CN101708838B - Highly oriented graphite material of nature flake graphite base and preparation method thereof - Google Patents

Highly oriented graphite material of nature flake graphite base and preparation method thereof Download PDF

Info

Publication number
CN101708838B
CN101708838B CN2009102729091A CN200910272909A CN101708838B CN 101708838 B CN101708838 B CN 101708838B CN 2009102729091 A CN2009102729091 A CN 2009102729091A CN 200910272909 A CN200910272909 A CN 200910272909A CN 101708838 B CN101708838 B CN 101708838B
Authority
CN
China
Prior art keywords
graphite material
flake graphite
nature
graphite
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN2009102729091A
Other languages
Chinese (zh)
Other versions
CN101708838A (en
Inventor
李轩科
袁观明
董志军
邓念
丛野
杨忠华
吴晓琴
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan University of Science and Engineering WUSE
Original Assignee
Wuhan University of Science and Engineering WUSE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan University of Science and Engineering WUSE filed Critical Wuhan University of Science and Engineering WUSE
Priority to CN2009102729091A priority Critical patent/CN101708838B/en
Publication of CN101708838A publication Critical patent/CN101708838A/en
Application granted granted Critical
Publication of CN101708838B publication Critical patent/CN101708838B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention particularly relates to a highly oriented graphite material of a nature flake graphite base and a preparation method thereof. The technical scheme is as follows: mixing and grinding 60-90wt% of nature flake graphite, 5-30wt% of agglomerant, and 1-25wt% of solvent; drying for 0.5-12h in an atmosphere furnace under the condition of 50-450 DEG C; carrying out hot-press forming in a mould; finally carbonizing at the temperature of 1000-1500 EDG C and graphitizing at the temperature of 2600-3000 DEG C to obtain the highly oriented graphite material. The highly oriented graphite material of the invention has wide source of raw materials, low price, simple preparation process, good repetitiveness and short production circle; the prepared graphite material has high uniform alignment of graphite crystal, thus further improving the heat conductivity of the graphite material; the heat conductivity after carbonization and graphitization can reach 320-750W/m.K, the volume density is respectively 1.9-2.0g/cm<3> and 2.0-2.1g/cm<3>, and the resistivity reaches 1.0 mu omega. m.

Description

Highly oriented graphite material of nature flake graphite base and preparation method thereof
Technical field
The invention belongs to the technical field of high oriented graphite material.Relate in particular to a kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.
Background technology
Developing rapidly of present many cutting edge technologies (as unicircuit, Electronic Packaging etc.), the raising of increase gradually, storage density and the travelling speed of number of electronic components and capacity all need the heat that operation produces to device to conduct in a certain direction or dissipation in time.For example, along with the miniaturization of computer and the quickening of arithmetic speed, especially notebook computer miniaturization requires to arrange more and the more and more higher miniaturized components of energy density in littler space, therefore how to allow the heat of device interior come out as early as possible, it is more and more important to become.And the key of heat radiation is how heat slewing to be derived from thermal source, i.e. the heat management of electron device.If heat management is insufficient, will cause the aging in advance or heat cracking of the hot physical damage of accelerated electron element and generation connecting portion of semiconductor element.Performance and serviceability for holding device, exploitation with high thermal conductivity, low thermal coefficient of expansion and low-density high-performance thermally conductive material seem particularly important and urgent (DTI Global WatchMission Report " Developments and trends in thermal management technologies-a mission to theUSA ", 2006.).Graphite material compare with traditional metal heat-conducting material have lower density, high thermal and lower thermal expansivity.
Traditional metal (as aluminium, copper etc.) heat sink material makes limitation such as its thermal conductivity declines to a great extent because autologous density is big, thermal expansivity is higher, material is impure, has been difficult to satisfy radiating requirements.Opposite heat tube reason material, most important performance requriements is that material has high thermal.Present many scientists have recognized that the property of utilizing graphite material can produce the material with some higher thermal conductivity performance.High-heat conductivity graphite material refers to have the graphite and the matrix material thereof of high heat conductance, be a class heat sink material of tool development prospect in recent years, have broad application prospects in the energy, computing technique, communication, electronics, laser and fields such as space science, energy-saving and emission-reduction.The normal temperature thermal conductivity of general graphite material only is (Qiu Haipeng about 70~150W/mK, Liu Lang. high heat conduction charcoal base functional materials. novel charcoal material, 2002,17,4), and the theoretical thermal conductivity of graphite (002) aspect up to 2100W/mK (J.C.Bokros.Chemistry and physics of carbon[M], Marcel Dekker Inc.NewYork, Vol.5,1969), its specific heat conductance ratio of material volume density (thermal conductivity with) is traditional metal materials copper, silver and aluminium 5~12 times.
Existing both at home and abroad at present many report and patents about high-heat conductivity graphite material.Traditional preparation method is normally with raw material crushing, calcining, pulverizing, screening, adding additives kneading and compacting again, impregnation-calcination repeatedly repeatedly then, last graphitization processing.The easy graphited pitch of the most employings of nearest improved method is binding agent (as coal-tar pitch, mesophase pitch etc.), with refinery coke (Liu Lang, Qiu Haipeng, Song Yongzhong, Shi Jingli. a kind of preparation method of high-heat conductivity graphite material. China, 01130544.4[P], 2003.06.04) or mesophase pitch Jiao (Liu Lang, Gao Xiaoqing, Guo Quangui, Shi Jingli. a kind of preparation method of high-heat conductivity graphite material. Chinese 200410012433.5[P], 2005.03.23) be mixed, (20~40MPa) processing obtain high conductive graphite goods in high temperature (2600~3000 ℃) hot pressing down again.But aforesaid method still more or less exist the production cycle long, cost is higher, preparation technology is to weak points such as equipment requirements harshnesses.
Summary of the invention
The present invention is intended to overcome the prior art deficiency, purpose provides that a kind of raw material sources are extensive, technology is simple, the preparation method of good reproducibility, highly oriented graphite material of nature flake graphite base with short production cycle, and the material for preparing with this method has high heat conduction characteristics.
For achieving the above object, the technical solution used in the present invention is: the natural flake graphite of 60~90wt%, the binding agent of 5~30wt% and the solvent of 1~25wt% are carried out mix grinding; In atmosphere furnace under 50~450 ℃ of conditions dry 0.5~12 hour again; Hot-forming in mould then, carry out 1000~1500 ℃ of charings at last and 2600~3000 ℃ of greyings promptly get high oriented graphite material.
In the technical program: natural flake graphite be particle diameter be 175~365 μ m, 365~495 μ m, 495~701 μ m, greater than more than one the natural flake graphite in four kinds of particle diameters of 701 μ m; Binding agent is more than one in mesophase pitch, coal-tar pitch, modified coal asphalt, the resol; Solvent is a kind of in water, dehydrated alcohol, methylene dichloride, ether, tetrahydrofuran (THF), Virahol, the normal hexane; Mix grinding is to carry out in mixing machine or ball mill, and mix grinding speed is 50~500 rev/mins, and the mix grinding time is 1~24 hour; Hot-formingly be: 300~800 ℃ of hot pressing temperatures, 0.1~30 ℃/minute of temperature rise rate, hot pressing pressure 5~40MPa, 1~20 hour heat-insulation pressure keeping time.
Because adopt technique scheme, the present invention is raw material with the natural flake graphite, low price, wide material sources; Preparation technology is simple, good reproducibility, with short production cycle; The prepared graphite material of the present invention can make the height-oriented arrangement of graphite crystal, thereby its thermal conductivity is further improved, and thermal conductivity can reach 320~750W/mK after charing and the greying, and volume density is respectively 1.9~2.0g/cm 3With 2.0~2.1g/cm 3, resistivity reaches 1 μ Ω .m.
Description of drawings
Fig. 1 is the texture synoptic diagram of the prepared a kind of high oriented graphite material of the present invention;
Fig. 2 is the x-ray diffraction pattern of A face among Fig. 1;
Fig. 3 is the x-ray diffraction pattern of B face among Fig. 1;
Fig. 4 is the x-ray diffraction pattern of C face among Fig. 1;
Fig. 5 is the low power SEM photo of C face among Fig. 1;
Fig. 6 is the high power SEM photo of C face among Fig. 1.
Embodiment
Below in conjunction with embodiment the present invention being further described, is not the restriction to its protection domain.
Embodiment 1
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 60~65wt%, the binding agent of 5~20wt% and the water of 15~25wt% are carried out mix grinding; In atmosphere furnace under 50~150 ℃ of conditions dry 0.5~10 hour again; Hot-forming in mould then, carry out 1000~1100 ℃ of charings at last and 2600~2700 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 175~365 μ m; Binding agent is a mesophase pitch; Mix grinding is to carry out in mixing machine, and mix grinding speed is 50~100 rev/mins, and the mix grinding time is 1~12 hour; Hot-formingly be: 300~350 ℃ of hot pressing temperatures, 0.1~5 ℃/minute of temperature rise rate, hot pressing pressure 5~8MPa, 1~6 hour heat-insulation pressure keeping time.
Embodiment 2
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 62~68wt%, the binding agent of 10~20wt% and the water of 12~25wt% are carried out mix grinding; In atmosphere furnace under 80~150 ℃ of conditions dry 5~10 hours again; Hot-forming in mould then, carry out 1050~1200 ℃ of charings at last and 2600~2800 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 365~495 μ m; Binding agent is a coal-tar pitch; Mix grinding is to carry out in ball mill, and mix grinding speed is 80~150 rev/mins, and the mix grinding time is 5~12 hours; Hot-formingly be: 330~450 ℃ of hot pressing temperatures, 1~10 ℃/minute of temperature rise rate, hot pressing pressure 6~10MPa, 3~8 hours heat-insulation pressure keeping time.
Embodiment 3
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 65~70wt%, the binding agent of 20~25wt% and the dehydrated alcohol of 5~15wt% are carried out mix grinding; In atmosphere furnace under 150~200 ℃ of conditions dry 1~5 hour again; Hot-forming in mould then, carry out 1300~1400 ℃ of charings at last and 2700~2900 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 495~701 μ m; Binding agent is a modified coal asphalt; Mix grinding is to carry out in ball mill, and mix grinding speed is 50~100 rev/mins, and the mix grinding time is 10~15 hours; Hot-formingly be: 400~550 ℃ of hot pressing temperatures, 10~15 ℃/minute of temperature rise rates, hot pressing pressure 10~20MPa, 5~16 hours heat-insulation pressure keeping time.
Embodiment 4
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 70~75wt%, the binding agent of 18~24wt% and the dehydrated alcohol of 1~12wt% are carried out mix grinding; In atmosphere furnace under 50~120 ℃ of conditions dry 2~8 hours again; Hot-forming in mould then, carry out 1200~1300 ℃ of charings at last and 2800~3000 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is greater than 701 μ m; Binding agent is a resol; Mix grinding is to carry out in mixing machine, and mix grinding speed is 300~500 rev/mins, and the mix grinding time is 12~20 hours; Hot-formingly be: 500~700 ℃ of hot pressing temperatures, 12~25 ℃/minute of temperature rise rates, hot pressing pressure 5~6MPa, 12~20 hours heat-insulation pressure keeping time.
Embodiment 5
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 72~80wt%, the binding agent of 10~15wt% and the methylene dichloride of 5~18wt% are carried out mix grinding; In atmosphere furnace under 60~200 ℃ of conditions dry 3~9 hours again; Hot-forming in mould then, carry out 1000~1200 ℃ of charings at last and 2750~2800 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 175~365 μ m and mixes by 1: 1 greater than two kinds of 701 μ m; Binding agent is that mesophase pitch and coal-tar pitch mixed by 1: 1; Mix grinding is to carry out in ball mill, and mix grinding speed is 250~500 rev/mins, and the mix grinding time is 10~24 hours; Hot-formingly be: 600~800 ℃ of hot pressing temperatures, 20~30 ℃/minute of temperature rise rates, hot pressing pressure 5~25MPa, 1~5 hour heat-insulation pressure keeping time.
Embodiment 6
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 75~85wt%, the binding agent of 8~12wt% and the methylene dichloride of 3~15wt% are carried out mix grinding; In atmosphere furnace under 150~250 ℃ of conditions dry 1~6 hour again; Hot-forming in mould then, carry out 1100~1400 ℃ of charings at last and 2700~2800 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 175~365 μ m and 365~495 μ m two kinds and mixed by 1: 1; Binding agent is that mesophase pitch closes modified coal asphalt by mixing in 1: 1; Mix grinding is to carry out in mixing machine, and mix grinding speed is 150~200 rev/mins, and the mix grinding time is 8~17 hours; Hot-formingly be: 400~450 ℃ of hot pressing temperatures, 0.1~0.5 ℃/minute of temperature rise rate, hot pressing pressure 30~40MPa, 1~6 hour heat-insulation pressure keeping time.
Embodiment 7
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 80~90wt%, the binding agent of 5~10wt% and the Virahol of 5~12wt% are carried out mix grinding; In atmosphere furnace under 70~200 ℃ of conditions dry 1~4 hour again; Hot-forming in mould then, carry out 1300~1500 ℃ of charings at last and 2600~2800 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 175~365 μ m and 495~701 μ m two kinds and mixed by 1: 1; Binding agent is that mesophase pitch and resol mixed by 1: 1; Mix grinding is to carry out in ball mill, and mix grinding speed is 250~400 rev/mins, and the mix grinding time is 20~24 hours; Hot-formingly be: 500~550 ℃ of hot pressing temperatures, 2~18 ℃/minute of temperature rise rates, hot pressing pressure 15~18MPa, 1~10 hour heat-insulation pressure keeping time.
Embodiment 8
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 60~65wt%, the binding agent of 20~30wt% and the Virahol of 5~20wt% are carried out mix grinding; In atmosphere furnace under 100~180 ℃ of conditions dry 4~10 hours again; Hot-forming in mould then, carry out 1250~1450 ℃ of charings at last and 2750~2950 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 365~495 μ m and 495~701 μ m two kinds and mixed by 1: 1; Binding agent is that coal-tar pitch and resol mixed by 1: 1; Mix grinding is to carry out in mixing machine, and mix grinding speed is 350~500 rev/mins, and the mix grinding time is 16~22 hours; Hot-formingly be: 350~550 ℃ of hot pressing temperatures, 20~25 ℃/minute of temperature rise rates, hot pressing pressure 5~8MPa, 1~6 hour heat-insulation pressure keeping time.
Embodiment 9
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 62~68wt%, the binding agent of 15~30wt% and the normal hexane of 2~20wt% are carried out mix grinding; In atmosphere furnace under 90~190 ℃ of conditions dry 5~8 hours again; Hot-forming in mould then, carry out 1200~1500 ℃ of charings at last and 2600~2900 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 365~495 μ m and mixes by 1: 1 greater than two kinds of 701 μ m; Binding agent is that modified coal asphalt and resol mixed by 1: 1; Mix grinding is to carry out in mixing machine, and mix grinding speed is 280~400 rev/mins, and the mix grinding time is 16~24 hours; Hot-formingly be: 400~450 ℃ of hot pressing temperatures, 0.1~5 ℃/minute of temperature rise rate, hot pressing pressure 35~38MPa, 15~18 hours heat-insulation pressure keeping time.
Embodiment 10
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 65~70wt%, the binding agent of 10~28wt% and the normal hexane of 2~25wt% are carried out mix grinding; In atmosphere furnace under 130~450 ℃ of conditions dry 10~12 hours again; Hot-forming in mould then, carry out 1350~1450 ℃ of charings at last and 2650~2850 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 495~701 μ m and mixes by 1: 1 greater than two kinds of 701 μ m; Binding agent is that coal-tar pitch and modified coal asphalt mixed by 1: 1; Mix grinding is to carry out in ball mill, and mix grinding speed is 330~450 rev/mins, and the mix grinding time is 10~22 hours; Hot-formingly be: 400~600 ℃ of hot pressing temperatures, 140~20 ℃/minute of temperature rise rates, hot pressing pressure 15~25MPa, 6~16 hours heat-insulation pressure keeping time.
Embodiment 11
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 70~75wt%, the binding agent of 15~22wt% and the tetrahydrofuran (THF) of 3~15wt% are carried out mix grinding; In atmosphere furnace under 50~350 ℃ of conditions dry 3~12 hours again; Hot-forming in mould then, carry out 1300~1500 ℃ of charings at last and 2800~3000 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 175~365 μ m, 365~495 μ m and 495~701 μ m three kinds and mixed by 1: 1: 1; Binding agent is that mesophase pitch, coal-tar pitch and modified coal asphalt mixed by 1: 1: 1; Mix grinding is to carry out in mixing machine, and mix grinding speed is 50~200 rev/mins, and the mix grinding time is 5~12 hours; Hot-formingly be: 500~750 ℃ of hot pressing temperatures, 3~15 ℃/minute of temperature rise rates, hot pressing pressure 20~35MPa, 8~16 hours heat-insulation pressure keeping time.
Embodiment 12
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 72~80wt%, the binding agent of 5~16wt% and the tetrahydrofuran (THF) of 4~20wt% are carried out mix grinding; In atmosphere furnace under 65~185 ℃ of conditions dry 8~12 hours again; Hot-forming in mould then, carry out 1200~1400 ℃ of charings at last and 2600~2800 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 175~365 μ m, 365~495 μ m and mixes by 1: 1: 1 greater than three kinds of 701 μ m; Binding agent is that mesophase pitch, coal-tar pitch and resol mixed by 1: 1: 1; Mix grinding is to carry out in ball mill, and mix grinding speed is 150~280 rev/mins, and the mix grinding time is 11~22 hours; Hot-formingly be: 550~650 ℃ of hot pressing temperatures, 15~20 ℃/minute of temperature rise rates, hot pressing pressure 10~16MPa, 5~8 hours heat-insulation pressure keeping time.
Embodiment 13
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 75~85wt%, the binding agent of 3~14wt% and the ether of 1~20wt% are carried out mix grinding; In atmosphere furnace under 100~130 ℃ of conditions dry 6~10 hours again; Hot-forming in mould then, carry out 1080~1150 ℃ of charings at last and 2600~2900 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 175~365 μ m, 495~701 μ m and mixes by 1: 1: 1 greater than three kinds of 701 μ m; Binding agent is that mesophase pitch, modified coal asphalt and resol mixed by 1: 1: 1; Mix grinding is to carry out in mixing machine, and mix grinding speed is 450~500 rev/mins, and the mix grinding time is 2~24 hours; Hot-formingly be: 400~650 ℃ of hot pressing temperatures, 0.5~15 ℃/minute of temperature rise rate, hot pressing pressure 12~25MPa, 2~5 hours heat-insulation pressure keeping time.
Embodiment 14
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 80~90wt%, the binding agent of 5~8wt% and the ether of 2~12wt% are carried out mix grinding; In atmosphere furnace under 90~160 ℃ of conditions dry 8~12 hours again; Hot-forming in mould then, carry out 1250~1460 ℃ of charings at last and 2600~2700 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite is that particle diameter is 365~495 μ m, 495~701 μ m and mixes by 1: 1: 1 greater than three kinds of 701 μ m; Binding agent is that coal-tar pitch, modified coal asphalt and resol mixed by 1: 1: 1; Mix grinding is to carry out in ball mill, and mix grinding speed is 320~480 rev/mins, and the mix grinding time is 8~20 hours; Hot-formingly be: 400~500 ℃ of hot pressing temperatures, 8~15 ℃/minute of temperature rise rates, hot pressing pressure 5~8MPa, 1~6 hour heat-insulation pressure keeping time.
Embodiment 15
A kind of highly oriented graphite material of nature flake graphite base and preparation method thereof.The natural flake graphite of 65~85wt%, the binding agent of 5~12wt% and the normal hexane of 3~25wt% are carried out mix grinding; In atmosphere furnace under 70~200 ℃ of conditions dry 4~12 hours again; Hot-forming in mould then, carry out 1400~1500 ℃ of charings at last and 2700~2800 ℃ of greyings promptly get high oriented graphite material.
In the present embodiment: natural flake graphite be particle diameter be 175~365 μ m, 365~495 μ m, 495~701 μ m and greater than four kinds of 701 μ m by 1: 1: 1: 1 mixes; Binding agent be mesophase pitch, coal-tar pitch, modified coal asphalt and resol by 1: 1: 1: 1 mixes; Mix grinding is to carry out in mixing machine, and mix grinding speed is 150~500 rev/mins, and the mix grinding time is 14~18 hours; Hot-formingly be: 600~800 ℃ of hot pressing temperatures, 16~25 ℃/minute of temperature rise rates, hot pressing pressure 15~35MPa, 5~15 hours heat-insulation pressure keeping time.
This embodiment is raw material with the natural flake graphite, low price, wide material sources; Preparation technology is simple, good reproducibility, with short production cycle.Prepared graphite material can make the height-oriented as shown in drawings arrangement of graphite crystal: Fig. 1, and (the A face is for along graphite crystal (002) face for the texture synoptic diagram of a kind of high oriented graphite material in this embodiment; B face and A face are 45; The C face is vertical graphite crystal (a 002) face); On x-ray diffractometer (CuK α) and scanning electronic microscope, its crystalline orientation, microtexture are tested respectively then.The result be the A face x-ray diffraction pattern as shown in Figure 2, have only the weak peak in the strong peak of graphite crystal (002) and (004); The x-ray diffraction pattern of B face the diffraction peak of other crystal face of graphite occurred as shown in Figure 3; The x-ray diffraction pattern of C face as shown in Figure 4, graphite crystal (002) peak intensity very weak (Fig. 4) is about 1/400 of A face and B face, this shows the natural flake graphite preferred orientation.Fig. 5 and Fig. 6 are the low power and the high power SEM photo of C face among Fig. 1, from figure further as can be seen the graphite synusia be arranged with preface, and high orientation.
With laser conductometer the finished product of embodiment 1~15 are tested, the thermal conductivity after charing and the greying can reach 320~750W/mK, and volume density is respectively 1.9~2.0g/cm 3With 2.0~2.1g/cm 3, resistivity reaches 1 μ Ω .m.

Claims (5)

1. the preparation method of a highly oriented graphite material of nature flake graphite base is characterized in that the natural flake graphite of 60~90wt%, the binding agent of 5~30wt% and the solvent of 1~25wt% are carried out mix grinding; In atmosphere furnace under 50~450 ℃ of conditions dry 0.5~12 hour again; Hot-forming in mould then, carry out 1000~1500 ℃ of charings at last and 2600~3000 ℃ of greyings promptly get high oriented graphite material;
Described mix grinding is to carry out in mixing machine or ball mill, and mix grinding speed is 50~500 rev/mins, and the mix grinding time is 1~24 hour;
Describedly hot-formingly be: 300~800 ℃ of hot pressing temperatures, 0.1~30 ℃/minute of temperature rise rate, hot pressing pressure 5~40MPa, 1~20 hour heat-insulation pressure keeping time.
2. the preparation method of highly oriented graphite material of nature flake graphite base according to claim 1, it is characterized in that described natural flake graphite be particle diameter be 175~365 μ m, 365~495 μ m, 495~701 μ m, greater than more than one the natural flake graphite in four kinds of particle diameters of 701 μ m.
3. the preparation method of highly oriented graphite material of nature flake graphite base according to claim 1 is characterized in that described binding agent is more than one in mesophase pitch, coal-tar pitch, modified coal asphalt, the resol.
4. the preparation method of highly oriented graphite material of nature flake graphite base according to claim 1 is characterized in that described solvent is a kind of in water, dehydrated alcohol, methylene dichloride, ether, tetrahydrofuran (THF), Virahol, the normal hexane.
5. according to the prepared high oriented graphite material of natural graphite base of preparation method of each described highly oriented graphite material of nature flake graphite base in the claim 1~4.
CN2009102729091A 2009-11-24 2009-11-24 Highly oriented graphite material of nature flake graphite base and preparation method thereof Expired - Fee Related CN101708838B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2009102729091A CN101708838B (en) 2009-11-24 2009-11-24 Highly oriented graphite material of nature flake graphite base and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2009102729091A CN101708838B (en) 2009-11-24 2009-11-24 Highly oriented graphite material of nature flake graphite base and preparation method thereof

Publications (2)

Publication Number Publication Date
CN101708838A CN101708838A (en) 2010-05-19
CN101708838B true CN101708838B (en) 2011-09-07

Family

ID=42401648

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2009102729091A Expired - Fee Related CN101708838B (en) 2009-11-24 2009-11-24 Highly oriented graphite material of nature flake graphite base and preparation method thereof

Country Status (1)

Country Link
CN (1) CN101708838B (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101798221B (en) * 2010-03-09 2012-10-10 武汉科技大学 Fine texture graphite material and preparation method thereof
CN102658226A (en) * 2012-05-08 2012-09-12 宜宾天原集团股份有限公司 Feeding method for coal briquette or formed coke production by using asphalt as adhesive
CN103450857A (en) * 2013-09-05 2013-12-18 中国科学院青岛生物能源与过程研究所 Composite graphite heat-conducting membrane material with controllable heat conductivity and preparation process thereof
CN105399083B (en) * 2015-11-19 2018-07-10 江西宁新新材料股份有限公司 Aluminum-graphite composite preparation process
CN106396681A (en) * 2016-10-08 2017-02-15 天津工业大学 Method for manufacturing graphite materials with high thermal conductivity
CN115141608A (en) * 2021-03-31 2022-10-04 国家能源投资集团有限责任公司 High-thermal-conductivity heat storage material, preparation method and application thereof, composition for preparing high-thermal-conductivity heat storage material and application thereof
CN113387703B (en) * 2021-04-06 2023-09-15 航天科工(长沙)新材料研究院有限公司 Directional graphite material and preparation method thereof
CN116803950A (en) * 2023-06-27 2023-09-26 陕西美兰德炭素有限责任公司 Preparation method and application of molded graphite sagger

Also Published As

Publication number Publication date
CN101708838A (en) 2010-05-19

Similar Documents

Publication Publication Date Title
CN101708838B (en) Highly oriented graphite material of nature flake graphite base and preparation method thereof
CN104591131B (en) A kind of graphene strengthens the preparation method of high heat conducting foam carbon
CN102060287B (en) Production method of low density foam carbon heat insulating material for inert atmosphere furnace
CN105884357B (en) It is a kind of for hot-forming graphite jig material and preparation method thereof
CN102219536B (en) B4C/SiC whisker/SiC multiphase ceramic matrix composite and preparation method thereof
CN102534331B (en) Method for preparing high conductivity diamond/aluminum composite material
CN105541328A (en) Graphene oxide based method for preparing highly oriented pyrolytic graphite film
CN103467000B (en) Compound thermal insulation material manufactured by using waste fibers and manufacturing method thereof
CN108584942A (en) A kind of preparation method of grapheme foam carbon composite
CN103171207A (en) Heat sink material and preparation method thereof
CN108893636A (en) A kind of preparation method of high thermal conductivity isotropic graphite ball reinforced aluminum matrix composites
CN105859291B (en) The preparation method of three-dimensional highly-conductive hot carbon based composites
CN103641484A (en) Method for preparing Si3N4/SiC composite ceramic powder from biomass power plant ash
CN103979930B (en) A kind of high-heat conductivity graphite material and its preparation method and application
CN102745994B (en) Silicon carbide-carbon composite material and preparation method thereof
CN106744835A (en) A kind of method that utilization maize straw prepares Graphene
Zhong et al. Binding natural graphite with mesophase pitch: A promising route to future carbon blocks
CN102897753B (en) Preparation method for graphite with high thermal conductivity
Fang et al. Improving the self-sintering of mesocarbon-microbeads for the manufacture of high performance graphite-parts
Zhao et al. Transformation of waste crystalline silicon into submicro β-SiC by multimode microwave sintering with low carbon emissions
CN101724907B (en) Method for preparing single-phase nano crystalline Mn3(Cu0.5Ge0.5)N negative thermal expansion bulk material
CN104446587B (en) There is along plane and thickness direction the preparation method of high thermal conductivity coefficient C-base composte material simultaneously
CN101619426A (en) Preparation method of carbon nanotube reinforced copper-based composite material
CN110668820A (en) Preparation method of high-performance carbon graphite product with superfine structure
CN108796258A (en) A kind of preparation method of high heat conduction isotropic graphite ball enhancing Cu-base composites

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20110907

Termination date: 20111124