CN115028165A - Preparation method of low-sulfur, super-thick and high-thermal conductivity natural flexible graphite paper - Google Patents
Preparation method of low-sulfur, super-thick and high-thermal conductivity natural flexible graphite paper Download PDFInfo
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- CN115028165A CN115028165A CN202210845638.XA CN202210845638A CN115028165A CN 115028165 A CN115028165 A CN 115028165A CN 202210845638 A CN202210845638 A CN 202210845638A CN 115028165 A CN115028165 A CN 115028165A
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Abstract
The invention discloses a preparation method of natural flexible graphite paper with low sulfur, super-thickness and high heat conductivity, which takes natural flake graphite particles as intercalation host materials, perchloric acid as an intercalating agent and nitric acid as an oxidizing agent, and perchloric acid/graphite intercalation compounds are prepared after oxidation intercalation reaction; then, preparing an intermediate expanded graphite by puffing treatment; and finally, further rolling the expanded graphite to prepare the high-thermal-conductivity natural flexible graphite paper material. The invention avoids the defects of the S-containing graphite paper as the S-containing substance or raw material is not involved in the preparation process. The natural flexible graphite paper prepared by the method has controllable thickness (0.3-0.6mm), extremely low S content and higher heat conductivity coefficient than similar products reported at home and abroad at present.
Description
Technical Field
The invention relates to a preparation method of natural flexible graphite paper.
Background
The natural flexible graphite paper is a paper-like graphite coiled material or plate, which is prepared by using natural phosphorus flake graphite powder as a raw material and performing purification, acidification intercalation, puffing, calendaring or rolling, namely the natural flexible graphite paper. The natural flexible graphite paper has the advantages of good chemical stability, high and low temperature resistance, corrosion resistance, radiation resistance, good heat conductivity, strong electric conductivity, good flexibility, good compression resilience and the like, and is widely applied to the sealing fields of electronics, petroleum, chemical engineering, metallurgy and the like at present.
In recent years, based on the high thermal conductivity of graphite microcrystals, which are the basic structural units of natural flexible graphite paper, researchers at home and abroad begin to pay attention to the research and development of high thermal conductivity natural flexible graphite paper materials. The flexible graphite paper has excellent performances of high thermal conductivity, low density, low thermal expansion coefficient, good high-temperature stability and the like, and is a thin film heat dissipation material with development prospect in recent years. The traditional metal material is replaced on some heat dissipation devices, so that the miniaturization and high power density of electronic devices are facilitated, and the weight of the devices can be effectively reduced; meanwhile, the heat dissipation structure can be used for high-end electronic device equipment, and the purposes of high-efficiency heat dissipation, safe use and long service life are achieved. The factors influencing the thermal conductivity of the natural flexible graphite paper are more, and mainly comprise the particle size, purity, intercalation reagent, expansion factor, calendering orientation and density of graphite worms and the like. In order to obtain natural flexible graphite paper with high thermal conductivity, a great deal of research work is carried out by domestic and foreign researchers. Vovchenko et al (Thermal conversion expanded graphite and its composites. Inorganic materials.2007,43(6):597-601 (Thermal evaluation of expanded graphite and its composites)) use concentrated sulfuric acid as an oxidizing intercalant, expand at different temperatures to produce graphite worms, and then roll to produce highly thermally conductive graphite paper. Through systematic research on the internal relation between the graphite paper with different densities and the thermal conductivity, the fact that the thermal conductivity of the graphite paper in the C-axis direction has an inflection point along with the change of the bulk density is found, and when the bulk density is lower than 1.5g/cm 3 When the density increases, the thermal conductivity decreases; when the density is higher than 1.5g/cm 3 And then increases with increasing density. Yuhang Liu et al (NH while amorphous expanded graphics files with amorphous continuous content by interconnecting cells carbon,53(2019)565- 4 ) 2 S 2 O 8 And H 2 SO 4 Is used as an oxidation intercalation agent, is thermally treated at 800 ℃ to prepare graphite worms, and is pressed to obtain the flexible graphite paper with electric conductivity and thermal conductivity2977S/cm and 854W/m.K are respectively reached. However, the thickness of the obtained flexible graphite paper is thin (0.046-0.23 mm), so that the heat transfer flux of the flexible graphite paper is limited. The American GrafTech company carries out deep and wide application research on high-heat-conductivity natural flexible graphite paper, and the developed high-heat-conductivity flexible graphite paper is used in the fields of digital information display screens, liquid crystal display screens, plasma display panels, mobile phones, notebook computers, flow field plates and the like, and has obvious heat dissipation effect. The flexible graphite paper has the advantages of uniform heat distribution in two dimensions, elimination of local hot spots, and unique capability of reducing contact temperature in the third dimension, which is incomparable with common aluminum and copper isotropic materials. This advantage of combining thermal conductivity and shielding makes flexible graphite paper a desirable material choice in solving thermal management problems. At present, GrafTech company in America has prepared a series of high-heat-conductivity flexible graphite paper products, the heat conductivity coefficient of the graphite paper products reaches more than 600W/m.K at most, but the thickness of the graphite paper products is below 0.3mm, so that the heat transfer flux of the graphite paper products is limited; in addition, the material is prepared by using concentrated H 2 SO 4 The S-containing organic silicon-based organic silicon-.
Disclosure of Invention
The invention aims to provide a preparation method of natural flexible graphite paper with low sulfur content, super-thick property and excellent heat conductivity.
The technical solution of the invention is as follows:
a preparation method of natural flexible graphite paper with low sulfur, super-thickness and high heat conductivity is characterized by comprising the following steps: natural flake graphite particles are used as intercalation host materials, perchloric acid is used as an intercalation agent, nitric acid is used as an oxidant, and a perchloric acid/graphite intercalation compound is prepared after oxidation intercalation reaction; then, preparing an intermediate expanded graphite by puffing treatment; and finally, further rolling the expanded graphite to prepare the high-thermal-conductivity natural flexible graphite paper material.
The average particle size of the natural crystalline flake graphite particles is 30-80 meshes, and the carbon content is more than 99.95 wt.%.
The dosage of the natural crystalline flake graphite particles, the perchloric acid and the nitric acid is respectively 28-40 wt%, 55-70 wt% and 1-6 wt% of the nitric acid.
The preparation method of the natural flexible graphite paper with low sulfur, super-thickness and high heat conductivity comprises the following specific steps:
(1) perchloric acid (HClO) in a proportion of 55 to 70wt.% 4 ) With 1-6 wt% nitric acid (HNO) 3 ) Adding HClO 4 With HNO 3 Mixing, adding 28-40 wt% of natural crystalline flake graphite particles, and stirring for 2-10 min to obtain a mixture;
(2) heating the mixture obtained in the step (1) to 20-120 ℃, and reacting for 10-40 min to obtain perchloric acid/graphite intercalation compound (HClO) 4 -GIC)；
(3) Washing the perchloric acid/graphite intercalation compound obtained in the step (2) with deionized water until the pH value is 5.5-7.0, and then drying the perchloric acid/graphite intercalation compound at 85-110 ℃ for 2-5 h to obtain a dried perchloric acid/graphite intercalation compound;
(4) performing expansion treatment on the dried perchloric acid/graphite intercalation compound obtained in the step (3), wherein the expansion temperature is 800-1000 ℃, the expansion time is 5-10 s, and cooling to room temperature after expansion to obtain expandable graphite;
(5) and (4) placing the expandable graphite obtained in the step (4) into a calender, and performing rolling treatment under the condition that the linear pressure is 60-90 MPa to obtain the high-thermal-conductivity natural graphite paper.
The concentration of the nitric acid is 60-70 wt.%; the concentration of perchloric acid is 70-75% by weight.
The invention provides a preparation method of low-sulfur-content high-heat-conductivity graphite paper. Concentrated H is used in the production process of general flexible graphite paper 2 SO 4 For the intercalating agent, SO is generated during the manufacturing process X Gas, which is harmful to human body and environment; in addition, S remains in the product, which will cause acidification corrosion of the contact parts in application. Meanwhile, the S-containing flexible graphite has poor high-temperature oxidation resistance and low tensile strength. The low-sulfur high-heat-conductivity graphite paper does not relate to S-containing substances or raw materials in the preparation process, so that the final materialThe material avoids the defects of the S-containing graphite paper.
The natural flexible graphite paper prepared by the method has controllable thickness (0.3-0.6mm), extremely low S content and higher heat conductivity coefficient than similar products reported at home and abroad at present.
The present invention will be further described with reference to the following examples.
Detailed Description
Example 1
Introducing HClO 4 ：HNO 3 : the natural crystalline flake graphite powder is prepared from the following components in parts by weight: 5.2: 30.8, mixing. In the mixing process, HClO is firstly mixed 4 Pouring with HNO 3 Then adding the natural crystalline flake graphite into the mixed acid, and stirring for 10 min. The natural flake graphite as described above had an average particle size of 32 mesh, a carbon content of 99.95wt.%, a nitric acid concentration of 65 wt.% and a perchloric acid concentration of 70 wt.%. The stirred mixture was heated to 40 ℃ and reacted at that temperature for 12min to obtain a perchloric acid/graphite intercalation compound. The resulting perchloric acid/graphite intercalation compound is then washed with deionized water to a pH of 5.8. And (3) putting the washings into a drying furnace, heating to 100 ℃ and drying for 4 h. And after drying, discharging from the furnace, naturally cooling to room temperature, then placing the dried material into a high-temperature puffing furnace at 950 ℃ for puffing, wherein the puffing time is 6s, and discharging from the furnace, cooling to room temperature to obtain the expandable graphite. And (3) putting the prepared expandable graphite into a calender for rolling treatment. The line pressure in the rolling process is 80MPa, the thickness of the final graphite paper is 0.38mm, and the volume density is 1.64g/cm 3 The basic physical properties are shown in Table 1.
Example 2
Adding HClO 4 、HNO 3 And natural crystalline flake graphite according to a weight ratio of 66: 5: 29 are mixed. In the mixing process, HClO is first mixed 4 Pouring with HNO 3 Then adding the natural crystalline flake graphite into the mixed acid, and stirring for 7 min. The natural flake graphite as described above had an average particle size of 40 mesh, a carbon content of 99.98 wt.%, a nitric acid concentration of 66 wt.% and a perchloric acid concentration of 71 wt.%. After stirring the mixtureThe mixture was heated to 75 ℃ and reacted at this temperature for 20min to give a perchloric acid/graphite intercalation compound. The resulting perchloric acid/graphite intercalation compound is then washed with deionized water to a pH of 6.0. And (3) putting the washed object into a drying furnace, heating to 105 ℃ for drying treatment, wherein the drying time is 3.5 h. And after drying, discharging from the furnace, naturally cooling to room temperature, then placing the dried material into a high-temperature expansion furnace at 940 ℃ for expansion, wherein the expansion time is 5s, and discharging from the furnace, cooling to room temperature to obtain the expandable graphite. And (3) putting the prepared expandable graphite into a calender for rolling treatment. The line pressure in the rolling process is 75MPa, the thickness of the final flexible graphite paper is 0.45mm, and the bulk density is 1.71g/cm 3 The basic physical properties are shown in Table 1.
Example 3
Introducing HClO 4 、HNO 3 And natural crystalline flake graphite in a weight ratio of 68: 2: 30 are mixed. In the mixing process, HClO is firstly mixed 4 Pouring with HNO 3 Then adding the natural crystalline flake graphite into the mixed acid and stirring for 3 min. The natural flake graphite as described above had an average particle size of 60 mesh, a carbon content of 99.92 wt.%, a nitric acid concentration of 67 wt.% and a perchloric acid concentration of 70 wt.%. The stirred mixture was heated to 70 ℃ and reacted at that temperature for 30min to obtain a perchloric acid/graphite intercalation compound. The resulting perchloric acid/graphite intercalation compound is then washed with deionized water to a pH of 6.5. And (3) putting the washings into a drying furnace, heating to 95 ℃ for drying treatment, wherein the drying time is 2.5 h. And (4) after drying, discharging from the furnace, naturally cooling to room temperature, then placing the dried material into a high-temperature expansion furnace at 880 ℃ for expansion, wherein the expansion time is 8s, and discharging from the furnace, cooling to room temperature to obtain the expandable graphite. And (3) putting the prepared expandable graphite into a calender for rolling treatment. The line pressure in the rolling process is 72MPa, the thickness of the final flexible graphite paper is 0.55mm, and the bulk density is 1.68g/cm 3 The basic physical properties are shown in Table 1.
Example 4
Introducing HClO 4 、HNO 3 And natural crystalline flake graphite according to a weight ratio of 64: 1: 35 are mixed. In the mixing process, HClO is firstly mixed 4 Pouring HNO into the container 3 Then adding the natural crystalline flake graphite into the mixed acid, and stirring for 4.5 min. Natural flake graphite as described above having an average particle size of 32 mesh and a carbon content of 99.98 wt.%; the concentration of nitric acid used was 67 wt.%, and the concentration of perchloric acid was 70 wt.%. The stirred mixture was heated to 40 ℃ and reacted at that temperature for 35min to obtain a perchloric acid/graphite intercalation compound. The resulting perchloric acid/graphite intercalation compound is then washed with deionized water to a pH of 6.8. And (3) putting the washings into a drying furnace, heating to 85 ℃ and drying for 4 h. And after drying, discharging from the furnace, naturally cooling to room temperature, then placing the dried material into a high-temperature puffing furnace at 1000 ℃ for puffing for 4s, and discharging from the furnace, cooling to room temperature to obtain the expandable graphite. And (3) putting the prepared expandable graphite into a calender for rolling treatment. The line pressure in the rolling process is 75MPa, the thickness of the final flexible graphite paper is 0.58mm, and the bulk density is 1.72g/cm 3 The basic physical properties are shown in Table 1.
Example 5
Introducing HClO 4 、HNO 3 And natural crystalline flake graphite in a weight ratio of 55: 5: 40 are mixed. In the mixing process, HClO is firstly mixed 4 Pouring with HNO 3 Then adding the natural crystalline flake graphite into the mixed acid, and stirring for 10 min. The natural flake graphite as described above had an average particle size of 80 mesh, a carbon content of 99.95wt.%, a nitric acid concentration of 68 wt.% and a perchloric acid concentration of 74 wt.%. The stirred mixture was heated to 55 ℃ and reacted at that temperature for 50min to obtain a perchloric acid/graphite intercalation compound. The resulting perchloric acid/graphite intercalation compound is then washed with deionized water to a pH of 6.9. And (3) putting the washings into a drying furnace, heating to 98 ℃ and drying for 3 h. And after drying, discharging from the furnace, naturally cooling to room temperature, then placing the dried material into a high-temperature puffing furnace at 1000 ℃ for puffing for 3s, and discharging from the furnace, cooling to room temperature to obtain the expandable graphite. And (3) putting the prepared expandable graphite into a calender for rolling treatment. The line pressure in the rolling process is 85MPa, the thickness of the final flexible graphite paper is 0.59mm, and the thickness of the final flexible graphite paper is larger than that of the final flexible graphite paperThe bulk density is 1.73g/cm 3 The basic physical properties are shown in Table 1.
Example 6
Introducing HClO 4 、HNO 3 And natural crystalline flake graphite in a weight ratio of 62.5: 2.5: 35 are mixed. In the mixing process, HClO is firstly mixed 4 Pouring with HNO 3 Then adding the natural crystalline flake graphite into the mixed acid, and stirring for 2 min. The natural flake graphite as described above had an average particle size of 80 mesh, a carbon content of 99.99 wt.%, a nitric acid concentration of 67 wt.% and a perchloric acid concentration of 70 wt.%. The stirred mixture was heated to 60 ℃ and reacted at that temperature for 60min to obtain a perchloric acid/graphite intercalation compound. The resulting perchloric acid/graphite intercalation compound is then washed with deionized water to a pH of 6.3. And (3) putting the washings into a drying furnace, heating to 85 ℃ and drying for 4 h. And after drying, discharging from the furnace, naturally cooling to room temperature, then placing the dried material into a high-temperature expansion furnace at 900 ℃ for expansion, wherein the expansion time is 4s, and discharging from the furnace, cooling to room temperature to obtain the expandable graphite. And (3) putting the prepared expandable graphite into a calender for rolling treatment. The line pressure in the rolling process is 40MPa, the thickness of the final flexible graphite paper is 0.53mm, and the bulk density is 1.73g/cm 3 The basic physical properties are shown in Table 1.
The basic physical properties of the natural flexible graphite paper material produced in the above examples are shown in table 1.
TABLE 1 basic physical Properties of Natural Flexible graphite paper Material
Remarking: at first: parallel to the direction of the graphite layer; and T: perpendicular to the direction of the graphite layers.
Claims (5)
1. A preparation method of natural flexible graphite paper with low sulfur, super-thickness and high heat conductivity is characterized by comprising the following steps: natural flake graphite particles are used as intercalation host materials, perchloric acid is used as an intercalation agent, nitric acid is used as an oxidant, and a perchloric acid/graphite intercalation compound is prepared after oxidation intercalation reaction; then, preparing an intermediate expanded graphite by puffing treatment; and finally, further rolling the expanded graphite to prepare the high-thermal-conductivity natural flexible graphite paper material.
2. The method for preparing the low-sulfur, ultra-thick and high-thermal conductivity natural flexible graphite paper according to claim 1, characterized in that: the average particle size of the natural crystalline flake graphite particles is 30-80 meshes, and the carbon content is more than 99.95 wt.%.
3. The method for preparing low-sulfur, ultra-thick and high-thermal conductivity natural flexible graphite paper according to claim 1 or 2, characterized in that: the dosage of the natural crystalline flake graphite particles, the perchloric acid and the nitric acid is respectively 28-40 wt%, 55-70 wt% and 1-6 wt% of the nitric acid.
4. The method for preparing the low-sulfur, ultra-thick and high-thermal conductivity natural flexible graphite paper according to claim 3, characterized in that: the method comprises the following specific steps:
(1) mixing 55-70 wt% perchloric acid and 1-6 wt% nitric acid to obtain HClO 4 With HNO 3 Mixing, adding 28-40 wt% of natural crystalline flake graphite particles, and stirring for 2-10 min to obtain a mixture;
(2) heating the mixture obtained in the step (1) to 20-120 ℃, and reacting for 10-40 min to obtain a perchloric acid/graphite interlayer compound;
(3) washing the perchloric acid/graphite intercalation compound obtained in the step (2) with deionized water until the pH value is 5.5-7.0, and then drying the perchloric acid/graphite intercalation compound at 85-110 ℃ for 2-5 h to obtain a dry perchloric acid/graphite intercalation compound;
(4) carrying out expansion treatment on the dried perchloric acid/graphite interlayer compound obtained in the step (3), wherein the expansion temperature is 800-1000 ℃, the expansion time is 5-10 s, and cooling to room temperature after expansion to obtain expandable graphite;
(5) and (4) placing the expandable graphite obtained in the step (4) into a calender, and performing rolling treatment under the condition that the linear pressure is 60-90 MPa to obtain the high-thermal-conductivity natural graphite paper.
5. The method for preparing the low-sulfur, ultra-thick and high-thermal conductivity natural flexible graphite paper according to claim 4, wherein the method comprises the following steps: the concentration of nitric acid is 60-70 wt.%; the concentration of perchloric acid is 70-75% by weight.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116534854A (en) * | 2023-04-25 | 2023-08-04 | 广东思泉新材料股份有限公司 | Expanded foaming graphite film, preparation method thereof and application thereof in semiconductor heat dissipation device |
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| CN1453209A (en) * | 2003-04-30 | 2003-11-05 | 中国科学院山西煤炭化学研究所 | Prepn of sulfur-free low-ash high-purity expanded graphite |
| CN103539111A (en) * | 2013-11-05 | 2014-01-29 | 中国科学院山西煤炭化学研究所 | Preparation method of high thermal conductivity natural flexible graphite film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1453209A (en) * | 2003-04-30 | 2003-11-05 | 中国科学院山西煤炭化学研究所 | Prepn of sulfur-free low-ash high-purity expanded graphite |
| CN103539111A (en) * | 2013-11-05 | 2014-01-29 | 中国科学院山西煤炭化学研究所 | Preparation method of high thermal conductivity natural flexible graphite film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116534854A (en) * | 2023-04-25 | 2023-08-04 | 广东思泉新材料股份有限公司 | Expanded foaming graphite film, preparation method thereof and application thereof in semiconductor heat dissipation device |
| CN116534854B (en) * | 2023-04-25 | 2024-05-10 | 广东思泉新材料股份有限公司 | Expanded foaming graphite film, preparation method thereof and application thereof in semiconductor heat dissipation device |
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