CN104961464A - Carbon-based composite with high rebound resilience and high heat conductivity coefficient along thickness direction and preparation method of carbon-based composite - Google Patents
Carbon-based composite with high rebound resilience and high heat conductivity coefficient along thickness direction and preparation method of carbon-based composite Download PDFInfo
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Abstract
The invention relates to a preparation method of a carbon-based composite with high rebound resilience and high heat conductivity coefficient simultaneously along a thickness direction. Graphite sheets in expanded graphite are connected to one another by arrayed carbon nano tubes; gaps among the graphite sheets are filled with the arrayed carbon nano tubes; the heat conductivity coefficient is greater than or equal to 25W/ (m.K) along the thickness direction; and after the graphite sheets are compressed by 10%, the rebound rate is greater than or equal to 90%. The arrayed carbon nano tubes grow through ferrocene carbon source solution; ferrocene cracks into iron atoms which are adhered to the graphite sheets of the expanded graphite, the carbon source solution cracks into carbon atoms which are adhered to surfaces of the iron atoms, so that the arrayed carbon nano tubes grow among the graphite sheets of the expanded graphite, heat flow can be transferred among the graphite sheets in the expanded graphite by high heat conductivity of the carbon nano tubes, the graphite sheets can be oriented along a perpendicular hot-pressing direction, namely a horizontal direction, the arrayed carbon nano tubes are connected to one another in the thickness direction, the graphite sheets and the gaps of the expanded graphite are filled with the arrayed carbon nano tubes, and the carbon-based composite with the high rebound resilience and the high heat conductivity coefficient along the thickness direction is obtained.
Description
Technical field
The present invention relates to the preparation method that a kind of through-thickness has snappiness and high thermal conductivity coefficient C-base composte material simultaneously, specifically the preparation method of a kind of expanded graphite and array carbon nano tube matrix material.
Background technology
Along with the fast development of science and technology, efficient heat conduction and heat radiation become the key issue of field of heat management.Improving constantly such as along with the electrical installation such as computer, mobile phone electronic component integration degree, the heat that the thermal value that its unit surface electron device improves constantly makes system produce increases suddenly.If there is no sufficient heat management guarantee, very easily cause related device premature aging or damage.Many electronic units need could normally to work at the temperature of 40 ~ 60 DEG C, and this proposes more and more higher requirement to thermally conductive material.The limitation such as density is comparatively large owing to existing for traditional metal heat-conducting material (as aluminium, copper etc.), the specific heat conductance ratio of material volume density (thermal conductivity coefficient with) is lower, thermal expansivity is higher, oxidizable, have been difficult to meet radiating requirements growing at present.Carbon material has higher thermal conductivity, lower density and good chemical resistance, is a class thermally conductive material most with prospects in recent years, thus has broad application prospects in fields such as the energy, communication, electronics.
Expanded graphite is a kind of loose porous vermiform material obtained through intercalation, expansion by natural flake graphite.Expanded graphite is owing to having the greying parietal layer of regular bulk, and the obstruction of phonon conduction is less, and heat transfer efficiency is very high, thus utilize expanded graphite to prepare research emphasis that carbon back highly heat-conductive material becomes people, also occurs the mandate or open of similar patent.State Intellectual Property Office of the People's Republic of China's grant number is that the patents of invention such as CN101407322B, CN100368342C, CN101458049A disclose the technology utilizing compression-expansion graphite-made for heat-conducting plate.
Above-described patent of invention disclose only traditional expanded graphite preparation method and pressing process, only obtain the graphite heat conducting material of anisotropic heat conductivity, and the compression resilience of material is poor.For graphite flake layer, the vibrations of the lattice of carbon atom are bases of material conducts heat, and therefore in graphite material, phonon transmission can only carry out travel at high speeds along graphite crystal face, and between graphite wafer surface layer due to hypertelorism, have a strong impact on the conduction of phonon.After the process of graphite pressing process, graphite crystal face under hot pressing function along in-plane orientation, thus in graphite heat-conducting fin only along in-plane having high thermal conductivity coefficient (being greater than 100W/ (mK)), and through-thickness thermal conductivity is very low, less than 10W/ (mK) (Zhi-Hai Feng, Tong-Qi Li, Zi-Jun Hu, Gao-Wen Zhao, Jun-Shan Wang, Bo-Yun Huang, Low cost preparation of high thermal conductivitycarbon blocks with ultra-high anisotropy from a commercial graphite paper, Carbon, 2012, 50 (10): 3947 – 3948.).All at 10W/ (mK) below, compression resilience is poor for the through-thickness thermal conductivity of the graphite heat conduction plate of the announcements such as patent application CN100368342C, CN103539111A of China.Therefore, existing published patent of invention obtain the compression resilience of graphite material through-thickness and thermal conductivity far can not meet the requirement of high integrated-optic device to the thermally conductive material capacity of heat transmission, have at carbon material and advantage basis develop the material that a kind of through-thickness has high resilience and a high thermal conductivity coefficient and seem particularly important.
Summary of the invention
The present invention is directed to the defect that graphite heat-conducting fin through-thickness thermal conductivity is too low and rebound resilience is poor prepared by existing expanded graphite, provide a kind of through-thickness to have C-base composte material of high resilience and high thermal conductivity coefficient and preparation method thereof.Through-thickness thermal conductivity reaches 25W/ (mK), and after compression 10%, rebound degree is more than or equal to the C-base composte material of 90%, as shown in Figure 1.
The present invention is by the following technical solutions:
A kind of through-thickness has the C-base composte material of high resilience and high thermal conductivity coefficient; Graphite flake layer in expanded graphite is connected by array carbon nano tube, and the space between graphite flake layer is filled by array carbon nano tube; The hot Xi Shuo≤25W/ (mK) of through-thickness Dao; Resilience Shuai≤90% after compression 10%.
A kind of through-thickness of the present invention has the preparation method of the C-base composte material of high resilience and high thermal conductivity coefficient, and step is as follows:
(1) by dehydrated alcohol and dimethylbenzene in mass ratio 0.1 ~ 10:1 be uniformly mixed and prepare carbon source solution, ferrocene is dissolved in above-mentioned carbon source solution, the ferrocene carbon source solution of configuration quality mark 1 ~ 5%;
(2) by rate of expansion be 100 ~ 300 expanded graphite be positioned in tube furnace, pass into argon shield, heated Tube-furnace is warming up to 700 ~ 900 DEG C, enters in tube furnace ferrocene carbon source injection of solution in order to grow array carbon nano tube on expanded graphite;
(3) expanded graphite of growth array carbon nano tube is placed in graphite jig, be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate controls at 200 ~ 300 DEG C/h, hot pressing temperature is 1500 ~ 2000 DEG C, hot pressing pressure is 5 ~ 40MPa, the heat-insulation pressure keeping time is 0.5 ~ 1h, treats that temperature is down to 100 DEG C of releases and is taken out sample.
In described step (2), the injection speed of ferrocene carbon source solution is 10 ~ 30mL/h, and growth time is 30 ~ 120min, and growth terminates under the protection of rare gas element, be cooled to room temperature and takes out.
Be described as follows:
(1) expanded graphite is a kind of vermiform graphite material; Rate of expansion refer to expansible black lead expand after with expansion front volume ratio; Directly can adopt commercially available prod;
(2) effect of ferrocene carbon source solution is for growing array carbon nano tube, in high temperature process furnances, ferrocene is cracked into iron atom and is attached to the graphite flake layer of expanded graphite, carbon source solution lyses becomes carbon atom and is adsorbed on iron atom surface, thus between the graphite flake layer of expanded graphite, grow array carbon nano tube, as Fig. 2;
(3) the array carbon nano tube Main Function of growth between the graphite flake layer of expanded graphite is the transmission utilizing the high thermal conductivity of carbon nanotube to realize graphite layers hot-fluid in expanded graphite, specifically, as Fig. 1 and 2, vertical-growth is in the array carbon nano tube of expanded graphite lamella, , connect the graphite flake layer of expanded graphite, fill the space between graphite flake layer, because carbon nanotube has high thermal conductivity (~ 2000W/ (mK)) along tube axial direction, the array carbon nano tube of dense arrangement provides a large amount of passage of heat between the graphite flake layer of expanded graphite, hot-fluid between the graphite flake layer making expanded graphite is by the array carbon nano tube transmission of interlayer, and then the thermal conductivity between the graphite flake layer of raising expanded graphite, space between the graphite flake layer being simultaneously filled with expanded graphite due to highdensity array carbon nano tube, and then improve its compression resilience,
(4) under hot pressing condition, the graphite flake layer of expanded graphite can along vertical hot pressing direction and horizontal direction orientation, now array carbon nano tube connects at thickness direction and fills lamella and the space of expanded graphite, and then acquisition through-thickness has high resilience and high thermal conductivity coefficient C-base composte material.
By the array carbon nano tube of above step in the growth of the graphite layers of expanded graphite and hot-forming, achieve the connection of high heat conduction array carbon nano tube to the graphite flake layer of expanded graphite and the filling in space, obtain through-thickness thermal conductivity and be more than or equal to 25W/ (mK), after compression 10%, rebound degree is more than or equal to the C-base composte material of 90%.
Beneficial effect of the present invention: matrix material expanded graphite of the present invention is easy to get, and the growthhabit of array carbon nano tube is controlled.In the present invention, the ordering of C-base composte material microtexture and densification can efficiently complete, can obtain the C-base composte material that through-thickness has high resilience and high thermal conductivity coefficient, the rebound resilience of its through-thickness and the capacity of heat transmission are far superior to traditional expanded graphite hot pressing coiled material and other expanded graphites and carbon nano tube compound material.
Accompanying drawing illustrates:
Fig. 1 is the microcosmic schematic diagram of C-base composte material of the present invention;
Fig. 2 is the scanning electron microscopic picture that array carbon nano tube grows at expanded graphite interlayer.
Embodiment
Provide embodiments of the invention below, be further illustrate of the present invention, instead of limit the scope of the invention.
Embodiment 1
Choose dehydrated alcohol and dimethylbenzene respectively 1.8g and 18g be configured to carbon source solution, in carbon source solution, add the ferrocene carbon source solution that 0.2g ferrocene is configured to massfraction 1%.By rate of expansion be 100 expanded graphite be positioned in tube furnace; pass into argon shield; heated Tube-furnace is warming up to 700 DEG C; inject above-mentioned ferrocene carbon source solution; the injection speed of described ferrocene carbon source solution controls at 10mL/h; growth time is 120min, and growth terminates rear stopping and injecting ferrocene carbon source solution, and under the protection of rare gas element, be cooled to room temperature taking-up.The expanded graphite of growth array carbon nano tube is placed in graphite jig, and be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate is 200 DEG C/h, hot pressing temperature is 1500 DEG C, hot pressing pressure is 5MPa, heat-insulation pressure keeping 0.5h, treats that temperature is down to 100 DEG C of releases and is taken out sample.Test sample through-thickness thermal conductivity is 25W/ (mK), is 95% by rebound degree after sample through-thickness compression 10%.
Embodiment 2
Choose dehydrated alcohol and each 9.5g of dimethylbenzene is configured to carbon source solution, in carbon source solution, add the ferrocene carbon source solution that 1g ferrocene is configured to massfraction 5%.By rate of expansion be 300 expanded graphite be positioned in tube furnace; pass into argon shield; heated Tube-furnace is warming up to 900 DEG C; inject above-mentioned ferrocene carbon source solution; the injection speed of described ferrocene carbon source solution controls at 30mL/h; growth time is 30min, and growth terminates rear stopping and injecting ferrocene carbon source solution, and under the protection of rare gas element, be cooled to room temperature taking-up.The expanded graphite of growth array carbon nano tube is placed in graphite jig, and be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate is 300 DEG C/h, hot pressing temperature is 2000 DEG C, hot pressing pressure is 40MPa, heat-insulation pressure keeping 1h, treats that temperature is down to 100 DEG C of releases and is taken out sample.Test sample through-thickness thermal conductivity is 35W/ (mK), is 98% by rebound degree after sample through-thickness compression 10%.
Embodiment 3
Choose dehydrated alcohol and each 9.6g of dimethylbenzene is configured to carbon source solution, in carbon source solution, add the ferrocene carbon source solution that 0.8g ferrocene is configured to massfraction 4%.By rate of expansion be 200 expanded graphite be positioned in tube furnace; pass into argon shield; heated Tube-furnace is warming up to 800 DEG C; inject above-mentioned ferrocene carbon source solution; the injection speed of described ferrocene carbon source solution controls at 20mL/h; growth time is 60min, and growth terminates rear stopping and injecting ferrocene carbon source solution, and under the protection of rare gas element, be cooled to room temperature taking-up.The expanded graphite of growth array carbon nano tube is placed in graphite jig, and be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate is 260 DEG C/h, hot pressing temperature is 1600 DEG C, hot pressing pressure is 30MPa, heat-insulation pressure keeping 0.6h, treats that temperature is down to 100 DEG C of releases and is taken out sample.Test sample through-thickness thermal conductivity is 27W/ (mK), is 90% by rebound degree after sample through-thickness compression 10%.
Embodiment 4
Choose dehydrated alcohol and dimethylbenzene respectively 18g and 1.8g be configured to carbon source solution, in carbon source solution, add the ferrocene carbon source solution that 0.2g ferrocene is configured to massfraction 1%.By rate of expansion be 100 expanded graphite be positioned in tube furnace; pass into argon shield; heated Tube-furnace is warming up to 750 DEG C; inject above-mentioned ferrocene carbon source solution; the injection speed of described ferrocene carbon source solution controls at 15mL/h; growth time is 50min, and growth terminates rear stopping and injecting ferrocene carbon source solution, and under the protection of rare gas element, be cooled to room temperature taking-up.The expanded graphite of growth array carbon nano tube is placed in graphite jig, and be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate is 200 DEG C/h, hot pressing temperature is 1800 DEG C, hot pressing pressure is 30MPa, heat-insulation pressure keeping 0.8h, treats that temperature is down to 100 DEG C of releases and is taken out sample.Test sample through-thickness thermal conductivity is 26W/ (mK), is 98% by rebound degree after sample through-thickness compression 10%.
Embodiment 5
Choose dehydrated alcohol and each 9.8g of dimethylbenzene is configured to carbon source solution, in carbon source solution, add the ferrocene carbon source solution that 0.4g ferrocene is configured to massfraction 2%.By rate of expansion be 200 expanded graphite be positioned in tube furnace; pass into argon shield; heated Tube-furnace is warming up to 750 DEG C; inject above-mentioned ferrocene carbon source solution; the injection speed of described ferrocene carbon source solution controls at 15mL/h; growth time is 60min, and growth terminates rear stopping and injecting ferrocene carbon source solution, and under the protection of rare gas element, be cooled to room temperature taking-up.The expanded graphite of growth array carbon nano tube is placed in graphite jig, and be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate is 280 DEG C/h, hot pressing temperature is 2000 DEG C, hot pressing pressure is 30MPa, heat-insulation pressure keeping 1h, treats that temperature is down to 100 DEG C of releases and is taken out sample.Test sample through-thickness thermal conductivity is 32W/ (mK), is 95% by rebound degree after sample through-thickness compression 10%.
Embodiment 6
Choose dehydrated alcohol and each 9.5g of dimethylbenzene is configured to carbon source solution, in carbon source solution, add the ferrocene carbon source solution that 1g ferrocene is configured to massfraction 5%.By rate of expansion be 100 expanded graphite be positioned in tube furnace; pass into argon shield; heated Tube-furnace is warming up to 700 DEG C; inject above-mentioned ferrocene carbon source solution; the injection speed of described ferrocene carbon source solution controls at 20mL/h; growth time is 60min, and growth terminates rear stopping and injecting ferrocene carbon source solution, and under the protection of rare gas element, be cooled to room temperature taking-up.The expanded graphite of growth array carbon nano tube is placed in graphite jig, and be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate is 200 DEG C/h, hot pressing temperature is 2000 DEG C, hot pressing pressure is 35MPa, heat-insulation pressure keeping 1h, treats that temperature is down to 100 DEG C of releases and is taken out sample.Test sample through-thickness thermal conductivity is 36W/ (mK), is 96% by rebound degree after sample through-thickness compression 10%.
The present invention's through-thickness that is open and that propose has the preparation method of snappiness and high thermal conductivity coefficient C-base composte material simultaneously, those skilled in the art are by using for reference present disclosure, the links such as appropriate change raw material and operational path realize, although method of the present invention and technology of preparing are described by preferred embodiment, person skilled obviously can change Method and Technology route as herein described or reconfigure not departing from content of the present invention, spirit and scope, realizes final technology of preparing.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are deemed to be included in spirit of the present invention, scope and content.
Claims (3)
1. a through-thickness has the C-base composte material of high resilience and high thermal conductivity coefficient; It is characterized in that, the graphite flake layer in expanded graphite is connected by array carbon nano tube, and the space between graphite flake layer is filled by array carbon nano tube; The hot Xi Shuo≤25W/ (mK) of through-thickness Dao; Resilience Shuai≤90% after compression 10%.
2. through-thickness has a preparation method for the C-base composte material of high resilience and high thermal conductivity coefficient, and step is as follows:
(1) by dehydrated alcohol and dimethylbenzene in mass ratio 0.1 ~ 10:1 be uniformly mixed and prepare carbon source solution, ferrocene is dissolved in above-mentioned carbon source solution, the ferrocene carbon source solution of configuration quality mark 1 ~ 5%;
(2) by rate of expansion be 100 ~ 300 expanded graphite be positioned in tube furnace, pass into argon shield, heated Tube-furnace is warming up to 700 ~ 900 DEG C, enters in tube furnace ferrocene carbon source injection of solution in order to grow array carbon nano tube on expanded graphite;
(3) expanded graphite of growth array carbon nano tube is placed in graphite jig, be placed in vacuum hotpressing stove and carry out high temperature hot pressing, heat-up rate controls at 200 ~ 300 DEG C/h, hot pressing temperature is 1500 ~ 2000 DEG C, hot pressing pressure is 5 ~ 40MPa, the heat-insulation pressure keeping time is 0.5 ~ 1h, treats that temperature is down to 100 DEG C of releases and is taken out sample.
3. method as claimed in claim 2, it is characterized in that in described step (2), the injection speed of ferrocene carbon source solution is 10 ~ 30mL/h, and growth time is 30 ~ 120min, and growth terminates under the protection of rare gas element, be cooled to room temperature and takes out.
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| CN106116580A (en) * | 2016-06-30 | 2016-11-16 | 东华大学 | A kind of flexible carbon film and preparation method thereof |
| CN106276859A (en) * | 2016-08-15 | 2017-01-04 | 天津大学 | A kind of preparation method of the CNT microsphere being coated with carbon film |
| CN108968703A (en) * | 2017-06-01 | 2018-12-11 | 佛山市顺德区美的电热电器制造有限公司 | Pot and cooking apparatus in ceramic inserts metal |
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| CN105439124A (en) * | 2015-12-17 | 2016-03-30 | 山西大同大学 | Method for growing nano carbon tube in pores of expanded graphite |
| CN105859291A (en) * | 2016-03-30 | 2016-08-17 | 天津大学 | Method for preparing three-dimensional high-thermal-conductivity carbon-based composite material |
| CN105859291B (en) * | 2016-03-30 | 2018-07-13 | 天津大学 | The preparation method of three-dimensional highly-conductive hot carbon based composites |
| CN106116580A (en) * | 2016-06-30 | 2016-11-16 | 东华大学 | A kind of flexible carbon film and preparation method thereof |
| CN106116580B (en) * | 2016-06-30 | 2018-07-17 | 东华大学 | A kind of flexibility carbon film and preparation method thereof |
| CN106276859A (en) * | 2016-08-15 | 2017-01-04 | 天津大学 | A kind of preparation method of the CNT microsphere being coated with carbon film |
| CN106276859B (en) * | 2016-08-15 | 2018-11-30 | 天津大学 | A kind of preparation method for the carbon nanotube microballoon being coated with carbon film |
| CN108968703A (en) * | 2017-06-01 | 2018-12-11 | 佛山市顺德区美的电热电器制造有限公司 | Pot and cooking apparatus in ceramic inserts metal |
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| CN110871270A (en) * | 2018-09-04 | 2020-03-10 | 天津大学 | Preparation method of high-elasticity high-heat-conductivity three-dimensional carbon nanotube composite material |
| WO2024001160A1 (en) * | 2022-12-23 | 2024-01-04 | 华北理工大学 | Expanded graphite/carbon nanotube composite material, and preparation method therefor and use thereof |
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