CN110451964A - A kind of preparation method of high orientation Graphite block material - Google Patents

A kind of preparation method of high orientation Graphite block material Download PDF

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Publication number
CN110451964A
CN110451964A CN201910852712.9A CN201910852712A CN110451964A CN 110451964 A CN110451964 A CN 110451964A CN 201910852712 A CN201910852712 A CN 201910852712A CN 110451964 A CN110451964 A CN 110451964A
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CN
China
Prior art keywords
graphite block
kapton
preparation
hot pressing
high orientation
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Pending
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CN201910852712.9A
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Chinese (zh)
Inventor
陈曲
唐文军
杨朝晖
吴晓宁
朱光福
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Beijing Zhongshiweiye Science And Technology Co Ltd
Wuxi Jones Tech Plc
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Beijing Zhongshiweiye Science And Technology Co Ltd
Wuxi Jones Tech Plc
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Priority to CN201910852712.9A priority Critical patent/CN110451964A/en
Publication of CN110451964A publication Critical patent/CN110451964A/en
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/522—Graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Abstract

The invention belongs to technical field of material, and in particular to a kind of preparation method of high orientation Graphite block material.The preparation method of high orientation Graphite block material of the present invention, the following steps are included: (1) stacks after cutting Kapton according to certain size, Kapton surface or every Kapton surface after stacking certain number of plies are coated with a layer binder, are stacked into laminated body；(2) the polyimide laminates body that heap is folded is placed in the tooling of hot pressing furnace, the temperature and pressure that hot pressing furnace is arranged is carbonized and is graphitized；(3) the polyimide laminates body after carbonization and graphitization is cut out or mechanical process, obtains complete graphite block product.The present invention can prepare the graphite block body of different size, method is simple, and the Graphite block material excellent heat transfer properties of preparation, using mesophase pitch or other easy graphited high molecular material phenolic resin or graphene oxide slurry as binder, there is lamination in avoidable graphite block.

Description

A kind of preparation method of high orientation Graphite block material
Technical field
The invention belongs to technical field of material, and in particular to a kind of preparation method of high orientation Graphite block material.
Background technique
In recent years, with the development of electronic industry, the heating problem that solve electronic equipment is also increasingly important.Currently, industry Boundary has been sought for the material with higher heat-sinking capability or heat-transfer capability to solve such problems, and stratiform high orientation Graphite block body material is a kind of good selection.The thermal conductivity of this high orientation graphite block body in the orientation direction is in 800W/ MK or more.
The existing common approach for preparing highly oriented graphite block body high conductivity material is chemical vapour deposition technique (CVD), And there is the defects of at high cost, the period is long by CVD, and then cannot achieve large-scale production.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of high orientation The preparation method of Graphite block material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of system of high orientation Graphite block material Preparation Method, which is characterized in that the preparation method of the high orientation Graphite block material has the feature that
A kind of preparation method of high orientation Graphite block material, comprising the following steps:
(1) it is stacked after cutting Kapton according to certain size, the polyimides after stacking certain number of plies Film surface or every Kapton surface are coated with a layer binder, continue to stack Kapton, until polyamides is sub- Amine thin-film laminate finished product thickness reaches 500 μm ~ 20cm；
(2) the polyimide laminates body that heap is folded is placed in the tooling of hot pressing furnace, the temperature and pressure of hot pressing furnace is set such as Under:
Carbonisation: hot pressing furnace carries out temperature programming to 1000 ~ 1500 DEG C, and pressure rises to 0.01 ~ 0.2kg/cm2, and in highest 30 ~ 300min of temperature；
Graphitizing process: after to carbodiimide procedure, 2700 ~ 3000 DEG C are continuously heating to, pressure rises to 20 ~ 400kg/cm2, and In 30 ~ 180min of highest temperature pressure-maintaining and heat-preservation, subsequent program is cooled to 1000 DEG C, terminator, cooled to room temperature；
(3) the folded burning sample in furnace is taken out, is cut out or mechanical process, obtains complete graphite block product.
The binder of the coating of Kapton surface described in step (1) is mesophase pitch, phenolic resin or oxidation Graphene slurry.
Compared with prior art, the invention has the following advantages that
(1) graphite block body of different size can be prepared, thickness is adjustable, and for thickness between 500 μm ~ 20cm, method is simple；
(2) the Graphite block material excellent heat transfer properties prepared, thermal coefficient is in 1200 ~ 2000W/mK；
(3) using mesophase pitch or other easily graphitization high molecular material such as phenolic resin or graphene oxide slurry as viscous Agent is tied, lamination occurs in avoidable graphite block.
Technical solution of the present invention is described further combined with specific embodiments below.
Specific embodiment
Embodiment 1
A kind of preparation method of high orientation Graphite block material, comprising the following steps:
(1) it is stacked after being cut with a thickness of 25 μm of Kapton according to the size of 127mm × 127mm, every stacking 10 layers of even spread, one layer of mesophase pitch binder continues to stack Kapton, until Kapton laminated body Finished product thickness reaches 10cm；
(2) the polyimide laminates body that heap is folded is placed in the tooling of hot pressing furnace, the temperature and pressure journey of hot pressing furnace is set Sequence is as follows:
Carbonisation: hot pressing furnace carries out temperature programming to 1100 DEG C, and pressure rises to 0.1kg/cm2, and keep the temperature 180min；
Graphitizing process: after to carbodiimide procedure, 2800 DEG C are continuously heating to, pressure rises to 300kg/cm2, and pressure-maintaining and heat-preservation 60min, subsequent program are cooled to 1000 DEG C, terminator, cooled to room temperature；
(3) the folded burning sample in furnace is taken out, obtains complete graphite block product by cutting out.
Embodiment 2
A kind of preparation method of high orientation Graphite block material, comprising the following steps:
(1) it is stacked after being cut with a thickness of 50 μm of Kapton according to the size of 127mm × 127mm, every stacking 10 layers of even spread, one layer of mesophase pitch binder continues to stack Kapton, until Kapton laminated body Finished product thickness reaches 20cm；
(2) the polyimide laminates body that heap is folded is placed in the tooling of hot pressing furnace, the temperature and pressure journey of hot pressing furnace is set Sequence is as follows:
Carbonisation: hot pressing furnace carries out temperature programming to 1500 DEG C, and pressure rises to 0.2kg/cm2, and keep the temperature 300min；
Graphitizing process: after to carbodiimide procedure, 3000 DEG C are continuously heating to, pressure rises to 300kg/cm2, and pressure-maintaining and heat-preservation 100min, subsequent program are cooled to 1000 DEG C, terminator, cooled to room temperature；
(3) the folded burning sample in furnace is taken out, obtains complete graphite block product by mechanical process.
Embodiment 3
A kind of preparation method of high orientation Graphite block material, comprising the following steps:
(1) it is stacked after being cut with a thickness of 25 μm of Kapton according to the size of 127mm × 127mm, at every Kapton surface applied adhesive phenolic resin continues to stack Kapton, until Kapton lamination Body finished product thickness reaches 500 μm；
(2) the polyimide laminates body that heap is folded is placed in the tooling of hot pressing furnace, the temperature and pressure journey of hot pressing furnace is set Sequence is as follows:
Carbonisation: hot pressing furnace carries out temperature programming to 1000 DEG C, and pressure rises to 0.1kg/cm2, and keep the temperature 180min；
Graphitizing process: after to carbodiimide procedure, 2800 DEG C are continuously heating to, pressure rises to 20kg/cm2, and pressure-maintaining and heat-preservation 180min, subsequent program are cooled to 1000 DEG C, terminator, cooled to room temperature；
(3) the folded burning sample in furnace is taken out, obtains complete graphite block product by cutting out.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to the present invention Essence any simple modification, change and equivalence change to the above embodiments, still fall within technical solution of the present invention In protection scope.

Claims (2)

1. a kind of preparation method of high orientation Graphite block material, which comprises the following steps:
(1) it is stacked after cutting Kapton according to certain size, the polyimides after stacking certain number of plies Film surface or every Kapton surface are coated with a layer binder, continue to stack Kapton, until polyamides is sub- Amine thin-film laminate finished product thickness reaches 500 μm ~ 20cm；
(2) the polyimide laminates body that heap is folded is placed in the tooling of hot pressing furnace, the temperature and pressure of hot pressing furnace is set such as Under:
Carbonisation: hot pressing furnace carries out temperature programming to 1000 ~ 1500 DEG C, and pressure rises to 0.01 ~ 0.2kg/cm2, and in the highest temperature 30 ~ 300min of degree heat preservation；
Graphitizing process: after to carbodiimide procedure, 2700 ~ 3000 DEG C are continuously heating to, pressure rises to 20 ~ 400kg/cm2, and In 30 ~ 180min of highest temperature pressure-maintaining and heat-preservation, subsequent program is cooled to 1000 DEG C, terminator, cooled to room temperature；
(3) the folded burning sample in furnace is taken out, is cut out or mechanical process, obtains complete graphite block product.
2. the preparation method of high orientation Graphite block material according to claim 1, which is characterized in that institute in step (1) The binder for stating the coating of Kapton surface is mesophase pitch, phenolic resin or graphene oxide slurry.
CN201910852712.9A 2019-09-10 2019-09-10 A kind of preparation method of high orientation Graphite block material Pending CN110451964A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113387703A (en) * 2021-04-06 2021-09-14 长沙新材料产业研究院有限公司 Oriented graphite material and preparation method thereof
CN113666369A (en) * 2021-09-10 2021-11-19 东莞市鸿亿导热材料有限公司 Alkene carbon film and preparation method thereof
CN116082047A (en) * 2021-11-05 2023-05-09 天津大学 Preparation method of heat dissipation in plane and high heat conduction orientation graphite plate outside plane constructed by hot pressing method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113387703A (en) * 2021-04-06 2021-09-14 长沙新材料产业研究院有限公司 Oriented graphite material and preparation method 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
CN113666369A (en) * 2021-09-10 2021-11-19 东莞市鸿亿导热材料有限公司 Alkene carbon film and preparation method thereof
CN116082047A (en) * 2021-11-05 2023-05-09 天津大学 Preparation method of heat dissipation in plane and high heat conduction orientation graphite plate outside plane constructed by hot pressing method

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Application publication date: 20191115