CN102508327A - Method for preparing aluminum and silicon carbide composite material reflector with high volume fraction - Google Patents
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 16
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 title abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 45
- 238000007747 plating Methods 0.000 claims abstract description 14
- 230000006641 stabilisation Effects 0.000 claims abstract description 5
- 238000011105 stabilization Methods 0.000 claims abstract description 5
- 238000007669 thermal treatment Methods 0.000 claims abstract 4
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 claims description 7
- 229910001096 P alloy Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000003082 abrasive agent Substances 0.000 claims 2
- 230000003252 repetitive effect Effects 0.000 claims 2
- 238000010792 warming Methods 0.000 claims 2
- 239000000126 substance Substances 0.000 claims 1
- 229910003460 diamond Inorganic materials 0.000 abstract description 8
- 239000010432 diamond Substances 0.000 abstract description 8
- 238000002310 reflectometry Methods 0.000 abstract description 5
- 230000003746 surface roughness Effects 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 1
- 239000000956 alloy Substances 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 229910052759 nickel Inorganic materials 0.000 abstract 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000011208 reinforced composite material Substances 0.000 description 2
- 229910000962 AlSiC Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及一种高体积分数的铝碳化硅复合材料反射镜的制备方法。尤其是铝碳化硅复合材料反射镜镜坯的研磨、镀层沉积速率控制及反射镜镜面光学研磨工艺。 The invention relates to a preparation method of a high-volume-fraction aluminum-silicon carbide composite reflector. Especially the grinding of aluminum-silicon carbide composite mirror blanks, the control of coating deposition rate and the optical grinding process of mirror mirrors. the
背景技术 Background technique
铝碳化硅复合材料具有质量轻、热导率高、热膨胀系数低、比强度高等特点，广泛应用于电子封装和精密仪器关键部件制造。已有报道的光学反射镜采用36%体积分数碳化硅的铝碳化硅复合材料反射镜坯化学镀镍磷的报道，是采用二次浸锌、碱性化学镀镍后再酸性化学镀镍磷。化学镀镍磷合金后，镀层具有耐酸、耐碱、耐磨及硬度高等特点,但这种工艺方法较复杂。反射镜是由低体积分数的铝碳化硅复合材料加工制成的，其热膨胀系数在10×10-6/k左右。一般的研磨方法用于铝碳化硅复合材料镍磷镀层研磨，镀层表面划痕多，反射镜面易产生光圈。其应用范围较小，不能适用于汽车工业和空间技术用的反射镜面。目前汽车工业和空间技术发展迅速，迫切需要一种热膨胀系数小于8.5×10-6/k，反射率为96%，反射镜面无光圈的高体积分数碳化硅颗粒增强的铝基复合材料（简称高体积分数的铝碳化硅复合材料）反射镜。申请人已申请的中国专利申请号201110101412.0公开了一种制备高体积分数铝基碳化硅颗粒增强复合材料方法以及201110259096.X公开了一种铝碳化硅复合材料表面化学镀镍磷合金工艺，但是目前还没有报导整个高体积分数的铝碳化硅复合材料反射镜的制备方法。 Aluminum silicon carbide composite materials have the characteristics of light weight, high thermal conductivity, low thermal expansion coefficient, and high specific strength. They are widely used in the manufacture of electronic packaging and key components of precision instruments. It has been reported that the optical mirror uses 36% silicon carbide aluminum-silicon carbide composite material mirror blank to be electroless nickel-phosphorus-plated. After electroless nickel-phosphorus alloy plating, the coating has the characteristics of acid resistance, alkali resistance, wear resistance and high hardness, but this process method is more complicated. The reflector is made of aluminum silicon carbide composite material with low volume fraction, and its thermal expansion coefficient is about 10×10 -6 /k. The general grinding method is used for grinding the nickel-phosphorus coating of the aluminum-silicon carbide composite material. There are many scratches on the surface of the coating, and the mirror surface is easy to produce apertures. Its scope of application is small and cannot be applied to reflective mirrors used in the automotive industry and space technology. At present, the automobile industry and space technology are developing rapidly, and there is an urgent need for a high-volume silicon carbide particle-reinforced aluminum-based composite material with a thermal expansion coefficient of less than 8.5×10 -6 /k, a reflectivity of 96%, and no aperture on the mirror surface (referred to as high volume fraction of AlSiC composite) mirrors. The Chinese patent application number 201110101412.0 that the applicant has applied for discloses a method for preparing a high volume fraction aluminum-based silicon carbide particle-reinforced composite material and 201110259096.X discloses a process for electroless nickel-phosphorus alloy plating on the surface of an aluminum-silicon carbide composite material, but currently The fabrication method of the whole high volume fraction aluminum silicon carbide composite mirror has not been reported yet.
本发明的目的在于提供一种体积分数为70%的铝碳化硅复合材料反射镜的制备方法。以实现其热膨胀系数小于8.0×10-6/k；能使反射镜的面形变形极小，粗糙度低，使反射镜的反射率为96%以上，反射镜面无光圈；适用范围广，能适用于汽车工业和空间技术用的反射镜。 The purpose of the present invention is to provide a method for preparing an aluminum-silicon carbide composite reflector with a volume fraction of 70%. In order to realize that its thermal expansion coefficient is less than 8.0×10 -6 /k; it can make the surface deformation of the mirror extremely small, the roughness is low, the reflectivity of the mirror is above 96%, and the mirror surface has no aperture; it has a wide range of applications and can Mirrors for the automotive industry and space technology.
本发明的技术方案是：包括以下步骤: Technical scheme of the present invention is: comprise the following steps:
（1）用体积分数为70%的铝碳化硅复合材料制备反射镜镜坯，其热膨胀系数为7.5×10-6/k； (1) The reflector blank is prepared with aluminum silicon carbide composite material with a volume fraction of 70%, and its thermal expansion coefficient is 7.5×10 -6 /k;
（2）镜坯的粗磨：在平面磨床用180目金刚石砂轮粗磨；若用高于180目金刚石砂轮粗磨，则砂轮易堵塞；低于180目金刚石砂轮粗磨，则粗糙度达不到要求，为后续精磨带来困难； (2) Coarse grinding of the mirror blank: use a 180-mesh diamond grinding wheel for rough grinding on a surface grinder; if you use a diamond grinding wheel higher than 180 mesh for rough grinding, the grinding wheel will be easily blocked; if you use a diamond grinding wheel lower than 180 mesh for rough grinding, the roughness will not reach To meet the requirements, it will bring difficulties for subsequent fine grinding;
（3）镜坯的第一次热处理，在温度为300～350℃保温60分钟，随炉冷却；否则，铝碳化硅复合材料的晶粒会长大，热膨胀系数增大； (3) For the first heat treatment of the mirror blank, keep it at a temperature of 300-350°C for 60 minutes, and then cool it with the furnace; otherwise, the grains of the aluminum-silicon carbide composite material will grow and the coefficient of thermal expansion will increase;
（4）镜坯的精磨：在平面磨床用2000目金刚石砂轮精磨镜坯的基准面和另一面； (4) Fine grinding of the mirror blank: use a 2000-mesh diamond grinding wheel to finely grind the reference surface and the other side of the mirror blank on a surface grinder;
（5）镜坯的稳定化处理： (5) Stabilization treatment of mirror blank:
①将镜坯放入加热炉内，在150～250℃，保温3～5小时； ① Put the mirror blank into the heating furnace, keep it warm for 3-5 hours at 150-250°C;
②快速将镜坯取出放入保温桶中，加入-180～220℃液氮，并高出镜坯顶部25～40mm,保温1～3小时； ②Quickly take out the mirror blank and put it into the heat preservation bucket, add liquid nitrogen at -180~220℃, and make it 25~40mm higher than the top of the mirror blank, and keep it warm for 1~3 hours;
③取出镜坯再放入加热炉内，在150～250℃，保温3～5小时； ③Take out the mirror blank and put it into the heating furnace, keep it warm for 3-5 hours at 150-250°C;
④按照②步和③步重复操作一次，随炉冷却； ④ Repeat step ② and step ③ once, and cool down with the furnace;
（6）镜坯的再研磨：用研磨机和0.5～1μm的Al2O3磨料对镜坯进行研磨，使平面度达到0.008～0.01 mm，表面粗糙度达到Ra0.02μm； (6) Re-grinding of the mirror blank: Grinding the mirror blank with a grinding machine and 0.5-1 μm Al 2 O 3 abrasive, so that the flatness reaches 0.008-0.01 mm, and the surface roughness reaches Ra0.02 μm;
（7）镜坯的化学镀镍磷合金，控制PH为3.5～4.0，施镀温度为80～85℃，镀速为3.5～5.0μm/hr；达到镀层100～120μm； (7) Electroless nickel-phosphorus alloy plating of the mirror blank, the pH is controlled at 3.5-4.0, the plating temperature is 80-85°C, and the plating rate is 3.5-5.0μm/hr; the coating layer reaches 100-120μm;
（8）第二次热处理，在温度350±20℃保温60分钟，随炉冷却； (8) For the second heat treatment, keep the temperature at 350±20°C for 60 minutes, and cool with the furnace;
（9）光学研磨：采用研磨机和0.3～0.5μm的Al2O3磨料对反射镜镀层进行研磨，达到Ra0.012μm。 (9) Optical grinding: Use a grinding machine and 0.3-0.5 μm Al 2 O 3 abrasive to grind the reflector coating to Ra0.012 μm.
所述反射镜的尺寸为150×150×10mm。 The size of the mirror is 150×150×10mm. the
本发明对体积分数为70%的铝碳化硅复合材料反射镜镜坯进行磨加工，热处理，精磨再研磨，保证反射镜平面度和粗糙度；通过控制镀液的PH值和施镀温度，达到镀层镍磷合金结晶细小；对镀层热处理增加镀层硬度，便于光学研磨；所制备的体积分数为70%的铝碳化硅复合材料反射镜反射率达97%，反射镜面无光圈；热膨胀系数为7.5×10-6/k，热导率为180W/m.K。本发明工艺简单、操作方便成本低，适用面广，可实现工业化生产。 The present invention grinds, heat-treats, finely grinds and then grinds the reflector blank of the aluminum-silicon carbide composite material with a volume fraction of 70%, so as to ensure the flatness and roughness of the reflector; by controlling the pH value of the plating solution and the plating temperature, The nickel-phosphorus alloy crystals of the coating are fine; the heat treatment of the coating increases the hardness of the coating, which is convenient for optical grinding; the prepared aluminum silicon carbide composite mirror with a volume fraction of 70% has a reflectivity of 97%, and the mirror surface has no aperture; the thermal expansion coefficient is 7.5 ×10 -6 /k, the thermal conductivity is 180W/mK. The invention has simple process, convenient operation, low cost, wide applicability and can realize industrialized production.
具体实施方式 Detailed ways
下面结合实例对本发明作进一步说明。 Below in conjunction with example the present invention will be further described.
实施例1 Example 1
（1）选用体积分数为70%的铝基碳化硅颗粒增强复合材料制备反射镜镜坯：镜坯尺寸为150×150×10mm； (1) Select aluminum-based silicon carbide particle-reinforced composite materials with a volume fraction of 70% to prepare mirror blanks: the size of the mirror blanks is 150×150×10mm;
（2）镜坯的粗磨：在平面磨床用180目金刚石砂轮粗磨,Ra0.2μm； (2) Coarse grinding of the mirror blank: rough grinding with a 180-mesh diamond grinding wheel on a surface grinder, Ra0.2μm;
（3）第一次热处理，在温度300℃保温60分钟，随炉冷却； (3) For the first heat treatment, keep the temperature at 300°C for 60 minutes and cool with the furnace;
（4）精磨：再用平面磨床和2000目金刚石砂轮精磨基准面和另一面，达到 Ra0.02μm； (4) Fine grinding: use a surface grinder and a 2000 mesh diamond grinding wheel to finely grind the reference plane and the other side to reach Ra0.02μm;
（5）镜坯的稳定化处理，①将镜坯放入加热炉内，升温至190℃，保温4小时后；②快速将镜坯取出放入保温桶中，从保温桶的底部加入液氮(-196℃)，液氮高出镜坯最高点30mm,在这种状态下保2小时后；③取出镜坯放入加热炉内再升温至190℃，保温4小时；④再将镜坯取出，放入保温桶中，按照②步和③步重复操作一次；随炉冷却 (5) Stabilization treatment of the mirror blank: ①Put the mirror blank in the heating furnace, raise the temperature to 190°C, and keep it warm for 4 hours; ②Quickly take out the mirror blank and put it into the insulation bucket, and add liquid nitrogen from the bottom of the insulation bucket (-196°C), the liquid nitrogen is 30mm higher than the highest point of the mirror blank, and keep it in this state for 2 hours; ③Take out the mirror blank and put it in the heating furnace, then raise the temperature to 190°C, and keep it for 4 hours; ④Take out the mirror blank , put it into the heat preservation bucket, repeat the operation according to step ② and step ③ once; cool with the furnace
（6）镜坯的再研磨：用研磨机和1μm的Al2O3磨料对镜坯进行研磨，使平面度达到0.008 mm，表面粗糙度达到Ra0.02μm； (6) Re-grinding of the mirror blank: Grinding the mirror blank with a grinding machine and 1 μm Al 2 O 3 abrasive, so that the flatness reaches 0.008 mm and the surface roughness reaches Ra0.02 μm;
（7）镜坯的化学镀镍磷合金，控制PH为4.0，施镀温度为85℃，镀速为3.5μm/hr；达到镀层120μm； (7) Electroless nickel-phosphorus alloy plating of the mirror blank, the pH is controlled at 4.0, the plating temperature is 85°C, and the plating speed is 3.5μm/hr; the coating layer reaches 120μm;
（8）第二次热处理，在温度350℃保温60分钟，随炉冷却； (8) For the second heat treatment, keep the temperature at 350°C for 60 minutes and cool with the furnace;
（9）光学研磨：采用研磨机和0.5μm的Al2O3磨料对反射镜镀层进行研磨，达到平面度为0.008 mm，Ra0.012μm。 (9) Optical grinding: Use a grinding machine and 0.5 μm Al 2 O 3 abrasive to grind the mirror coating to achieve a flatness of 0.008 mm and a Ra of 0.012 μm.
通过以上步骤制备的铝碳化硅复合材料反射镜，镀层经400℃，保温60分钟后水淬，镀层没有脱落，也没有产生裂纹和起泡；取样测量铝碳化硅复合材料的物理性能，热膨胀系数为7.5×10-6/k，热导率为180W/m.K。经实际应用，反射率达97%，反射镜面无光圈。 The aluminum silicon carbide composite reflector prepared by the above steps, the coating was water quenched after 400 ° C for 60 minutes, and the coating did not fall off, nor did cracks and bubbles occur; samples were taken to measure the physical properties of the aluminum silicon carbide composite material, thermal expansion coefficient It is 7.5×10 -6 /k, and the thermal conductivity is 180W/mK. After practical application, the reflectivity reaches 97%, and the reflecting mirror has no aperture.
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