CN110453100A - A method for preparing graphite/copper composite material by intercalation in situ - Google Patents
A method for preparing graphite/copper composite material by intercalation in situ Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 104
- 239000010439 graphite Substances 0.000 title claims abstract description 104
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 39
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 36
- 239000010949 copper Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000009830 intercalation Methods 0.000 title claims description 45
- 230000002687 intercalation Effects 0.000 title claims description 45
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000007800 oxidant agent Substances 0.000 claims abstract description 7
- 238000007731 hot pressing Methods 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 45
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000012286 potassium permanganate Substances 0.000 claims description 15
- 230000001007 puffing effect Effects 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005204 segregation Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000138 intercalating agent Substances 0.000 abstract 1
- 238000005452 bending Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- C01B32/22—Intercalation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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Abstract
Description
技术领域technical field
本发明属于金属-石墨复合材料制备技术领域，具体涉及一种原位插层制备石墨/铜复合材料的方法。The invention belongs to the technical field of metal-graphite composite material preparation, and in particular relates to a method for preparing graphite/copper composite material by in-situ intercalation.
背景技术Background technique
近年来，由于石墨/金属基复合材料有众多优良的性能，它既有金属的高导电、高强度、良好延展性，同时具备石墨良好的润滑性能、减震性、耐腐蚀性、热稳定性和比重低等特性，广泛应用于航空航天、舰船、高铁和汽车工业领域，尤其是电剁、电机、电刷、自润滑轴承和受电弓等电工部件。In recent years, due to the many excellent properties of graphite/metal matrix composites, it not only has the high conductivity, high strength, and good ductility of metals, but also has the good lubricating properties, shock absorption, corrosion resistance, and thermal stability of graphite. It is widely used in the fields of aerospace, shipbuilding, high-speed rail and automobile industry, especially for electrical components such as electric chopping machines, motors, brushes, self-lubricating bearings and pantographs.
但在传统工艺中，因材料密度差别大（铜8.8×103kg/m3 ，石墨2.25×103kg/m3）且石墨粉凝聚性强、分散性差，机械混合粉末不均匀，易产生偏析，同时碳与铜界面只能通过机械互锁链接在一起，界面之间结合强度低，造成产品质量不稳定。高温浸渗法中的石墨与铜即使在1100℃ 时其润湿角也高达140℃，石墨很难在铜溶体中成均匀悬浮状分布，也易产生偏析。金属在材料内不能形成连续的三维网络，很难保持烧结体的强度和稳定性。However, in the traditional process, due to the large difference in material density (copper 8.8×103kg/m 3 , graphite 2.25×103kg/m 3 ), graphite powder has strong agglomeration and poor dispersion, mechanically mixed powder is uneven, and segregation is easy to occur. The copper interface can only be linked together through mechanical interlocking, and the bonding strength between the interfaces is low, resulting in unstable product quality. The wetting angle of graphite and copper in the high-temperature infiltration method is as high as 140°C even at 1100°C. It is difficult for graphite to distribute uniformly in suspension in the copper solution, and it is also prone to segregation. The metal cannot form a continuous three-dimensional network in the material, and it is difficult to maintain the strength and stability of the sintered body.
发明内容Contents of the invention
为了克服现有技术中的不足，解决石墨在铜溶体中易偏析、石墨与铜烧结体的强度和稳定性差的技术问题，一种原位插层制备石墨/铜复合材料的方法。In order to overcome the deficiencies in the prior art and solve the technical problems of easy segregation of graphite in copper solution and poor strength and stability of graphite and copper sintered body, a method for preparing graphite/copper composite material by in-situ intercalation is provided.
本发明的设计思路为：本发明采用天然鳞片石墨为原料，在其中加入氧化剂和插层剂制备可膨胀石墨；将可膨胀石墨和铜粉在v型混料机中充分混匀；再将混匀后的物料放入真空热压炉中原位插层膨胀；最后将原位插层后的物料放入真空热压炉中热压烧结，制得具有三维网络结构且分散均匀的高性能石墨/铜复合材料。The design concept of the present invention is as follows: the present invention uses natural flake graphite as raw material, adds oxidant and intercalation agent to prepare expandable graphite; fully mixes expandable graphite and copper powder in a v-type mixer; then mixes The homogenized material is put into a vacuum hot-pressed furnace for in-situ intercalation expansion; finally, the in-situ intercalated material is put into a vacuum hot-pressed furnace for hot-pressing and sintering to obtain a high-performance graphite with a three-dimensional network structure and uniform dispersion. copper composite.
本发明通过以下技术方案予以实现。The present invention is achieved through the following technical solutions.
一种原位插层制备石墨/铜复合材料的方法，包括以下步骤：A method for preparing graphite/copper composite material by intercalation in situ, comprising the following steps:
S1、将天然鳞片石墨与高锰酸钾粉末混合，然后向混合物料中加入高氯酸和乙酸，采用高锰酸钾做氧化剂，高氯酸和乙酸做插层剂，持续搅拌反应物，进行氧化插层反应，其中反应温度为20~30℃，反应时间为60~90 min，充分反应后制得可膨胀石墨原料；S1. Mix natural flake graphite with potassium permanganate powder, then add perchloric acid and acetic acid to the mixed material, use potassium permanganate as oxidant, perchloric acid and acetic acid as intercalation agent, keep stirring the reactants, and carry out Oxidative intercalation reaction, wherein the reaction temperature is 20-30°C, the reaction time is 60-90 min, and the expandable graphite raw material is obtained after sufficient reaction;
S2、将步骤S1制得的可膨胀石墨原料水洗，直至滤液的pH值为5~7，可膨胀石墨原料抽滤脱水后，在45~60 ℃的条件下烘干，制得可膨胀石墨；S2. Washing the expandable graphite raw material prepared in step S1 until the pH value of the filtrate is 5-7, and drying the expandable graphite raw material at 45-60° C. to obtain expandable graphite after suction filtration and dehydration;
S3、将步骤S2制得的可膨胀石墨与铜粉在v型混料机中充分混合，混合时间为6~20 h；S3, fully mixing the expandable graphite and copper powder prepared in step S2 in a v-type mixer, the mixing time is 6 ~ 20 h;
S4、将步骤S3混合后的物料放入石墨磨具中，然后放置在真空烧结炉中，先进行原位插层膨化处理，温度为250℃~800℃，真空度为10~100 Pa，压力为0.1~1MPa，当压力不再发生变化，即原位插层膨化完全后，真空烧结炉继续升温， 再进行真空热压烧结，温度为850℃~1050℃，真空度为10~100 Pa，压力为20~40MPa，制得石墨/铜复合材料。S4. Put the mixed material in step S3 into a graphite abrasive tool, and then place it in a vacuum sintering furnace for in-situ intercalation puffing treatment. The temperature is 250°C~800°C, the vacuum degree is 10~100 Pa, and the pressure 0.1~1MPa, when the pressure no longer changes, that is, after the in-situ intercalation puffing is complete, the vacuum sintering furnace continues to heat up, and then vacuum hot pressing sintering is carried out, the temperature is 850°C~1050°C, and the vacuum degree is 10~100 Pa. The pressure is 20~40MPa, and the graphite/copper composite material is prepared.
进一步地，所述天然鳞片石墨的粒度为32目，含碳量为99%。Further, the particle size of the natural flake graphite is 32 mesh, and the carbon content is 99%.
进一步地，在所述步骤S1中，制备可膨胀石墨原料所采用的原料组成及其质量百分比为：天然鳞片石墨：高锰酸钾：高氯酸：乙酸=1:0.4~0.8:1~5:0.5~2。Further, in the step S1, the composition and mass percentage of the raw materials used to prepare the expandable graphite raw materials are: natural flake graphite: potassium permanganate: perchloric acid: acetic acid=1:0.4~0.8:1~5 :0.5~2.
进一步地，在所述步骤S2中，可膨胀石墨与铜粉的质量比为10~50%。Further, in the step S2, the mass ratio of expandable graphite to copper powder is 10-50%.
本发明与现有技术相比具有以下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明提供的一种原位插层制备石墨/铜复合材料的方法，能将铜粉均匀插入石墨层间，不仅解决由于铜和石墨比重相差过大所造成的偏析问题，而且促进复合材料分散均匀性，从而提升复合材料的综合性能。The present invention provides a method for preparing graphite/copper composite materials by intercalation in situ, which can evenly insert copper powder between graphite layers, which not only solves the segregation problem caused by the large difference in specific gravity between copper and graphite, but also promotes the dispersion of composite materials. Uniformity, thereby improving the comprehensive performance of composite materials.
总体上说，在石墨含量相同的条件下，和未经过原位插层处理制备的石墨/铜复合材料的性能相比，抗弯强度提升20~50%，抗压强度提升15~40%，导电性能提升20~40%。Generally speaking, under the condition of the same graphite content, compared with the performance of graphite/copper composites prepared without in-situ intercalation treatment, the flexural strength is increased by 20-50%, and the compressive strength is increased by 15-40%. Conductivity improved by 20~40%.
具体实施方式Detailed ways
为详细说明本发明的技术方案、结构特征、所实现的技术效果，以下结合具体实施方式详予说明。下列实施例仅用于说明本发明，而不应视为限制本发明的范围。 实施例1In order to describe in detail the technical solution, structural features, and achieved technical effects of the present invention, it will be described in detail below in conjunction with specific embodiments. The following examples are only for illustrating the present invention and should not be considered as limiting the scope of the present invention. Example 1
一种原位插层制备石墨/铜复合材料的方法，包括以下步骤：A method for preparing graphite/copper composite material by intercalation in situ, comprising the following steps:
S1、将天然鳞片石墨与高锰酸钾粉末混合，天然鳞片石墨的粒度为32目，含碳量为99%，然后向混合物料中加入高氯酸和乙酸，所采用的原料的质量百分比为：天然鳞片石墨：高锰酸钾：高氯酸：乙酸=1:0.4:1.5:0.5；采用高锰酸钾做氧化剂，高氯酸和乙酸做插层剂，持续搅拌反应物，进行氧化插层反应，其中反应温度为20℃，反应时间为60min，充分反应后制得可膨胀石墨原料；S1, natural flake graphite is mixed with potassium permanganate powder, and the particle size of natural flake graphite is 32 orders, and carbon content is 99%, then in mixed material, add perchloric acid and acetic acid, the mass percent of the raw material that adopts is : Natural flake graphite: Potassium permanganate: Perchloric acid: Acetic acid = 1:0.4:1.5:0.5; Potassium permanganate is used as the oxidant, perchloric acid and acetic acid are used as the intercalation agent, and the reactants are continuously stirred for oxidation intercalation Layer reaction, wherein the reaction temperature is 20°C, the reaction time is 60min, and the expandable graphite raw material is obtained after sufficient reaction;
S2、将步骤S1制得的可膨胀石墨原料水洗，直至滤液的pH值为5.5，可膨胀石墨原料抽滤脱水后，在45~60 ℃的条件下烘干，制得可膨胀石墨；S2. Washing the expandable graphite raw material prepared in step S1 until the pH value of the filtrate is 5.5, and drying the expandable graphite raw material at 45-60° C. to obtain expandable graphite after suction filtration and dehydration;
S3、将步骤S2制得的可膨胀石墨与铜粉在v型混料机中充分混合，可膨胀石墨与铜粉的质量比为10%，混合时间为8h；S3, fully mix the expandable graphite and copper powder prepared in step S2 in a v-type mixer, the mass ratio of expandable graphite and copper powder is 10%, and the mixing time is 8h;
S4、将步骤S3混合后的物料放入石墨磨具中，然后放置在真空烧结炉中进行原位插层膨化处理，温度为300℃，真空度为30 Pa，压力为0.2MPa；当压力不再发生变化，即膨化完全后，继续升温， 再进行真空热压烧结，温度为1000℃，真空度为30 Pa，压力为40MPa，制得石墨/铜复合材料。S4. Put the mixed material in step S3 into a graphite abrasive, and then place it in a vacuum sintering furnace for in-situ intercalation puffing treatment. The temperature is 300°C, the vacuum degree is 30 Pa, and the pressure is 0.2 MPa; when the pressure is not Then change, that is, after the puffing is complete, continue to heat up, and then carry out vacuum hot-press sintering at a temperature of 1000°C, a vacuum degree of 30 Pa, and a pressure of 40 MPa to obtain a graphite/copper composite material.
本实施例1制得的石墨/铜复合材料的抗弯强度为143MPa，抗压强度为138MPa，电导率为54%IACS。The bending strength of the graphite/copper composite material prepared in Example 1 is 143 MPa, the compressive strength is 138 MPa, and the electrical conductivity is 54% IACS.
鳞片石墨不经步骤S1、S2和S4原位插层膨化处理，其它步骤同上述内容：未原位插层膨化的石墨/铜复合材料的抗弯强度为105 MPa，抗压强度为108 MPa，电导率为43%IACS。经原位插层膨化制备的石墨/铜复合材料比未原位插层膨化的石墨/铜复合材料的抗弯强度、抗压强度和电导率分别提高了36.2%，27.8%和25.6%。The flake graphite is not processed by in-situ intercalation and expansion in steps S1, S2 and S4, and other steps are the same as above: the flexural strength of the graphite/copper composite material that is not in-situ intercalation and expansion is 105 MPa, and the compressive strength is 108 MPa. The conductivity is 43% IACS. The flexural strength, compressive strength and electrical conductivity of graphite/copper composites prepared by in-situ intercalation and expansion increased by 36.2%, 27.8% and 25.6%, respectively, compared with those without in-situ intercalation and expansion.
实施例2Example 2
一种原位插层制备石墨/铜复合材料的方法，包括以下步骤：A method for preparing graphite/copper composite material by intercalation in situ, comprising the following steps:
S1、将天然鳞片石墨与高锰酸钾粉末混合，天然鳞片石墨的粒度为32目，含碳量为99%，然后向混合物料中加入高氯酸和乙酸，所采用的原料的质量百分比为：天然鳞片石墨：高锰酸钾：高氯酸：乙酸=1:0.6:3:1.2；采用高锰酸钾做氧化剂，高氯酸和乙酸做插层剂，持续搅拌反应物，进行氧化插层反应，其中反应温度为25℃，反应时间为70min，充分反应后制得可膨胀石墨原料；S1, natural flake graphite is mixed with potassium permanganate powder, and the particle size of natural flake graphite is 32 orders, and carbon content is 99%, then in mixed material, add perchloric acid and acetic acid, the mass percent of the raw material that adopts is : Natural flake graphite: Potassium permanganate: Perchloric acid: Acetic acid = 1:0.6:3:1.2; Potassium permanganate is used as the oxidant, perchloric acid and acetic acid are used as the intercalation agent, and the reactant is continuously stirred for oxidation intercalation Layer reaction, wherein the reaction temperature is 25°C, the reaction time is 70min, and the expandable graphite raw material is obtained after sufficient reaction;
S2、将步骤S1制得的可膨胀石墨原料水洗，直至滤液的pH值为6，可膨胀石墨原料抽滤脱水后，在50 ℃的条件下烘干，制得可膨胀石墨；S2. Washing the expandable graphite raw material prepared in step S1 until the pH value of the filtrate is 6, and drying the expandable graphite raw material at 50° C. to obtain expandable graphite after suction filtration and dehydration;
S3、将步骤S2制得的可膨胀石墨与铜粉在v型混料机中充分混合，可膨胀石墨与铜粉的质量比为30%，混合时间为12h；S3, fully mix the expandable graphite and copper powder prepared in step S2 in a v-type mixer, the mass ratio of expandable graphite and copper powder is 30%, and the mixing time is 12h;
S4、将步骤S3混合后的物料放入石墨磨具中，然后放置在真空烧结炉中进行原位插层膨化处理，真空度为50 Pa，压力为0.5MPa；S4. Put the mixed material in step S3 into a graphite abrasive tool, and then place it in a vacuum sintering furnace for in-situ intercalation puffing treatment, with a vacuum degree of 50 Pa and a pressure of 0.5 MPa;
S5、将步骤S4原位插层膨化后的物料放入石墨磨具中再进行真空热压烧结，真空度为50 Pa，压力为30MPa，制得石墨/铜复合材料。S5. Put the in-situ intercalated and puffed material in step S4 into a graphite abrasive tool, and then perform vacuum hot-press sintering at a vacuum degree of 50 Pa and a pressure of 30 MPa to obtain a graphite/copper composite material.
S4、将步骤S3混合后的物料放入石墨磨具中，然后放置在真空烧结炉中进行原位插层膨化处理，温度为450℃，真空度为50 Pa，压力为0.5MPa；当压力不再发生变化，即膨化完全后，继续升温， 再进行真空热压烧结，温度为950℃，真空度为50 Pa，压力为30MPa，制得石墨/铜复合材料。S4. Put the mixed material in step S3 into a graphite abrasive tool, and then place it in a vacuum sintering furnace for in-situ intercalation puffing treatment. The temperature is 450°C, the vacuum degree is 50 Pa, and the pressure is 0.5 MPa; when the pressure is not Then change, that is, after the puffing is complete, continue to heat up, and then carry out vacuum hot-press sintering at a temperature of 950°C, a vacuum of 50 Pa, and a pressure of 30 MPa to obtain a graphite/copper composite material.
本实施例2制得的石墨/铜复合材料的抗弯强度为45.2 MPa，抗压强度为42.9MPa，电导率为25.9%IACS。The bending strength of the graphite/copper composite material prepared in Example 2 is 45.2 MPa, the compressive strength is 42.9 MPa, and the electrical conductivity is 25.9%IACS.
鳞片石墨不经步骤S1、S2和S4原位插层膨化处理，其它步骤同上述内容：未原位插层膨化的石墨/铜复合材料的抗弯强度33.5MPa，抗压强度32.4MPa，电导率为21.1%IACS。经原位插层膨化制备的石墨/铜复合材料比未原位插层膨化的石墨/铜复合材料的抗弯强度、抗压强度和电导率分别提高了34.9%，32.4%和22.7%。The flake graphite is not processed by in-situ intercalation and expansion in steps S1, S2 and S4, and other steps are the same as above: the flexural strength of graphite/copper composite material without in-situ intercalation and expansion is 33.5MPa, the compressive strength is 32.4MPa, and the electrical conductivity It is 21.1% IACS. The flexural strength, compressive strength and electrical conductivity of graphite/copper composites prepared by in-situ intercalation and expansion increased by 34.9%, 32.4% and 22.7%, respectively, compared with those without in-situ intercalation and expansion.
实施例3Example 3
一种原位插层制备石墨/铜复合材料的方法，包括以下步骤：A method for preparing graphite/copper composite material by intercalation in situ, comprising the following steps:
S1、将天然鳞片石墨与高锰酸钾粉末混合，天然鳞片石墨的粒度为32目，含碳量为99%，然后向混合物料中加入高氯酸和乙酸，所采用的原料的质量百分比为：天然鳞片石墨：高锰酸钾：高氯酸：乙酸=1:0.8:4:2；采用高锰酸钾做氧化剂，高氯酸和乙酸做插层剂，持续搅拌反应物，进行氧化插层反应，其中反应温度为30℃，反应时间为80min，充分反应后制得可膨胀石墨原料；S1, natural flake graphite is mixed with potassium permanganate powder, and the particle size of natural flake graphite is 32 orders, and carbon content is 99%, then in mixed material, add perchloric acid and acetic acid, the mass percent of the raw material that adopts is : Natural flake graphite: Potassium permanganate: Perchloric acid: Acetic acid = 1:0.8:4:2; Potassium permanganate is used as the oxidant, perchloric acid and acetic acid are used as the intercalation agent, and the reactant is continuously stirred for oxidation intercalation Layer reaction, wherein the reaction temperature is 30°C, the reaction time is 80min, and the expandable graphite raw material is obtained after sufficient reaction;
S2、将步骤S1制得的可膨胀石墨原料水洗，直至滤液的pH值为6.5，可膨胀石墨原料抽滤脱水后，在55℃的条件下烘干，制得可膨胀石墨；S2. Wash the expandable graphite raw material prepared in step S1 until the pH value of the filtrate is 6.5, and then dry the expandable graphite raw material at 55° C. to obtain expandable graphite after suction filtration and dehydration;
S3、将步骤S2制得的可膨胀石墨与铜粉在v型混料机中充分混合，可膨胀石墨与铜粉的质量比为50%，混合时间为16h；S3, fully mix the expandable graphite and copper powder prepared in step S2 in a v-type mixer, the mass ratio of expandable graphite and copper powder is 50%, and the mixing time is 16h;
S4、将步骤S3混合后的物料放入石墨磨具中，然后放置在真空烧结炉中进行原位插层膨化处理，温度为600℃，真空度为80 Pa，压力为0.8MPa；当压力不再发生变化，即膨化完全后，继续升温， 再进行真空热压烧结，温度为900℃，真空度为80 Pa，压力为20MPa，制得石墨/铜复合材料。S4. Put the mixed material in step S3 into a graphite abrasive, and then place it in a vacuum sintering furnace for in-situ intercalation puffing treatment. The temperature is 600°C, the vacuum degree is 80 Pa, and the pressure is 0.8 MPa; when the pressure is not Then change, that is, after the puffing is complete, continue to raise the temperature, and then carry out vacuum hot-press sintering at a temperature of 900°C, a vacuum degree of 80 Pa, and a pressure of 20 MPa to obtain a graphite/copper composite material.
本实施例3制得的石墨/铜复合材料的抗弯强度为14.9 MPa，抗压强度为28.9MPa，电导率为5.7%IACS。The bending strength of the graphite/copper composite material prepared in Example 3 is 14.9 MPa, the compressive strength is 28.9 MPa, and the electrical conductivity is 5.7%IACS.
鳞片石墨不经步骤S1、S2和S4原位插层膨化处理，其它步骤同上述内容：未原位插层膨化的石墨/铜复合材料的抗弯强度11.8MPa，抗压强度24.6MPa，电导率为4.3%IACS。经原位插层膨化制备的石墨/铜复合材料比未原位插层膨化的石墨/铜复合材料的抗弯强度、抗压强度和电导率分别提高了26.3%，17.5%和32.6%。The flake graphite is not processed by in-situ intercalation and expansion in steps S1, S2 and S4, and other steps are the same as above: the flexural strength of graphite/copper composite material without in-situ intercalation and expansion is 11.8MPa, the compressive strength is 24.6MPa, and the electrical conductivity It is 4.3% IACS. The flexural strength, compressive strength and electrical conductivity of graphite/copper composites prepared by in-situ intercalation and expansion increased by 26.3%, 17.5% and 32.6%, respectively, compared with those without in-situ intercalation and expansion.
本发明并不受上述实施方式的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The present invention is not limited by the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the present invention. within the scope of protection.
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