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CN117551424A - Oil-based thermosensitive active grinding fluid and microwave-assisted fixed abrasive grinding method - Google Patents

Oil-based thermosensitive active grinding fluid and microwave-assisted fixed abrasive grinding method Download PDF

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Publication number
CN117551424A
CN117551424A CN202311501800.7A CN202311501800A CN117551424A CN 117551424 A CN117551424 A CN 117551424A CN 202311501800 A CN202311501800 A CN 202311501800A CN 117551424 A CN117551424 A CN 117551424A
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grinding
microwave
workpiece
oil
fixed abrasive
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CN117551424B (en
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黄水泉
杨飞燕
黄传真
黄含
穆德魁
王真
徐龙华
曲美娜
许征凯
张迪嘉
郭保苏
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Yanshan University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions
    • 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
    • B24B57/00Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
    • B24B57/02Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Grinding And Polishing Of Tertiary Curved Surfaces And Surfaces With Complex Shapes (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The invention discloses an oil-based thermosensitive active grinding fluid and a microwave-assisted fixed abrasive grinding method, wherein the oil-based thermosensitive active grinding fluid comprises the following components: the mass percent of the propylene glycol is 0.5-5%, the mass percent of the triethanolamine is 0.5-5%, the mass percent of the thermosensitive oxidant is 1-10%, and the balance is vegetable oil. The thermal decomposition initiator in the thermally-induced thermosensitive active grinding fluid is decomposed to generate free radicals with strong chemical activity, so that the hard and brittle materials under the action of mechanical force are quickly subjected to chemical modification, and a relatively softer modification layer is generated on the surface of the matrix; under the action of microwave heating, the thermosensitive active grinding fluid is used as a conducting medium to transfer heat to the surface of a workpiece to be processed, so that the plastic deformation capacity of the surface modified layer material of the workpiece is improved; the diamond fixed abrasive millstone mechanically removes the surface material of the workpiece softened by microwave heating, the low-hardness modified layer is broken and peeled off in a layered manner, and the rapidly exposed new surface is further modified and removed, so that high processing efficiency is obtained.

Description

一种油基热敏活性研磨液及微波辅助固结磨料研磨方法An oil-based heat-sensitive active grinding fluid and microwave-assisted bonded abrasive grinding method

技术领域Technical field

本发明涉及难加工材料超精密加工技术领域,涉及一种油基热敏活性研磨液及微波辅助固结磨料研磨方法,该研磨液及研磨方法尤其适用于脆性晶体材料。The invention relates to the technical field of ultra-precision machining of difficult-to-machine materials, and relates to an oil-based heat-sensitive active grinding fluid and a microwave-assisted bonded abrasive grinding method. The grinding fluid and grinding method are particularly suitable for brittle crystal materials.

背景技术Background technique

这里的陈述仅提供与本发明相关的背景技术,而不必然地构成现有技术。The statements herein merely provide background information related to the present invention and do not necessarily constitute prior art.

脆性晶体材料,如单晶硅、氧化铝、碳化硅、氮化镓,是能源、通信、交通和医疗领域的核心材料。脆性半导体材料制备的功率器件和射频器件则被广泛应用于新能源汽车、5G通讯、光伏发电、轨道交通、智能电网和航空航天等现代工业领域。但是,上述脆性晶体材料具有硬度高、脆性大以及化学性质稳定等特点,是典型的难加工材料。工件表面质量及加工精度会显著影响半导体器件的性能、能耗和寿命,因此实现脆性材料高效率、低损伤和超精密加工显得尤为重要。Brittle crystal materials, such as single crystal silicon, alumina, silicon carbide, and gallium nitride, are core materials in the fields of energy, communications, transportation, and medical care. Power devices and radio frequency devices made of brittle semiconductor materials are widely used in modern industrial fields such as new energy vehicles, 5G communications, photovoltaic power generation, rail transportation, smart grids, and aerospace. However, the above-mentioned brittle crystalline materials have the characteristics of high hardness, great brittleness and stable chemical properties, and are typically difficult-to-process materials. The surface quality and processing accuracy of the workpiece will significantly affect the performance, energy consumption and life of semiconductor devices. Therefore, it is particularly important to achieve high efficiency, low damage and ultra-precision processing of brittle materials.

国内外主要采用磨削、研磨和抛光对线切割而成的脆性晶体材料进行超精密加工,控制形状精度、表面质量及亚表面损伤深度。研磨通常采用1~15μm的游离金刚石磨料机械去除磨削过程产生的损伤层,CN110421481A提供了一种游离磨料机械研磨加工硬脆蓝宝石的方法,但高硬度和强耐磨的材料特性以及三体磨损去除材料的加工方式,导致游离磨料研磨蓝宝石时材料去除速率极低、工件面形精度差。CN110539209A则提供了一种游离磨料研磨和固结磨料研磨相结合加工蓝宝石晶圆的方法,固结磨料磨盘研磨可有效增大研磨压力,提高材料去除速率,同时获得高的加工精度,但是二体磨损机械去除材料的加工方式导致研磨表面和亚表面质量相对较差,显著增加了后续化学机械抛光处理的时间和成本。鉴于第三代半导体材料高硬度、强耐磨、高脆性的材料特性,现有研磨方法加工硬脆材料存在效率极低或加工表面质量差的问题,亟需研发一种能兼顾表面质量与加工效率的研磨方法,降低整个脆性材料,特别是硬脆材料的制造加工成本,加速高效能半导体器件的发展。Grinding, grinding and polishing are mainly used at home and abroad for ultra-precision processing of brittle crystal materials made by wire cutting to control shape accuracy, surface quality and sub-surface damage depth. Grinding usually uses 1 to 15 μm free diamond abrasives to mechanically remove the damage layer generated during the grinding process. CN110421481A provides a method of mechanical grinding and processing of hard and brittle sapphire with free abrasives, but the material properties of high hardness and strong wear resistance and three-body wear The processing method of material removal results in extremely low material removal rate and poor surface accuracy of the workpiece when grinding sapphire with free abrasives. CN110539209A provides a method for processing sapphire wafers by combining free abrasive grinding and fixed abrasive grinding. Fixed abrasive disc grinding can effectively increase the grinding pressure, improve the material removal rate, and obtain high processing accuracy at the same time. However, the two-body method The processing method of abrasive mechanical removal of material results in relatively poor grinding surface and subsurface quality, significantly increasing the time and cost of subsequent chemical mechanical polishing treatments. In view of the material characteristics of third-generation semiconductor materials such as high hardness, strong wear resistance, and high brittleness, existing grinding methods for processing hard and brittle materials have problems such as extremely low efficiency or poor surface quality. There is an urgent need to develop a method that can take into account both surface quality and processing. Efficient grinding methods reduce the manufacturing and processing costs of brittle materials, especially hard and brittle materials, and accelerate the development of high-efficiency semiconductor devices.

发明内容Contents of the invention

针对难加工脆性晶体材料研磨效率与表面质量之间的突出矛盾,本发明提供一种油基热敏活性研磨液及微波辅助固结磨料研磨方法。In view of the prominent contradiction between grinding efficiency and surface quality of difficult-to-process brittle crystalline materials, the present invention provides an oil-based heat-sensitive active grinding fluid and a microwave-assisted fixed abrasive grinding method.

为了实现上述目的,本发明是通过如下的技术方案来实现:In order to achieve the above objects, the present invention is achieved through the following technical solutions:

第一方面,本发明提供一种油基热敏活性研磨液,包括以下组分:丙二醇的质量百分数为0.5%~5%,三乙醇胺的质量百分数为0.5%~5%,热敏氧化剂的质量百分数为1%~10%,余量为植物油。In a first aspect, the present invention provides an oil-based heat-sensitive active grinding fluid, which includes the following components: a mass percentage of propylene glycol of 0.5% to 5%, a mass percentage of triethanolamine of 0.5% to 5%, and a mass percentage of heat-sensitive oxidant. The percentage is 1% to 10%, and the balance is vegetable oil.

在一些实施例中,所述热敏氧化剂选自过氧化氢、过氧化碳酸二环己酯(DCPD)或过氧化二碳酸二异丙酯(IPP)中的一种或多种的组合。In some embodiments, the heat-sensitive oxidant is selected from one or a combination of one or more of hydrogen peroxide, dicyclohexyl peroxycarbonate (DCPD), or diisopropyl peroxydicarbonate (IPP).

热分解引发剂是指能受热分解产生自由基对机械力作用下的硬脆材料进行可控化学改性的热分解型引发剂。Thermal decomposition initiator refers to a thermal decomposition initiator that can be thermally decomposed to produce free radicals for controllable chemical modification of hard and brittle materials under the action of mechanical force.

油基热敏活性研磨液的主要作用原理:微波诱导热敏活性研磨液中热分解型引发剂分解产生强化学活性的自由基,快速对机械力作用下的硬脆材料进行化学改性,促进基体表面产生一层相对更软的改性层;微波加热作用下,热敏活性研磨液作为传导介质将热量传递到待加工工件表面,提高工件表层改性层材料的塑性变形能力;金刚石固结磨料磨盘机械去除被微波加热软化的工件表层材料,低硬度的改性层破碎、层状剥落,快速暴露的新生面被进一步改性和去除,获得高的加工效率;利用丙二醇和三乙醇胺协同调控金刚石磨粒与改性层间的接触应力,实现难加工硬脆材料的高效率、低损伤超精密研磨加工。The main working principle of oil-based thermally active polishing fluid: microwave-induced thermal decomposition initiator in the thermally active polishing fluid decomposes to produce highly chemically active free radicals, which can quickly chemically modify hard and brittle materials under the action of mechanical force, and promote A relatively softer modified layer is produced on the surface of the substrate; under the action of microwave heating, the heat-sensitive active grinding fluid acts as a conductive medium to transfer heat to the surface of the workpiece to be processed, improving the plastic deformation ability of the modified layer material on the surface of the workpiece; diamond consolidation The abrasive disc mechanically removes the surface material of the workpiece softened by microwave heating. The modified layer with low hardness is broken and peeled off in layers. The newly exposed surface is further modified and removed to obtain high processing efficiency. Propylene glycol and triethanolamine are used to synergistically regulate diamond. The contact stress between the abrasive particles and the modified layer enables high-efficiency, low-damage ultra-precision grinding of hard and brittle materials that are difficult to machine.

具体如下:有机过氧类热分解引发剂过氧化碳酸二环己酯(DCPD)、过氧化二碳酸二异丙酯(IPP)受热分解反应的方程式如下:The details are as follows: The thermal decomposition reaction equations of the organic peroxy thermal decomposition initiators dicyclohexyl peroxycarbonate (DCPD) and diisopropyl peroxydicarbonate (IPP) are as follows:

无机过氧类热分解引发剂过氧化氢受热分解反应的方程式如下:The equation for the thermal decomposition reaction of hydrogen peroxide, an inorganic peroxy thermal decomposition initiator, is as follows:

脆性晶体材料表面与自由基反应的化学方程式如下:The chemical equation for the reaction between the surface of brittle crystalline materials and free radicals is as follows:

其中,B是脆性工件材料。Among them, B is the brittle workpiece material.

在一些实施例中,所述植物油为大豆油、棕榈油或菜籽油。In some embodiments, the vegetable oil is soybean oil, palm oil, or rapeseed oil.

第二方面,本发明提供所述油基热敏活性研磨液的制备方法,包括如下步骤:In a second aspect, the present invention provides a method for preparing the oil-based heat-sensitive active grinding fluid, which includes the following steps:

将丙二醇、三乙醇胺和植物油按比例混合均匀后,向混合液中加入热敏氧化剂,混合均匀,即得研磨液。After mixing propylene glycol, triethanolamine and vegetable oil in proportion, add a heat-sensitive oxidant to the mixture and mix evenly to obtain a grinding liquid.

第三方面,本发明提供一种微波辅助固结磨料研磨方法,包括如下步骤:将所述油基热敏活性研磨液加入固结磨料研磨盘上;In a third aspect, the present invention provides a microwave-assisted fixed abrasive grinding method, which includes the following steps: adding the oil-based heat-sensitive active grinding fluid to the fixed abrasive grinding disc;

驱动待研磨工件和研磨盘旋转、对磨;Drive the workpiece to be ground and the grinding disc to rotate and grind against each other;

利用微波对研磨体系进行加热,同时诱导热敏活性研磨液中油机热敏活性研磨液分解产生活性自由基对机械应力作用下的工件进行化学改性;Use microwaves to heat the grinding system, and at the same time induce the decomposition of the oil machine's thermally active grinding fluid in the thermally active grinding fluid to produce active free radicals to chemically modify the workpiece under mechanical stress;

研磨去除工件表面的软化材料,即可。Grinding removes the softened material from the surface of the workpiece.

化学改性可以降低工件表面材料的硬度、提高脆性材料的断裂韧性,同时利用微波的加热效应提高改性层材料的塑性。Chemical modification can reduce the hardness of the surface material of the workpiece and improve the fracture toughness of brittle materials. At the same time, the heating effect of microwave is used to improve the plasticity of the modified layer material.

通过配置油基热敏活性研磨液,搭建具备微波加热功能且温度可调的微波-固结金刚石磨料研磨系统,利用微波能量加热待加工工件,提高材料的塑性变形能力,同时诱导热敏活性研磨液中热分解型引发剂分解产生活性自由基对机械应力作用下的工件表层材料进行化学改性,引发脆性工件材料表面形成一层低硬度、低弹性模量及高断裂韧性的改性层,增大材料脆-塑性转变去除的临界切削深度,减小甚至消除单一机械应力去除造成的加工损伤,提高材料的去除速率和加工表面质量。By configuring an oil-based thermally active grinding fluid, a microwave-consolidated diamond abrasive grinding system with microwave heating function and adjustable temperature is constructed, using microwave energy to heat the workpiece to be processed, improving the plastic deformation ability of the material, and inducing thermally active grinding at the same time The thermal decomposition initiator in the liquid decomposes to generate active free radicals to chemically modify the surface material of the workpiece under mechanical stress, causing the surface of the brittle workpiece material to form a modified layer with low hardness, low elastic modulus and high fracture toughness. Increase the critical cutting depth for material brittle-plastic transition removal, reduce or even eliminate processing damage caused by single mechanical stress removal, and improve material removal rate and processing surface quality.

在一些实施例中,研磨去除工件表面软化材料的临界磨削深度dc的表达式如下:In some embodiments, the expression of the critical grinding depth d c for grinding to remove softened material from the workpiece surface is as follows:

dc=λ(H/E)1/2(Kc/H)2d c =λ(H/E) 1/2 (K c /H) 2 ;

其中,λ是脆性材料的脆性-塑性转变因子,H是微波软化后的材料的硬度,E是微波软化后的材料的弹性模量,Kc是微波软化后的材料的断裂韧性。Among them, λ is the brittleness-plastic transition factor of brittle materials, H is the hardness of the microwave-softened material, E is the elastic modulus of the microwave-softened material, and K c is the fracture toughness of the microwave-softened material.

在一些实施例中,采用微波对研磨体系加热至40~300℃。In some embodiments, microwaves are used to heat the grinding system to 40-300°C.

在一些实施例中,所述研磨盘中金刚石磨料的粒度为0.2~3.0μm。In some embodiments, the particle size of the diamond abrasive in the grinding disc is 0.2-3.0 μm.

在一些实施例中,研磨压力为50~100g/cm2In some embodiments, the grinding pressure is 50-100g/cm 2 ;

优选的,所述研磨盘转速为150~300rpm;Preferably, the rotation speed of the grinding disc is 150-300 rpm;

优选的,所述工件转速为100~150rpm;Preferably, the rotation speed of the workpiece is 100-150 rpm;

优选的,所述研磨液流量50~100mL/min。Preferably, the flow rate of the grinding liquid is 50-100 mL/min.

在一些实施例中,还包括利用原子力显微镜测量研磨后工件的表面粗糙度Sa和利用聚焦离子束-透射电镜技术观测研磨后工件的亚表面的步骤。In some embodiments, the method further includes the steps of measuring the surface roughness S a of the polished workpiece using an atomic force microscope and observing the subsurface of the polished workpiece using focused ion beam-transmission electron microscopy technology.

在一些实施例中,微波辅助固结磨料研磨系统的搭建步骤为:In some embodiments, the construction steps of the microwave-assisted fixed abrasive grinding system are:

在研磨平台外部设置具有可视窗口的微波辐射屏蔽罩;Set a microwave radiation shield with a visible window outside the grinding platform;

在屏蔽罩内部,沿研磨平台集中或均匀设置有一个或多个微波发生器,微波发生器与待加工工件的距离为5~10cm;Inside the shielding cover, one or more microwave generators are concentrated or evenly arranged along the grinding platform. The distance between the microwave generator and the workpiece to be processed is 5 to 10 cm;

将待加工工件和研磨盘分别安装,即可进行后续操作。Install the workpiece to be processed and the grinding disc separately for subsequent operations.

上述本发明的一种或多种实施例取得的有益效果如下:The beneficial effects achieved by one or more embodiments of the present invention are as follows:

1、本发明利用热敏活性研磨液对机械力作用下的工件进行微波辅助可控化学改性,软化工件表面材料,增大材料脆-塑性转变去除的临界切削深度,以此减小甚至消除单一机械应力去除造成的加工损伤,同时提高材料的去除速率。研磨后的工件表面无微裂纹损伤和破碎,工件表面粗糙度Sa可达1.0~10.0nm。材料去除率可达15.0~30.0μm/min。本发明可同时实现难加工材料的高表面质量、低机械损伤和高材料去除速率的超精密研磨加工。1. The present invention uses heat-sensitive active grinding fluid to carry out microwave-assisted controllable chemical modification of the workpiece under the action of mechanical force, soften the surface material of the workpiece, increase the critical cutting depth for material brittle-plastic transition removal, thereby reducing or even Eliminates processing damage caused by single mechanical stress removal while increasing material removal rate. There is no microcrack damage or breakage on the surface of the workpiece after grinding, and the surface roughness Sa of the workpiece can reach 1.0~10.0nm. The material removal rate can reach 15.0~30.0μm/min. The invention can simultaneously achieve ultra-precision grinding processing of high surface quality, low mechanical damage and high material removal rate of difficult-to-machine materials.

2、本发明利用固结磨料研磨盘,磨粒的密度分布具有可控性,磨削效率高,磨盘耐磨性好,耐用度高,同时活性研磨液对机械力作用下的工件进行微波辅助可控化学改性,扩大化学反应可控速度范围,适配不同参数下的机械作用力,调控化学与机械研磨的协同效应,有效提高材料表面质量和加工效率,可实现硬脆难加工材料高效率、低损伤超精密研磨加工。2. The present invention uses a fixed abrasive grinding disc. The density distribution of the abrasive particles is controllable, the grinding efficiency is high, the grinding disc has good wear resistance and high durability. At the same time, the active grinding fluid provides microwave assistance to the workpiece under the action of mechanical force. Controllable chemical modification can expand the controllable speed range of chemical reactions, adapt to mechanical forces under different parameters, regulate the synergistic effect of chemical and mechanical grinding, effectively improve the surface quality and processing efficiency of materials, and achieve high performance for hard, brittle and difficult-to-machine materials. Efficient, low-damage ultra-precision grinding processing.

附图说明Description of the drawings

构成本发明的一部分的说明书附图用来提供对本发明的进一步理解,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。The description and drawings that constitute a part of the present invention are used to provide a further understanding of the present invention. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention.

图1本发明微波辅助固结磨料研磨方法中制备金刚石固结磨料磨盘的金刚石磨粒SEM显微图(a和b)和金刚石固结磨料磨盘(c)的图片;Figure 1: SEM micrographs (a and b) of diamond abrasive grains (a and b) and pictures of diamond fixed abrasive discs (c) prepared in the microwave-assisted bonded abrasive grinding method of the present invention;

图2本发明微波辅助固结磨料研磨方法中研磨平台的示意图,1-工作台、2-待加工工件、3-液池、4-金刚石固结磨料磨盘、5-磨屑过滤装置、6-热敏活性研磨液供液装置、7-热敏引发剂浓度指示装置、8-微波发生装置;Figure 2 is a schematic diagram of the grinding platform in the microwave-assisted fixed abrasive grinding method of the present invention, 1-workbench, 2-workpiece to be processed, 3-liquid pool, 4-diamond fixed abrasive grinding disc, 5-grinding dust filtering device, 6- Thermal active grinding liquid supply device, 7-thermal initiator concentration indicating device, 8-microwave generating device;

图3本发明微波辅助固结磨料研磨方法中去离子水和油基热敏活性研磨液作用下金刚石固结磨料研磨碳化硅和氧化铝晶体的材料去除速率对比图;Figure 3 is a comparison chart of the material removal rates of diamond-bonded abrasives grinding silicon carbide and alumina crystals under the action of deionized water and oil-based heat-sensitive active grinding fluid in the microwave-assisted bonded abrasive grinding method of the present invention;

图4本发明微波辅助固结磨料研磨方法中去离子水和油基热敏活性研磨液作用下金刚石固结磨料研磨氧化铝单晶的SEM显微图;Figure 4 is an SEM micrograph of alumina single crystals ground by diamond-bonded abrasives under the action of deionized water and oil-based heat-sensitive active polishing fluid in the microwave-assisted bonded abrasive grinding method of the present invention;

图5本发明微波辅助固结磨料研磨方法中油基热敏活性研磨液制备及脆性材料微波辅助固结磨料研磨加工的工艺流程图。Figure 5 is a process flow chart for the preparation of oil-based heat-sensitive active grinding fluid and the microwave-assisted fixed abrasive grinding processing of brittle materials in the microwave-assisted fixed abrasive grinding method of the present invention.

具体实施方式Detailed ways

应该指出,以下详细说明都是例示性的,旨在对本发明提供进一步的说明。除非另有指明,本发明使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present invention. Unless otherwise specified, all technical and scientific terms used herein have the same meanings commonly understood by one of ordinary skill in the art to which this invention belongs.

实施例1Example 1

结合实施例对本发明一种脆性材料的微波辅助固结磨料研磨方法及油基热敏活性研磨液做进一步描述:A microwave-assisted fixed abrasive grinding method for brittle materials and an oil-based heat-sensitive active grinding fluid of the present invention will be further described with reference to the examples:

本实施例中加工工件选择2英寸的硬脆碳化硅和氧化铝晶圆,采用实验室设计定制的磨抛一体机作为试验平台,微波发生器可将待加工工件以及活性研磨液加热到80℃,平均粒度3μm的金刚石固结磨料磨盘对磨上述工件,如图2所示,进行研磨加工。研磨加工后,采用酒精超声清洗样品10min。利用天平(精度0.001mg)称量研磨前后工件材料的质量,计算出材料去除率;利用原子力显微镜测量研磨后工件的表面粗糙度Sa,测量范围50μm×50μm,利用场发射扫描电镜观测研磨后工件的表面。In this embodiment, a 2-inch hard and brittle silicon carbide and alumina wafer is selected as the workpiece to be processed. A grinding and polishing machine designed and customized in the laboratory is used as the test platform. The microwave generator can heat the workpiece to be processed and the active grinding fluid to 80°C. , a diamond bonded abrasive disc with an average particle size of 3 μm is used to grind the above workpiece, as shown in Figure 2, for grinding processing. After grinding, the samples were ultrasonically cleaned with alcohol for 10 minutes. Use a balance (accuracy 0.001 mg) to weigh the mass of the workpiece material before and after grinding, and calculate the material removal rate; use an atomic force microscope to measure the surface roughness S a of the workpiece after grinding, with a measurement range of 50 μm × 50 μm, and use a field emission scanning electron microscope to observe the workpiece after grinding. The surface of the workpiece.

具体实施步骤如下:The specific implementation steps are as follows:

S1、根据热分解型引发剂与热相互作用产生自由基活性种的化学原理,以及自由基活性种和惰性材料相互反应形成软化层的化学原理,针对硬脆材料硬度高、脆性大、化学性质稳定的特点,配置具备微波加热产生自由基活性种且对机械应力作用中的工件材料能进行可控化学改性的活性研磨液:S1. Based on the chemical principle that thermal decomposition initiators interact with heat to generate free radical active species, and the chemical principle that free radical active species and inert materials react with each other to form a softening layer, for hard and brittle materials with high hardness, brittleness, and chemical properties Stable characteristics, equipped with active grinding fluid that generates free radical active species by microwave heating and can perform controllable chemical modification of workpiece materials under mechanical stress:

S11、化学实验操作箱里将一定量的丙二醇、三乙醇胺和植物油依次倒入烧杯内,室温机械搅拌混合3~5min,得到丙二醇-三乙醇胺混合油溶液;S11. Pour a certain amount of propylene glycol, triethanolamine and vegetable oil into a beaker in sequence in the chemical experiment operation box, and mechanically stir and mix at room temperature for 3 to 5 minutes to obtain a propylene glycol-triethanolamine mixed oil solution;

S12、将一定量的热分解型引发剂复配物缓慢加入到丙二醇-三乙醇胺混合油溶液,室温机械搅拌1~2min,热分解引发剂复配物溶解或分散到丙二醇-三乙醇胺混合油溶液中,获得具有热敏活性的研磨液;S12. Slowly add a certain amount of the thermal decomposition initiator compound to the propylene glycol-trolamine mixed oil solution, stir mechanically at room temperature for 1 to 2 minutes, and dissolve or disperse the thermal decomposition initiator compound into the propylene glycol-trolamine mixed oil solution. , a grinding fluid with heat-sensitive activity is obtained;

S13、将配制好的热敏活性研磨液倒入到避光的试剂瓶中待用。S13. Pour the prepared heat-sensitive active grinding fluid into a light-proof reagent bottle for later use.

S2、搭建具备微波加热功能且温度可调的微波-固结金刚石磨料研磨平台:S2. Build a microwave-consolidated diamond abrasive grinding platform with microwave heating function and adjustable temperature:

S21、将微波发生器固定于工件与磨盘接触界面5cm处,微波发生器可旋转移动,能将能量聚焦于指定区域;S21. Fix the microwave generator 5cm from the contact interface between the workpiece and the grinding disc. The microwave generator can rotate and move to focus the energy on the designated area;

S22、利用天平称量研磨前工件的质量,接着将双开门的屏蔽罩安装到研磨台的正前方,将工件通过真空吸附装夹到连接着上驱动电机的工作台上,将3μm粒度的固结金刚石磨料研磨盘固定到与下驱动电机连接的转盘上;S22. Use a balance to weigh the mass of the workpiece before grinding, then install the double-door shielding cover directly in front of the grinding table, clamp the workpiece to the workbench connected to the upper drive motor through vacuum adsorption, and place the 3 μm particle size solid The bonded diamond abrasive grinding disc is fixed to the turntable connected to the lower drive motor;

S23、将S1配置的热敏活性研磨液按一定流量加入到金刚石固结磨料研磨盘上。S23. Add the heat-sensitive active grinding fluid configured in S1 to the diamond bonded abrasive grinding disc at a certain flow rate.

S3、根据S1得到的热敏活性研磨液中引发剂复配物的成分、含量和溶液的流量,以及工件材料改性层的硬度、弹性模量、断裂韧性和界面分离强度分别设置微波发生器的功率、研磨压力、研磨盘转速和工件转速等工艺参数,工艺参数的选择是根据工件改性层的力学性能,启动自动磨抛一体机进行工件材料的微波加热化学改性、机械研磨去除改性层的动态去除材料的微波辅助机械研磨加工:S3. Set the microwave generator respectively according to the composition, content and flow rate of the initiator compound in the heat-sensitive active grinding fluid obtained in S1, as well as the hardness, elastic modulus, fracture toughness and interface separation strength of the workpiece material modification layer. Process parameters such as power, grinding pressure, grinding disc rotation speed and workpiece rotation speed. The selection of process parameters is based on the mechanical properties of the workpiece modification layer. The automatic grinding and polishing machine is started to perform microwave heating chemical modification and mechanical grinding removal of the workpiece material. Microwave-assisted mechanical grinding processing of dynamically removing material from the sexual layer:

对工件进行对磨的具体操作步骤包括:The specific steps for grinding the workpiece include:

S31、启动下驱动电机带动固结金刚石磨料研磨盘旋转,启动上驱动电机带动工件旋转,同时施加正压力控制固结金刚石磨料研磨盘与工件进行对磨。S31. Start the lower drive motor to drive the fixed diamond abrasive grinding disc to rotate, start the upper drive motor to drive the workpiece to rotate, and at the same time apply positive pressure to control the fixed diamond abrasive grinding disc and the workpiece to grind against each other.

S32、调整微波发生器,利用微波能量加热待加工工件,同时诱导热敏活性研磨液中热分解型引发剂分解产生活性自由基对机械应力作用下的工件进行化学改性,降低工件表面材料的硬度和弹性模量,同时提高脆性材料的断裂韧性。S32. Adjust the microwave generator, use microwave energy to heat the workpiece to be processed, and at the same time induce the thermal decomposition initiator in the heat-sensitive active grinding fluid to decompose to generate active free radicals to chemically modify the workpiece under the action of mechanical stress and reduce the deterioration of the surface material of the workpiece. Hardness and elastic modulus, while improving the fracture toughness of brittle materials.

步骤S3的基础上对磨去除工件表面软化的材料,金刚石磨粒机械去除工件表面软化材料的临界切削深度dc的表达式如下:On the basis of step S3, the softened material on the surface of the workpiece is removed by grinding. The expression of the critical cutting depth d c for mechanically removing the softened material on the surface of the workpiece with diamond abrasive grains is as follows:

dc=λ(H/E)1/2(Kc/H)2d c =λ(H/E) 1/2 (K c /H) 2 ;

其中,λ是光敏材料的脆-塑性转变因子,H是光敏材料的硬度,E是光敏材料的弹性模量,Kc是光敏材料的断裂韧性。Among them, λ is the brittle-plastic transition factor of the photosensitive material, H is the hardness of the photosensitive material, E is the elastic modulus of the photosensitive material, and K c is the fracture toughness of the photosensitive material.

S33、10~30min后关闭试验机,取下工件,随后利用酒精超声清洗工件10min,利用天平称量研磨后工件的质量,计算得到工件材料的去除率,利用原子力显微镜测量研磨后工件的表面粗糙度Sa,测量范围50μm×50μm,利用场发射扫描电镜观测研磨后工件的表面。S33. After 10 to 30 minutes, turn off the testing machine, remove the workpiece, and then clean the workpiece ultrasonically with alcohol for 10 minutes. Use a balance to weigh the mass of the ground workpiece, calculate the removal rate of the workpiece material, and use an atomic force microscope to measure the surface roughness of the ground workpiece. Degree Sa , measuring range 50μm×50μm, use field emission scanning electron microscope to observe the surface of the workpiece after grinding.

S34、利用原子力显微镜测量研磨后工件的表面粗糙度Sa,利用场发射扫描电镜观测研磨后工件的表面,利用聚焦离子束-透射电镜技术观测研磨后工件的亚表面。S34. Use an atomic force microscope to measure the surface roughness S a of the polished workpiece, use a field emission scanning electron microscope to observe the surface of the polished workpiece, and use focused ion beam-transmission electron microscopy technology to observe the subsurface of the polished workpiece.

研磨液:研磨液C,组成为:94%大豆油、5%过氧化碳酸二环己酯(DCPD)、0.5%丙二醇、0.5%三乙醇胺。Grinding liquid: Grinding liquid C, composed of: 94% soybean oil, 5% dicyclohexyl peroxycarbonate (DCPD), 0.5% propylene glycol, and 0.5% triethanolamine.

研磨方法:研磨温度80℃,研磨压力100g/cm2,磨盘转速为200rpm,工件转速50rpm,研磨液流量50mL/min,研磨时间20分钟,微波发生器处于工作状态,保证磨盘表面温度处于80℃左右波动;固结磨料磨盘中金刚石磨粒的粒度是250nm~1000nm。Grinding method: grinding temperature 80°C, grinding pressure 100g/cm 2 , grinding disc rotation speed 200rpm, workpiece rotation speed 50rpm, grinding fluid flow 50mL/min, grinding time 20 minutes, the microwave generator is in working condition, and the grinding disc surface temperature is guaranteed to be 80°C Fluctuates left and right; the particle size of the diamond abrasive grains in the fixed abrasive disc is 250nm ~ 1000nm.

对比例1Comparative example 1

研磨液A为去离子水,其他均与实施例1相同。Grinding liquid A is deionized water, and everything else is the same as in Example 1.

对比例2Comparative example 2

研磨液B中包括:99%大豆油、0.5%丙二醇、0.5%三乙醇胺;其他均与实施例1相同。Grinding liquid B includes: 99% soybean oil, 0.5% propylene glycol, and 0.5% triethanolamine; everything else is the same as in Example 1.

试验结果:test results:

如图3所示,研磨液A微波辅助固结磨料研磨加工的碳化硅和氧化铝晶圆的表面粗糙度Sa=41.3nm和36.6nm,工件材料去除速率MRR=7.3μm/min和3.9μm/min。As shown in Figure 3, the surface roughness S a of silicon carbide and alumina wafers processed by microwave-assisted fixed abrasive grinding with polishing liquid A is 41.3nm and 36.6nm, and the workpiece material removal rate MRR is 7.3μm/min and 3.9μm. /min.

研磨液B微波辅助固结磨料研磨加工的碳化硅和氧化铝晶圆的表面粗糙度Sa=33.1nm和24.8nm,工件材料去除速率MRR=6.3μm/min和2.3μm/min。The surface roughness S a of silicon carbide and alumina wafers processed by polishing liquid B with microwave-assisted fixed abrasive grinding is 33.1nm and 24.8nm, and the workpiece material removal rate MRR is 6.3μm/min and 2.3μm/min.

研磨液C微波辅助固结磨料研磨加工的碳化硅和氧化铝晶圆的表面粗糙度Sa=11.3nm和8.6nm,工件材料去除速率MRR=20.5μm/min和10.9μm/min。The surface roughness S a of silicon carbide and alumina wafers processed by polishing liquid C microwave-assisted fixed abrasive grinding is 11.3nm and 8.6nm, and the workpiece material removal rate MRR is 20.5μm/min and 10.9μm/min.

图4进一步证明,基于油基热敏活性研磨液的微波辅助固结磨料研磨加工可有效降低碳化硅和氧化铝晶体表面的脆性破碎,改善研磨表面的机械损伤。Figure 4 further proves that microwave-assisted fixed abrasive grinding processing based on oil-based thermally active grinding fluid can effectively reduce the brittle fracture of silicon carbide and aluminum oxide crystal surfaces and improve the mechanical damage of the grinding surface.

通过上述三组试验对比金刚石固结磨料机械研磨与微波辅助固结磨料研磨的加工效果,发现本发明的研磨加工方法加工效果显著优于传统机械研磨加工方法。Through the above three sets of tests to compare the processing effects of diamond fixed abrasive mechanical grinding and microwave-assisted fixed abrasive grinding, it was found that the processing effect of the grinding processing method of the present invention is significantly better than the traditional mechanical grinding processing method.

特别地,对照组A采用去离子,微波加热超过100℃会产生高温水蒸气,存在一定安全隐患,因此本实施例仅将温度控制于80℃附近,但实际加工过程中,因采用的是大豆油、橄榄油等植物油作为基础液,温度可进一步提高到300℃,将更有利于改性层表层材料的位错滑移,进而提高塑性变形能力,获得更好的研磨性能。In particular, control group A uses deionization. Microwave heating exceeding 100°C will produce high-temperature water vapor, which poses certain safety risks. Therefore, this example only controls the temperature around 80°C. However, in the actual processing process, due to the use of large Vegetable oils such as soybean oil and olive oil are used as the base liquid, and the temperature can be further increased to 300°C, which will be more conducive to the dislocation slip of the surface material of the modified layer, thereby improving the plastic deformation ability and obtaining better grinding performance.

实施例2Example 2

研磨液:组成为:93%大豆油、2%过氧化二碳酸二异丙酯、4%丙二醇、1%三乙醇胺。其他均与实施例1相同。Grinding liquid: composed of: 93% soybean oil, 2% diisopropyl peroxydicarbonate, 4% propylene glycol, and 1% triethanolamine. Others are the same as Example 1.

实施例3Example 3

研磨液:组成为:87%大豆油、7%过氧化氢、2%丙二醇、4%三乙醇胺。其他均与实施例1相同。Grinding fluid: composed of: 87% soybean oil, 7% hydrogen peroxide, 2% propylene glycol, and 4% triethanolamine. Others are the same as Example 1.

实施例4Example 4

研磨方法:研磨温度200℃,研磨压力50g/cm2,磨盘转速为300rpm,工件转速150rpm,研磨液流量70mL/min,研磨时间20分钟,微波发生器处于工作状态,保证磨盘表面温度处于200℃左右波动。Grinding method: grinding temperature 200°C, grinding pressure 50g/cm 2 , grinding disc rotation speed 300rpm, workpiece rotation speed 150rpm, grinding fluid flow 70mL/min, grinding time 20 minutes, microwave generator in working condition, ensure the grinding disc surface temperature is 200°C Fluctuate left and right.

实施例5Example 5

研磨方法:研磨温度300℃,研磨压力100g/cm2,磨盘转速为150rpm,工件转速150rpm,研磨液流量100mL/min,研磨时间20分钟,微波发生器处于工作状态,保证磨盘表面温度处于300℃左右波动。Grinding method: grinding temperature 300°C, grinding pressure 100g/cm 2 , grinding disc rotation speed 150rpm, workpiece rotation speed 150rpm, grinding fluid flow 100mL/min, grinding time 20 minutes, the microwave generator is in working condition, and the surface temperature of the grinding disc is guaranteed to be 300°C. Fluctuate left and right.

以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.

Claims (11)

1. An oil-based thermosensitive active grinding fluid is characterized in that: the composition comprises the following components: the mass percent of the propylene glycol is 0.5-5%, the mass percent of the triethanolamine is 0.5-5%, the mass percent of the thermosensitive oxidant is 1-10%, and the balance is vegetable oil.
2. The oil-based heat sensitive active abrasive slurry of claim 1, wherein: the thermosensitive oxidant is selected from one or a combination of more of hydrogen peroxide, dicyclohexyl peroxycarbonate or diisopropyl peroxydicarbonate;
preferably, the vegetable oil is soybean oil, palm oil or rapeseed oil.
3. The method for preparing the oil-based thermosensitive active polishing liquid according to claim 1 or 2, characterized in that: the method comprises the following steps:
and (3) uniformly mixing propylene glycol, triethanolamine and vegetable oil according to a proportion, adding a thermosensitive oxidant into the mixed solution, and uniformly mixing to obtain the grinding fluid.
4. A microwave-assisted fixed abrasive grinding method is characterized in that: the method comprises the following steps: adding the oil-based heat-sensitive active abrasive slurry of claim 1 or 2 to a fixed abrasive grinding disc;
driving a workpiece to be ground and a grinding disc to rotate and perform counter grinding;
heating the grinding system by utilizing microwaves, and simultaneously inducing the decomposition of the thermosensitive active grinding fluid of the oil machine in the thermosensitive active grinding fluid to generate active free radicals to chemically modify the workpiece under the action of mechanical stress;
grinding to remove the softened material on the surface of the workpiece.
5. A method of microwave-assisted fixed abrasive lapping according to claim 3, wherein: critical grinding depth d for grinding and removing workpiece surface softening material c The expression of (2) is as follows:
d c =λ(H/E) 1/2 (K c /H) 2
wherein lambda is the brittle-plastic transition factor of the brittle material, H is the hardness of the material after microwave softening, E is the elastic modulus of the material after microwave softening, K c Is the fracture toughness of the material after microwave softening.
6. A method of microwave-assisted fixed abrasive lapping according to claim 3, comprising the steps of: and heating the grinding system to 40-300 ℃ by adopting microwaves.
7. A method of microwave-assisted fixed abrasive lapping according to claim 3, comprising the steps of: the granularity of the diamond abrasive in the grinding disc is 0.2-3.0 mu m.
8. A method of microwave-assisted fixed abrasive lapping according to claim 3, comprising the steps of: the grinding pressure is 50-100 g/cm 2
9. The method for microwave-assisted fixed abrasive lapping according to claim 7, comprising the steps of: the rotating speed of the grinding disc is 150-300 rpm;
preferably, the rotating speed of the workpiece is 100-150 rpm;
preferably, the flow rate of the grinding fluid is 50-100 mL/min.
10. A method of microwave-assisted fixed abrasive lapping according to claim 3, comprising the steps of: further comprises measuring the surface roughness S of the workpiece after grinding by using an atomic force microscope a And observing the subsurface of the workpiece after grinding by using a focused ion beam-transmission electron microscope technique.
11. A method of microwave-assisted fixed abrasive lapping according to claim 3, comprising the steps of: the method for constructing the microwave-assisted fixed abrasive grinding system comprises the following steps of:
a microwave radiation shielding cover with a visible window is arranged outside the grinding platform;
one or more microwave generators are arranged in the shielding cover in a centralized or uniform manner along the grinding platform, and the distance between the microwave generators and a workpiece to be processed is 5-10 cm;
and respectively installing the workpiece to be processed and the grinding disc, and then carrying out subsequent operation.
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