CN104495795A - Graphite flake and preparation method thereof - Google Patents
Graphite flake and preparation method thereof Download PDFInfo
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- CN104495795A CN104495795A CN201410680391.6A CN201410680391A CN104495795A CN 104495795 A CN104495795 A CN 104495795A CN 201410680391 A CN201410680391 A CN 201410680391A CN 104495795 A CN104495795 A CN 104495795A
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Abstract
The invention provides a preparation method of graphite flake. The preparation method comprises following steps: lamination of organic polymer thin film, hot pressing moulding, carbonization, graphitization, and obtaining of the graphite flake. The preparation method is simple; the organic polymer thin film is taken as a raw material; the layer number of the organic polymer thin film is controlled, so that the thickness of the obtained graphite flake is controllable; and at the same time, longitudinal heat conduction capability of the graphite flake is increased via combination of hot pressing moulding, carbonization, and graphitization. The preparation method can be used for preparing the graphite flake with a thickness of 0.05 to 1.00mm, facing heat conductivity coefficient of 780 to 860W/mK, and longitudinal heat conductivity coefficient of 15 to 30W/mK.
Description
Technical field
The invention belongs to graphite material technical field, be specifically related to a kind of graphite flake and preparation method thereof.
Background technology
The developing trend miniaturization of high-end electronic industrial devices, compact construction and high power density, and the heat dispersion of high-end electronic industrial devices and the job stability of device and reliability closely bound up, become important factor of its development of restriction.Solve the heat dissipation problem of high-end electronic industrial devices, except good heat dissipation design, the heat sink material that, thermal conductivity light in the urgent need to quality is high.Traditional metal (aluminium, copper) radiating piece is because itself density is comparatively large, thermal expansivity is higher, impure its thermal conductivity that causes of material can decline to a great extent.
High-heat conductivity graphite material becomes the effective way solving high power electronic device heat dissipation problem.High-heat conductivity graphite material quality light (being only the 1/2-1/5 of conventional metals thermally conductive material), thermal conductivity is high, corrosion-resistant, thermal expansivity is little, and the aforementioned device that need dispel the heat replaces traditional metal materials, is not only conducive to miniaturization microminiaturization and the high power density of electron device, and effectively can alleviate the weight of device, increase useful load, can realize high efficiency and heat radiation, use safety, life-span are long.Be commonly used for electronics industry heat conduction, the graphite-structure material of heat radiation have graphite flake, expandable graphite sheet (also known as natural stone ink film) and rostone ink film.
High-power LED lamp can adopt graphite flake replacement heat conductive silica gel in the past, High thermal-conductive silicone grease is served as heat-conducting pad and used, and the replacement of this thermally conductive material can increase its comprehensive heat-sinking capability, reduces overall dimensions and the weight of high-power LED lamp simultaneously.But graphite flake conventional in current industrial is normally raw material with natural flake graphite, carries out intercalation chemistry reaction by acidification, then through washing, dry and high-temperature expansion acquisition high power expanded graphite worm, then obtain through calendering, pressing process.
Publication number is the preparation method that the patent documentation of CN102244153A provides a kind of graphite heat radiation fin, and the method is by Graphite Powder 99 through strong acid treatment, with metal powder compound, then obtains through high temperature puffing.Publication number is the heat radiation graphite flake that the patent documentation of CN10191751A provides that a kind of thickness is 0.05-0.5mm, preparation technology is that Graphite Powder 99 is through acidifying or high temperature purification process, again through expanded, most heel boron nitride, carbon black or copper powder carry out composite, prepare graphite flake coiled material.The graphite heat radiation fin that above-mentioned patent documentation provides is in fact all to conventional flex graphite flake modification gained, belong to natural graphite flakes field, above-mentioned processing method not only making processes is loaded down with trivial details, in process, acidification and washing process easily produce a large amount of waste water, quality product is correlated with material purity simultaneously, the not easily obtained desirable material for high power device heat radiation.
Rostone ink film, its thickness is generally less than 0.050mm, and with its low density, the feature of high heat conduction is applied in portable electronic piece field more and more.Graphite film outstanding advantages is that plane thermal conductivity is high, can to more than 1600W/mK, but due to the thinner and longitudinal capacity of heat transmission not good (being generally 5-15W/mK) of graphite film itself, in portable electronic piece field, be usually applied to effect smart mobile phone screen rear or CPU playing auxiliary heat dissipation, for longitudinal heat radiation have outstanding demand as high-power LED lamp etc. then and inapplicable.The method of conductive graphite sheet is prepared in the superposition of present stage favourable use artificial graphite film or modification, but still there is the problems such as the uncontrollable and longitudinal heat conductivility of thickness is not good.The patent documentation being CN202652815U as the patent No. is mutually superposed by some electrographite films, then glued membrane is coated on graphite basic layer outside, this electrographite sheet be formed by stacking, owing to there is space between electrographite membrane layer, can affect its longitudinal heat-conducting effect.Publication number is that the patent documentation of CN103770415A discloses a kind of method utilizing graphite modified dose of modifying artificial graphite film, but the method cannot increase the thickness of electrographite film effectively, and longitudinal capacity of heat transmission is poor.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of graphite flake and preparation method thereof, and the thickness of the graphite flake adopting preparation method provided by the present invention to prepare is controlled, has good longitudinal capacity of heat transmission.
The invention provides a kind of preparation method of graphite flake, comprise the following steps:
By hot-forming for the organic polymer thin film of lamination, successively through carbonization and greying, obtain graphite flake.
Preferably, described organic polymer thin film is selected from one or both in Kapton or aromatic series polyoxadiazoles quasi-copolymer film.
Preferably, described organic polymer thin film is Kapton.
Preferably, the thickness in monolayer of described organic polymer thin film is 35 μm ~ 75 μm, and the thickness of the organic polymer thin film of described lamination is 0.1mm ~ 2.5mm.
Preferably, described hot-forming temperature is 400 ~ 700 DEG C, and described hot-forming pressure is 8MPa ~ 20MPa.
Preferably, the temperature rise rate of described hot-forming temperature is less than 20 DEG C/min.
Preferably, the temperature of described carbonization is 1000 ~ 1500 DEG C.
Preferably, the temperature rise rate of described carbonization is less than 2 DEG C/min.
Preferably, described graphited temperature is 2600 ~ 2900 DEG C.
Present invention also offers a kind of graphite flake prepared by above-mentioned preparation method.
Compared with prior art, the invention provides a kind of preparation method of graphite flake, comprise the following steps: by organic polymer thin film lamination, hot-forming, carbonization, greying, obtain graphite flake.Preparation method's technique of graphite flake provided by the present invention is simple, using organic polymer thin film as raw material, by controlling the number of plies of organic polymer thin film, makes the graphite flake thickness that obtains controlled; Meanwhile, in conjunction with hot-forming, carbonization, graphited step, longitudinal capacity of heat transmission of graphite flake can be strengthened.
Result shows, the present invention can prepare the graphite flake that thickness is 0.05mm ~ 1.00mm, graphite flake be 780 ~ 860W/mK towards thermal conductivity, longitudinal thermal conductivity is 15 ~ 30W/mK.
Embodiment
The invention provides a kind of preparation method of graphite flake, it is characterized in that, comprise the following steps:
By hot-forming for lamination organic polymer thin film, successively through carbonization and greying, obtain graphite flake.
The present invention is that graphite flake prepared by raw material with organic polymer thin film, described organic polymer thin film be selected from Kapton or aromatic series polyoxadiazoles base polymer (POD) film one or both, preferably, described organic polymer thin film is the Kapton of two-way stretch.
First organic polymer thin film is carried out lamination by the present invention, concrete, is fitly superimposed by the organic polymer thin film reduced in advance according to thickness requirements.Wherein, the thickness in monolayer of described organic polymer thin film is 35 μm ~ 75 μm, and in one embodiment of the invention, the thickness in monolayer of described organic polymer thin film is preferably 50 μm; Further, the thickness of the organic polymer thin film of lamination is 0.1mm ~ 2.5mm, is preferably 0.2mm ~ 2.0mm, is more preferably 0.5mm ~ 1.0mm.
By hot-forming for the organic polymer thin film of lamination.Describedly hot-formingly to be specially: be placed in by the polymeric film of lamination in the middle of two briquettings, be positioned in hot pressing furnace, under nitrogen or argon, be warming up to by polymeric film between 400 ~ 700 DEG C, namely hot-forming temperature is 400 ~ 700 DEG C; Described polymeric film is applied to the pressure of 8MPa ~ 20MPa, namely hot-forming pressure is 8MPa ~ 20MPa, obtains hot-forming polymeric film.Wherein, described hot-forming temperature is for being preferably 500 ~ 650 DEG C, and described hot-forming temperature rise rate is less than 20 DEG C/min, is preferably 10 DEG C/min; Described hot-forming pressure is preferably 10MPa ~ 15MPa.
The present invention, by the organic polymer thin film after hot-forming, successively through carbonization and greying, obtains graphite flake.
In the present invention, described carbonization is preferably carried out as follows:
Organic polymer thin film after hot-forming is placed in carbonization mould, under the condition vacuumized, carries out carbonization.The temperature of described carbonization is 1000 ~ 1500 DEG C, is preferably 1200 ~ 1500 DEG C; The temperature rise rate of described carbonization is less than 2 DEG C/min, is preferably 1 DEG C/min.
Film cooling after carbonization is placed in graphitizing furnace, under an argon atmosphere, carries out greying, obtain graphite flake.Described graphited temperature is 2600 ~ 2900 DEG C, and in one embodiment, described graphited temperature is preferably 2800 DEG C; In another embodiment, described graphited temperature is preferably 2850 DEG C.Described graphited temperature rise rate is 5 ~ 40 DEG C/min, is preferably 15 ~ 20 DEG C/min.Described graphitizing furnace is preferably the graphitizing furnace of heating in medium frequency.Above-mentioned obtained graphite flake, after pressure treatment, can strengthen its mechanical strength further.
Present invention also offers a kind of graphite flake prepared by aforesaid method.The graphite flake that thickness is 0.05mm ~ 1.00mm can be prepared according to preparation method provided by the present invention.
Preparation method's technique of graphite flake provided by the present invention is simple, using organic polymer thin film as raw material, by controlling the number of plies of organic polymer thin film, makes the graphite flake thickness that obtains controlled; Meanwhile, in conjunction with hot-forming, carbonization, graphited step, longitudinal capacity of heat transmission of graphite flake can be strengthened.The field high to longitudinal heat conduction demand is applicable to, such as great power LED cooling etc. prepared by the present invention.
Result shows, the present invention can prepare the graphite flake that thickness is 0.05mm ~ 1.00mm, graphite flake be 780 ~ 860W/mK towards thermal conductivity, longitudinal thermal conductivity is 15 ~ 30W/mK.
In order to understand the present invention further, be described graphite flake provided by the invention and preparation method thereof below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
Be 257*257mm by 10 chip sizes, the Kapton of 50 micron thickness fitly stacks, thickness is about 0.5mm, be positioned in the middle of two graphite briquettings (described two graphite briquetting sizes are greater than the size of Kapton), be placed in hot pressing furnace, with the speed rapid temperature increases to 600 DEG C of 10 DEG C/min, apply the pressure of about 10MPa simultaneously.Transfer in carbonization mould subsequently, under vacuumized conditions, be warming up to 1200 DEG C with the heat-up rate of 1 DEG C/min.After lowering the temperature, carbonization mould is transferred in graphitizing furnace, under an argon atmosphere, is warming up to 2900 DEG C with the temperature rise rate of 20 DEG C/min, and constant temperature 1h.
The electrographite sheet thickness preparing gained is about 0.43mm, and utilize laser heat conducting instrument to test and show that towards thermal conductivity be 860W/mK, longitudinal thermal conductivity is 18W/mK.
Embodiment 2
Be 257*257mm by 20 chip sizes, the Kapton of 50 micron thickness fitly stacks, thickness is about 1mm, be positioned in the middle of two graphite briquettings (graphite briquetting size is greater than the size of Kapton), be placed in hot pressing furnace, with the speed rapid temperature increases to 550 DEG C of 10 DEG C/min, apply the pressure of about 12MPa simultaneously.Transfer in carbonization mould subsequently, under vacuumized conditions, be warming up to 1500 DEG C with the heat-up rate of 1 DEG C/min.After lowering the temperature, carbonization mould is transferred in graphitizing furnace, under an argon atmosphere, is warming up to 2850 DEG C with the temperature rise rate of 15 DEG C/min, and constant temperature 1h.
The electrographite sheet thickness preparing gained is about 0.86mm, and utilize laser heat conducting instrument to test and show that towards thermal conductivity be 820W/mK, longitudinal thermal conductivity is 23W/mK.
Embodiment 3
Be 257*300mm by 15 chip sizes, the Kapton of 35 micron thickness fitly stacks, thickness is about 0.5mm, be positioned in the middle of two graphite briquettings (graphite briquetting size is greater than the size of Kapton), be placed in hot pressing furnace, with the speed rapid temperature increases to 500 DEG C of 10 DEG C/min, apply the pressure of about 10MPa simultaneously.Transfer in carbonization mould subsequently, under vacuumized conditions, be warming up to 1200 DEG C with the heat-up rate of 1 DEG C/min.After lowering the temperature, carbonization mould is transferred in graphitizing furnace, under an argon atmosphere, is warming up to 2800 DEG C with the temperature rise rate of 18 DEG C/min, and constant temperature 1h.
The electrographite sheet thickness preparing gained is about 0.38mm, and utilize laser heat conducting instrument to test and show that towards thermal conductivity be 800W/mK, longitudinal thermal conductivity is 15W/Mk.
Embodiment 4
Be 257*350mm by 10 chip sizes, the Kapton of 75 micron thickness fitly stacks, laminated thickness is about 0.75mm, be positioned in the middle of two briquettings (graphite briquetting size is greater than the size of Kapton), be placed in hot pressing furnace, with the speed rapid temperature increases to 550 DEG C of 15 DEG C/min, apply the pressure of about 15MPa simultaneously.Transfer in carbonization mould subsequently, under vacuumized conditions, be warming up to 1450 DEG C with the heat-up rate of 1 DEG C/min.After lowering the temperature, carbonization mould is transferred in graphitizing furnace, under an argon atmosphere, is warming up to 2900 DEG C with the temperature rise rate of 20 DEG C/min, and constant temperature 1h.
The electrographite sheet thickness preparing gained is about 0.6mm, and utilize laser heat conducting instrument to test and show that towards thermal conductivity be 780W/mK, longitudinal thermal conductivity is 30W/mK.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for graphite flake, is characterized in that, comprises the following steps:
By hot-forming for the organic polymer thin film of lamination, successively through carbonization and greying, obtain graphite flake.
2. preparation method according to claim 1, is characterized in that, described organic polymer thin film be selected from Kapton or aromatic series polyoxadiazoles quasi-copolymer film one or both.
3. preparation method according to claim 1, is characterized in that, described organic polymer thin film is Kapton.
4. preparation method according to claim 1, is characterized in that, the thickness in monolayer of described organic polymer thin film is 35 μm ~ 75 μm, and the thickness of the organic polymer thin film of described lamination is 0.1mm ~ 2.5mm.
5. preparation method according to claim 1, is characterized in that, described hot-forming temperature is 400 ~ 700 DEG C, and described hot-forming pressure is 8MPa ~ 20MPa.
6. preparation method according to claim 5, is characterized in that, the temperature rise rate of described hot-forming temperature is less than 20 DEG C/min.
7. preparation method according to claim 1, is characterized in that, the temperature of described carbonization is 1000 ~ 1500 DEG C.
8. preparation method according to claim 1, is characterized in that, the temperature rise rate of described carbonization is less than 2 DEG C/min.
9. preparation method according to claim 1, is characterized in that, described graphited temperature is 2600 ~ 2900 DEG C.
10. the graphite flake prepared by claim 1 ~ 9 any one preparation method.
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| CN104909358A (en) * | 2015-05-25 | 2015-09-16 | 镇江博昊科技有限公司 | Preparation method of large-size high-heat conduction graphite membrane |
| CN105439132A (en) * | 2015-12-17 | 2016-03-30 | 云南云天化股份有限公司 | Graphite material with high thermal conduction performance and preparation method thereof |
| CN105600782A (en) * | 2016-03-04 | 2016-05-25 | 深圳丹邦科技股份有限公司 | Graphene film prepared from flexible polyimide and preparing method thereof |
| CN105752959A (en) * | 2016-03-04 | 2016-07-13 | 深圳丹邦科技股份有限公司 | Thermoplastic polyimide film carbonization composite film and preparation method thereof |
| CN106185899A (en) * | 2016-07-11 | 2016-12-07 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of axial high thermal conductivity flexible graphite cake |
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| CN107922193A (en) * | 2015-06-18 | 2018-04-17 | 帝国创新有限公司 | Two-dimentional carbon material |
| CN109071233A (en) * | 2016-04-22 | 2018-12-21 | 株式会社钟化 | The manufacturing method of high orientation graphite and high orientation graphite |
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| CN110451964A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | A kind of preparation method of high orientation Graphite block material |
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| CN109874344A (en) * | 2015-04-15 | 2019-06-11 | 株式会社钟化 | The charge of ion beam converts film |
| CN104909358A (en) * | 2015-05-25 | 2015-09-16 | 镇江博昊科技有限公司 | Preparation method of large-size high-heat conduction graphite membrane |
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| WO2017148106A1 (en) * | 2016-03-04 | 2017-09-08 | 深圳丹邦科技股份有限公司 | Thermoplastic polyimide thin-film carbonized composite membrane, and preparation method therefor |
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| US11078081B2 (en) | 2016-03-04 | 2021-08-03 | Shenzhen Danbond Technology Co., Ltd | Graphene film prepared with flexible polyimide and preparation method thereof |
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| CN105600782A (en) * | 2016-03-04 | 2016-05-25 | 深圳丹邦科技股份有限公司 | Graphene film prepared from flexible polyimide and preparing method thereof |
| US11001739B2 (en) * | 2016-03-04 | 2021-05-11 | Shenzhen Danbond Technology Co., Ltd | Carbonized composite thermoplastic polyimide film and preparation method thereof |
| CN109071233A (en) * | 2016-04-22 | 2018-12-21 | 株式会社钟化 | The manufacturing method of high orientation graphite and high orientation graphite |
| CN106185899A (en) * | 2016-07-11 | 2016-12-07 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of axial high thermal conductivity flexible graphite cake |
| CN106626578A (en) * | 2016-12-30 | 2017-05-10 | 株洲晨昕中高频设备有限公司 | Heat conduction graphite plate and preparation method thereof |
| CN110451964A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | A kind of preparation method of high orientation Graphite block material |
| CN113085294A (en) * | 2021-04-26 | 2021-07-09 | 湖南沛德新材料有限公司 | Graphite flake with controllable thickness and preparation process thereof |
| CN115520862A (en) * | 2022-10-10 | 2022-12-27 | 中汇睿能凤阳新材料科技有限公司 | Preparation method of artificial high-thermal-conductivity ultrathin graphite film |
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Effective date of registration: 20170821 Address after: 401220 Changshou District of Chongqing economic and Technological Development Zone United Road No. 22 Co-patentee after: Yutianhua Co., Ltd., Yunnan Patentee after: Chongqing Yuntianhua hanen New Material Development Co Ltd Address before: 650228 Dianchi Road, Yunnan, China, No. 1417, No. Patentee before: Yutianhua Co., Ltd., Yunnan |
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