CN108129148A - 一种低膨胀石墨材料的制备方法 - Google Patents
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- 238000004898 kneading Methods 0.000 claims abstract description 13
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 6
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- 238000005087 graphitization Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 21
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- 230000000087 stabilizing effect Effects 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009760 electrical discharge machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种低膨胀石墨材料的制备方法。主要原料包括球型人造石墨粉与沥青,依次经过磨粉、整形、筛分、配料、混捏、等静压成型、焙烧、石墨化等工艺步骤后制得低膨胀石墨材料。本低膨胀石墨材料制备工艺操作简单,充分利用资源,成品率高,节约成本,且具有良好的耐热膨胀性。
Description
技术领域
本发明涉及石墨材料制备领域,具体涉及一种低膨胀石墨材料的制备方法。
技术背景
石墨制品以其稳定的化学性质与优异的耐高温性质得到了各行各业的广泛认可,目前广泛用于太阳能光伏、模具、电子半导体、电火花加工、冶金、化工、核工业和石英等行业,但是部分高精尖行业在需求一些精密零部件时,对石墨制品的热膨胀性就提出了更高程度的需求。
发明内容
本发明的目的,在于解决现有技术存在的上述问题,提供一种低膨胀石墨材料的制备方法。
本发明采用沥青为粘结剂,将粘结剂按比例加入到人造石墨粉中,经过充分混捏之后再将其按照程序进行等静压成型,对成型之后的坯料依次进行焙烧、石墨化等处理即可得所述低膨胀石墨材料。
所述的人造石墨粉的整形为人造石墨粉在整形机中进行表面修整处理,处理之后得到球型度良好的人造石墨粉。
所述的沥青所占比例为30%~40%,人造石墨粉所占比例为60%~70%。
所述的沥青与人造石墨粉的混合物充分混捏,混捏过程需要进行加热,加热温度为150℃~350℃。
所述的人造石墨粉粒径≤10μm。
所述的等静压成型,在成型过程中需将经过充分混捏的原料加入到模具中进行密封,抽真空至10KPa~40KPa,再移至等静压机中压制成型,压型压力为80MPa~150MPa,先以7~10MPa/min的升压速率上升至所设定成型压力,稳压5~10min,再以8~16MPa/min的泄压速率泄压至70~80MPa,稳压5~10min;再以8~16MPa/min的泄压速率泄压至30~40MPa,稳压2~5min;最后以8~16MPa/min的泄压速率泄压至室压。
所述的焙烧,其处理过程为分段进行,具体步骤为,将压制好的生坯放入坩埚内,再把坩埚放入焙烧炉中进行焙烧,焙烧是在真空设备里进行的,在升温区间100℃~350℃时,升温速度为1.0℃/h~1.5℃/h,在升温区间350℃~600℃时,升温速度为0.5℃/h~1.0℃/h,在升温区间600℃~900℃时,升温速度为1.0℃/h~1.5℃/h,在升温区间900℃~1300℃时,升温速度为2.0℃/h~3.0℃/h。
所述的石墨化处理的过程具体为先将炭化后的样品均匀升温至1350℃~1550℃,保温2~5h,再均匀升温至2650℃~2950℃,最后以0.5℃/h~1.0℃/h的降温速率降至90℃出炉,自然冷却,即可得所述低膨胀石墨材料。
本发明实现的有益效果:
本发明的低膨胀石墨材料由于采用了球型人造石墨粉为主要原料,在根本上降低了石墨材料的膨胀性,再加上采用特殊的成型方式,在不影响其膨胀性的基础上,使其拥有更高的机械强度。
附图说明
图1是本发明的加工流程图。
具体实施方式
下面结合具体实施例,进一步阐述本发明的实施方式。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例
①将粒径≤50μm的人造石墨粉加入到整形机中,在经过整形处理后,将整形后的人造石墨粉进行筛分,选取粒径≤10μm的人造石墨粉待用。
②将35kg在200℃下呈熔融状态的沥青加入到65kg粒径≤10μm的人造石墨粉中,进行混捏处理,混捏过程需进行加热处理,加热温度为250℃,混捏时间为90min。
③将步骤②中混捏完成的原料全部转移到等静压模具中,对其抽真空至40KPa,再将其移至等静压机中压制成型,先以8MPa/min的升压速率上升至140MPa,稳压10min,再以10MPa/min的泄压速率泄压至80MPa,稳压5min;再以10MPa/min的泄压速率泄压至40MPa,稳压5min;最后以10MPa/min的泄压速率泄压至室压,即可得生坯。
④将步骤③中所得生坯放入坩埚内,再将坩埚转移至真空焙烧炉,在升温区间100℃~350℃时,升温速度为1.0℃/h,在升温区间350℃~600℃时,升温速度为0.5℃/h,在升温区间600℃~900℃时,升温速度为1.5℃/h,在升温区间900℃~1300℃时,升温速度为2.0℃/h。
⑤将步骤④中焙烧后坯料进行石墨化处理,具体为先将炭化后的样品均匀升温至1500℃,保温4h,再均匀升温至2800℃,最后以1.0℃/h的降温速率降至90℃出炉,自然冷却,即可得到低膨胀石墨材料。
Claims (8)
1.一种低膨胀石墨材料的制备方法,其特征在于:它采用沥青为粘结剂,将粘结剂按比例加入到经过整形处理后的人造石墨粉中,经过充分混捏之后再将其按照程序进行等静压成型,对成型之后的坯料依次进行焙烧、石墨化等处理即可得所述低膨胀石墨材料。
2.根据权利要求1所述的低膨胀石墨材料的制备方法,其特征在于:所述的人造石墨粉的整形为人造石墨粉在整形机中进行表面修整处理,处理之后得到球型度良好的人造石墨粉。
3.根据权利要求1所述的低膨胀石墨材料的制备方法,其特征在于:所述的沥青所占比例为30%~40%,人造石墨粉所占比例为60%~70%。
4.根据权利要求1所述的低膨胀石墨材料的制备方法,其特征在于:所述的沥青与人造石墨粉的混合物充分混捏,混捏过程需要进行加热,加热温度为150℃~350℃。
5.根据权利要求1所述的低膨胀石墨材料的制备方法,其特征在于:所述的人造石墨粉粒径≤10μm。
6.根据权利要求1所述的低膨胀石墨材料的制备方法,其特征在于:所述的等静压成型,在成型过程中需将经过充分混捏的原料加入到模具中进行密封,抽真空至10KPa~40KPa,再移至等静压机中压制成型,压型压力为80MPa~150MPa,先以7~10MPa/min的升压速率上升至所设定成型压力,稳压5~10min,再以8~16MPa/min的泄压速率泄压至70~80MPa,稳压5~10min;再以8~16MPa/min的泄压速率泄压至30~40MPa,稳压2~5min;最后以8~16MPa/min的泄压速率泄压至室压。
7.根据权利要求1所述的低膨胀石墨材料的制备方法,其特征在于:所述的焙烧,其处理过程为分段进行,具体步骤为,将压制好的生坯放入坩埚内,再把坩埚放入焙烧炉中进行焙烧,焙烧是在真空设备里进行的,在升温区间100℃~350℃时,升温速度为1.0℃/h~1.5℃/h,在升温区间350℃~600℃时,升温速度为0.5℃/h~1.0℃/h,在升温区间600℃~900℃时,升温速度为1.0℃/h~1.5℃/h,在升温区间900℃~1300℃时,升温速度为2.0℃/h~3.0℃/h。
8.根据权利要求1所述的低膨胀石墨材料的制备方法,其特征在于:所述的石墨化处理的过程具体为先将炭化后的样品均匀升温至1350℃~1550℃,保温2~5h,再均匀升温至2650℃~2950℃,最后以0.5℃/h~1.0℃/h的降温速率降至90℃出炉,自然冷却,即可得所述低膨胀石墨材料。
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CN111072015A (zh) * | 2019-12-20 | 2020-04-28 | 厦门大学 | 一种低膨胀热还原氧化石墨烯的制备方法 |
CN112321301A (zh) * | 2020-10-19 | 2021-02-05 | 湖南长宇科技发展有限公司 | 一种火箭发动机喷管用的高导热低膨胀石墨及其制备方法 |
CN112624764A (zh) * | 2020-12-30 | 2021-04-09 | 巴中意科碳素股份有限公司 | 一种防止等静压石墨烧结开裂的方法 |
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Cited By (5)
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CN109694250A (zh) * | 2018-06-19 | 2019-04-30 | 安徽锦美碳材科技发展有限公司 | 一种制备石墨匣钵的方法 |
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CN112321301A (zh) * | 2020-10-19 | 2021-02-05 | 湖南长宇科技发展有限公司 | 一种火箭发动机喷管用的高导热低膨胀石墨及其制备方法 |
CN112624764A (zh) * | 2020-12-30 | 2021-04-09 | 巴中意科碳素股份有限公司 | 一种防止等静压石墨烧结开裂的方法 |
CN112624764B (zh) * | 2020-12-30 | 2022-07-29 | 巴中意科碳素股份有限公司 | 一种防止等静压石墨烧结开裂的方法 |
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