CN116970342B - 一种碳化硅加工用多晶金刚石磨抛剂及其制备方法 - Google Patents
一种碳化硅加工用多晶金刚石磨抛剂及其制备方法 Download PDFInfo
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- CN116970342B CN116970342B CN202310956596.1A CN202310956596A CN116970342B CN 116970342 B CN116970342 B CN 116970342B CN 202310956596 A CN202310956596 A CN 202310956596A CN 116970342 B CN116970342 B CN 116970342B
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- polycrystalline diamond
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 40
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000003672 processing method Methods 0.000 title description 2
- 238000003756 stirring Methods 0.000 claims abstract description 47
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 22
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
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- KFUSXMDYOPXKKT-UHFFFAOYSA-N 2-[(2-methylphenoxy)methyl]oxirane Chemical compound CC1=CC=CC=C1OCC1OC1 KFUSXMDYOPXKKT-UHFFFAOYSA-N 0.000 claims description 10
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 claims description 9
- BHIZVZJETFVJMJ-UHFFFAOYSA-N 2-hydroxypropyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OCC(C)O BHIZVZJETFVJMJ-UHFFFAOYSA-N 0.000 claims description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 8
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- 229950003429 sorbitan palmitate Drugs 0.000 claims description 8
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 8
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- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
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- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 2
- AVFZOVWCLRSYKC-UHFFFAOYSA-N 1-methylpyrrolidine Chemical compound CN1CCCC1 AVFZOVWCLRSYKC-UHFFFAOYSA-N 0.000 claims description 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 2
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- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
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- YKDMBTQVKVEMSA-UHFFFAOYSA-N diethylene glycol distearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCOCCOC(=O)CCCCCCCCCCCCCCCCC YKDMBTQVKVEMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229940111071 diethylene glycol distearate Drugs 0.000 claims description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 2
- TVACALAUIQMRDF-UHFFFAOYSA-N dodecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(O)=O TVACALAUIQMRDF-UHFFFAOYSA-N 0.000 claims description 2
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 2
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- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000001593 sorbitan monooleate Substances 0.000 claims description 2
- 235000011069 sorbitan monooleate Nutrition 0.000 claims description 2
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims 1
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
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- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
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- 238000000407 epitaxy Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/10—Treatment with macromolecular organic compounds
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- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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- C10M2201/041—Carbon; Graphite; Carbon black
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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Abstract
本发明公开了一种碳化硅加工用多晶金刚石磨抛剂,以重量份数计,磨抛剂由如下组分制成:改性多晶金刚石0.5~35份、D120溶剂油60~80份、分散剂0.5~5份、悬浮剂1~10份、润滑剂0.5~5份、表面活性剂0.5~5份;制备方法包括如下步骤:将改性多晶金刚石、D120溶剂油加入到配液桶中,超声搅拌5~10min,然后加入分散剂和悬浮剂,超声搅拌5~10min,最后加入润滑剂和表面活性剂,超声搅拌5~10min,混合均匀后得到所述磨抛剂;改性多晶金刚石微粉能够在介质中长期、稳定分散,制备得到的磨抛剂具有良好的冷却性和清洗性、优越的润滑性、高悬浮性、高团聚抑制能力。
Description
技术领域
本发明涉及磨抛剂领域,具体涉及一种碳化硅加工用多晶金刚石磨抛剂及其制备方法。
背景技术
单晶碳化硅(Silicon Carbide,SiC)作为第三代半导体材料(也称为宽禁带半导体材料),与硅(Silicon,Si)和砷化镓(Gallium Arsenide,GaAs)为代表的第一代与第二代半导体材料相比,具有显著的使用性能优势,如节能、大功率等,是光电器件的理想衬底材料。目前,各领域传统硅基半导体器件在很多方面的性能已经接近极限,因此SiC将成为突破相关瓶颈的优选材料。另一方面,应用于半导体领域的碳化硅衬底对平坦度、TTV、表面粗糙度等方面要具有更高的精度要求。但是,由于碳化硅单晶的硬度极高且耐腐蚀性优良,导致碳化硅衬底的加工性较差,难以在维持高研磨速度的同时保持高质量表面。
由于碳化硅硬度仅次于金刚石,故在对碳化硅单晶衬底进行研磨时,通常采用金刚石作为磨料,多晶金刚石拥有高的去除率和韧性,具有自锐性,与单晶金刚石比起来,更不容易产生表面划伤,因此多晶金刚石微粉磨抛剂是碳化硅晶片加工主要研磨材料。
目前,市面上常用的研磨液可分为水性和油性研磨液两种,但是,由于金刚石微粉比表面积大、比表面能高、处于热力学不稳定状态,所以在介质中分散稳定性差、容易发生团聚,研磨液长期放置时,会出现分层、失效等情况;同时为了保证磨料的悬浮稳定性,研磨液的润滑作用有限,导致其去除率偏低,不利于加工效率的提高,使得研磨液在应用过程中受到很大程度的制约。
中国专利文献CN201010223346.X公开了一种纳米级抛光液及其调配方法,该抛光液由单晶人造金刚石微粉、氧化铝微粉、硅胶、表面活性剂、分散剂、润滑剂、化学pH值调节剂和溶剂配置而成,具体质量百分比为:金刚石微粉0.1~10%,氧化铝微粉0.1~5%,硅胶0.1~10%,表面活性剂0.3~10%,分散剂0.05~4%,润滑剂0.5~1%,化学pH值调节剂0.01~1%,溶剂60~98.2%。实现了理想的抛光效果,满足了GaN外延用衬底(碳化硅,蓝宝石)进行减薄研磨工艺的要求,为半导体抛光工艺提供了良好的技术手段。
中国专利文献CN201210560797.1公开了一种油性金刚石研磨液及其制备方法,该研磨液各组分的重量配比为:金刚石微粉:0.001~10%;表面活性剂:0.001~20%;分散剂:0~20%;pH值调节剂:0~10%;润湿剂:0~10%;其余为油。
无论水基还是油基的研磨液,制备的关键都是金刚石微粒在介质中的长期、稳定分散。金刚石微粒较小的尺寸、极大的比表面积、较高的表面能、表面缺少邻近的配位原子,导致颗粒表面存在大量的不饱和键,彼此之间极易产生自发团聚现象,形成二次粒子。因此导致了现有的研磨液仍存在性能不稳定,不能长期储存,使用过程中易产生分散不均匀、易沉淀、吸附性差、使用后清洗困难等问题。
发明内容
为了解决现有技术存在的不足,本发明的目的在于提供一种碳化硅加工用多晶金刚石磨抛剂及其制备方法,制备得到的磨抛剂具有良好的冷却性和清洗性、优越的润滑性、高悬浮性、高团聚抑制能力,改性多晶金刚石微粉能够在介质中长期、稳定分散,具有非常优异的技术效果、经济效益和环保效益,有良好的大规模推广前景和应用价值。
为了实现上述目的,本发明采用如下技术方案:
一种碳化硅加工用多晶金刚石磨抛剂,以重量份数计,由如下组分制成:改性多晶金刚石0.5~35份、D120溶剂油60~80份、分散剂0.5~5份、悬浮剂1~10份、润滑剂0.5~5份、表面活性剂0.5~5份。
优选的,所述改性多晶金刚石的制备方法包括如下步骤:
(1)将多晶金刚石真空干燥,待冷却后加入到硫酸中,然后加入KMnO4粉末,超声处理,密封搅拌反应,待产物冷却后洗涤至中性、干燥过夜,得到羧基化多晶金刚石;
(2)将羧基化多晶金刚石、邻甲苯基缩水甘油醚、磷酸加入到反应容器中,在氮气氛围下搅拌反应,将产物过滤、洗涤、干燥,得到预改性多晶金刚石;
(3)将预改性多晶金刚石分散至丙交酯中,超声处理,然后加入辛酸亚锡,在氮气氛围下搅拌反应,将产物过滤、洗涤、干燥,得到改性多晶金刚石。
优选的,步骤(1)中,所述多晶金刚石微粉表面光滑,两端呈锐边,相邻棱边线多数构成锐角或钝角,粒径为1~10μm。
优选的,步骤(1)中,真空干燥条件为50~70℃下干燥18~24h;硫酸浓度为95~98wt%,超声处理时间为0.5~1h。
优选的,步骤(1)中,多晶金刚石、硫酸、KMnO4的重量比为10:120~150:8~14;搅拌反应条件为150~180℃下反应3~6h。
优选的,步骤(2)中,羧基化多晶金刚石、邻甲苯基缩水甘油醚的重量比为10:150~180:1~5,搅拌反应条件为70~100℃下反应4~8h。
优选的,步骤(3)中,预改性多晶金刚石、丙交酯、辛酸亚锡的重量比为10:50~80:1~2;超声处理时间为1~2h;搅拌反应条件为110~140℃下反应18~24h。
优选的,所述分散剂为丙二醇甲醚醋酸酯、烷羟基氨基酰胺、月桂醇、壬基酚聚氧乙烯醚、脂肪胺聚氧乙烯醚中的一种或多种;所述悬浮剂为羧甲基纤维素、改性聚脲、N-甲基吡咯烷酮、甲基吡咯烷、蓖麻油衍生物中的一种或多种。
优选的,所述润滑剂为甘油三硬脂酸酯、丙二醇单十二酸酯、二乙二醇双硬脂酸酯、硼酸酯中的一种或多种;所述表面活性剂为十二烷基苯磺酸、单十二烷基磷酸酯、单十四烷基磷酸酯、失水山梨醇棕榈酸酯、失水山梨醇单油酸酯、脂肪醇聚乙二醇酯中的一种或多种。
本发明还要求保护一种所述磨抛剂的制备方法,其特征在于,包括如下步骤:按重量份将改性多晶金刚石、D120溶剂油加入到配液桶中,超声搅拌5~10min;然后加入分散剂和悬浮剂,超声搅拌5~10min;最后加入润滑剂和表面活性剂,超声搅拌5~10min,混合均匀后得到一种碳化硅加工用多晶金刚石磨抛剂。
与现有技术相比,本发明具有如下有益效果:
1)本发明提供了一种碳化硅加工用多晶金刚石磨抛剂,悬浮剂能够改善多晶金刚石微粉在体系中的分散性、悬浮性,减缓金刚石微粉的沉淀速度;润滑剂能够在研磨铜盘表面形成一层油膜,以减小衬底与研磨盘之间的摩擦,从而起到减小盘温、TTV的效果;经过改性处理的多晶金刚石粉,能够在介质中均匀分散、长时间悬浮,不仅能够防止金刚石微粉团聚造成衬底损伤,提高良品率,同时还能有效增加磨抛剂的使用寿命,从而降低碳化硅的研磨成本。
2)本发明提供了一种改性多晶金刚石,首先用浓硫酸、KMnO4处理多晶金刚石,将其表面的含氧活性基团氧化为羧基,然后利用羧基化多晶金刚石与邻甲苯基缩水甘油醚,在磷酸催化剂的作用下进行开环反应,通过羧基与环氧基的反应得到含苯羟基酯,一方面能够增加金刚石微粒之间的空间位阻改善其悬浮性能,另一方面刚性苯环的引入能够增加多晶金刚石的自锐性从而提升其抛光效率,同时,引入的羟基能够引发环状丙交酯在多晶金刚石表面发生开环聚合反应,将聚乳酸接枝到多晶金刚石表面;以共价结合的方式将聚乳酸链键接到金刚石表面,聚酯链舒展开后能够使金刚石微粒彼此错开,从而赋予微粒良好的分散性和分散稳定性;同时,聚乳酸能够在金刚石微粒表面构筑一层膜,使微粒能够在油相中相互弹开,削弱微粒之间的相互作用能,阻止金刚石微粒的重新团聚,从而实现改性多晶金刚石微粒的稳定分散。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本发明的某些实施例示意图,因此不应被看作是对范围的限定,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他相关的附图。
图1为羧基化多晶金刚石制备预改性多晶金刚石的反应过程;
图2为多晶金刚石的粒径分布示意图;
图3为改性多晶金刚石镜下示意图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚,以下结合实施例,对本发明作进一步的详细说明。当然,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
如无特殊说明外,本发明中的化学试剂和材料均通过市场途径购买或通过市场途径购买的原料合成。
下面通过具体实施例,来对本发明作进一步的说明。
实施例1
一种碳化硅加工用多晶金刚石磨抛剂的制备方法,包括如下步骤:
(1)将10g粒径为1~10μm的多晶金刚石(D50=2.857μm)在70℃下真空干燥24h,待冷却后加入到150g 98wt%硫酸中,然后加入14g KMnO4粉末,超声处理1h,密封、180℃下搅拌反应6h,待产物冷却后洗涤至中性、干燥过夜,得到羧基化多晶金刚石;
(2)将10g羧基化多晶金刚石、180g邻甲苯基缩水甘油醚、5g磷酸加入到反应容器中,在氮气氛围、100℃下搅拌反应8h,将产物过滤、洗涤、干燥,得到预改性多晶金刚石;
(3)将10g预改性多晶金刚石分散至80g丙交酯中,超声处理2h,然后加入2g辛酸亚锡,在氮气氛围、140℃下搅拌反应24h,将产物过滤、洗涤、干燥,得到改性多晶金刚石;
(4)将25g改性多晶金刚石、70g D120溶剂油加入到配液桶中,超声搅拌7min;然后加入3g丙二醇甲醚醋酸酯和8g N-甲基吡咯烷酮,超声搅拌8min;最后加入4g丙二醇单十二酸酯和3.5g失水山梨醇棕榈酸酯,超声搅拌8min,混合均匀后得到一种碳化硅加工用多晶金刚石磨抛剂。
实施例2
一种碳化硅加工用多晶金刚石磨抛剂的制备方法,包括如下步骤:
(1)将10g粒径为1~10μm的多晶金刚石(D50=2.857μm)在50℃下真空干燥18h,待冷却后加入到120g 98wt%硫酸中,然后加入8g KMnO4粉末,超声处理0.5h,密封、150℃下搅拌反应3h,待产物冷却后洗涤至中性、干燥过夜,得到羧基化多晶金刚石;
(2)将10g羧基化多晶金刚石、150g邻甲苯基缩水甘油醚、1g磷酸加入到反应容器中,在氮气氛围、70℃下搅拌反应4h,将产物过滤、洗涤、干燥,得到预改性多晶金刚石;
(3)将10g预改性多晶金刚石分散至50g丙交酯中,超声处理1h,然后加入1g辛酸亚锡,在氮气氛围、110℃下搅拌反应18h,将产物过滤、洗涤、干燥,得到改性多晶金刚石;
(4)将25g改性多晶金刚石、70g D120溶剂油加入到配液桶中,超声搅拌7min;然后加入3g丙二醇甲醚醋酸酯和8g N-甲基吡咯烷酮,超声搅拌8min;最后加入4g丙二醇单十二酸酯和3.5g失水山梨醇棕榈酸酯,超声搅拌8min,混合均匀后得到一种碳化硅加工用多晶金刚石磨抛剂。
实施例3
一种碳化硅加工用多晶金刚石磨抛剂的制备方法,包括如下步骤:
(1)将10g粒径为1~10μm的多晶金刚石(D50=2.857μm)在60℃下真空干燥20h,待冷却后加入到130g 98wt%硫酸中,然后加入10g KMnO4粉末,超声处理0.5h,密封、160℃下搅拌反应4h,待产物冷却后洗涤至中性、干燥过夜,得到羧基化多晶金刚石;
(2)将10g羧基化多晶金刚石、160g邻甲苯基缩水甘油醚、3g磷酸加入到反应容器中,在氮气氛围、80℃下搅拌反应6h,将产物过滤、洗涤、干燥,得到预改性多晶金刚石;
(3)将10g预改性多晶金刚石分散至60g丙交酯中,超声处理1h,然后加入1g辛酸亚锡,在氮气氛围、120℃下搅拌反应20h,将产物过滤、洗涤、干燥,得到改性多晶金刚石;
(4)将25g改性多晶金刚石、70g D120溶剂油加入到配液桶中,超声搅拌7min;然后加入3g丙二醇甲醚醋酸酯和8g N-甲基吡咯烷酮,超声搅拌8min;最后加入4g丙二醇单十二酸酯和3.5g失水山梨醇棕榈酸酯,超声搅拌8min,混合均匀后得到一种碳化硅加工用多晶金刚石磨抛剂。
实施例4
一种碳化硅加工用多晶金刚石磨抛剂的制备方法,包括如下步骤:
(1)将10g粒径为1~10μm的多晶金刚石(D50=2.857μm)在60℃下真空干燥22h,待冷却后加入到140g 98wt%硫酸中,然后加入12g KMnO4粉末,超声处理0.5h,密封、170℃下搅拌反应5h,待产物冷却后洗涤至中性、干燥过夜,得到羧基化多晶金刚石;
(2)将10g羧基化多晶金刚石、170g邻甲苯基缩水甘油醚、4g磷酸加入到反应容器中,在氮气氛围、90℃下搅拌反应7h,将产物过滤、洗涤、干燥,得到预改性多晶金刚石;
(3)将10g预改性多晶金刚石分散至70g丙交酯中,超声处理1h,然后加入1g辛酸亚锡,在氮气氛围、130℃下搅拌反应22h,将产物过滤、洗涤、干燥,得到改性多晶金刚石;
(4)将25g改性多晶金刚石、70g D120溶剂油加入到配液桶中,超声搅拌7min;然后加入3g丙二醇甲醚醋酸酯和8g N-甲基吡咯烷酮,超声搅拌8min;最后加入4g丙二醇单十二酸酯和3.5g失水山梨醇棕榈酸酯,超声搅拌8min,混合均匀后得到一种碳化硅加工用多晶金刚石磨抛剂。
对比例1
一种多晶金刚石磨抛剂的制备方法,包括如下步骤:
(1)将10g粒径为1~10μm的多晶金刚石(D50=2.857μm)在50~70℃下真空干燥18~24h,待冷却后加入到120~150g 98wt%硫酸中,然后加入8~14g KMnO4粉末,超声处理0.5~1h,密封、150~180℃下搅拌反应3~6h,待产物冷却后洗涤至中性、干燥过夜,得到羧基化多晶金刚石;
(2)将10g羧基化多晶金刚石、150~180g邻甲苯基缩水甘油醚、1~5g磷酸加入到反应容器中,在氮气氛围、70~100℃下搅拌反应4~8h,将产物过滤、洗涤、干燥,得到预改性多晶金刚石;
(3)将25g预改性多晶金刚石、70g D120溶剂油加入到配液桶中,超声搅拌7min;然后加入3g丙二醇甲醚醋酸酯和8g N-甲基吡咯烷酮,超声搅拌8min;最后加入4g丙二醇单十二酸酯和3.5g失水山梨醇棕榈酸酯,超声搅拌8min,混合均匀后得到一种多晶金刚石磨抛剂。
对比例2
一种多晶金刚石磨抛剂的制备方法,包括如下步骤:
将25g多晶金刚石、70g D120溶剂油加入到配液桶中,超声搅拌7min;然后加入3g丙二醇甲醚醋酸酯和8g N-甲基吡咯烷酮,超声搅拌8min;最后加入4g丙二醇单十二酸酯和3.5g失水山梨醇棕榈酸酯,超声搅拌8min,混合均匀后得到一种多晶金刚石磨抛剂。
以下对实施例1~4、对比例1制备得到的磨抛剂进行性能测试。
将制备好的磨抛剂静置14天观察磨抛剂是否发生分层、聚沉现象,实施例1~4无分层或聚沉现象,稳定性良好,对比例1在第4天发生分层聚沉现象,稳定性一般,对比例2在第2天发生分层聚沉现象,稳定性差。
采用双面研磨机同时加工4片6寸碳化硅晶片,压力为100g/cm2,上盘转速为20rpm,下盘转速为50rpm,料液供给流量为2mL/min,20min后下机量测碳化硅晶片的划痕深度、TTV和抛光速率,取4片平均值。抛光速率通过抛光前后碳化硅晶片厚度变化来计算,即抛光速率=抛光前后的移除量/抛光时间,晶片厚度变化用千分表测量。盘温通过铜盘机自带测温系统得到。具体数据见表1。
表1磨抛剂综合性能评价数据
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (9)
1.一种碳化硅加工用多晶金刚石磨抛剂,其特征在于,以重量份数计,由如下组分制成:改性多晶金刚石0.5~35份、D120溶剂油60~80份、分散剂0.5~5份、悬浮剂1~10份、润滑剂0.5~5份、表面活性剂0.5~5份;
所述改性多晶金刚石的制备方法包括如下步骤:
(1)将多晶金刚石真空干燥,待冷却后加入到硫酸中,然后加入KMnO4粉末,超声处理,密封搅拌反应,待产物冷却后洗涤至中性、干燥过夜,得到羧基化多晶金刚石;
(2)将羧基化多晶金刚石、邻甲苯基缩水甘油醚、磷酸加入到反应容器中,在氮气氛围下搅拌反应,将产物过滤、洗涤、干燥,得到预改性多晶金刚石;
(3)将预改性多晶金刚石分散至丙交酯中,超声处理,然后加入辛酸亚锡,在氮气氛围下搅拌反应,将产物过滤、洗涤、干燥,得到改性多晶金刚石。
2.根据权利要求1所述的磨抛剂,其特征在于,步骤(1)中,所述多晶金刚石的粒径为1~10μm。
3.根据权利要求1所述的磨抛剂,其特征在于,步骤(1)中,真空干燥条件为50~70℃下干燥18~24h;硫酸浓度为95~98wt%,超声处理时间为0.5~1h。
4.根据权利要求1所述的磨抛剂,其特征在于,步骤(1)中,多晶金刚石、硫酸、KMnO4的重量比为10:120~150:8~14;搅拌反应条件为150~180℃下反应3~6h。
5.根据权利要求1所述的磨抛剂,其特征在于,步骤(2)中,羧基化多晶金刚石、邻甲苯基缩水甘油醚的重量比为10:150~180:1~5,搅拌反应条件为70~100℃下反应4~8h。
6.根据权利要求1所述的磨抛剂,其特征在于,步骤(3)中,预改性多晶金刚石、丙交酯、辛酸亚锡的重量比为10:50~80:1~2;超声处理时间为1~2h;搅拌反应条件为110~140℃下反应18~24h。
7.根据权利要求1所述的磨抛剂,其特征在于,所述分散剂为丙二醇甲醚醋酸酯、烷羟基氨基酰胺、月桂醇、壬基酚聚氧乙烯醚、脂肪胺聚氧乙烯醚中的一种或多种;所述悬浮剂为羧甲基纤维素、改性聚脲、N-甲基吡咯烷酮、甲基吡咯烷、蓖麻油衍生物中的一种或多种。
8.根据权利要求1所述的磨抛剂,其特征在于,所述润滑剂为甘油三硬脂酸酯、丙二醇单十二酸酯、二乙二醇双硬脂酸酯、硼酸酯中的一种或多种;所述表面活性剂为十二烷基苯磺酸、单十二烷基磷酸酯、单十四烷基磷酸酯、失水山梨醇棕榈酸酯、失水山梨醇单油酸酯、脂肪醇聚乙二醇酯中的一种或多种。
9.一种如权利要求1~8任一项所述磨抛剂的制备方法,其特征在于,包括如下步骤:按重量份将改性多晶金刚石、D120溶剂油加入到配液桶中,超声搅拌5~10min;然后加入分散剂和悬浮剂,超声搅拌5~10min;最后加入润滑剂和表面活性剂,超声搅拌5~10min,混合均匀后得到一种碳化硅加工用多晶金刚石磨抛剂。
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