CN113621964A - 一种铝基碳化硅表面低反射率膜层及其制备方法 - Google Patents
一种铝基碳化硅表面低反射率膜层及其制备方法 Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 41
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 40
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 40
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002310 reflectometry Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 29
- 239000011701 zinc Substances 0.000 claims abstract description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000007747 plating Methods 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052802 copper Inorganic materials 0.000 claims abstract description 22
- 239000010949 copper Substances 0.000 claims abstract description 22
- 238000007598 dipping method Methods 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 33
- 239000003921 oil Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- LEKPFOXEZRZPGW-UHFFFAOYSA-N copper;dicyanide Chemical compound [Cu+2].N#[C-].N#[C-] LEKPFOXEZRZPGW-UHFFFAOYSA-N 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- 229940099690 malic acid Drugs 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 3
- 235000006666 potassium iodate Nutrition 0.000 claims description 3
- 239000001230 potassium iodate Substances 0.000 claims description 3
- 229940093930 potassium iodate Drugs 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 229960004249 sodium acetate Drugs 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 235000019263 trisodium citrate Nutrition 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
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- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
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Abstract
一种涉及铝基碳化硅材料表面改性的技术领域的铝基碳化硅表面低反射率膜层及其制备方法，铝基碳化硅表面低反射率膜层包含清洁面，清洁面外依次设有浸锌层、化学镀镍层、铜层和氧化膜层，铜层厚度为4～6μm，氧化膜层厚度小于等于2μm，380nm～10μm波长范围内的光在此膜层上的镜面反射率不高于2％，对结构件的精度影响不超过5μm，其制备方法是先对铝基碳化硅材料进行除油，酸洗，浸锌，化学镀镍等工序将材料表面进行改性，再经过电镀铜和化学氧化方法，最终得到反射率不高于2％的低反射率膜层。
Description
技术领域
本发明涉及铝基碳化硅材料表面改性的技术领域，尤其是涉及一种铝基碳化硅表面低反射率膜层及其制备方法。
背景技术
铝基碳化硅材料是采用铝合金作基体，以碳化硅颗粒作增强相，通过粉末冶金技术烧结制成的一种颗粒增强金属基复合材料；铝基碳化硅复合材料拥有一般金属合金材料所不具备的低密度、高比强度、高比刚度、高耐磨性、低热膨胀系数、高耐蚀性和可采用传统金属加工工艺加工等优良性能，它还具备良好的尺寸稳定性、导热性以及耐磨、耐疲劳等优异的力学性能和物理性能，在航空航天的各类空间飞行器与先进武器装备研制中得以广泛应用；由于铝基碳化硅活性较差，表面不易成膜，所制成的结构件在某特殊环境中使用，零件表面需要较低的反射率以及吸收杂光的性能，目前并无在铝基碳化硅材料表面制备低反射率膜层的工艺方法。
发明内容
为了克服背景技术中的不足，本发明公开了一种铝基碳化硅表面低反射率膜层及其制备方法，使得光在此方法得到的膜层上镜面反射率低，并且需要和铝基碳化硅复合材料基体结合牢固，不易脱落，满足特殊环境下的需求。
为实现上述发明目的，本发明采用如下技术方案：
一种铝基碳化硅表面低反射率膜层，包含铝基碳化硅结构件，所述铝基碳化硅结构件设有清洁面，所述清洁面外依次设有浸锌层、化学镀镍层、铜层和氧化膜层，所述铜层厚度为4～6μm，所述氧化膜层厚度小于等于2μm。
进一步，所述浸锌层厚度小于等于1μm。
进一步，所述化学镀镍层厚度小于等于2μm。
一种铝基碳化硅表面低反射率膜层的制备方法，包含如下步骤：S1、对铝基碳化硅材料制成的结构件表面依次进行除油处理、水洗、弱浸蚀和再水洗，得到活性较强的清洁面；S2、对S1步骤中得到的清洁面进行浸锌处理，得到浸锌层；S3、对S2步骤中得到的浸锌层表面进行化学镀镍处理，完成对铝基碳化硅材料制成的结构件表面的改性，得到改性表面；S4、对S3步骤中得到的改性表面进行镀铜处理，得到铜层；S5、在S4步骤中得到的铜层表面进行化学氧化处理，最终得到黑色的低反射率膜层，使得380nm～10μm波长范围内的光在此膜层上的镜面反射率≤2％，对结构件的精度影响不超过5μm。
进一步，在S1步骤中的除油处理包含有机溶剂除油和化学除油，除油处理时间超过25min，除油处理后先进行热水洗，再进行冷水洗。
进一步，在S1步骤中弱浸蚀采用的浸蚀液原料包含铬酸酐、氢氟酸和硝酸，弱浸蚀之后进行冷水洗。
进一步，在S2步骤中，浸锌处理工艺依次为一次浸锌、冷水清洗、退锌、二次浸锌和冷水清洗。
进一步，在S3步骤中，化学镀镍采用的化学原料包含硫酸镍、氯化镍、次亚磷酸钠、乙酸钠、柠檬酸三钠、苹果酸、碘酸钾。
进一步，在S4步骤中的镀铜方式选用氰化镀铜工艺。
进一步，对S5步骤中的低反射率膜层还需在水洗干燥后，进行防锈处理。
由于采用如上所述的技术方案，本发明具有如下有益效果：
本发明铝基碳化硅表面的低反射率膜层为黑色，380nm～10μm波长范围内的光在此膜层上的镜面反射率不高于2％，对结构件的精度影响不超过5μm；本发明铝基碳化硅表面的低反射率膜层的方法通过先对铝基碳化硅材料进行除油，酸洗，浸锌，化学镀镍等工序将材料表面进行改性，再经过镀铜和化学氧化方法得到低反射率膜层，这种黑色的低反射率膜层附着力好，反射率低，能够用于光路中吸收杂散光的铝基碳化硅材料结构件，可广泛的用于航天相机、光电设备等军民用光学领域。
附图说明
图1是本发明的工艺流程示意图；
图2是本发明在傅立叶变换红外光谱仪上测试3～5μm波段的光在此膜层上的反射率测试数值变化图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明的技术方案进行说明：
一种铝基碳化硅表面低反射率膜层，是在铝基碳化硅(SiCp/Al)材料的结构件表面进行制备，且铝基碳化硅材料中碳化硅含量为50％以下，具体碳化硅含量能够为40％，或为20％；铝基碳化硅结构件设有清洁面，也即需要制备低反射率膜层的表面，清洁面外依次设有浸锌层、化学镀镍层、铜层和氧化膜层，铜层厚度为4～6μm(具体可为4μm，5μm，6μm)，氧化膜层厚度小于等于2μm(具体可为2μm，1.5μm，0.5μm)；根据需要，浸锌层厚度小于等于1μm(具体可为1μm，0.6μm，0.3μm)；此外，化学镀镍层厚度小于等于2μm(具体可为2μm，1.2μm，0.7μm)。
一种铝基碳化硅表面低反射率膜层的制备方法，如图1所示，包含如下步骤：
S1、对铝基碳化硅材料制成的结构件表面依次进行除油处理、水洗、弱浸蚀和再水洗，得到活性较强的清洁面；根据需要，在S1步骤中的除油处理包含有机溶剂除油和化学除油，总的除油处理时间超过25min，除油处理后先进行热水洗，再进行冷水洗，防止除油液残留，其中有机溶剂除油所使用的化学原料为汽油、酒精等，化学除油能够使用铝合金清洗剂；此外，弱浸蚀采用的浸蚀液原料包含铬酸酐、氢氟酸和硝酸，弱浸蚀之后进行冷水清洗；
S2、对S1步骤中得到的清洁面进行浸锌处理，得到≤1μm的浸锌层；浸锌处理工艺依次为一次浸锌、冷水清洗、退锌、二次浸锌和冷水清洗，其中一次浸锌和二次浸锌均采用四元浸锌剂，并采用硝酸进行退锌；
S3、对S2步骤中得到的浸锌层表面进行化学镀镍处理，得到≤2μm的化学镀镍层，完成对铝基碳化硅材料制成的结构件表面的改性，得到改性表面，其中化学镀镍采用的化学原料包含硫酸镍、氯化镍、次亚磷酸钠、乙酸钠、柠檬酸三钠、苹果酸、碘酸钾；
S4、对S3步骤中得到的改性表面进行镀铜处理，得到厚度为4～6μm的铜层；其中镀铜方法可以广泛选择镀铜工艺，但对于结构复杂的零件优选分散能力和覆盖能力好的氰化镀铜工艺；
S5、在S4步骤中得到的铜层表面进行化学氧化处理，并保证氧化膜层厚度不超过2μm，最终得到黑色的低反射率膜层，使得380nm～10μm波长范围内的光在此膜层上的镜面反射率≤2％，对结构件的精度影响不超过5μm，根据需要，最好将该低反射率膜层水洗干燥后，进行防锈处理；如图2所示，在傅立叶变换红外光谱仪上，测试3～5μm波段的光在此低反射率膜层上的反射率满足需求。
本发明未详述部分为现有技术，对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明；因此，无论从哪一点来看，均应将上述实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内，不应将权利要求中的任何附图标记视为限制所涉及的权利要求内容。
Claims (10)
1.一种铝基碳化硅表面低反射率膜层，其特征是：包含铝基碳化硅结构件，所述铝基碳化硅结构件设有清洁面，所述清洁面外依次设有浸锌层、化学镀镍层、铜层和氧化膜层，所述铜层厚度为4～6μm，所述氧化膜层厚度小于等于2μm。
2.根据权利要求1所述的铝基碳化硅表面低反射率膜层，其特征是：所述浸锌层厚度小于等于1μm。
3.根据权利要求1所述的铝基碳化硅表面低反射率膜层，其特征是：所述化学镀镍层厚度小于等于2μm。
4.一种如权利要求1-3任一所述铝基碳化硅表面低反射率膜层的制备方法，其特征是：包含如下步骤：
S1、对铝基碳化硅材料制成的结构件表面依次进行除油处理、水洗、弱浸蚀和再水洗，得到活性较强的清洁面。
S2、对S1步骤中得到的清洁面进行浸锌处理，得到浸锌层。
S3、对S2步骤中得到的浸锌层表面进行化学镀镍处理，完成对铝基碳化硅材料制成的结构件表面的改性，得到改性表面。
S4、对S3步骤中得到的改性表面进行镀铜处理，得到铜层。
S5、在S4步骤中得到的铜层表面进行化学氧化处理，最终得到黑色的低反射率膜层，使得380nm～10μm波长范围内的光在此膜层上的镜面反射率≤2％，对结构件的精度影响不超过5μm。
5.根据权利要求4所述的铝基碳化硅表面低反射率膜层的制备方法，其特征是：在S1步骤中的除油处理包含有机溶剂除油和化学除油，除油处理时间超过25min，除油处理后先进行热水洗，再进行冷水洗。
6.根据权利要求4所述的铝基碳化硅表面低反射率膜层的制备方法，其特征是：在S1步骤中弱浸蚀采用的浸蚀液原料包含铬酸酐、氢氟酸和硝酸，弱浸蚀之后进行冷水洗。
7.根据权利要求4所述的铝基碳化硅表面低反射率膜层的制备方法，其特征是：在S2步骤中，浸锌处理工艺依次为一次浸锌、冷水清洗、退锌、二次浸锌和冷水清洗。
8.根据权利要求4所述的铝基碳化硅表面低反射率膜层的制备方法，其特征是：在S3步骤中，化学镀镍采用的化学原料包含硫酸镍、氯化镍、次亚磷酸钠、乙酸钠、柠檬酸三钠、苹果酸、碘酸钾。
9.根据权利要求4所述的铝基碳化硅表面低反射率膜层的制备方法，其特征是：在S4步骤中的镀铜方式选用氰化镀铜工艺。
10.根据权利要求4所述的铝基碳化硅表面低反射率膜层的制备方法，其特征是：对S5步骤中的低反射率膜层还需在水洗干燥后，进行防锈处理。
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