtained after step (2) kneading is added roll shaft pelleter while hot, by four film-makings (roll surface temperature 230 DEG C, rotating speed 20r/min), by air-cooled for the sheet stock obtained be down to room temperature after be crushed to D50=25 micron, it is subsequently placed in V-type batch mixer preliminary mixing 1h(rotating speed 100r/min) after, the material of mixing is carried out comminution by gas stream to D50=9 micron, put into the rotating speed 200r/min mixing 2h(batch mixer in V-type batch mixer again), 4h is stood after blanking, the material being uniformly mixed, now in compound, the quality of volatile matter accounts for the 8.35wt% of compound gross mass；
(4) mixed material after step (3) is slowly put in φ 166mm nitrile rubber mould, counterweight vibrations compacting, evacuation 20min, put into equal pressing equipment, first rise to 150MPa, voltage stabilizing 8min with the rate of pressure rise of 10MPa/min after glue sealing；Again with 15MPa/min pressure release speed pressure release to 90MPa, voltage stabilizing 18min；Finally with 5MPa/min pressure release speed pressure release to chamber pressure, the demoulding, after the demoulding, obtain regular column type green compact sample, be placed in room temperature environment and stand 24h；
(5) green compact sample step (4) obtained loads in stainless steel crucible, fill up the graphous graphite powder that granularity is below 0.5mm, ram-jolt, sample distance sidewall of crucible is more than 80mm, distance crucible top, more than 220mm, proceeds by roasting carbonization process: (a) is first warming up to 300 DEG C with the heating rate of 6.5 DEG C/h；B () is warming up to 400 DEG C with the heating rate of 4.5 DEG C/h again；C () is then warming up to 700 DEG C with the heating rate of 1.5 DEG C/h；D () is warming up to 850 DEG C with the heating rate of 2 DEG C/h again；E () is warming up to 1100 DEG C with the heating rate of 2.5 DEG C/h again；(f) finally with the rate of temperature fall of 5 DEG C/h to being cooled to room temperature, obtain carbonization sample, carbonization qualification rate more than 88%；
(6) sample after step (5) carbonization is placed in medium acheson furnace it is uniformly heating to 1850 DEG C, be incubated 5h, then be uniformly heating to 2100 DEG C, start with 15m3/h Speed be passed through chlorine, when temperature rises to 2820 DEG C, stop power transmission, chlorine continues conveying 10h, finally it is down to 90 DEG C with the rate of temperature fall of 5 DEG C/h come out of the stove, natural cooling, i.e. can get hyperfine structure, high intensity, high densification, High Purity, low-ash graphite jig original blank, and graphitization qualification rate reaches more than 98%.
Its mean diameter of graphite jig material prepared by the present embodiment is 9 μm, and bulk density is 1.89g/cm3, comprcssive strength is 102.2MPa, and rupture strength is 60.1MPa, resistivity 18.5 μ Ω m, and Shore hardness is 55, the porosity 15%, and ash 7.5 ppm, product qualified rate is more than 84%；Wherein, GB/T 24528-2009 touchstone bulk density is used；Compressive resistance is 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 is according to GB/T 9345.1-2008.Whole graphite jig material production cycle is 5 months.

Claims (10)

1. one kind is used for hot-forming graphite jig material, it is characterized in that, the raw material of described graphite jig material includes that mesophase pitch carbon microspheres, Colophonium and crystalline flake graphite, the mass ratio of wherein said mesophase pitch carbon microspheres and crystalline flake graphite are (19:1) ~ (7:3)；The addition of described Colophonium accounts for the 5% ~ 20% of raw material gross mass.
2. graphite jig material as claimed in claim 1, it is characterised in that the softening point temperature of described Colophonium is 200 ~ 205 DEG C, and the purity of described crystalline flake graphite is more than 99%.
3. the preparation method of a graphite jig material as claimed in claim 1 or 2, it is characterised in that comprise the following steps:
(1) Colophonium is made asphalt grout；
(2) asphalt grout mesophase pitch carbon microspheres, crystalline flake graphite and step (1) obtained, under conditions of evacuation, kneading roller roll sheet, pulverize after cooling, add in mixer batch mixing and stand；
(3) mixed material after step (2) is carried out isostatic pressing, after the demoulding, obtain green compact sample；
(4) green compact sample step (3) obtained carries out roasting carbonization process after standing；
(5) sample that step (4) roasting carbonization processes is carried out graphitization, i.e. obtain described graphite jig material.
4. preparation method as claimed in claim 3, it is characterized in that, the detailed process of the isostatic pressing in described step (3) is: mixed material first loads compacting evacuation in mould and processes, it is re-fed in isostatic pressing machine rising to 120 ~ 150MPa voltage stabilizing 10～15min with 7～10MPa/min rate of pressure rise, again with 15～20MPa/min pressure release speed pressure releases to 70～90MPa, voltage stabilizing 5～10min；Finally with 10～15MPa/min pressure release speed pressure releases to chamber pressure.
5. preparation method as claimed in claim 3, it is characterised in that in described step (4), roasting carbonization processing procedure segmentation is carried out, and it concretely comprises the following steps: (a) is first warming up to 300～302 DEG C with the heating rate of 8～10 DEG C/h；B () is warming up to 450～452 DEG C with the heating rate of 2.9～3.1 DEG C/h again；C () is then warming up to 649～651 DEG C with the heating rate of 1.4～1.6 DEG C/h；D () is warming up to 850～852 DEG C with the heating rate of 1.9～2.1 DEG C/h again；E () is warming up to 1008～1012 DEG C with the heating rate of 2.9～3.1 DEG C/h again；F () is finally come out of the stove to 60 ~ 80 DEG C with the rate of temperature fall of 5 DEG C/h, natural cooling.
6. preparation method as claimed in claim 3, it is characterised in that in described step (5), graphited detailed process is: be first uniformly heating to 1550～1850 DEG C, is incubated 2～5h, then is uniformly heating to when 2680～2820 DEG C stop power transmission；Wherein in temperature-rise period, starting to be passed through chlorine when temperature reaches 2100 DEG C ~ 2150 DEG C, continue to be passed through chlorine 10～12h after stopping power-off, the speed that is passed through of chlorine is 12 ~ 15m3/h；Stopping the rate of temperature fall after power transmission is 2～6 DEG C/h.
7. the preparation method as described in any one of claim 3～6, it is characterized in that, in described step (2), the detailed process of kneading is: be placed in vacuum kneader by the mesophase pitch carbon microspheres that granularity is 7～8 microns, open wide mixing 1～2h with the temperature of 120～140 DEG C, be subsequently adding asphalt grout, evacuation kneading 1～2h, being warming up to 220 ~ 240 DEG C of vacuum kneading 1 ~ 2h again, wherein kneader forward rotational speed controls 80～120r/min.
8. the preparation method as described in any one of claim 3～6, it is characterised in that in described step (2), after pulverizing, the granularity of mixed material is 9～10 microns, and the volatile matter quality of mixed material accounts for the 5wt% ~ 15wt% of mixed material quality.
9. the preparation method as described in any one of claim 3～6, it is characterised in that the mixed material time of repose in described step (2) is 3～5h；Green compact sample time of repose in described step (4) is 24～48h.
10. the preparation method as described in any one of claim 3～6, it is characterized in that, in described step (1), the concrete preparation process of asphalt grout is: mixed according to the amount that mass ratio is (4:1) ~ (3:2) with ethyl acetate by Colophonium, stirs 0.5 ~ 1h with the mixing speed of 80 ~ 120r/min.
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CN112321300A (en) * 2020-10-19 2021-02-05 湖南长宇科技发展有限公司 High-thermal-conductivity low-porosity graphite for curved glass hot bending die and preparation method thereof
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
CN112457015A (en) * 2020-12-21 2021-03-09 柯良节 Novel graphite radiator and preparation method thereof
CN113213937A (en) * 2021-04-29 2021-08-06 杨斌 Preparation process of one-step formed ultrahigh-purity isostatic pressing graphite material
CN114314580A (en) * 2021-12-30 2022-04-12 宁波杉杉新材料科技有限公司 Composite graphite negative electrode material and preparation method and application thereof

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CN112457015A (en) * 2020-12-21 2021-03-09 柯良节 Novel graphite radiator and preparation method thereof
CN113213937A (en) * 2021-04-29 2021-08-06 杨斌 Preparation process of one-step formed ultrahigh-purity isostatic pressing graphite material
CN114314580A (en) * 2021-12-30 2022-04-12 宁波杉杉新材料科技有限公司 Composite graphite negative electrode material and preparation method and application thereof

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