WO2015176639A1 - 超细磨料生物高分子柔性抛光膜及其制备方法 - Google Patents

超细磨料生物高分子柔性抛光膜及其制备方法 Download PDF

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Publication number
WO2015176639A1
WO2015176639A1 PCT/CN2015/079259 CN2015079259W WO2015176639A1 WO 2015176639 A1 WO2015176639 A1 WO 2015176639A1 CN 2015079259 W CN2015079259 W CN 2015079259W WO 2015176639 A1 WO2015176639 A1 WO 2015176639A1
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WIPO (PCT)
Prior art keywords
polishing film
abrasive
biopolymer
coupling agent
flexible polishing
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PCT/CN2015/079259
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English (en)
French (fr)
Inventor
陆静
徐西鹏
黄辉
宋运运
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华侨大学
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Application filed by 华侨大学 filed Critical 华侨大学
Priority to JP2016567237A priority Critical patent/JP6586963B2/ja
Priority to KR1020167030929A priority patent/KR102358778B1/ko
Priority to US15/312,957 priority patent/US10286524B2/en
Publication of WO2015176639A1 publication Critical patent/WO2015176639A1/zh

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D11/00—Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B19/00—Single-purpose machines or devices for particular grinding operations not covered by any other main group
    • B24B19/22—Single-purpose machines or devices for particular grinding operations not covered by any other main group characterised by a special design with respect to properties of the material of non-metallic articles to be ground
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/11—Lapping tools
    • B24B37/20—Lapping pads for working plane surfaces
    • B24B37/22—Lapping pads for working plane surfaces characterised by a multi-layered structure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/11—Lapping tools
    • B24B37/20—Lapping pads for working plane surfaces
    • B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
    • B24B37/245—Pads with fixed abrasives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D11/00—Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
    • B24D11/001—Manufacture of flexible abrasive materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
    • B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives

Definitions

  • the invention relates to an ultra-precision grinding and polishing tool, which is a biopolymer flexible polishing film containing ultrafine abrasive.
  • the ultra-precision polishing methods of such materials mainly include three methods: free abrasive polishing, fixed abrasive polishing and special processing.
  • the abrasive particles are randomly distributed and the trajectory is uncontrollable, forming a three-dimensional integral motion, and the processing efficiency is low.
  • the size of the abrasive grains is small, agglomerates are easily formed, causing scratches on the surface of the workpiece and affecting the processing quality.
  • the corrosive slurry and free abrasive used are not only wasteful but also pollute the environment.
  • the grinding disc for fixed abrasive polishing has high rigidity, and the dressing in the polishing process is difficult and complicated, and the condition control during the processing is very strict, otherwise it is easy to cause hard damage to the workpiece, and there is also a problem of fine-grained abrasive agglomeration.
  • the new special processing can obtain better surface quality, it is often very demanding on equipment, and it is difficult to achieve efficient and rapid processing of large-surface workpieces, which cannot be widely applied to large-scale industrial production.
  • the object of the present invention is to provide an ultrafine abrasive polishing film product based on a degradable biopolymer material in view of the problems existing in the existing ultra-precision grinding and polishing tools.
  • the preparation method is simple, the shape and size of the diaphragm are not limited, and only water is used as the polishing liquid in the processing process, which is used for ultra-precision non-destructive processing, and has the characteristics of green environmental protection and no pollution.
  • the technical proposal of the invention is: an ultrafine abrasive biopolymer flexible polishing film, the substrate comprises: surface modified superfine abrasive 0.1-10 Wt%, drying control chemical additive 5-15 wt% and biopolymer sol 1-10 wt%; the above substrate is uniformly mixed, solidified by physical or chemical crosslinking, and formed after drying;
  • the surface modification is to chemically coat the ultrafine abrasive by a coupling agent to improve the dispersibility and holding power of the abrasive in the polymer substrate.
  • the coupling agent is one of a silane coupling agent, a titanate coupling agent, a lignin coupling agent, or a combination thereof.
  • the ultrafine abrasive is one or a combination of diamond, carbide, boride, oxide, and the particle size of the ultrafine abrasive is 5 nm-40. Mm.
  • the drying control chemical additive comprises a filler, a water holding agent and a pore former, and the filler is one or a combination of nano SiO 2 , nano CaCO 3 , nano polyimide and nano calcium magnesium powder; water holding agent Is one of sucrose, lactose, fructose, glycerol or a combination thereof; the pore forming agent is NaHCO 3 , NaCl, sodium dodecyl sulfate (SDS), sodium dodecylbenzenesulfonate or a combination thereof
  • the biopolymer material is starch, modified cellulose, chitosan, agarose, glucomannan, sodium alginate, gelatin, carrageenan, xanthan gum, pectin, soybean gum, polylactic acid. One or a combination thereof.
  • the drying may be carried out by a drying method such as constant temperature drying or infrared drying.
  • a preparation method of ultrafine abrasive biopolymer flexible polishing film comprises the following steps:
  • modification treatment the ultrafine abrasive particles are added to the aqueous solution of the coupling agent for modification treatment;
  • the mixed sol is formed by spraying or scraping, and then solidified by physical or chemical crosslinking, and dried to form a polishing film.
  • the ratio of the ultrafine abrasive particles and the coupling agent ranges from 100: 0.1 to 10 by mass.
  • the ultrafine abrasive biopolymer flexible polishing film of the invention can be widely used for ceramic substrates, semiconductor wafers, optical crystals, decorative and engineering stone materials, especially ultra-precision processing of large-sized planes.
  • the superfine abrasive in the polishing film of the invention is surface-modified by the coupling agent, effectively solves the problem of agglomeration of the abrasive, and enhances the ability of the biopolymer substrate to hold the inorganic abrasive; and because the polishing film has good flexibility It can realize the wear of the abrasive grains, avoiding the scratching of the workpiece by the hard large particles while the solid abrasive is processed efficiently; the polishing film of the invention also contains the drying control chemical additive, so that the polishing film has good mechanical properties. And shelf life; the selected biopolymer material can be degraded by microorganisms and is an environmentally friendly polishing tool.
  • the ultrafine abrasive biopolymer flexible polishing film of the invention has the following substrate selection:
  • Ultrafine abrasive diamond
  • Drying control chemical additives including filler nano SiO 2 , water holding agent sucrose and pore forming agent sodium dodecyl sulfate (SDS);
  • the biopolymer substrate starch, carrageenan combination
  • Coupling agent an aqueous solution of KH-550 silane coupling agent.
  • the preparation method of the ultrafine abrasive biopolymer flexible polishing film of the invention comprises the following steps:
  • particle size is 500
  • the diamond of nm was added to an aqueous solution of KH-550 silane coupling agent (coupling agent concentration: 0.005%, diamond addition amount: 1%) for ultrasonication for 30 minutes.
  • Substrate mixing treated diamond powder (after surface treatment, the functional group formed by hydrolysis of the coupling agent is adsorbed on the diamond, filtered to obtain diamond powder), SiO 2 having a particle size of 30 nm, SDS, sucrose, carrageenan and The starch was uniformly mixed by mechanical stirring in deionized water, and their mass percentage concentrations were 1%, 3%, 0.1%, 3%, 6%, and 4%, respectively.
  • the polishing film was attached to the polishing disc of the AUTOPOL-1000S automatic grinding and polishing machine, and the grinding disc speed was set to 120. Rpm, the sample plate speed is set to 60 rpm, the polishing pressure is set to 3 kg, and the SiC wafer with the original roughness of 10 nm is polished for 2 h with a surface roughness of 0.3. Nm, and the surface of the wafer is free of scratches and pits.
  • the ultrafine abrasive biopolymer flexible polishing film of the invention has the following substrate selection:
  • Ultrafine abrasive alumina
  • Drying control chemical additive CaCO 3 having a filler particle size of 20 nm, a water-retaining agent glycerin and a pore former NaCl crystal grain;
  • the biopolymer substrate a combination of chitosan and sodium alginate.
  • TTS titanate coupling agent TTS titanate coupling agent
  • the preparation method of the ultrafine abrasive biopolymer flexible polishing film of the invention comprises the following steps:
  • Substrate mixing treated alumina, CaCO 3 with a particle size of 20 nm, NaCl crystal grains, glycerol, chitosan and sodium alginate were uniformly mixed by mechanical stirring in deionized water, and the mass percentage concentrations were respectively It is 2%, 1%, 0.2%, 3%, 3.5%, 5%.
  • the sol is applied to a circular sprayed tin plate and immersed in a calcium ion solution to form a gel film.
  • the polishing film of the present invention can be prepared by gently peeling off from the universal board and attaching the smooth surface of the film to the round backing.
  • the polishing film was attached to the polishing disc of the AUTOPOL-1000S automatic grinding and polishing machine, and the grinding disc speed was set to 90. Rpm, the sample plate speed is set to 80 rpm, the polishing pressure is set to 2 kg, and the single crystal Si piece with the original roughness of 500 nm is polished for 30 min, and the surface roughness is 0.6. Nm, and the surface of the wafer is free of scratches and pits.
  • Physical or chemical cross-linking includes: molecular entanglement caused by temperature change (gelatin, agarose); ion cross-linking (sodium alginate, carrageenan, sodium alginate and soybean gum, carrageenan and xanthan gum); Hydrogen bonding or hydrophobic interaction (starch, modified cellulose, chitosan, glucomannan and pectin); crystallization (polylactic acid).
  • the coupling agent is a silane coupling agent (for example, KH540, KH550, KH580) Or a combination of a titanate coupling agent (for example, KR-TTS, KP-TTS, and KR-41B, etc.), a lignin coupling agent (for example, a solvent-type high-boiling alcohol HBS, etc.) or a combination thereof.
  • a silane coupling agent for example, KH540, KH550, KH580
  • a combination of a titanate coupling agent for example, KR-TTS, KP-TTS, and KR-41B, etc.
  • a lignin coupling agent for example, a solvent-type high-boiling alcohol HBS, etc.
  • the ultrafine abrasive is one or a combination of diamond, carbide (eg, silicon carbide, etc.), boride (eg, boron nitride, etc.), oxide (eg, alumina, silica, yttria, etc.).
  • carbide eg, silicon carbide, etc.
  • boride eg, boron nitride, etc.
  • oxide eg, alumina, silica, yttria, etc.
  • Ultrafine abrasives range in size from 50 nm to 40 ⁇ m. Can be 50 nm, 100 nm, 250 nm, 500 nm, 1 Mm, 5 ⁇ m, 10 ⁇ m, etc.
  • the drying control chemical additive includes a filler, a water holding agent, and a pore former.
  • the filler may be one or a combination of nano SiO 2 , nano CaCO 3 , nano polyimide, and nano calcium magnesium powder;
  • the water holding agent may be one of sucrose, lactose, fructose, glycerol, and the like.
  • the pore former may be one or a combination of NaHCO 3 , NaCl, sodium dodecyl sulfate (SDS), sodium dodecylbenzene sulfonate, and the like.
  • the biopolymer substrate may be starch, modified cellulose, chitosan, agarose, glucomannan, sodium alginate, gelatin, carrageenan, xanthan gum, pectin, soybean gum, polylactic acid. One or several combinations of the others.
  • the ultrafine abrasive biopolymer flexible polishing film of the invention has the surface modification of the superfine abrasive in the polishing film by the coupling agent, effectively solves the problem of agglomeration of the abrasive, and enhances the ability of the biopolymer substrate to control the inorganic abrasive. And because the polishing film has good flexibility, the wear of the abrasive particles can be achieved, and the solid abrasive is efficiently processed while avoiding the scratch of the workpiece by the hard large particles, and can be widely used for the ceramic substrate and the semiconductor crystal. Round, optical crystals, decorative and engineered stone, especially ultra-precision machining of large-size flat surfaces.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Polishing Bodies And Polishing Tools (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

公开了一种超细磨料生物高分子柔性抛光膜及其制备方法，属于生物高分子材料和超精密加工相结合领域。抛光膜基材为可降解的生物高分子材料，选用填充剂、持水剂和造孔剂等干燥控制化学添加剂增强抛光膜的机械性能，通过偶联剂表面化学改性的方法实现超细磨料在抛光膜中的均匀分散和有效把持。与传统的化学机械抛光方式相比，不存在游离磨料浪费严重和腐蚀性抛光液对环境的污染问题，相较于商业的抛光膜产品，生物高分子基材具有一定的柔性，能实现对磨粒的容没，不会产生划痕和机械损伤，可达到超精密无损加工。该抛光膜具有制备工艺简单、抛光效果好、加工效率高、工件易清洗、绿色环保等特点。

Description

超细磨料生物高分子柔性抛光膜及其制备方法 技术领域
本发明涉及一种超精密磨抛工具，是含超细磨料的生物高分子柔性抛光膜。
背景技术
近些年，随着信息技术和光电技术的快速发展，对陶瓷基板、半导体晶圆、光学晶体、装饰及工程石材的加工，都提出了越来越高的要求。尤其是半导体晶片的加工，不仅要求表面超光滑、超平坦，而且不能有残余应力、表面和亚表面损伤。
这类材料的超精密抛光方法主要有游离磨料抛光、固结磨料抛光和特种加工三种方式。游离磨料抛光过程中，磨粒随机分布并且轨迹不可控，形成三维一体运动，加工效率较低。当磨粒尺寸较小时，容易形成团聚体，造成工件表面划伤，影响加工质量。采用的腐蚀性研磨液和游离磨料不仅浪费严重还污染环境。固结磨料抛光用的磨盘刚度大，抛光过程中的修整比较困难繁琐，加工过程中条件控制非常严格，否则易对工件产生硬损伤，且同样存在细粒度磨料团聚的问题。新型的特种加工，虽然能获得较好的表面质量，但是往往对设备要求非常高，且很难实现大平面工件的高效快速加工，无法广泛应用到大规模的工业化生产中。
国内外研究学者也针对上述问题开发了一类半固着的磨抛工具，比如冰盘、树脂抛光片、亲水性抛光膜等，在一定程度上解决细粒度磨料的分散问题。但这类工具的磨料把持能力较低，加工过程中多数处于游离状态，且高分子聚合物很难降解，废弃物后期处理比较麻烦。
发明内容
本发明的目的是针对现有超精密磨抛工具存在的问题，提出一种基于可降解生物高分子材料的超细磨料抛光膜产品。其制备方法简单，膜片的形状和尺寸不受限制，加工过程中只需要水作为抛光液，用于超精密无损加工，具有绿色环保无污染的特点。
本发明的技术方案是：一种超细磨料生物高分子柔性抛光膜，其基材包括：经过表面改性的超细磨料0.1-10 wt%、干燥控制化学添加剂5-15 wt%和生物高分子溶胶1-10 wt%；上述基材均匀混合，通过物理或化学交联固化成型，干燥后形成；
所述的表面改性是通过偶联剂对超细磨料进行化学包覆以提高磨料在高分子基材中的分散性和把持力。
所述的偶联剂为硅烷偶联剂、钛酸酯偶联剂、木质素偶联剂的一种或者其组合。
所述的超细磨料为金刚石、碳化物、硼化物、氧化物的一种或者几种组合，超细磨料的粒径在5 nm-40 µm。
所述的干燥控制化学添加剂包括填充剂、持水剂和造孔剂，填充剂为纳米SiO2、纳米CaCO3、纳米聚酰亚胺和纳米钙镁粉的一种或其组合；持水剂为蔗糖、乳糖、果糖、丙三醇的一种或其组合；造孔剂为NaHCO3、NaCl、十二烷基硫酸钠（SDS）、十二烷基苯磺酸钠的一种或其组合，前两者的混合比例范围为，填充剂：持水剂=1～3 wt%：3～10 wt%，造孔剂的添加浓度根据工具表面孔隙率的要求进行调整。
所述的生物高分子材料为淀粉、改性纤维素、壳聚糖、琼脂糖、葡甘聚糖，海藻酸钠、明胶、卡拉胶、黄原胶、果胶、豆胶、聚乳酸中的一种或其组合。
所述的干燥可以采用恒温干燥或红外干燥等干燥方法。
一种超细磨料生物高分子柔性抛光膜的制备方法，包括如下步骤：
（1）改性处理： 超细磨粒添加到偶联剂的水溶液中改性处理；
（2）基材混合： 处理后的超细磨粒、干燥控制添加剂以及生物高分子溶胶以0.1%～2%：4% ～14%：1.5%～5%比例混合均匀；
（3）成型干燥：将混合溶胶通过喷涂或刮抹成型，再物理或化学交联固化，干燥后制成抛光膜。
其中，步骤（1）中，超细磨粒和偶联剂比例范围为质量比100：0.1～10。
本发明的技术效果：
本发明的超细磨料生物高分子柔性抛光膜可以广泛的用于陶瓷基板、半导体晶圆、光学晶体、装饰及工程石材，特别是大尺寸平面的超精密加工。本发明的抛光膜中超细磨料经偶联剂表面改性，有效解决了磨料的团聚问题，且增强了生物高分子基材对无机磨料的把持能力；又由于该抛光膜具有良好的柔韧性，可以实现磨粒的容没，在固结磨料高效加工的同时避免了硬质大颗粒对工件的划伤；本发明的抛光膜中还含有干燥控制化学添加剂，使得抛光膜具有良好的机械性能和储存寿命；所选的生物高分子材料可以被微生物降解，是一种环保型的抛光工具。
具体的实施方式
实施例1
本发明超细磨料生物高分子柔性抛光膜，其基材选用：
超细磨料：金刚石；
干燥控制化学添加剂：包括填充剂纳米SiO2、持水剂蔗糖和造孔剂十二烷基硫酸钠（SDS）；
所述的生物高分子基材：淀粉、卡拉胶组合；
偶联剂：KH-550硅烷偶联剂的水溶液。
本发明超细磨料生物高分子柔性抛光膜的制备方法，包括如下步骤：
（1）改性处理：粒度为500 nm的金刚石添加到KH-550硅烷偶联剂的水溶液（偶联剂浓度0.005%，金刚石的添加量1%）中超声30分钟。
（2）基材混合：处理后的金刚石粉（表面处理后，偶联剂水解形成的官能团吸附在金刚石上，过滤得到金刚石粉）、粒径30 nm的SiO2、SDS、蔗糖、卡拉胶和淀粉在去离子水中通过机械搅拌混合均匀，它们的质量百分比浓度分别为1%、3%、0.1%、3%、6%、4%。
（3）成型干燥：将溶胶通过涂布机均匀的涂布到无纺布表面，喷洒雾化的钠离子溶液形成凝胶。恒温干燥后粘附到背胶上，制成本发明的抛光膜。
将抛光膜贴到AUTOPOL-1000S自动研磨抛光机的抛光盘上，研磨盘速度设为120 rpm，载样盘速度设为60 rpm，抛光压力设为3 kg，对原始粗糙度10 nm的SiC晶片抛光2 h，表面粗糙度达到0.3 nm，且晶片表面无划痕和凹坑。
实施例2
本发明超细磨料生物高分子柔性抛光膜，其基材选用：
超细磨料：氧化铝；
干燥控制化学添加剂：包括填充剂粒径20nm的CaCO3、持水剂丙三醇和造孔剂NaCl晶粒；
所述的生物高分子基材：壳聚糖和海藻酸钠组合。
偶联剂：TTS钛酸酯偶联剂
本发明超细磨料生物高分子柔性抛光膜的制备方法，包括如下步骤：
（1）改性处理：在常温下，将粒度为10 µm的氧化铝添加到TTS钛酸酯偶联剂（氧化铝和TTS的量分别为2%和0.02%）中超声10分钟。
（2）基材混合：处理后的氧化铝、粒径20nm的CaCO3、NaCl晶粒、丙三醇、壳聚糖和海藻酸钠在去离子水中通过机械搅拌混合均匀，其质量百分比浓度分别为2%、1%、0.2%、3%、3.5%、5%。
（3）成型干燥：将溶胶涂覆到圆形喷锡万能板上，浸泡到钙离子溶液中形成凝胶膜。红外干燥后从万能板上轻轻撕下，将膜片光滑面贴到圆形背胶上，就可以制成本发明的抛光膜。
将这种抛光膜贴到AUTOPOL -1000S自动研磨抛光机的抛光盘上，研磨盘速度设为90 rpm，载样盘速度设为80 rpm，抛光压力设为2 kg，对原始粗糙度500 nm的单晶Si片抛光30 min，表面粗糙度达到0.6 nm，且晶片表面无划痕和凹坑。
需要说明的是上述两个实施例仅用来进一步本发明超细磨料生物高分子柔性抛光膜及制备方法，还包括并不限于下述选择：
物理或化学交联包括：温度变化引起的分子缠结（明胶、琼脂糖）；离子交联作用（海藻酸钠、卡拉胶、海藻酸钠和豆胶复合、卡拉胶和黄原胶复合）；氢键或疏水作用（淀粉、改性纤维素、壳聚糖、葡甘聚糖和果胶）；结晶作用（聚乳酸）。
所述的偶联剂为硅烷偶联剂（例如KH540、KH550、KH580 等）、钛酸酯偶联剂（例如KR-TTS、KP-TTS和KR-41B等）、木质素偶联剂（例如溶剂型高沸醇HBS等）的一种或其组合。
所述的超细磨料为金刚石、碳化物（例如碳化硅等）、硼化物（例如氮化硼等）、氧化物（例如氧化铝、氧化硅、氧化铈等）的一种或者几种组合。
超细磨料的粒径在50 nm - 40 µm。可以为50 nm、100 nm、250 nm、500 nm、1 µm、5 µm、10 µm等。
所述的干燥控制化学添加剂包括填充剂、持水剂和造孔剂。填充剂和持水性的混合比例范围为，填充剂：持水剂=1～3 wt%：3～10 wt%，造孔剂的添加浓度范围可根据所制备工具的孔隙率要求进行适当调整，一般可以采用0.1-2%，优选为0.5-1.5%。
填充剂可以为纳米SiO2、纳米CaCO3、纳米聚酰亚胺和纳米钙镁粉等中的一种或者几种组合；持水剂可以为蔗糖、乳糖、果糖、丙三醇等中的一种或者几种组合；造孔剂可以为NaHCO3、NaCl、十二烷基硫酸钠（SDS）、十二烷基苯磺酸钠等中的一种或者几种组合。
所述的生物高分子基材可以为淀粉、改性纤维素、壳聚糖、琼脂糖、葡甘聚糖，海藻酸钠、明胶、卡拉胶、黄原胶、果胶、豆胶、聚乳酸等中的一种或者几种组合。
工业实用性
本发明的超细磨料生物高分子柔性抛光膜，其抛光膜中超细磨料经偶联剂表面改性，有效解决了磨料的团聚问题，且增强了生物高分子基材对无机磨料的把持能力；又由于该抛光膜具有良好的柔韧性，可以实现磨粒的容没，在固结磨料高效加工的同时避免了硬质大颗粒对工件的划伤，可以广泛的用于陶瓷基板、半导体晶圆、光学晶体、装饰及工程石材，特别是大尺寸平面的超精密加工。

Claims (11)

  1. 一种超细磨料生物高分子柔性抛光膜，其特征是：其基材包括：经过表面改性的超细磨料0.1-10 wt%、干燥控制化学添加剂5-15 wt%和生物高分子溶胶1-10 wt%；所述基材按比例均匀混合，通过物理或化学交联固化成型，干燥后形成；
    所述的表面改性是通过偶联剂对超细磨料进行化学包覆以提高磨料在高分子基材中的分散性和把持力。
  2. 根据权利要求1所述的超细磨料生物高分子柔性抛光膜，其特征是所述的偶联剂为硅烷偶联剂、钛酸酯偶联剂、木质素偶联剂的一种或者其组合。
  3. 根据权利要求1所述的超细磨料生物高分子柔性抛光膜，其特征是所述的超细磨料为金刚石、碳化物、硼化物、氧化物的一种或者几种组合，超细磨料的粒径在5 nm-40 µm。
  4. 根据权利要求1所述的超细磨料生物高分子柔性抛光膜，其特征是所述的干燥控制化学添加剂包括填充剂、持水剂和造孔剂，填充剂为纳米SiO2、纳米CaCO3、纳米聚酰亚胺和纳米钙镁粉的一种或其组合；持水剂为蔗糖、乳糖、果糖、丙三醇的一种或其组合；造孔剂为NaHCO3、NaCl、十二烷基硫酸钠、十二烷基苯磺酸钠的一种或其组合，前两者的混合比例范围为，填充剂：持水剂=1～3 wt%：3～10 wt%，造孔剂的添加浓度根据工具表面孔隙率的要求进行调整。
  5. 根据权利要求1所述的超细磨料生物高分子柔性抛光膜，其特征是所述的生物高分子材料为淀粉、改性纤维素、壳聚糖、琼脂糖、葡甘聚糖，海藻酸钠、明胶、卡拉胶、黄原胶、果胶、豆胶、聚乳酸中的一种或其组合。
  6. 如权利要求1至5任一项所述的超细磨料生物高分子柔性抛光膜的制备方法，包括如下步骤：
    （1） 改性处理：超细磨粒添加到偶联剂的水溶液中改性处理；
    （2） 基材混合：处理后的超细磨粒、干燥控制化学添加剂以及生物高分子溶胶以0.1%～10%：5%～15%：1%～10%比例混合均匀；
    （3）成型干燥：将混合溶胶通过喷涂或刮抹成型，再物理或化学交联固化，干燥后制成抛光膜。
  7. 如权利要求6所述的超细磨料生物高分子柔性抛光膜的制备方法，其特征是：
    所述步骤（1）超细磨粒和偶联剂的比例范围为质量比100：0.1～10。
  8. 如权利要求6所述的超细磨料生物高分子柔性抛光膜的制备方法，其特征是：包括如下步骤：
    （1）改性处理：将粒度为500 nm的金刚石添加到KH-550硅烷偶联剂的水溶液中改性处理；
    （2）基材混合：处理后的金刚石粉、粒径30 nm的SiO2、十二烷基硫酸钠、蔗糖、卡拉胶和淀粉在去离子水中通过机械搅拌混合均匀，它们的质量百分比浓度分别为1%、3%、0.1%、3%、6%、4%；
    （3）成型干燥：将溶胶通过涂布机均匀的涂布到无纺布表面，喷洒雾化的钠离子溶液形成凝胶；恒温干燥制成抛光膜。
  9. 如权利要求8所述的超细磨料生物高分子柔性抛光膜的制备方法，其特征是，所述步骤（1）中偶联剂浓度0.005%，金刚石的添加量1% 。
  10. 如权利要求6所述的超细磨料生物高分子柔性抛光膜的制备方法，其特征是：包括如下步骤：
    （1）改性处理：将粒度为10 µm的氧化铝添加到TTS钛酸酯偶联剂中，超声10分钟，进行改性处理；
    （2）基材混合：处理后的氧化铝、粒径20nm的CaCO3、NaCl晶粒、丙三醇、壳聚糖和海藻酸钠在去离子水中通过机械搅拌混合均匀，其质量百分比浓度分别为2%、1%、0.2%、3%、3.5%、5%；
    （3）成型干燥：将溶胶涂覆到圆形喷锡万能板上，浸泡到钙离子溶液中形成凝胶膜；红外干燥制成抛光膜。
  11. 如权利要求10所述的超细磨料生物高分子柔性抛光膜的制备方法，其特征是，所述步骤（1）氧化铝和TTS的量分别为2%和0.02%。
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