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CN107052913B - RB-SiC optical element polishing process processing methods - Google Patents

RB-SiC optical element polishing process processing methods Download PDF

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CN107052913B
CN107052913B CN201710397592.9A CN201710397592A CN107052913B CN 107052913 B CN107052913 B CN 107052913B CN 201710397592 A CN201710397592 A CN 201710397592A CN 107052913 B CN107052913 B CN 107052913B
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CN107052913A (en
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惠迎雪
刘卫国
张进
周顺
徐均琪
赵杨勇
熊涛
房沫岑
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Xian Technological University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B13/00Machines or devices designed for grinding or polishing optical surfaces on lenses or surfaces of similar shape on other work; Accessories therefor

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Abstract

本发明公开了一种RB‑SiC光学元件抛光工艺加工方法,该方法首先利用电感耦合等离子体抛光技术实现RB‑SiC光学元件的精磨抛光,之后利用射频磁控溅射表面平坦化技术在光学表面沉积纳米级平坦化层、最后利用离子束抛光修形技术辅助自由基微波等离子体抛光技术实现光学元件超光滑表面加工。相比于现有技术,本发明利用等离子体抛光技术替代传统的光学加工方法,结合纳米级的平坦化层制备技术和离子束修形抛光技术,极大地缩短了中大口径RB‑SiC元件的加工周期,构建了以高效率、高精度和低损耗的特点RB‑SiC光学元件抛光加工新方法。

The invention discloses a polishing process method for RB-SiC optical components. The method first uses inductively coupled plasma polishing technology to realize fine grinding and polishing of RB-SiC optical components, and then utilizes radio frequency magnetron sputtering surface planarization technology in the optical Deposit a nanoscale planarization layer on the surface, and finally use ion beam polishing technology to assist free radical microwave plasma polishing technology to achieve ultra-smooth surface processing of optical components. Compared with the prior art, the present invention uses plasma polishing technology to replace the traditional optical processing method, combined with nanoscale planarization layer preparation technology and ion beam modification polishing technology, which greatly shortens the cost of medium and large diameter RB‑SiC components. The processing cycle has established a new method of polishing RB‑SiC optical components with the characteristics of high efficiency, high precision and low loss.

Description

RB-SiC光学元件抛光工艺加工方法RB-SiC optical component polishing process processing method

技术领域technical field

本发明涉及本发明涉及光学元件表面超光滑精密加工技术领域,尤其涉及RB-SiC光学元件抛光工艺加工方法。The present invention relates to the technical field of ultra-smooth precision machining on the surface of optical elements, in particular to a polishing process method for RB-SiC optical elements.

背景技术Background technique

近年来,随着航空航天事业的蓬勃发展,社会生产飞速进步,人类对太空领域的探索热情越来越强烈,航空航天技术为人类观测太空、研究地球及整个浩瀚的宇宙空间作出了重大贡献。许多国家开始重视对航空航天技术以及空间光学的研究,空间望远镜、遥感侦察相机等大型空间系统为了满足使用要求,需要拥有足够高的分辨率及足够大的口径,但口径的增大,相应的会增加整个光学系统的重量,因此,不但需要提高光学系统的成像质量,而且需要减轻其重量,来降低发射成本,人们便对空间光学系统反射镜的材料及制造工艺提出一定要求。In recent years, with the vigorous development of the aerospace industry and the rapid progress of social production, human beings have become more and more enthusiastic about exploring the space field. Aerospace technology has made significant contributions to human observation of space, research on the earth and the entire vast space. Many countries have begun to attach importance to the research of aerospace technology and space optics. In order to meet the requirements of use, large-scale space systems such as space telescopes and remote sensing reconnaissance cameras need to have a high enough resolution and a large enough aperture, but the increase of the aperture, the corresponding It will increase the weight of the entire optical system. Therefore, it is not only necessary to improve the imaging quality of the optical system, but also to reduce its weight to reduce the launch cost. People put forward certain requirements for the material and manufacturing process of the space optical system reflector.

碳化硅(SiC)作为一种新型的空间反射镜加工材料,其具有密度较低、强度及弹性模量较高、热膨胀系数较小、导热性能良好、化学稳定性高等一系列优点,成为理想的大口径、轻量化反射镜基底材料。从上世纪70年代末开始,美国、德国、日本等发达国家对SiC材料应用于反射镜基底做了许多研究,积累了丰富的研究经验,我国在这方面起步相对较晚,在最近的几年里也取得了一定的研究成果。As a new type of space mirror processing material, silicon carbide (SiC) has a series of advantages such as low density, high strength and elastic modulus, small thermal expansion coefficient, good thermal conductivity, and high chemical stability. Large-diameter, lightweight mirror base material. Since the end of the 1970s, the United States, Germany, Japan and other developed countries have done a lot of research on the application of SiC materials to mirror substrates, and accumulated rich research experience. my country started relatively late in this regard. In recent years Some research results have also been obtained.

反应烧结法作为一种制备SiC反射镜的方法,其工艺简单、烧结温度低,是制备大口径、复杂形状反应烧结碳化硅(RB-SiC) 材料优先选用的方法。As a method for preparing SiC mirrors, the reaction sintering method has a simple process and low sintering temperature, and is the preferred method for preparing large-diameter and complex-shaped reaction-bonded silicon carbide (RB-SiC) materials.

RB-SiC是由Si和SiC组成的具有两相结构的材料(Si含量约占14%),由于二者物理特性的差异,致使抛光过程中Si的去除速率要比SiC快一些,导致RB-SiC抛光后表面质量下降,粗糙度增大,反射率减小,散射现象严重,根本无法满足高质量超光滑光学系统的要求。RB-SiC is a material with a two-phase structure composed of Si and SiC (Si content is about 14%). Due to the difference in physical properties between the two, the removal rate of Si during the polishing process is faster than that of SiC, resulting in RB-SiC After polishing, the surface quality of SiC decreases, the roughness increases, the reflectivity decreases, and the scattering phenomenon is serious, which cannot meet the requirements of high-quality ultra-smooth optical systems at all.

已有的RB-SiC抛光方法是由长春精密光学机械物理研究所和中科院化学物理研究所(发明专利:授权号200710159200.1)提出了一系列基于RB-SiC表面改性沉积工艺方法,其核心在于,中间过程利于镀膜方法在SiC表面沉积数微米至数十微米的Si薄膜(或其他材料改性层)。The existing RB-SiC polishing method is a series of RB-SiC surface modification deposition process methods based on the Changchun Institute of Precision Optical Mechanical Physics and the Institute of Chemical Physics of the Chinese Academy of Sciences (invention patent: authorization number 200710159200.1), the core of which is, The intermediate process is beneficial to the coating method to deposit Si films (or other material modification layers) of several microns to tens of microns on the SiC surface.

目前在该材料领域,主要发展了一种基于磁控溅射改性的RB-SiC加工方法,具体过程为:At present, in the field of this material, a RB-SiC processing method based on magnetron sputtering modification has been mainly developed. The specific process is as follows:

第一步,采用传统的磨削加工方法,对SiC进行磨削加工,使得材料的表面粗糙度Ra达到10nm以下(或者RMS达到20nm以下,)可以进行光学干涉测量;The first step is to use the traditional grinding method to grind SiC, so that the surface roughness Ra of the material can reach below 10nm (or RMS below 20nm), which can be used for optical interferometry;

第二步,采用磁控溅射方法,在RB-SiC表面沉积数十微米的Si薄膜,该方法的核心在于,RB-SiC的应用主要在于实现光学高反射,因此,在RB-SiC基底上沉积足够厚的Si改性层,由于Si膜相对于RB-SiC,材料单一,硬度低,易于加工;The second step is to use the magnetron sputtering method to deposit tens of microns of Si film on the surface of RB-SiC. The core of this method is that the application of RB-SiC is mainly to achieve high optical reflection. Therefore, on the RB-SiC substrate Deposit a sufficiently thick Si modified layer. Compared with RB-SiC, the Si film has a single material, low hardness and easy processing;

第三步,采用数控小工具抛光方法,对沉积在RB-SiC上的Si薄膜进行抛光,实现超光滑表面加工和面形修正。In the third step, the Si thin film deposited on the RB-SiC is polished using the CNC small tool polishing method to achieve ultra-smooth surface processing and surface shape correction.

现有的传统光学加工方法存在如下几个问题,第一是加工效率低,周期长,第二是,很难大面积(通常尺寸大于150mm)实现超光滑表面(粗糙度RMS小于1nm,面形RMS低于λ/5)。这是因为:磁控溅射沉积速率不高,沉积数十微米厚的Si层,导致加工时间较长,其二,磁控溅射沉积Si薄膜,随着膜厚达到微米量级时,薄膜的粗糙度将会劣化,通常由7~8nm劣化至十几纳米。The existing traditional optical processing methods have the following problems. First, the processing efficiency is low and the cycle time is long. Second, it is difficult to achieve an ultra-smooth surface (roughness RMS less than 1nm, surface shape RMS below λ/5). This is because: the deposition rate of magnetron sputtering is not high, and the deposition of tens of microns thick Si layer results in longer processing time. Second, magnetron sputtering deposits Si thin films. The roughness will deteriorate, usually from 7~8nm to more than ten nanometers.

鉴于此,如何设计一种可降低RB-SiC光学元件表面粗糙度,提高表面质量的超光滑表面加工方法,特别是如何设计一种操作简便、易于实现的表面抛光加工方法,有效控制光学元件表面面形,抑制表面及亚表面损伤,降低表面光学损耗。In view of this, how to design an ultra-smooth surface processing method that can reduce the surface roughness of RB-SiC optical components and improve surface quality, especially how to design a surface polishing processing method that is easy to operate and easy to implement, can effectively control the surface of optical components. Surface shape, inhibit surface and sub-surface damage, reduce surface optical loss.

发明内容Contents of the invention

针对已有传统机械抛光方法抛光RB-SiC所导致的材料表面质量下降,表面粗糙度较大,材料表面亚表面损伤严重,特别地,超长的加工周期和极低的加工效率,本发明的目的是提供RB-SiC光学元件抛光工艺加工方法,克服已有该材料抛光方法中所存在的问题。Aiming at the degradation of the surface quality of the material caused by polishing RB-SiC by the existing traditional mechanical polishing method, the surface roughness is large, the subsurface damage of the material surface is serious, especially, the ultra-long processing cycle and the extremely low processing efficiency, the present invention The purpose of the invention is to provide a processing method for polishing the RB-SiC optical element and overcome the problems existing in the existing polishing method for the material.

为了实现上述目的,本发明所采用的技术方案为:In order to achieve the above object, the technical solution adopted in the present invention is:

RB-SiC光学元件抛光工艺加工方法,包括以下步骤:The RB-SiC optical element polishing process processing method includes the following steps:

步骤1,首先对RB-SiC毛坯料进行抛光刻蚀加工,实现光学元件的精密磨削,使光学元件表面粗糙度值收敛到20纳米以内;Step 1. Firstly, the RB-SiC blank is polished and etched to realize the precision grinding of the optical element, so that the surface roughness value of the optical element converges to within 20 nanometers;

步骤2,利用射频磁控溅射技术(RF-MS)在RB-SiC光学元件表面沉积纳米级平坦化层;Step 2, using radio frequency magnetron sputtering (RF-MS) to deposit a nanoscale planarization layer on the surface of the RB-SiC optical element;

步骤3,利用自由基微波等离子体源技术(RPS)对RB-SiC基底表面沉积的平坦化层进行抛光加工,利用自由基等离子体技术,将等离子体限定于等离子源本体之内,通过真空室流导控制,形成大面积均匀活性自由基,使得活性基与平坦化层材料发生化学化学反应,实现光学元件表面超光滑抛光加工;Step 3, use the radical microwave plasma source technology (RPS) to polish the planarization layer deposited on the surface of the RB-SiC substrate, use the radical plasma technology to confine the plasma within the plasma source body, and pass through the vacuum chamber Conductance control, forming a large area of uniform active radicals, making the active radicals chemically react with the material of the planarization layer, and realizing ultra-smooth polishing of the surface of optical components;

步骤4,利用离子束修形抛光技术(IBF),对光学元件表面平坦化层进行修形和抛光,通过对表面的高确定性去除,实现光学元件表面面形修正。Step 4: Use ion beam modification polishing technology (IBF) to modify and polish the planarization layer on the surface of the optical element, and realize the surface shape modification of the optical element by removing the surface with high certainty.

所述步骤1中ICP刻蚀抛光装置,其本底真空2.0×10-4Pa,工作真空控制在0.5~10Pa。The ICP etching and polishing device in the step 1 has a background vacuum of 2.0×10 -4 Pa and a working vacuum of 0.5-10 Pa.

初始毛坯料表面粗糙度RMS>100nm时,偏压功率维持100~150W,反应活性气体采用高纯度四氟化碳(纯度99.99%)。When the initial blank surface roughness RMS>100nm, the bias power is maintained at 100~150W, and the reactive gas uses high-purity carbon tetrafluoride (purity 99.99%).

针对RMS>100nm初始RB-SiC工件,射频功率150W,偏压功率150W,刻蚀气体流量为25~30sccm,工作气压2~5Pa。For the initial RB-SiC workpiece with RMS>100nm, the RF power is 150W, the bias power is 150W, the etching gas flow rate is 25~30sccm, and the working pressure is 2~5Pa.

所述步骤4中采用13.56MHz的射频离子源,利用三维运动控制系统控制离子源加工轨迹和驻留时间,所采用真空腔室本底真空1.0×10-4Pa,以高纯度氩气(纯度99.99%)为工作气体。In the step 4 , a 13.56MHz radio frequency ion source is used, and the three-dimensional motion control system is used to control the processing trajectory and residence time of the ion source. 99.99%) is the working gas.

步骤2中工作真空度1.2Pa,靶功率密度控制在5~10W/cm2In step 2, the working vacuum degree is 1.2Pa, and the target power density is controlled at 5~10W/cm 2 .

步骤3中通过真空气体流导和真空泵抽速控制,形成均匀性<5%活性基区,抛光时典型的真空度在50~100Pa。In step 3, the conductance of the vacuum gas and the pumping speed of the vacuum pump are controlled to form an active base area with a uniformity of <5%. The typical vacuum degree during polishing is 50-100Pa.

步骤4离子束能量控制在800eV以下,束斑尺寸控制在10mm以下,刻蚀效率1.0×10-3~0.02mm3/min。In step 4, the ion beam energy is controlled below 800eV, the beam spot size is controlled below 10mm, and the etching efficiency is 1.0×10 -3 ~0.02mm 3 /min.

本发明所述方法具有以下优点:The method of the present invention has the following advantages:

1、本加工方法极大的缩短了已有加工方法的加工周期,提高了效率。这主要体现在,在初抛阶段,本发明创造性直接将ICP等离子体刻蚀加工方法应用于SiC粗坯表面加工,通过工艺优化,利用对含氟气体和氧气的比例调整,可以实现SiC表面粗糙度由RMS100~200nm达到RMS10~20nm,面形优于4微米,提高了加工效率,彻底解决了传统方法难以加工高硬度的SiC材料,本方法可将加工周期缩短1/3~1/2;1. This processing method greatly shortens the processing cycle of existing processing methods and improves efficiency. This is mainly reflected in the fact that in the initial polishing stage, the invention creatively directly applies the ICP plasma etching processing method to the surface processing of the SiC rough billet. Through process optimization, the SiC surface can be roughened by adjusting the ratio of fluorine-containing gas and oxygen. The thickness is from RMS100~200nm to RMS10~20nm, and the surface shape is better than 4 microns, which improves the processing efficiency and completely solves the difficulty of processing SiC materials with high hardness by traditional methods. This method can shorten the processing cycle by 1/3~1/2;

2、传统工艺中改性方法的思路是基于RB-SiC脆硬难于加工,且材料组分复杂(包含有不同比例的Si和SiC),由于其组分不一致,所有在小工具抛光或传统的磨削加工过程中,导致了不同物相Si和SiC的去除效率的差异,几乎不可能实现光滑表面加工,于是,改性方法被提出,其核心是在RB-SiC表面沉积足够厚的Si层,只要能保证其与基底RB-SiC膜基结合强度,后续的方法仅是对硅层进行抛光,不涉及基底RB-SiC材料的抛光,故而,改性的方法一定要使沉积硅层足够厚,以避免后续方法加工至基底。本发明在磁控溅射沉积过程中,仅需镀制100~500nm的Si平坦化层,而改性的方法需要镀制2~200μm,由于中频磁控溅射沉积速率较低,在此工艺环节,本发明所采用方法加工效率也大大优于已有加工方法;2. The idea of the modification method in the traditional process is based on the fact that RB-SiC is brittle and hard to process, and the material composition is complex (including Si and SiC in different proportions). Due to its inconsistent composition, all in small tool polishing or traditional During the grinding process, the removal efficiency of Si and SiC in different phases is different, and it is almost impossible to achieve smooth surface processing. Therefore, a modification method was proposed, the core of which is to deposit a sufficiently thick Si layer on the surface of RB-SiC , as long as its bonding strength with the substrate RB-SiC film can be guaranteed, the subsequent method is only to polish the silicon layer, and does not involve the polishing of the substrate RB-SiC material. Therefore, the modification method must make the deposited silicon layer thick enough , to avoid subsequent processing to the substrate. In the magnetron sputtering deposition process of the present invention, only a 100-500nm Si planarization layer needs to be plated, while the modified method needs to be plated with a 2-200μm layer. Due to the low deposition rate of the intermediate frequency magnetron sputtering, this process link, the processing efficiency of the method adopted by the present invention is also much better than the existing processing method;

3、传统工艺中采用磁控溅射沉积硅层的目的是表面改性,而本发明采用磁控溅射沉积硅层的目的是平坦化,膜层厚度在数百纳米以内时,薄膜沉积后可实现材料表面质量在一定程度上的优化,主要表现在表面粗糙度变小,中频加工误差变小,本发明专利正基于这一考虑,在薄膜沉积过程中,通过优化调整工艺参数,在保证膜基结合强度的条件下,镀制100~500nm薄膜层,可将材料表面粗糙度优化至RMS2nm以下;3. The purpose of using magnetron sputtering to deposit a silicon layer in the traditional process is surface modification, while the purpose of using magnetron sputtering to deposit a silicon layer in the present invention is to planarize. When the film thickness is within hundreds of nanometers, after film deposition The surface quality of the material can be optimized to a certain extent, mainly manifested in the reduction of the surface roughness and the reduction of the intermediate frequency processing error. The patent of the present invention is based on this consideration. During the film deposition process, the process parameters are optimized and adjusted to ensure Under the condition of the bonding strength of the film base, the surface roughness of the material can be optimized to below RMS2nm by plating a 100~500nm thin film layer;

4、利用等离子体实现含氟反应气体的激发(注意,不需要离化),利用这些活性基作用于材料表面,由于抑制了活性离子或其他离子的作用,故在抛光过程中不会发生物理溅射刻蚀作用,而仅利用Si和SiC与含氟活性基的化学反应,实现大面积均匀刻蚀抛光,有效抑制了平坦化层与光学元件基底的热失配问题引起的膜层龟裂或脱落,而且由于其反应速度是由活性基的浓度确定,故而,可以很容易的实行表面平坦化层纳米量级的刻蚀精度,在前面步骤的基础上,进一步使材料表面粗糙度减小到RMS1nm以下;4. Use plasma to realize the excitation of fluorine-containing reactive gas (note that ionization is not required), and use these active groups to act on the surface of the material. Since the action of active ions or other ions is suppressed, no physical damage will occur during the polishing process. Sputter etching, but only use the chemical reaction between Si and SiC and fluorine-containing active groups to achieve large-area uniform etching and polishing, effectively suppressing the cracking of the film layer caused by the thermal mismatch between the planarization layer and the optical element substrate or fall off, and because its reaction rate is determined by the concentration of active groups, it is easy to implement the etching precision of the surface planarization layer at the nanometer level, and further reduce the surface roughness of the material on the basis of the previous steps To below RMS1nm;

5、离子束抛光修形方法是目前在非接触抛光修形方法中应用较为成熟的一种方法,该方法并不能直接用于RB-SiC材料的抛光修形,其原因也是在于RB-SiC不同物相的溅刻效率不同,而导致抛光过程中面形劣化。而本发明中,由于利用磁控溅射沉积有平坦化层,因此离子束抛光修形方法可直接作用于Si薄膜表面,实现了大面积光学元件的面形保持;5. The ion beam polishing modification method is a relatively mature method used in the non-contact polishing modification method at present. This method cannot be directly used for the polishing modification of RB-SiC materials. The reason is that RB-SiC is different. The sputtering efficiency of the phases is different, which leads to the deterioration of the surface shape during the polishing process. However, in the present invention, due to the use of magnetron sputtering to deposit a planarization layer, the ion beam polishing modification method can directly act on the surface of the Si film, realizing the surface shape maintenance of large-area optical elements;

6、本发明所采用的抛光方法均是以等离子体抛光和离子束抛光加工为主,均是非接触加工,刻蚀过程中不存在接触应力和应变,可实现全口径高精度粗糙度,在兼顾面形和表面质量的同时,可实现光学元件的高效化整形抛光,极大提高了抛光效率,降低时间成本。这对SiC这种脆硬材料而言,彻底避免了传统加工方法或小工具等接触式加工方法对元件的表面及亚表面损伤,不会产生应力问题。6. The polishing methods adopted in the present invention are all based on plasma polishing and ion beam polishing, both of which are non-contact processing. There is no contact stress and strain in the etching process, and full-caliber high-precision roughness can be achieved. While improving the surface shape and surface quality, it can achieve high-efficiency shaping and polishing of optical components, greatly improving polishing efficiency and reducing time costs. For brittle and hard materials such as SiC, this completely avoids damage to the surface and subsurface of components by traditional processing methods or contact processing methods such as small tools, and will not cause stress problems.

附图说明Description of drawings

读者在参照附图阅读了本发明的具体实施方式以后,将会更清楚地了解本发明的各个方面。其中,Readers will have a clearer understanding of various aspects of the present invention after reading the detailed description of the present invention with reference to the accompanying drawings. in,

图1为本发明实施例中的加工工艺流程示意图;Fig. 1 is the schematic diagram of processing technology flow in the embodiment of the present invention;

图2为本发明实施例中ICP刻蚀工作原理示意图;2 is a schematic diagram of the working principle of ICP etching in an embodiment of the present invention;

图3为本发明实施例中射频磁控溅射原理示意图;3 is a schematic diagram of the principle of radio frequency magnetron sputtering in an embodiment of the present invention;

图4为本发明实施例中采用自由基等离子源原理示意图;4 is a schematic diagram of the principle of using a free radical plasma source in an embodiment of the present invention;

图5为不同工艺下的光学元件表面粗糙度测试结果图;Figure 5 is a graph of the surface roughness test results of optical elements under different processes;

其中,a为初步经过ICP刻蚀后的反应烧结碳化硅基底表面粗糙度测试图,b为在反应烧结碳化硅基底表面沉积硅平坦化层的表面粗糙度测试图,c为RPS刻蚀平坦化层后的表面粗糙度测试图。Among them, a is the surface roughness test diagram of the reaction sintered silicon carbide substrate after preliminary ICP etching, b is the surface roughness test diagram of the silicon planarization layer deposited on the surface of the reaction sintered silicon carbide substrate, and c is the RPS etching planarization Surface roughness test chart after layer.

具体实施方式Detailed ways

为了使本申请所揭示的技术内容更加详尽与完备,可参照附图以及本发明的下述各种具体实施例。In order to make the technical content disclosed in this application more detailed and complete, reference may be made to the accompanying drawings and the following various specific embodiments of the present invention.

一种RB-SiC光学元件抛光工艺加工方法,包括以下步骤:A polishing process method for RB-SiC optical components, comprising the following steps:

步骤1,首先对RB-SiC毛坯料进行抛光刻蚀加工,实现光学元件的精密磨削,使光学元件表面粗糙度值收敛到20纳米以内;Step 1. Firstly, the RB-SiC blank is polished and etched to realize the precision grinding of the optical element, so that the surface roughness value of the optical element converges to within 20 nanometers;

步骤2,利用射频磁控溅射技术(RF-MS)在RB-SiC光学元件表面沉积纳米级平坦化层;Step 2, using radio frequency magnetron sputtering (RF-MS) to deposit a nanoscale planarization layer on the surface of the RB-SiC optical element;

步骤3,利用自由基微波等离子体源技术(RPS)对RB-SiC基底表面沉积的平坦化层进行抛光加工,利用自由基等离子体技术,将等离子体限定于等离子源本体之内,通过真空室流导控制,形成大面积均匀活性自由基,使得活性基与平坦化层材料发生化学化学反应,实现光学元件表面超光滑抛光加工;Step 3, use the radical microwave plasma source technology (RPS) to polish the planarization layer deposited on the surface of the RB-SiC substrate, use the radical plasma technology to confine the plasma within the plasma source body, and pass through the vacuum chamber Conductance control, forming a large area of uniform active radicals, making the active radicals chemically react with the material of the planarization layer, and realizing ultra-smooth polishing of the surface of optical components;

步骤4,利用离子束修形抛光技术(IBF),对光学元件表面平坦化层进行修形和抛光,通过对表面的高确定性去除,实现光学元件表面面形修正。Step 4: Use ion beam modification polishing technology (IBF) to modify and polish the planarization layer on the surface of the optical element, and realize the surface shape modification of the optical element by removing the surface with high certainty.

所述步骤1中ICP刻蚀抛光装置,其本底真空2.0×10-4Pa,工作真空控制在0.5~10Pa。The ICP etching and polishing device in the step 1 has a background vacuum of 2.0×10 -4 Pa and a working vacuum of 0.5-10 Pa.

初始毛坯料表面粗糙度RMS>100nm时,偏压功率维持100~150W,反应活性气体采用高纯度四氟化碳(纯度99.99%)。When the initial blank surface roughness RMS>100nm, the bias power is maintained at 100~150W, and the reactive gas uses high-purity carbon tetrafluoride (purity 99.99%).

针对RMS>100nm初始RB-SiC工件,射频功率150W,偏压功率150W,刻蚀气体流量为25~30sccm,工作气压2~5Pa。For the initial RB-SiC workpiece with RMS>100nm, the RF power is 150W, the bias power is 150W, the etching gas flow rate is 25~30sccm, and the working pressure is 2~5Pa.

所述步骤4中采用13.56MHz的射频离子源,利用三维运动控制系统控制离子源加工轨迹和驻留时间,所采用真空腔室本底真空1.0×10-4Pa,以高纯度氩气(纯度99.99%)为工作气体。In the step 4 , a 13.56MHz radio frequency ion source is used, and the three-dimensional motion control system is used to control the processing trajectory and residence time of the ion source. 99.99%) is the working gas.

步骤2中工作真空度1.2Pa,靶功率密度控制在5~10W/cm2In step 2, the working vacuum degree is 1.2Pa, and the target power density is controlled at 5~10W/cm 2 .

步骤3中通过真空气体流导和真空泵抽速控制,形成均匀性<5%活性基区,抛光时典型的真空度在50~100Pa。In step 3, the conductance of the vacuum gas and the pumping speed of the vacuum pump are controlled to form an active base area with a uniformity of <5%. The typical vacuum degree during polishing is 50-100Pa.

步骤4离子束能量控制在800eV以下,束斑尺寸控制在10mm以下,刻蚀效率1.0×10-3~0.02mm3/min。In step 4, the ion beam energy is controlled below 800eV, the beam spot size is controlled below 10mm, and the etching efficiency is 1.0×10 -3 ~0.02mm 3 /min.

下面参照附图,对本发明各个方面的具体实施方式作进一步的详细描述。The specific implementation manners of various aspects of the present invention will be further described in detail below with reference to the accompanying drawings.

本发明涉及的反应烧结碳化硅光学元件表面平坦化加工方法,能够实现反应烧结碳化硅光学元件表面的平坦化加工效果,粗糙度可小于1nm。The surface flattening processing method of the reaction sintered silicon carbide optical element involved in the present invention can realize the flattening processing effect of the surface of the reaction sintered silicon carbide optical element, and the roughness can be less than 1 nm.

参见图1:See Figure 1:

本发明将ICP等离子体抛光技术、射频磁控溅射平坦化层沉积技术(RF-MS)、自由基等离子体源抛光技术(PR2)和离子束修形抛光技术相结合,构建一套完整的抛光工艺流程。该工艺方法的基本思路在于利用等离子体技术实现RB-SiC光学元件的无损抛光,克服传统光学加工方法引入的应力及损伤问题,其二是利用物理气相沉积方法,利用在光学元件表面沉积平坦化层的思路,在改善光学元件表面粗糙度的同时,使得光学元件表面材质同一化,从而使得离子束修形抛光成为可能,而纳米级的平坦化层厚度则保证了工艺周期的高效性。The present invention combines ICP plasma polishing technology, radio frequency magnetron sputtering planarization layer deposition technology (RF-MS), free radical plasma source polishing technology (PR2) and ion beam modification polishing technology to construct a complete set of Polishing process. The basic idea of this process is to use plasma technology to realize non-destructive polishing of RB-SiC optical components, to overcome the stress and damage problems introduced by traditional optical processing methods, and the second is to use physical vapor deposition method to planarize the surface of optical components. The idea of layer, while improving the surface roughness of the optical element, makes the surface material of the optical element uniform, thus making ion beam modification and polishing possible, and the thickness of the nano-level planarization layer ensures the efficiency of the process cycle.

为实现如上目的,本发明专利的具体方案为:In order to achieve the above object, the specific scheme of the patent of the present invention is:

1)首先利用ICP抛光刻蚀技术实现RB-SiC毛坯样品的进行刻蚀加工,针对不同粗糙度的光学元件,着重通过偏压功率和反应气体流量工艺参数,使光学元件毛坯样品的表面粗糙度值收敛于20纳米以下,实现光学元件样品的精磨和抛亮工序。1) First, use ICP polishing and etching technology to realize the etching process of RB-SiC blank samples. For optical components with different roughness, focus on the bias power and reaction gas flow process parameters to make the surface roughness of optical component blank samples The value converges below 20 nanometers to realize the fine grinding and polishing process of optical component samples.

2)之后,利用射频磁控溅射技术在精磨抛亮后的RB-SiC工件表面沉积Si平坦化层,通过射频磁控溅射过程中的靶功率密度,气体质量流量、工作气压等参数进行调节,确定合适的沉积速率15nm/min~20nm/min),通过光学元件旋转,实现Si平坦化层均匀沉积,并使光学元件表面粗糙度值降至2nm以下,同时为保证后续离子束修形工艺需要,平坦化层厚度控制在100~500nm。2) Afterwards, use radio frequency magnetron sputtering technology to deposit a Si planarization layer on the surface of the RB-SiC workpiece after fine grinding and polishing. Adjust to determine the appropriate deposition rate (15nm/min~20nm/min), through the rotation of the optical element, realize the uniform deposition of the Si planarization layer, and reduce the surface roughness value of the optical element to below 2nm. According to the requirements of the forming process, the thickness of the planarization layer is controlled at 100~500nm.

3)第三步利用RPS刻蚀抛光技术对RB-SiC表面沉积的平坦化层进行刻蚀抛光,利用该方法可以实现大面积(>Ф300mm口径)复杂表面的抛光加工,RPS技术通过2.45GHz的微波激励源,使得N2气电离形成等离子体,由于未施加任何引出电极,等离子体被约束在等离子体源内部,此时通入高纯度的含氟气体和氧气等活性气体在等离子体的作用下被激活,少量离化的活性气体仍然被约束在等离子体源内部,而大量的被激活的活性基,在真空流导的控制下,形成了一个大面积的均匀区,直接作用于光学元件表面,通过活性基气体与Si的化学反应,实现抛光的效果,最终优化表面粗糙度至1nm以下。3) The third step is to use RPS etching and polishing technology to etch and polish the planarization layer deposited on the surface of RB-SiC. This method can realize the polishing of large-area (> Ф 300mm caliber) complex surfaces. RPS technology passes 2.45GHz The microwave excitation source makes the N2 gas ionize to form plasma. Since no extraction electrode is applied, the plasma is confined inside the plasma source. At this time, high-purity fluorine-containing gas and oxygen and other active gases are introduced into the plasma Activated under the action of the ionized active gas, a small amount of ionized active gas is still confined inside the plasma source, while a large number of activated active radicals form a large-area uniform area under the control of vacuum conductance, directly acting on the optical The surface of the component is polished through the chemical reaction between the active radical gas and Si, and the surface roughness is finally optimized to less than 1nm.

4)最后,利用离子束抛光技术对RPS抛光后的RB-SiC光学元件进行离子束修形抛光,通过对离子源特征参数调整控制去除函数,继而通过实际面形和理想面形差值,获得元件表面各点驻留时间,通过三维运动控制系统,实现学元件的面形修正,修正面形可达1/5~1/10λ4) Finally, use ion beam polishing technology to perform ion beam modification and polishing on the RB-SiC optical element after RPS polishing, control the removal function by adjusting the characteristic parameters of the ion source, and then use the difference between the actual surface shape and the ideal surface shape to obtain The residence time of each point on the surface of the component, through the three-dimensional motion control system, realizes the surface shape correction of the chemical component, and the corrected surface shape can reach 1/5~1/10 λ .

实施例1:Example 1:

1)ICP刻蚀:参见图2,ICP刻蚀设备真空腔室的本底真空2.0×10-4Pa,工作真空控制在0.5~10Pa 。将口径150mm,厚度10mm的反应烧结碳化硅样品(RMS在209.72nm)放入ICP刻蚀设备真空腔室的基台上,依次打开预抽阀、前级阀,当复合真空计气压值降至5Pa时,打开分子泵,按下启动按钮,待分子泵转速达到400r/min,打开高阀,同时关闭预抽阀,当复合真空计气压值低于10-1Pa时,将气体流量计上CF4气体流量计开关拨到阀控位置,调节流量计的旋钮,将两种气体流量分别设置为25sccm然后打开气体总阀,调节高阀,让气压稳定在1Pa,通过时间控制器将刻蚀时间设置为3000s,此时同时打开射频电源和偏压电源,调节匹配旋钮,分别将射频功率和偏压功率设置为150W,待刻蚀结束后,按顺序依次关闭气体总阀、气体流量计开关、分子泵停止按钮,直至分子泵转速降为0,再关闭高阀、前级阀,冷却两分钟后,按下充气阀按钮,充气结束后按下开盖按钮,取出刻蚀后的样片进行表面粗糙度测试,测试结果RMS值为16.702nm。1) ICP etching: see Figure 2, the background vacuum of the vacuum chamber of the ICP etching equipment is 2.0×10 -4 Pa, and the working vacuum is controlled at 0.5~10Pa. Put the reaction sintered silicon carbide sample (RMS at 209.72nm) with a diameter of 150mm and a thickness of 10mm on the base of the vacuum chamber of the ICP etching equipment, and open the pre-pumping valve and the front-stage valve in sequence. When the pressure value of the composite vacuum gauge drops to At 5Pa, turn on the molecular pump and press the start button. When the speed of the molecular pump reaches 400r/min, open the high valve and close the pre-pumping valve at the same time. When the pressure value of the composite vacuum gauge is lower than 10 -1 Pa, turn on the gas flowmeter Switch the switch of the CF 4 gas flowmeter to the valve control position, adjust the knob of the flowmeter, set the flow rates of the two gases to 25sccm respectively, then open the main gas valve, adjust the high valve, let the air pressure stabilize at 1Pa, and pass the time controller to etch The time is set to 3000s. At this time, turn on the RF power supply and the bias power supply at the same time, adjust the matching knob, and set the RF power and bias power to 150W respectively. After the etching is completed, turn off the main gas valve and the gas flow meter switch in sequence. , Molecular pump stop button, until the molecular pump speed drops to 0, then close the high valve and front valve, after cooling for two minutes, press the inflation valve button, after the inflation is completed, press the open button, take out the etched sample for Surface roughness test, the test result RMS value is 16.702nm.

2)射频磁控溅射沉积平坦化层:2) Deposit planarization layer by radio frequency magnetron sputtering:

在ICP刻蚀后的反应烧结碳化硅基底上利用射频磁控溅射技术镀制Si平坦化层。参见图3,采用通用射频磁控溅射设备,所用溅射靶材为高纯度硅靶,纯度为99.9995%,工作气体确定为氩气,纯度为99.99%,射频频率为13.56MHz。本底真空抽至8.0×10-4Pa,然后将氩气流量设定为40sccm,工作气压设定为1.2Pa,同时将预镀基片通过旋转样品台旋转至对应溅射靶的上方位置,靶基距为80mm;打开射频电源,将射频功率密度调至10W/cm2,放电后先预溅射15min,再关闭挡板,沉积薄膜厚度为386nm;关闭射频电源、进气阀及分子泵和真空腔室之间的挡板阀,保压退火15min,关闭电离规,打开充气阀,充气结束后取出样品,测试其表面粗糙度RMS值为1.6599nm。A Si planarization layer was plated on the reaction sintered silicon carbide substrate after ICP etching by using radio frequency magnetron sputtering technology. Referring to Fig. 3, general-purpose radio frequency magnetron sputtering equipment is used, the sputtering target used is a high-purity silicon target with a purity of 99.9995%, the working gas is determined to be argon with a purity of 99.99%, and the radio frequency is 13.56MHz. The background vacuum was evacuated to 8.0×10 -4 Pa, and then the argon flow rate was set to 40 sccm, and the working pressure was set to 1.2 Pa. At the same time, the pre-coated substrate was rotated to the position above the corresponding sputtering target by rotating the sample stage. The target base distance is 80mm; turn on the RF power supply, adjust the RF power density to 10W/cm 2 , pre-sputter for 15 minutes after discharge, and then close the baffle, the thickness of the deposited film is 386nm; turn off the RF power supply, intake valve and molecular pump The baffle valve between the vacuum chamber and the vacuum chamber was annealed for 15 minutes under pressure, the ionization gauge was closed, the inflation valve was opened, and the sample was taken out after inflation, and the RMS value of the surface roughness was tested to be 1.6599nm.

3)RPS刻蚀抛光:参见图3,将真空室抽至本底真空2.0×10-3Pa,通入500Sccm高纯N2(纯度99.999%),打开2.45GHz微波电源,将微波电源设定在1.5KW,稳定15min之后,将N2流量降至100Sccm,通入450SccmCF4(纯度99.99%)和30Sccm的O2(纯度99.999%),调节真空气体抽速,将真空度设定在60Pa,对光学元件表面进行抛光,当Si平坦化层去除150nm后,测试刻蚀平坦化层后的表面粗糙度RMS值为0.79706nm。其中垂直方向分布的磁力线将电子约束在靶材表面附近,延长其在等离子体中的运动轨迹,提高电子参与气体分子碰撞和电离过程的几率。3) RPS etching and polishing: see Figure 3, evacuate the vacuum chamber to a background vacuum of 2.0×10 -3 Pa, feed 500Sccm high-purity N 2 (purity 99.999%), turn on the 2.45GHz microwave power supply, and set the microwave power supply to At 1.5KW, after stabilizing for 15 minutes, reduce the N 2 flow rate to 100Sccm, feed 450Sccm CF 4 (purity 99.99%) and 30Sccm O 2 (purity 99.999%), adjust the vacuum gas pumping speed, and set the vacuum degree at 60Pa. The surface of the optical element was polished, and when the Si planarization layer was removed by 150nm, the RMS value of the surface roughness after etching the planarization layer was tested to be 0.79706nm. Among them, the magnetic field lines distributed in the vertical direction confine electrons near the surface of the target, prolong their trajectory in the plasma, and increase the probability of electrons participating in gas molecule collisions and ionization processes.

4)离子束抛光:参见图4,设定典型的离子源工作参数:本底真空1.0×10-4Pa,射频功率180W,束压500V,加速栅电压100V,氩气(99.99%)流量5Sccm,工作真空度5.0×10-2Pa,束斑直径控制在Ф10~5mm变化,确定去除效率控制在5.0×10-3~0.01mm3/min,变化,最终实现实现光学元件的面形修正至1/10λ。4) Ion beam polishing: see Figure 4, set typical ion source working parameters: background vacuum 1.0×10 -4 Pa, RF power 180W, beam voltage 500V, accelerating grid voltage 100V, argon (99.99%) flow rate 5Sccm , the working vacuum degree is 5.0×10 -2 Pa, the diameter of the beam spot is controlled at Ф 10~5mm, and the removal efficiency is determined to be controlled at 5.0×10 -3 ~0.01mm 3 /min, and finally the surface shape correction of the optical element is realized. to 1/10λ.

本实施例中,采用13.56MHz的射频离子源,利用三维运动控制系统控制离子源加工轨迹和驻留时间,所采用真空腔室本底真空1.0×10-4Pa,以高纯度氩气(纯度99.99%)为工作气体。In this embodiment, a 13.56MHz radio frequency ion source is used, and the three-dimensional motion control system is used to control the processing trajectory and residence time of the ion source. The background vacuum of the vacuum chamber used is 1.0×10 -4 Pa. 99.99%) is the working gas.

参见图5,是利用泰勒霍普森的Taly Surf CCI2000型非接触式白光干涉仪对ICP精磨抛光、磁控溅射平坦化沉积,以及RPS抛光之后样品表面粗糙度进行测量,其中,图5(a)是ICP精磨抛光后样品表面的测试点粗糙度情况,由图可知,RMS已由毛坯料的209.72nm下降至RMS16.702nm,当镀制一层硅平坦化层之后,样品表面粗糙度下降至RMS1.6599nm(如图5(b)所示),而最终采用RPS抛光之后,RB-SiC表面粗糙度下降至0.79706nm,下降至1nm以下,成功实现超光滑表面加工。See Figure 5, which uses Taylor Hobson's Taly Surf CCI2000 non-contact white light interferometer to measure the surface roughness of the sample after ICP fine grinding and polishing, magnetron sputtering planarization deposition, and RPS polishing, among them, Figure 5 (a) is the roughness of the test point on the surface of the sample after ICP fine grinding and polishing. It can be seen from the figure that the RMS has dropped from 209.72nm of the blank to RMS16.702nm. After plating a layer of silicon planarization layer, the surface of the sample is rough The surface roughness of RB-SiC dropped to RMS1.6599nm (as shown in Figure 5(b)), and after RPS polishing was finally used, the surface roughness of RB-SiC dropped to 0.79706nm, down to below 1nm, successfully achieving ultra-smooth surface processing.

以上所述为本发明的优选实施方式,但对于本领域普通技术人员来说,其内容并不仅限于实施例,通过阅读本发明的说明书,在不脱离本发明原理的前提下作出一些更改和变化,凡属于本发明思路下的技术方案,均在本发明权利要求的保护范围。The above is a preferred embodiment of the present invention, but for those of ordinary skill in the art, its content is not limited to the examples. By reading the description of the present invention, some changes and changes can be made without departing from the principles of the present invention. , All technical solutions under the idea of the present invention are within the protection scope of the claims of the present invention.

Claims (8)

  1. The RB-SiC optical element polishing process machining method comprises the following steps:
    step 1, firstly, polishing and etching RB-SiC blank materials to realize precise grinding of optical elements, so that the roughness value of the surfaces of the optical elements is converged within 20 nanometers;
    step 2, depositing a nanoscale planarization layer on the surface of the RB-SiC optical element by utilizing a radio frequency magnetron sputtering technology (RF-MS);
    step 3, polishing the planarization layer deposited on the surface of the RB-SiC substrate by utilizing a free radical microwave plasma source technology (RPS), limiting plasma in a plasma source body by utilizing the free radical plasma technology, and forming large-area uniform active free radicals by controlling the conductance of a vacuum chamber, so that the active radicals and the planarization layer material perform chemical reaction to realize the ultra-smooth polishing processing of the surface of the optical element;
    and 4, utilizing an ion beam shape-modifying polishing technology (IBF) to modify and polish the surface planarization layer of the optical element, and realizing the surface shape modification of the surface of the optical element by removing the surface with high certainty.
  2. 2. The RB-SiC optical element polishing process machining method according to claim 1, characterized in that: the polishing etching in the step 1 is an ICP etching polishing device with a background vacuum of 2.0 multiplied by 10-4Pa, and the working vacuum is controlled to be 0.5-10 Pa.
  3. 3. The RB-SiC optical element polishing process machining method according to claim 2, characterized in that: when the initial blank surface roughness RMS is more than 100nm, the bias power is maintained at 100-150W, and the reactive gas is carbon tetrafluoride with the purity of 99.99%.
  4. 4. The RB-SiC optical element polishing process machining method according to claim 3, characterized in that: aiming at an initial RB-SiC workpiece with RMS of more than 100nm, the radio frequency power is 150W, the bias power is 150W, the etching gas flow is 25-30 sccm, and the working pressure is 2-5 Pa.
  5. 5. The RB-SiC optical element polishing process machining method according to claim 4, wherein: in the step 4, a 13.56MHz radio frequency ion source is adopted, a three-dimensional motion control system is used for controlling the processing track and the residence time of the ion source, and the background vacuum of a vacuum chamber is 1.0 multiplied by 10-4Pa, argon with the purity of 99.99 percent is used as working gas.
  6. 6. RB-SiC optical element polishing according to claim 5The technical processing method is characterized in that: in the step 2, the working vacuum degree is 1.2Pa, and the target power density is controlled to be 5-10W/cm2
  7. 7. The RB-SiC optical element polishing process machining method according to claim 6, characterized in that: and 3, forming an active base region with the uniformity of less than 5% by controlling the vacuum gas conductance and the pumping speed of a vacuum pump, wherein the typical vacuum degree is 50-100 Pa during polishing.
  8. 8. The RB-SiC optical element polishing process machining method according to claim 7, characterized in that: step 4, controlling the ion beam energy below 800eV, controlling the beam spot size below 10mm, and controlling the etching efficiency to be 1.0 multiplied by 10-3~0.02mm3/min。
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