JP4363890B2 - Water-based polishing fluid - Google Patents
Water-based polishing fluid Download PDFInfo
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- JP4363890B2 JP4363890B2 JP2003124946A JP2003124946A JP4363890B2 JP 4363890 B2 JP4363890 B2 JP 4363890B2 JP 2003124946 A JP2003124946 A JP 2003124946A JP 2003124946 A JP2003124946 A JP 2003124946A JP 4363890 B2 JP4363890 B2 JP 4363890B2
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Description
【0001】
【発明の属する技術分野】
本発明は、超硬金属、ステンレス、チタン等の金属類、炭化珪素、窒化ガリウム等のセラミックス類、サファイヤ、結晶化ガラス等の電子材料等の各種の硬質材料を研磨する際に使用される水系研磨加工液に関するものである。
【0002】
【従来の技術】
硬質材料の研磨は、研磨砥粒が分散している研磨加工液をかけながら研磨パッドを材料の研磨面に定加重で押し付けることで行われる。番手の小さな(粒子の粗い)研磨砥粒から始めて段階的に番手を大きくする。最近ではダイヤモンド砥粒の粒子が小さく揃ったものを得られるようになったため、研磨の初期段階からダイヤモンド砥粒を使って平坦度の高い研磨面を効率的に仕上げることができるようになっている。研磨加工液は水系と非水系(油性系)があるが、取扱いが簡単なため主に水系が使用されている。
【0003】
かかる研磨に使用される研磨加工液は、研磨砥粒を均一に分散して研磨面に潤沢に送り込む、研磨定盤と研磨面の間を潤滑にする、研磨定盤と研磨面の摩擦熱を冷却する、というような役割を負っている。従来の研磨加工液として、例えば特許文献1に記載されているようなアルキレングリコールモノアルキルエーテル、高級脂肪酸その塩を含むものが示されている。特許文献2には、グリコール化合物、高級脂肪酸金属塩を含む研磨加工液が記載されている。
【0004】
【特許文献1】
特開平8−287456号公報
【特許文献2】
特開2000−141210号公報
【0005】
【発明が解決しようとする課題】
本件出願の発明者による追試験のためアルキレングリコールと高級脂肪酸塩の研磨加工液でステンレスのような硬質材料を研磨したところ、研磨面の仕上がりの表面粗さは良かったが、研磨加工中の滑りが良すぎて研磨レートが上がらないという結果がでている。
【0006】
本発明は、特許文献1や特許文献2に示された従来の研磨加工液を改良するためになされたもので、研磨砥粒を安定して均一に分散でき、研磨能、浸透性がよく、摩擦熱の冷却効率が優れた研磨加工液を提供するものである。
【0007】
【課題を解決するための手段】
前記の目的を達成するためになされた本発明の水系研磨加工液は、蓚酸、マロン酸、コハク酸、アジピン酸、アゼライン酸、セバシン酸、乳酸、グルコン酸、リンゴ酸、酒石酸、クエン酸、フタル酸、トリメシン酸、及びトリメリット酸から選ばれる少なくとも一種類の酸と、ナトリウム、カリウム、及びアンモニウムから選ばれる少なくとも一種類の塩基とからなるカルボン酸塩と、
エチレングリコール、ジエチレングリコール、プロピレングリコール、ジプロピレングリコール、及び分子量100〜1000のポリエチレングリコールから選ばれる少なくとも一種類のグリコールと、
リン酸及びピロリン酸の何れかの塩とを含有する水溶液に、
3〜10μmの粒径のダイヤモンド砥粒を分散させている。
【0008】
アルキレングリコールとしては、例えばエチレングリコール、ジエチレングリコール、プロピレングリコール、ジプロピレングリコール、分子量100〜1000のポリエチレングリコールが使用できる。
【0009】
アルキレングリコールの混合水溶液中の割合は、1〜90%が好ましく、20〜40%であればさらに好ましい。1%未満ではダイヤモンド砥粒が沈降する傾向がみられ、研磨面の表面粗さが悪くなる。90%以上であると粘性が高くなりすぎ、他の添加物の溶解性も悪くなってしまう。
【0010】
カルボン酸塩の酸の具体例は、カプリル酸、ペラルゴン酸、カプリン酸等のモノカルボン酸、蓚酸、マロン酸、コハク酸、アジピン酸、アゼライン酸、セバシン酸等のジカルボン酸、乳酸、グルコン酸、リンゴ酸、酒石酸、クエン酸等のオキシカルボン酸、フタル酸、トリメシン酸、トリメリット酸等の芳香族カルボン酸、ニトリロトリ酢酸、エチレンジアミンテトラ酢酸等がある。カルボン酸塩の塩基としてはナトリウム、カリウム、アンモニウム、トリエタノールアミン等の水溶性アミンが使用できる。これらの酸と塩基は任意に組み合わされる。
リン酸とピロリン酸との何れかの塩が、リン酸3ナトリウム、又はピロリン酸カリウムであることが好ましい。
【0011】
カルボン酸塩の水系研磨加工液中の割合は0.01〜5%が好ましい。0.01%以下では研磨能が低く加工レートが上がらない。5%以上加えてもさほど研磨能が上がらないので無駄になる。
【0012】
また水系研磨加工液に分散させるダイヤモンド砥粒の種類は、単結晶、多結晶どちらでもよく、天然又は合成のダイヤモンドを使用できる。粒径は、研磨能を向上させ加工レートを上げるため、0.5μm以上が好ましく、さらに好ましくは1μm以上が良い。大きいほど研磨能が上がるが、研磨面の表面粗さが大きくなってしまうため、通常は10μm程度までの粒子径が使われる。
3〜10μmの粒径のダイヤモンド砥粒を分散させているものであると、特に好ましい。
【0013】
本発明の水系研磨加工液には、上記成分の他に防錆剤、界面活性剤、防腐剤を含有することもできる。
【0014】
【発明の実施の形態】
本発明の水系研磨加工液は、以下のように調製される。アルキレングリコールを適当量の純水に溶かし、そこにカルボン酸塩を溶かして水溶液を準備する。その水溶液にリン酸塩の純水溶液を加え、さらに防錆剤等の他の添加成分を加えてから純水で濃度調整をして混合水溶液を得る。この混合水溶液にダイヤモンド砥粒を加えミキサーで高速攪拌するとダイヤモンド砥粒が分散浮遊状態となり、水系研磨加工液が得られる。
【0015】
尚、混合水溶液を得るために全量の純水に全成分を同時に加えることも、溶解が潤沢に進めば問題ない。またダイヤモンド砥粒を分散させるため、必要なら超音波分散機やビーズミルを併用してもよい。
【0016】
本発明の水系研磨加工液は、図1に示すような研磨機で、硬質材料のワーク1を研磨する際に使用される。ワーク1は、荷重回転軸14に繋がるセラミック板12にワックスによって複数枚貼り付けられる。荷重回転軸14は図示しない回転駆動源に繋がっている。数本の円形溝11が削条された回転定盤10は、受盥(不図示)を伴って回転駆動源に繋がっている。水系研磨加工液は、タンク15に貯蔵され、配管パイプによりバルブ16を経て給液ノズル17から回転定盤10の上に向けて噴霧される。回転定盤10の受盥の下方ドレインにつながる配管パイプからポンプ18でタンク15に吸い上げられる。このようにして水系研磨加工液は、タンク15→バルブ16→ワーク1と研磨パッド13の摺接面(研磨面)→ドレイン(不図示)→ポンプ18→タンク15と循環してゆく。
【0017】
研磨加工のときには、回転定盤10が回転し、セラミック板12が回転すると、ワーク1が荷重を受けながら回転定盤10に摺接する。このとき水系研磨加工液は、溝11に溜まりながら回転定盤10の上を濡らしているため、ワーク1と回転定盤10との摺接面で研磨機能を果たす。
【0018】
【実施例】
以下、本発明を適用する実施例と本発明を適用外の比較例の水系研磨加工液を試作し研磨加工に供した例を説明する。
【0019】
参考のために表1に示す配合によって実施例1、比較例1、実施例2、比較例2、実施例3、実施例4、表2に示す配合によって比較例3、比較例4、比較例5、比較例6、比較例7、比較例8、実施例5の水系研磨加工液を、上記の手順により調製した。
【0020】
【表1】
【0021】
【表2】
【0022】
各実施例および比較例で試作した水系研磨加工液を使い、図1に示す研磨加工機で以下のとおり研磨加工をした。予めフェーシングした錫下定盤を用い硬質材料のワーク用テストピースとしてSUS304(5mm×5mm)をセラミックス上定盤にワックスで貼り付けた。水系研磨加工液を30秒毎に3ミリリットル噴霧しながら、セラミックス板に36.5kgの荷重をかけ60rpmで60分研磨した。
【0023】
研磨の終了したテストピースの研磨面を表面粗さ計(東京精密社製サーフコム590A)で測定した。テストピースの研磨前後の重量差から加工レートを算出した。表面粗さRa(nm)、加工レートmg/mgのデータを、表1および表2に併せて記載してある。表1および表2から明らかなように本発明の水系研磨加工液を使った研磨面の表面粗さの値は小さく、加工レート、すなわち同一定条件下における研磨による減量が大きいことが分かる。
【0024】
【発明の効果】
以上、詳細に説明したように、本発明の水系研磨加工液は研磨砥粒を安定して均一に分散でき、研磨能、浸透性がよく、摩擦熱の冷却効率が優れている。そのため本発明の水系研磨加工液を使うことによって、研磨加工面の表面粗さが小さいものとなる。また研磨加工による減量が大きく短時間で研磨できるようになる。すなわち、本発明の水系研磨加工液は、研磨精度の向上と研磨加工の時間短縮に資するところが大である。
【図面の簡単な説明】
【図1】研磨加工機による研磨加工の状態を示す図である。
【符号の説明】
1はワーク、10は定盤、11は溝、12はセラミック板、14は荷重回転軸、15はタンク、16はバルブ、17は給液ノズル、18はポンプである。[0001]
BACKGROUND OF THE INVENTION
The present invention is an aqueous system used when polishing various hard materials such as super hard metals, metals such as stainless steel and titanium, ceramics such as silicon carbide and gallium nitride, and electronic materials such as sapphire and crystallized glass. It relates to a polishing liquid.
[0002]
[Prior art]
The polishing of the hard material is performed by pressing the polishing pad against the polishing surface of the material with a constant load while applying a polishing liquid in which polishing abrasive grains are dispersed. Start with a small (grainy) abrasive grain and increase the count step by step. Recently, it has become possible to obtain diamond grains that are small in size, and it has become possible to efficiently finish polished surfaces with high flatness using diamond grains from the initial stage of polishing. . There are two types of polishing liquids, water-based and non-aqueous (oil-based), but water-based is mainly used because it is easy to handle.
[0003]
The polishing liquid used for such polishing is to uniformly disperse the abrasive grains and send them abundantly to the polishing surface, to lubricate between the polishing surface plate and the polishing surface, to generate frictional heat between the polishing surface plate and the polishing surface. It has a role of cooling. As conventional polishing processing liquids, for example, those containing alkylene glycol monoalkyl ethers and higher fatty acid salts thereof as described in Patent Document 1 are shown. Patent Document 2 describes a polishing liquid containing a glycol compound and a higher fatty acid metal salt.
[0004]
[Patent Document 1]
JP-A-8-287456 [Patent Document 2]
Japanese Patent Laid-Open No. 2000-141210
[Problems to be solved by the invention]
When a hard material such as stainless steel was polished with a polishing liquid of alkylene glycol and a higher fatty acid salt for a follow-up test by the inventors of the present application, the surface roughness of the polished surface was good, but slipping during polishing The result is that the polishing rate does not increase because of too good.
[0006]
The present invention was made in order to improve the conventional polishing liquid shown in Patent Document 1 and Patent Document 2, and can stably and uniformly disperse abrasive grains, and has good polishing ability and permeability. It is an object of the present invention to provide a polishing liquid with excellent frictional heat cooling efficiency.
[0007]
[Means for Solving the Problems]
The aqueous polishing liquid of the present invention made to achieve the above object includes oxalic acid, malonic acid, succinic acid, adipic acid, azelaic acid, sebacic acid, lactic acid, gluconic acid, malic acid, tartaric acid, citric acid, phthalate A carboxylate comprising at least one acid selected from acids, trimesic acid, and trimellitic acid, and at least one base selected from sodium, potassium, and ammonium;
At least one glycol selected from ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, and polyethylene glycol having a molecular weight of 100 to 1000;
The aqueous solution containing any of the salt of phosphoric acid and pyrophosphoric acid,
Diamond abrasive grains having a particle diameter of 3 to 10 μm are dispersed.
[0008]
Examples of the alkylene glycol include ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, and polyethylene glycol having a molecular weight of 100 to 1000.
[0009]
The proportion of the alkylene glycol in the mixed aqueous solution is preferably 1 to 90%, more preferably 20 to 40%. If it is less than 1%, the diamond abrasive grains tend to settle and the surface roughness of the polished surface becomes poor. If it is 90% or more, the viscosity becomes too high, and the solubility of other additives also deteriorates.
[0010]
Specific examples of the acid mosquitoes carboxylic acid salt, caprylic acid, pelargonic acid, monocarboxylic acids such as capric acid, oxalic acid, malonic acid, succinic acid, adipic acid, azelaic acid, dicarboxylic acids such as sebacic acid, lactic acid, gluconic acid , Oxycarboxylic acids such as malic acid, tartaric acid and citric acid, aromatic carboxylic acids such as phthalic acid, trimesic acid and trimellitic acid, nitrilotriacetic acid, ethylenediaminetetraacetic acid and the like. Sodium as the base for mosquito carboxylic acid salts, potassium, ammonium, water soluble amines such as triethanolamine can be used. These acids and bases are arbitrarily combined.
It is preferable that any salt of phosphoric acid and pyrophosphoric acid is trisodium phosphate or potassium pyrophosphate.
[0011]
Mosquito carboxylic proportion of the aqueous polishing liquid of salt from 0.01 to 5% is preferred. If it is 0.01% or less, the polishing ability is low and the processing rate does not increase. Even if 5% or more is added, the polishing ability is not improved so much that it is wasted.
[0012]
The type of diamond abrasive particles dispersed in the aqueous polishing liquid may be either single crystal or polycrystalline, and natural or synthetic diamond can be used. The particle size is preferably 0.5 μm or more, more preferably 1 μm or more in order to improve the polishing ability and increase the processing rate. The larger the size, the higher the polishing ability. However, since the surface roughness of the polished surface increases, a particle size up to about 10 μm is usually used.
It is particularly preferable that diamond abrasive grains having a particle diameter of 3 to 10 μm are dispersed.
[0013]
The aqueous polishing liquid of the present invention may contain a rust inhibitor, a surfactant and a preservative in addition to the above components.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
The aqueous polishing liquid of the present invention is prepared as follows. Dissolved alkylene glycol in purified water appropriate amount, to prepare a solution by dissolving it in mosquito carboxylic acid salt. A pure aqueous solution of phosphate is added to the aqueous solution, and other additive components such as a rust inhibitor are added, and then the concentration is adjusted with pure water to obtain a mixed aqueous solution. When diamond abrasive grains are added to this mixed aqueous solution and stirred at high speed with a mixer, the diamond abrasive grains are dispersed and suspended, and an aqueous polishing liquid is obtained.
[0015]
In addition, in order to obtain mixed aqueous solution, adding all components simultaneously to the whole amount of pure water is not a problem as long as the dissolution proceeds sufficiently. Further, in order to disperse the diamond abrasive grains, an ultrasonic disperser or a bead mill may be used together if necessary.
[0016]
The aqueous polishing liquid of the present invention is used when a hard material workpiece 1 is polished by a polishing machine as shown in FIG. A plurality of workpieces 1 are affixed to a
[0017]
At the time of polishing, when the
[0018]
【Example】
Hereinafter, an example in which a water-based polishing liquid of an example to which the present invention is applied and a comparative example to which the present invention is not applied is made and subjected to polishing will be described.
[0019]
For reference, Example 1, Comparative Example 1, Example 2, Comparative Example 2, Example 3, Example 4, and Comparative Example 3, Comparative Example 4, and Comparative Example according to Table 2 5, Comparative Example 6, Comparative Example 7, Comparative Example 8, and Example 5 were prepared by the above-described procedure.
[0020]
[Table 1]
[0021]
[Table 2]
[0022]
Using the water-based polishing fluids produced in each example and comparative example, polishing was performed as follows with the polishing machine shown in FIG. SUS304 (5 mm × 5 mm) as a hard material workpiece test piece was affixed to the ceramic upper surface plate with wax using a pre-facing tin lower surface plate. While spraying 3 ml of aqueous polishing liquid every 30 seconds, a load of 36.5 kg was applied to the ceramic plate and polished at 60 rpm for 60 minutes.
[0023]
The polished surface of the test piece after polishing was measured with a surface roughness meter (Surfcom 590A manufactured by Tokyo Seimitsu Co., Ltd.). The processing rate was calculated from the weight difference before and after polishing the test piece. Data of surface roughness Ra (nm) and processing rate mg / mg are shown in Table 1 and Table 2 together. As is apparent from Tables 1 and 2, the surface roughness value of the polished surface using the aqueous polishing liquid of the present invention is small, and it can be seen that the processing rate, that is, the weight loss due to polishing under the same constant condition is large.
[0024]
【The invention's effect】
As described above in detail, the aqueous polishing liquid of the present invention can stably and uniformly disperse abrasive grains, has good polishing ability and permeability, and has excellent frictional heat cooling efficiency. Therefore, by using the aqueous polishing liquid of the present invention, the surface roughness of the polished surface becomes small. Further, the weight loss due to polishing is large, and polishing can be performed in a short time. That is, the water-based polishing liquid of the present invention greatly contributes to improvement of polishing accuracy and shortening of polishing time.
[Brief description of the drawings]
FIG. 1 is a diagram showing a state of polishing by a polishing machine.
[Explanation of symbols]
1 is a work, 10 is a surface plate, 11 is a groove, 12 is a ceramic plate, 14 is a load rotating shaft, 15 is a tank, 16 is a valve, 17 is a liquid supply nozzle, and 18 is a pump.
Claims (3)
エチレングリコール、ジエチレングリコール、プロピレングリコール、ジプロピレングリコール、及び分子量100〜1000のポリエチレングリコールから選ばれる少なくとも一種類のグリコールと、
リン酸及びピロリン酸の何れかの塩とを含有する水溶液に、
3〜10μmの粒径のダイヤモンド砥粒を分散させてなる水系研磨加工液。 At least one acid selected from succinic acid, malonic acid, succinic acid, adipic acid, azelaic acid, sebacic acid, lactic acid, gluconic acid, malic acid, tartaric acid, citric acid, phthalic acid, trimesic acid, and trimellitic acid; A carboxylate comprising at least one base selected from sodium, potassium, and ammonium;
At least one glycol selected from ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, and polyethylene glycol having a molecular weight of 100 to 1000;
The aqueous solution containing any of the salt of phosphoric acid and pyrophosphoric acid,
An aqueous polishing liquid in which diamond abrasive grains having a particle diameter of 3 to 10 μm are dispersed.
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JP2003124946A JP4363890B2 (en) | 2003-04-30 | 2003-04-30 | Water-based polishing fluid |
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JP5065574B2 (en) | 2005-01-12 | 2012-11-07 | 住友電気工業株式会社 | Polishing method of GaN substrate |
JP2008246668A (en) * | 2008-07-07 | 2008-10-16 | Yushiro Chem Ind Co Ltd | Aqueous abrasive particle dispersion medium composite, processing aqueous slurry, and processing method using them |
EP2406341B1 (en) | 2009-03-13 | 2020-04-29 | Saint-Gobain Ceramics & Plastics, Inc. | Chemical mechanical planarization using nanodiamond |
JP5965906B2 (en) * | 2010-09-08 | 2016-08-10 | ビーエーエスエフ ソシエタス・ヨーロピアBasf Se | Aqueous polishing composition and method for chemical mechanical polishing of a substrate comprising a silicon oxide dielectric film and a polysilicon film |
JP5195966B2 (en) * | 2011-06-20 | 2013-05-15 | 住友電気工業株式会社 | Polishing method of GaN substrate |
KR20190040360A (en) | 2016-09-23 | 2019-04-17 | 생-고뱅 세라믹스 앤드 플라스틱스, 인코포레이티드 | Chemical mechanical planarization slurry and method of forming the same |
CN111647356A (en) * | 2020-06-09 | 2020-09-11 | 苏州特鲁利电子材料有限公司 | Diamond polishing solution and preparation method thereof |
KR20220149320A (en) * | 2021-04-30 | 2022-11-08 | 주식회사 케이씨텍 | Polishing slurry composition |
CN113618497A (en) * | 2021-07-09 | 2021-11-09 | 维达力实业(赤壁)有限公司 | Polishing liquid for polishing microcrystalline ceramic and microcrystalline ceramic polishing method |
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