CN108793152A - A kind of preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance - Google Patents
A kind of preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance Download PDFInfo
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- CN108793152A CN108793152A CN201810717399.3A CN201810717399A CN108793152A CN 108793152 A CN108793152 A CN 108793152A CN 201810717399 A CN201810717399 A CN 201810717399A CN 108793152 A CN108793152 A CN 108793152A
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Abstract
The present invention relates to pyrolyzed carbon materials field, specially a kind of preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance.This approach includes the following steps：(1) preparation of pyrolytic graphite：Using chemical vapor deposition method, using intermediate frequency furnace by controlling temperature, gas flow and reaction time etc., deposited pyrolyzing graphite material is prepared on graphite matrix；(2) the high temperature and pressure heat treatment of pyrolytic graphite：The deposited pyrolyzing graphite material being prepared is processed into required size, it is placed in the smooth graphite jig in surface, after high temperature and pressure is heat-treated, the annealed state pyrolytic graphite with super-high heat-conductive performance is obtained, annealed state pyrolytic graphite prepared by the method reaches 1600W/ (mk) or more in the directions ab thermal conductivity.
Description
Technical field
The present invention relates to pyrolyzed carbon materials field, specially a kind of annealed state pyrolytic graphite with super-high heat-conductive performance
Preparation method.
Background technology
With the fast development of China's aeronautical and space technology, the component integrated level of electronic equipment is higher and higher, heat consumption
And the increase of heat flow density also at double, while lightweight to material is it is also proposed that harsh requirement, the gold such as traditional aluminium, copper, silver
The heat conductivility and high density for belonging to material can no longer meet its demand.Compared with metal material, high-heat conductivity graphite material has
The features such as light weight, thermal coefficient is big, can not only meet the heat-conductive characteristic of device as heat sink material, while can be effective
The weight for mitigating device is most a kind of heat sink material of development potentiality in recent years.
Annealed state pyrolytic graphite (APG, Annealed Pyrolytic Graphite) with super-high heat-conductive performance is heat
Graphite (PG, Pyrolytic Graphite) is solved under pressure through a kind of new material obtained from high-temperature heat treatment, is somebody's turn to do
Material has the anisotropy of height, reaches 1600W/ (mk) or more in thermal conductivities of the ab into level, is the four of metallic copper
Times or more, and its density is only a quarter of copper or so (< 2.3g/cm3).The states such as the seventies in last century is beautiful, adds, which just carry out, moves back
The material and its composite material are successfully applied to the systems such as Aeronautics and Astronautics by the development work of fiery state pyrolytic graphite, the eighties
In, the U.S. has prepared the APG materials that thermal conductivity is more than 1700W/ (mk) at present.
And also there are much reports and patent about high-heat conductivity graphite material in the country, such as：Chinese patent (publication number
CN103011141A), carbonized under protective atmosphere using such as Kapton, and through (2500~3000 DEG C) processing of graphitization
Obtained from high heat conduction graphite film, thermal conductivity also can reach 1600W/ (mk), but its thickness only have 0.0125mm~
0.075mm, increasing thickness thermal conductivity can be remarkably decreased, and limit its application in Aeronautics and Astronautics field.
Invention content
The object of the present invention is to provide a kind of preparation methods of the annealed state pyrolytic graphite with super-high heat-conductive performance, to open up
Application of the wide high-heat conductivity graphite material in Aeronautics and Astronautics field as cooling fin.
The technical scheme is that：
A kind of preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance, includes the following steps：
(1) preparation of pyrolytic graphite：
It using chemical vapor deposition method, is placed in induction furnace using graphite as depositing base, opening vacuum pump will feel
It answers furnace air to be discharged, when vacuum degree reaches 300Pa or less in induction furnace, is powered and heats up to induction furnace；When temperature reaches setting
Depositing temperature when, be proportionally passed through carrier gas and reaction gas simultaneously, the reaction time is 5 minutes~40 hours, is prepared
Deposited pyrolyzing graphite material；
(2) the high temperature and pressure heat treatment of pyrolytic graphite：
The deposited pyrolyzing graphite material being prepared is processed into required size, is placed on the smooth graphite mo(u)ld in surface
In tool, be heat-treated under conditions of applying pressure and vacuum or protective atmosphere, apply the pressure that pressure generates be 0.5~
10MPa is heat-treated 0.5~20 hour at 2800~3100 DEG C of predetermined temperature, then cools to room temperature with the furnace, obtains having super
The annealed state pyrolyzing graphite material of high thermal conductivity.
The preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance, carrier gas be nitrogen or argon gas, instead
It is hydrocarbon gas to answer gas.
The preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance, hydrocarbon gas account for carrier gas and reaction
The 20%~40% of total gas flow rate, remaining is carrier gas.
The preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance, depositing temperature be 1700 DEG C~
2100℃。
The present invention design philosophy be：
The present invention prepares pyrolyzing graphite material using chemical vapor deposition method first using intermediate frequency furnace, because of pyrolysis
The thermal conductivity of graphite only has 350~400W/ (mk), cannot be satisfied the cooling requirements of Aeronautics and Astronautics electronic component.Graphite
The anharmonic vibration that the high thermal conductivity of material relies primarily on lattice transmits heat, and crystallite dimension is bigger, and the heat transmitted is more.
Based on this present invention pyrolytic graphite is subjected to high temperature and pressure heat treatment in graphitizing furnace, the crystallite dimension of pyrolytic graphite is made to increase
Greatly, lamellar structure tends to be more complete, prepares the annealed state pyrolyzing graphite material with super-high heat-conductive performance.
It advantages of the present invention and has the beneficial effect that：
1, the present invention provides a kind of preparation method of super-high heat-conductive annealed state pyrolytic graphite, includes the following steps：(1) it is pyrolyzed
The preparation of graphite：Using chemical vapor deposition method, using intermediate frequency furnace by controlling temperature, gas flow and reaction time
Deng preparing pyrolytic graphite on graphite matrix；(2) the high temperature and pressure heat treatment of pyrolytic graphite：It is thermally treated resulting in by high temperature and pressure
Annealed state pyrolytic graphite with super-high heat-conductive performance.It is thus possible to which preparing the annealed state that thickness is 0.5mm~20mm is pyrolyzed stone
Ink material.
2, the lamellar structure of annealed state pyrolytic graphite of the present invention is more complete, have extraordinary heat conductivility, ab to
Thermal conductivity in face can reach 1600W/ (mk) or more.
Description of the drawings：
Fig. 1 pyrolytic graphite precipitation equipment schematic diagrames.In figure, 1 induction furnace；2 hydrocarbon gas and carrier gas air inlet；3 graphite-baseds
Body；4 tail gas gas outlets.
Fig. 2 super-high heat-conductive annealed state pyrolytic graphite stereoscan photographs.
Specific implementation mode
As shown in Figure 1, pyrolytic graphite precipitation equipment is equipped with induction furnace 1 in the present invention, carbon is respectively set in the both ends of induction furnace 1
Hydrogen and carrier gas air inlet 2, tail gas gas outlet 4.In use, graphite matrix 3 is placed in induction furnace 1 first, vacuum is opened
Air in induction furnace 1 is discharged pump, and when vacuum degree reaches 300Pa or less in induction furnace 1, be powered heating.When temperature reaches setting
Depositing temperature (1700 DEG C~2100 DEG C) when, proportionally simultaneously be passed through hydrocarbon gas (such as：Methane, ethylene, acetylene, ethane,
Propane etc.) and carrier gas, the reaction time is 5 minutes~40 hours, and deposited pyrolytic graphite (PG) material is prepared, and deposits thickness
Degree is 0.1mm~20mm.
After deposited pyrolytic graphite (PG) material being prepared is machined to required size, it is put into high-temperature heat treatment
In stove, pressure is applied to it by the smooth graphite jig in surface, high temperature (2800~3100 is carried out under vacuum or protective atmosphere
DEG C), high pressure (0.5~10MPa) heat treatment, cool to room temperature with the furnace, obtain having the annealed state pyrolysis stone of super-high heat-conductive performance
Ink material.
In the following, being further elaborated on to the present invention by embodiment.
Embodiment 1
In the present embodiment, 2000 DEG C of depositing temperature, propane gas flow 0.4m3/ h, nitrogen flow 0.6m3/ h, depositing base
It is 6 pieces of graphite cakes that size is 420 × 100mm, graphite plate surface passes through polishing treatment.Graphite cake is fitted into induction furnace, is beaten
It opens vacuum pump and excludes induction furnace air, be warming up to 2000 DEG C according to the heating rate of 15 DEG C/min, at this time vacuum in induction furnace
Degree is 150Pa, while being passed through nitrogen and propane progress chemical vapor deposition.Sedimentation time 5h, obtain specification be 420 ×
The deposited pyrolytic graphite plank of 100 × 1.5mm.
PG plates are processed into the PG pieces of 200 × 90 × 1mm, are put into graphitizing furnace the 0.5MPa that pressurizes, at 2900 DEG C into
Row heat treatment 1 hour, cools to room temperature with the furnace, obtains the annealed state pyrolytic graphite piece with super-high heat-conductive performance after heat treatment,
Its thermal conductivity is 1721W/ (mk).
As shown in Fig. 2, observing Fracture Profile in Metallic Materials using scanning electron microscope, it is found that graphite platelet structure is very complete.
Embodiment 2
In the present embodiment, 1950 DEG C of depositing temperature, propane gas flow 0.45m3/ h, nitrogen flow 0.8m3/ h deposits base
Body is 6 pieces of graphite cakes that size is 420 × 120mm, and graphite plate surface passes through polishing treatment.Graphite cake is fitted into induction furnace,
It opens vacuum pump and excludes induction furnace air, 1950 DEG C are warming up to according to the heating rate of 15 DEG C/min, it is true in induction furnace at this time
Reciprocal of duty cycle is 160Pa, while being passed through nitrogen and propane progress chemical vapor deposition.Sedimentation time 30h, it is 420 to obtain specification
The deposited pyrolytic graphite plank of × 120 × 7mm.
PG plates are processed into the PG pieces of 100 × 60 × 4mm, are put into graphitizing furnace the 0.5MPa that pressurizes, at 3000 DEG C into
Row heat treatment 3 hours, cools to room temperature with the furnace, obtains the annealed state pyrolytic graphite piece with super-high heat-conductive performance after heat treatment,
Its thermal conductivity is 1736W/ (mk).Fracture Profile in Metallic Materials is observed using scanning electron microscope, it is found that graphite platelet structure is very complete
It is whole.
Embodiment 3
In the present embodiment, 2100 DEG C of depositing temperature, propane gas flow 0.35m3/ h, nitrogen flow 0.9m3/ h deposits base
Body is 6 pieces of graphite cakes that size is 420 × 150mm, and polishing treatment is passed through on surface.Graphite cake is fitted into induction furnace, is opened true
Sky pump excludes induction furnace air, is warming up to 2100 DEG C according to the heating rate of 15 DEG C/min, vacuum degree is in induction furnace at this time
100Pa, while being passed through nitrogen and propane progress chemical vapor deposition.Sedimentation time 40h, obtain specification be 420 × 150 ×
The deposited pyrolytic graphite plank of 15mm.
PG plates are processed into the PG pieces of 200 × 100 × 12mm, are put into graphitizing furnace the 5MPa that pressurizes, at 2800 DEG C into
Row heat treatment 8 hours, cools to room temperature with the furnace, obtains the annealed state pyrolytic graphite piece with super-high heat-conductive performance after heat treatment,
Its thermal conductivity is 1679W/ (mk).Fracture Profile in Metallic Materials is observed using scanning electron microscope, it is found that graphite platelet structure is very complete
It is whole.
Embodiment 4
In the present embodiment, 1850 DEG C of depositing temperature, acetylene gas flow 0.2m3/ h, nitrogen flow 0.8m3/ h, depositing base
It is 6 pieces of graphite cakes that size is 420 × 100mm, polishing treatment is passed through on surface.Graphite cake is fitted into induction furnace, vacuum is opened
Pump excludes induction furnace air, is warming up to 1850 DEG C according to the heating rate of 15 DEG C/min, vacuum degree is in induction furnace at this time
200Pa, while being passed through nitrogen and acetylene progress chemical vapor deposition.Sedimentation time 30h, obtain specification be 420 × 100 ×
The deposited pyrolytic graphite plank of 10mm.
PG plates are processed into the PG pieces of 150 × 80 × 8mm, are put into graphitizing furnace the 8MPa that pressurizes, are carried out at 3100 DEG C
Heat treatment 2 hours, cools to room temperature with the furnace, obtains the annealed state pyrolytic graphite piece with super-high heat-conductive performance after heat treatment,
Thermal conductivity is 1805W/ (mk).Fracture Profile in Metallic Materials is observed using scanning electron microscope, it is found that graphite platelet structure is very complete.
Claims (4)
1. a kind of preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance, it is characterised in that：Include the following steps：
(1) preparation of pyrolytic graphite：
It using chemical vapor deposition method, is placed in induction furnace using graphite as depositing base, opens vacuum pump by induction furnace
Interior air is discharged, and when vacuum degree reaches 300Pa or less in induction furnace, is powered and heats up to induction furnace；When temperature reaches the heavy of setting
When accumulated temperature is spent, it is proportionally passed through carrier gas and reaction gas simultaneously, the reaction time is 5 minutes~40 hours, and deposition is prepared
State pyrolyzing graphite material；
(2) the high temperature and pressure heat treatment of pyrolytic graphite：
The deposited pyrolyzing graphite material being prepared is processed into required size, is placed on the smooth graphite jig in surface
In, be heat-treated under conditions of applying pressure and vacuum or protective atmosphere, apply the pressure that pressure generates be 0.5~
10MPa is heat-treated 0.5~20 hour at 2800~3100 DEG C of predetermined temperature, then cools to room temperature with the furnace, obtains having super
The annealed state pyrolyzing graphite material of high thermal conductivity.
2. the preparation method of the annealed state pyrolytic graphite described in accordance with the claim 1 with super-high heat-conductive performance, feature exist
In：Carrier gas is nitrogen or argon gas, and reaction gas is hydrocarbon gas.
3. the preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance, feature exist according to claim 2
In：Hydrocarbon gas accounts for the 20%~40% of carrier gas and reaction gas total flow, remaining is carrier gas.
4. the preparation method of the annealed state pyrolytic graphite described in accordance with the claim 1 with super-high heat-conductive performance, feature exist
In：Depositing temperature is 1700 DEG C~2100 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112813496A (en) * | 2021-01-11 | 2021-05-18 | 上海第二工业大学 | Preparation method of highly oriented pyrolytic graphite |
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| CN1792124A (en) * | 2003-09-19 | 2006-06-21 | 通用电气公司 | Bulk high thermal conductivity feedstock and method of making thereof |
| US20060210465A1 (en) * | 2005-03-04 | 2006-09-21 | The Morgan Crucible Company Plc | Anisotropic material treatment heater tubes |
| CN1872677A (en) * | 2005-06-03 | 2006-12-06 | 中国矿业大学（北京校区） | High heat conducting foam material of graphite, and fabricating method |
| CN101660137A (en) * | 2009-09-11 | 2010-03-03 | 华东理工大学 | Pyrolytic graphite composite coating and applications thereof |
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