JP2006249129A - Method for producing polishing agent and polishing agent - Google Patents
Method for producing polishing agent and polishing agent Download PDFInfo
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- JP2006249129A JP2006249129A JP2005063728A JP2005063728A JP2006249129A JP 2006249129 A JP2006249129 A JP 2006249129A JP 2005063728 A JP2005063728 A JP 2005063728A JP 2005063728 A JP2005063728 A JP 2005063728A JP 2006249129 A JP2006249129 A JP 2006249129A
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- abrasive
- cerium
- producing
- polishing agent
- hydroxide particles
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 44
- 238000005498 polishing Methods 0.000 title claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 89
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 39
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 31
- 150000003839 salts Chemical class 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000000151 deposition Methods 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- 150000000703 Cerium Chemical class 0.000 claims description 5
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 claims description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 3
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 3
- OKJMLYFJRFYBPS-UHFFFAOYSA-J tetraazanium;cerium(4+);tetrasulfate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OKJMLYFJRFYBPS-UHFFFAOYSA-J 0.000 claims description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical group [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 2
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 description 18
- 235000011114 ammonium hydroxide Nutrition 0.000 description 12
- 239000011521 glass Substances 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 7
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
- 229910000420 cerium oxide Inorganic materials 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
本発明は、研磨剤の製造方法及び研磨剤に関する。 The present invention relates to a method for producing an abrasive and an abrasive.
現在の超々大規模集積回路では、実装密度を高める傾向にあり、種々の微細加工技術が研究、開発されている。既に、デザインルールは、サブハーフミクロンのオーダーになっている。このような厳しい微細化の要求を満足するために開発されている技術の一つにＣＭＰ（ケミカルメカニカルポリッシング）技術がある。この技術は、半導体装置の製造工程において、露光を施す層を平坦化し、露光技術の負担を軽減し、歩留まりを安定させることができるため、例えば、層間絶縁膜の平坦化、シャロー・トレンチ分離等を行う際に必須となる技術である。 In the present ultra-large scale integrated circuit, there is a tendency to increase the mounting density, and various fine processing techniques are being researched and developed. Already, the design rules are on the order of sub-half microns. One of the techniques that have been developed in order to satisfy such demands for strict miniaturization is a CMP (Chemical Mechanical Polishing) technique. Since this technology can flatten the layer to be exposed in the semiconductor device manufacturing process, reduce the burden of the exposure technology, and stabilize the yield, for example, flattening the interlayer insulating film, shallow trench isolation, etc. This technology is indispensable when performing.
従来、半導体装置の製造工程において、フォトマスク用ガラス表面研磨剤として、酸化セリウム研磨剤が用いられている。酸化セリウム粒子はシリカ粒子やアルミナ粒子に比べ硬度が低く、従って研磨表面に傷が入り難いことから仕上げ鏡面研磨に有用である。また、酸化セリウムは強い酸化剤として知られるように、化学的活性な性質を有している。この利点を活かして、半導体絶縁膜用ＣＭＰ研磨剤への適用が有用である。 Conventionally, a cerium oxide abrasive has been used as a glass surface abrasive for a photomask in a semiconductor device manufacturing process. Cerium oxide particles have a lower hardness than silica particles and alumina particles, and are therefore useful for finishing mirror polishing because scratches are less likely to enter the polished surface. Moreover, cerium oxide has a chemically active property as known as a strong oxidizing agent. Taking advantage of this advantage, application to a CMP polishing agent for a semiconductor insulating film is useful.
しかしながら、フォトマスクガラス表面研磨剤としての酸化セリウム研磨剤をそのまま半導体絶縁膜研磨剤として適用すると、粒子が大きく、その為絶縁膜表面に目視で観察できる研磨傷が入ってしまう。粒子径を小さくすると、研磨傷は入りにくくなるが、研磨速度が低下してしまう。酸化セリウム研磨剤による研磨は、酸化セリウムの化学的作用と粒子による機械的除去作用で加工が進行するとされている。粒子による機械的除去作用があると研磨傷が入る。今後、益々半導体素子の多層化・高精細化が予想されており、半導体素子の歩留まり向上には研磨傷フリーで、かつ高平坦化が可能な研磨剤が求められる。特許文献１には、半導体絶縁膜研磨剤として、４価の金属水酸化物粒子とアニオン性添加剤を媒体に分散させたスラリーを含む研磨剤を用いることにより、被研磨面を傷無く、高平坦化に研磨することが可能であることが記載されている。
しかしながら、特許文献１に記載されたスラリーを含む研磨剤を静置しておくと、金属水酸化物粒子の粒径及びスラリーのｐＨが増加もしくは低下してしまい、研磨傷の増加や研磨速度の低下につながるという問題があった。本発明は、経時的に安定な研磨剤の製造方法及び研磨剤を提供するものである。 However, if the abrasive containing the slurry described in Patent Document 1 is allowed to stand, the particle size of the metal hydroxide particles and the pH of the slurry will increase or decrease, resulting in an increase in polishing scratches and polishing rate. There was a problem that led to a decline. The present invention provides a method for producing an abrasive that is stable over time and an abrasive.
本発明者らは、上記課題を解決するため鋭意検討の結果、金属水酸化物粒子析出時のｐＨを制御することにより、研磨剤製造後も研磨剤中に含まれる金属水酸化物粒子の粒径と研磨剤のｐＨを安定に保つことができることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above-mentioned problems, the inventors of the present invention controlled the pH at the time of precipitation of the metal hydroxide particles, so that the particles of the metal hydroxide particles contained in the abrasive even after the production of the abrasive were produced. The inventors have found that the diameter and pH of the abrasive can be kept stable, and have completed the present invention.
すなわち、本発明は以下の通りである。
１．金属塩を含む水溶液にアルカリ液を加えて金属水酸化物粒子を析出させる工程を有する研磨剤の製造方法であって、ｐＨ４．０〜７．５で金属水酸化物粒子を析出させることを特徴とする研磨剤の製造方法。
２．アルカリ液がアンモニア水である項１記載の研磨剤の製造方法。
３．金属塩が４価の金属塩である項１又は２記載の研磨剤の製造方法。
４．４価の金属塩がセリウム塩である項３記載の研磨剤の製造方法。
５．セリウム塩が、硝酸セリウムアンモニウム、硝酸セリウム、硫酸セリウムアンモニウム、酢酸セリウム、塩化セリウムの群から選択される少なくとも１種または２種以上のセリウム塩である項４記載の研磨剤の製造方法。
６．金属塩を含む水溶液の金属塩の濃度が０．２〜５０重量％である項１〜５のいずれかに記載の研磨剤の製造方法。
７．更に、析出させた金属水酸化物粒子を溶液中に分散する工程を有する項１〜６記載のいずれかに記載の研磨剤の製造方法。
８．金属水酸化物粒子を分散する溶液が水である項７に記載の研磨剤の製造方法。
９．項１〜８のいずれかに記載の研磨剤の製造方法により得られた研磨剤。
１０．平均粒径が２００ｎｍ以下の金属水酸化物粒子を含有する項９記載の研磨剤。
１１．製造７日後のｐＨ変化率が１０％以下である項９又は１０記載の研磨剤。
That is, the present invention is as follows.
1. A method for producing an abrasive having a step of depositing metal hydroxide particles by adding an alkali solution to an aqueous solution containing a metal salt, wherein the metal hydroxide particles are precipitated at a pH of 4.0 to 7.5. A method for producing an abrasive.
2. Item 2. The method for producing an abrasive according to Item 1, wherein the alkaline liquid is aqueous ammonia.
3. Item 3. The method for producing an abrasive according to Item 1 or 2, wherein the metal salt is a tetravalent metal salt.
Item 4. The method for producing an abrasive according to Item 3, wherein the tetravalent metal salt is a cerium salt.
5. Item 5. The method for producing an abrasive according to Item 4, wherein the cerium salt is at least one or two or more cerium salts selected from the group consisting of cerium ammonium nitrate, cerium nitrate, cerium ammonium sulfate, cerium acetate, and cerium chloride.
6). The manufacturing method of the abrasive | polishing agent in any one of claim | item 1 -5 whose density | concentration of the metal salt of the aqueous solution containing a metal salt is 0.2 to 50 weight%.
7). Item 7. The method for producing an abrasive according to any one of Items 1 to 6, further comprising a step of dispersing the precipitated metal hydroxide particles in the solution.
8). Item 8. The method for producing an abrasive according to Item 7, wherein the solution in which the metal hydroxide particles are dispersed is water.
9. Item 10. An abrasive obtained by the method for producing an abrasive according to any one of Items 1 to 8.
10. Item 10. The abrasive according to Item 9, containing metal hydroxide particles having an average particle size of 200 nm or less.
11. The abrasive | polishing agent of claim | item 9 or 10 whose pH change rate 7 days after manufacture is 10% or less.
本発明によると、経時的な安定性に優れる研磨剤が得られ、半導体素子製造技術である基板表面の平坦化工程などにおいて使用される研磨剤の製造方法及び研磨剤として有用である。 According to the present invention, an abrasive having excellent stability over time can be obtained, and it is useful as a method for producing an abrasive and an abrasive used in a step of planarizing a substrate surface, which is a semiconductor element manufacturing technique.
本発明の研磨剤の製造方法は、金属塩を含む水溶液にアルカリ液を加えて金属水酸化物粒子を析出させる工程を有する研磨剤の製造方法であって、ｐＨ４．０〜７．５で金属水酸化物粒子を析出させることを特徴とする。 The manufacturing method of the abrasive | polishing agent of this invention is a manufacturing method of the abrasive | polishing agent which has the process of adding an alkali liquid to the aqueous solution containing a metal salt, and depositing metal hydroxide particle | grains, Comprising: It is metal at pH 4.0-7.5. It is characterized by depositing hydroxide particles.
本発明においては、金属塩とアルカリ液とを用いて、ｐＨ４．０〜７．５で金属水酸化物粒子を析出させる。特にｐＨ４．５〜６．５で析出した金属水酸化物粒子は、粒径・ｐＨの変化がほとんどなく、好ましい。金属水酸化物粒子を析出させるｐＨが４．０未満では析出した金属水酸化物粒子の粒径が経時的に次第に減少してしまい、ｐＨが７．５を超えると析出した金属水酸化物粒子が凝結してしまい分散することが困難になってしまう。金属水酸化物粒子を析出させる方法として、金属塩とアルカリ液を混合する手法が使用できる。この方法は、例えば「希土類の科学」（足立吟也編、化学同人）３０４〜３０５頁に説明されている。 In the present invention, metal hydroxide particles are precipitated at a pH of 4.0 to 7.5 using a metal salt and an alkali solution. In particular, metal hydroxide particles precipitated at pH 4.5 to 6.5 are preferable since there is almost no change in particle size and pH. When the pH at which the metal hydroxide particles are precipitated is less than 4.0, the particle size of the precipitated metal hydroxide particles gradually decreases with time, and when the pH exceeds 7.5, the precipitated metal hydroxide particles. Will condense and become difficult to disperse. As a method for precipitating the metal hydroxide particles, a method of mixing a metal salt and an alkali solution can be used. This method is described in, for example, “Science of rare earths” (edited by Adiya Ginya, Kagaku Dojin) pages 304-305.
本発明において用いられる金属塩としては、４価の金属塩が好ましく、中でもセリウム塩がより好ましく、更に硝酸セリウムアンモニウム、硝酸セリウム、硫酸セリウムアンモニウム、酢酸セリウム、塩化セリウムの群から選択されることが特に好ましい。特に収率の観点からは硝酸セリウムアンモニウムが極めて好ましい。金属塩の濃度が、０．１〜５０重量％の水溶液を用いることが好ましい。中でも１〜１０重量％の水溶液であればより好ましく、０．５〜１重量％の水溶液であれば特に好ましい。金属塩の水溶液濃度が０．１重量％に満たないと収率が劣る傾向にあり、５０重量％を超えると、金属水酸化物粒子の分散性が低下する傾向にある。 The metal salt used in the present invention is preferably a tetravalent metal salt, more preferably a cerium salt, and further selected from the group of cerium ammonium nitrate, cerium nitrate, cerium ammonium sulfate, cerium acetate, and cerium chloride. Particularly preferred. In particular, cerium ammonium nitrate is extremely preferable from the viewpoint of yield. It is preferable to use an aqueous solution having a metal salt concentration of 0.1 to 50% by weight. Of these, an aqueous solution of 1 to 10% by weight is more preferred, and an aqueous solution of 0.5 to 1% by weight is particularly preferred. If the aqueous solution concentration of the metal salt is less than 0.1% by weight, the yield tends to be inferior, and if it exceeds 50% by weight, the dispersibility of the metal hydroxide particles tends to decrease.
本発明において用いられるアルカリ液としては、金属水酸化物粒子を析出できるものであれば特に制限は無いが、例えば、アンモニア水、水酸化カリウム、水酸化ナトリウム等が使用できる。金属不純物低減の観点からは、アルカリ液としては、好ましくはアンモニア水が用いられる。金属水酸化物粒子の析出は、金属塩の水溶液に、ｐＨの値が４．０〜７．５、好ましくは４．５〜６．５になるまでアルカリ液を混合することにより行う。 The alkali solution used in the present invention is not particularly limited as long as it can precipitate metal hydroxide particles, and for example, ammonia water, potassium hydroxide, sodium hydroxide, and the like can be used. From the viewpoint of reducing metal impurities, ammonia water is preferably used as the alkaline liquid. Precipitation of metal hydroxide particles is carried out by mixing an alkali solution in an aqueous solution of metal salt until the pH value is 4.0 to 7.5, preferably 4.5 to 6.5.
金属塩の水溶液とアルカリ液の混合で得られた金属水酸化物粒子は、遠心分離などで固液分離を行い洗浄することが好ましい。本発明の研磨剤の製造方法としては、さらに金属水酸化物粒子を溶液中に分散する工程を有することが好ましく、溶液が水であることがより好ましい。例えば洗浄した金属水酸化物粒子に純水等の溶液を加えて分散処理を施すことにより研磨剤を製造することができる。分散方法としてはホモジナイザー、超音波分散機、ビーズミルなどを用いることができる。研磨傷低減の観点からは、分散処理後の金属水酸化物微粒子の粒径は、光子相関法を用いて測定し、２次粒子の平均粒径が２００ｎｍ以下であることが好ましく、３０〜１８０ｎｍがより好ましく、５０〜１５０ｎｍが特に好ましい。 The metal hydroxide particles obtained by mixing an aqueous solution of a metal salt and an alkali solution are preferably washed by solid-liquid separation such as by centrifugation. As a manufacturing method of the abrasive | polishing agent of this invention, it is preferable to have a process which disperse | distributes a metal hydroxide particle further in a solution, and it is more preferable that a solution is water. For example, the abrasive can be produced by adding a solution such as pure water to the washed metal hydroxide particles and applying a dispersion treatment. As a dispersion method, a homogenizer, an ultrasonic disperser, a bead mill, or the like can be used. From the viewpoint of reducing polishing scratches, the particle size of the metal hydroxide fine particles after the dispersion treatment is measured using a photon correlation method, and the average particle size of the secondary particles is preferably 200 nm or less, preferably 30 to 180 nm. Is more preferable, and 50 to 150 nm is particularly preferable.
また、研磨剤中の金属水酸化物粒子（２次粒子）の平均粒径の変化率は、研磨剤製造７日後に、１０％以下であることが好ましく、５％以下であることがより好ましい。本発明の研磨剤は、製造７日後のｐＨ変化率が１０％以下であることが好ましい。すなわち、分散が終了した時点から７日後以降の研磨剤（金属水酸化物粒子が溶液中に分散されたスラリー）のｐＨが１０％以内の変化であることが好ましい。研磨剤製造７日後のｐＨの変化率はより好ましくは５％以下で、特に好ましくは２％以下である。ｐＨの測定は、分散の終了した研磨剤を容器に密封し常温で静置保存し、ガラス電極式水素イオン濃度計を用いて測定した。製造７日後のｐＨ変化率が１０％以下とするためには、前記のように金属塩とアルカリ液とを用いて、ｐＨ４．０〜７．５で金属水酸化物粒子を析出させる。特にｐＨ４．５〜６．５で析出させると好ましい。 Further, the change rate of the average particle diameter of the metal hydroxide particles (secondary particles) in the abrasive is preferably 10% or less, more preferably 5% or less after 7 days from the production of the abrasive. . The polishing agent of the present invention preferably has a pH change rate of 10% or less after 7 days of production. That is, it is preferable that the pH of the abrasive (slurry in which the metal hydroxide particles are dispersed in the solution) after 7 days from the end of the dispersion be within 10%. The pH change rate after 7 days from the production of the abrasive is more preferably 5% or less, and particularly preferably 2% or less. The pH was measured by using a glass electrode-type hydrogen ion concentration meter after sealing the dispersed abrasive in a container and storing it at room temperature. In order to make the pH change rate 7 days after the production 10% or less, the metal hydroxide particles are precipitated at pH 4.0 to 7.5 using the metal salt and the alkali liquid as described above. In particular, it is preferable to deposit at pH 4.5 to 6.5.
（実施例１）
０．１０５ｋｇのＣｅ（ＮＨ４）２（ＮＯ３）６を９．４６ｋｇの純水と混合し、金属塩の水溶液を作製する。次にガラス電極式水素イオン濃度計（株式会社堀場製作所製、商品名Ｄ−２１）を用いてｐＨ値を確認しながら、金属塩の水溶液にアルカリ液であるアンモニア水（２．５重量％水溶液）を混合・攪拌する。ｐＨの値が６．０になったら、一度アンモニア水の混合を終了し、攪拌を行う。ｐＨ値が低下したら、さらにアンモニア水を追加混合し、終ｐＨ値が６．１３である金属水酸化物粒子（水酸化セリウム粒子）が析出した水酸化セリウム粒子含有懸濁液を得た。得られた水酸化セリウム粒子含有懸濁液は遠心分離（株式会社日立製作所製ＨＩＭＡＣ ＣＥＮＴＲＩＦＵＧＥ ＣＴ５ＤＬを使用、条件：３０００ｒｐｍ、１５分間）することによって、固液分離を施して液体と共に金属不純物を除去した後に、固形分１．２重量％になるように、１．６ｋｇの純水を加えた。
Example 1
0.105 kg of Ce (NH 4 ) 2 (NO 3 ) 6 is mixed with 9.46 kg of pure water to prepare an aqueous solution of a metal salt. Next, while confirming the pH value using a glass electrode-type hydrogen ion concentration meter (manufactured by Horiba, Ltd., trade name D-21), an aqueous ammonia solution (2.5 wt% aqueous solution) as an alkali solution while confirming the pH value. ) Is mixed and stirred. When the pH value becomes 6.0, mixing of the ammonia water is once stopped and stirring is performed. When the pH value decreased, ammonia water was further added to obtain a cerium hydroxide particle-containing suspension in which metal hydroxide particles (cerium hydroxide particles) having a final pH value of 6.13 were deposited. The obtained cerium hydroxide particle-containing suspension was subjected to solid-liquid separation by centrifugation (using Hitachi, Ltd. HIMAC CENTRIFUGE CT5DL, conditions: 3000 rpm, 15 minutes) to remove metal impurities along with the liquid. Later, 1.6 kg of pure water was added to a solid content of 1.2% by weight.
この懸濁液を超音波洗浄器（シャープマニュファクチャリングシステム製ＵＴ２０５、出力２００Ｗ）にかけて分散処理を行い、９０分おきに２０ｃｃ程度サンプリングを行い、粒径の変化を光子相関法（マルバーン製、ゼータサイザ）にて測定する。粒径が２００ｎｍ以下になったら超音波洗浄器を停止し、研磨剤を得た。この時の研磨剤中に含まれる金属水酸化物（水酸化セリウム）粒子の平均粒径は、１０１．９ｎｍであった。また、ｐＨ値は４．１４であった。分散処理終了後、得られた研磨剤を容器に密封して静置しておき、１日おきに、研磨剤のｐＨと水酸化セリウム粒子の粒径を測定した。粒径は光子相関法を用いて測定を行った。また、ｐＨに関してはガラス電極式水素イオン濃度計を用いて測定した。研磨剤を静置して７日後のｐＨは４．１０（変化率１％）、水酸化セリウム粒子の平均粒径は１０６．１ｎｍ（変化率４．１％）であった。 This suspension is subjected to dispersion treatment by applying an ultrasonic cleaner (UT205 manufactured by Sharp Manufacturing System, output 200 W), sampling about 20 cc every 90 minutes, and the change in particle size is measured by the photon correlation method (Malvern, Zetasizer). ) To measure. When the particle size became 200 nm or less, the ultrasonic cleaner was stopped to obtain an abrasive. The average particle diameter of the metal hydroxide (cerium hydroxide) particles contained in the abrasive at this time was 101.9 nm. The pH value was 4.14. After the dispersion treatment was completed, the obtained abrasive was sealed in a container and allowed to stand, and the pH of the abrasive and the particle size of the cerium hydroxide particles were measured every other day. The particle size was measured using the photon correlation method. The pH was measured using a glass electrode type hydrogen ion concentration meter. Seven days after the abrasive was allowed to stand, the pH was 4.10 (change rate 1%), and the average particle size of the cerium hydroxide particles was 106.1 nm (change rate 4.1%).
（実施例２）
０．４７ｋｇのＣｅ（ＮＨ４）２（ＮＯ３）６と８．４３ｋｇの純水を混合し、金属塩の水溶液を作製する。次にガラス電極式水素イオン濃度計（株式会社堀場製作所製、商品名Ｄ−２１）を用いてｐＨ値を確認しながら、金属塩の水溶液にアルカリ液であるアンモニア水（２．５重量％水溶液）を混合・攪拌する。ｐＨの値が６．０になったら、一度アンモニア水の混合を終了し、攪拌を行う。ｐＨ値が低下したらさらにアンモニア水を追加混合し、終ｐＨ値が５．７２である金属水酸化物粒子（水酸化セリウム粒子）が析出した水酸化セリウム粒子含有懸濁液を得た。得られた水酸化セリウム粒子含有懸濁液は遠心分離（株式会社日立製作所製ＨＩＭＡＣ ＣＥＮＴＲＩＦＵＧＥ ＣＴ５ＤＬを使用、条件：３０００ｒｐｍ、１５分間）することによって、固液分離を施して液体と共に金属不純物を除去し、固形分１．２重量％になるように７．７９ｋｇの純水を加え、超音波洗浄器（シャープマニュファクチャリングシステム製ＵＴ２０５、出力２００Ｗ）にかけて分散処理を行い、９０分おきに２０ｃｃ程度サンプリングを行い、粒径の変化を光子相関法（マルバーン製、ゼータサイザ）にて測定し、粒径が２００ｎｍ以下になったら超音波洗浄器を停止し、研磨剤を得た。
(Example 2)
0.47 kg of Ce (NH 4 ) 2 (NO 3 ) 6 and 8.43 kg of pure water are mixed to prepare an aqueous solution of a metal salt. Next, while confirming the pH value using a glass electrode-type hydrogen ion concentration meter (manufactured by Horiba, Ltd., trade name D-21), an aqueous ammonia solution (2.5 wt% aqueous solution) as an alkali solution while confirming the pH value. ) Is mixed and stirred. When the pH value becomes 6.0, mixing of the ammonia water is once stopped and stirring is performed. When the pH value decreased, additional ammonia water was further mixed to obtain a cerium hydroxide particle-containing suspension in which metal hydroxide particles (cerium hydroxide particles) having a final pH value of 5.72 were precipitated. The obtained cerium hydroxide particle-containing suspension is centrifuged (using Hitachi, Ltd., HIMAC CENTRIFUGE CT5DL, conditions: 3000 rpm, 15 minutes) to perform solid-liquid separation to remove metal impurities along with the liquid. Add 7.79 kg of pure water to a solid content of 1.2% by weight, disperse it with an ultrasonic cleaner (UT205 manufactured by Sharp Manufacturing System, output 200 W), and sample about 20 cc every 90 minutes. The particle size change was measured by a photon correlation method (Malvern, Zetasizer). When the particle size became 200 nm or less, the ultrasonic cleaner was stopped to obtain an abrasive.
得られた研磨剤中の水酸化セリウム粒子の平均粒径は、１２４．１ｎｍであった。また、研磨剤のｐＨ値は３．７４であった。研磨剤を容器に密封して静置しておき、１日おきに、研磨剤中の水酸化セリウム粒子の粒径と研磨剤のｐＨを測定した。粒径は光子相関法を用いて測定を行った。また、ｐＨに関してはガラス電極式水素イオン濃度計を用いて測定した。研磨剤を静置して８日後の水酸化セリウム粒子の平均粒径は１２４．９ｎｍ（変化率０．６％）、研磨剤のｐＨは３．７２（変化率０．５％）であった。 The average particle diameter of the cerium hydroxide particles in the obtained abrasive was 124.1 nm. The pH value of the abrasive was 3.74. The abrasive was sealed in a container and allowed to stand, and the particle size of the cerium hydroxide particles in the abrasive and the pH of the abrasive were measured every other day. The particle size was measured using the photon correlation method. The pH was measured using a glass electrode type hydrogen ion concentration meter. The average particle diameter of the cerium hydroxide particles 8 days after standing the abrasive was 124.9 nm (change rate 0.6%), and the pH of the abrasive was 3.72 (change rate 0.5%). .
（実施例３）
０．１１ｋｇのＣｅ（ＮＨ４）２（ＮＯ３）６を９．４６ｋｇの純水と混合し、金属塩の水溶液を作製する。次にガラス電極式水素イオン濃度計（株式会社堀場製作所製、商品名Ｄ−２１）を用いてｐＨ値を確認しながら、金属塩の水溶液にアルカリ液であるアンモニア水（２．５重量％水溶液）を混合・攪拌する。ｐＨ計の値が５．０になったら、一度アンモニア水の混合を終了し、攪拌を行う。ｐＨ値が低下したらさらにアンモニア水を追加混合し、終ｐＨ値が５．０５である金属水酸化物粒子（水酸化セリウム粒子）が析出した水酸化セリウム粒子含有懸濁液を得た。得られた水酸化セリウム粒子含有懸濁液は遠心分離（株式会社日立製作所製ＨＩＭＡＣ ＣＥＮＴＲＩＦＵＧＥ ＣＴ５ＤＬを使用、条件：３０００ｒｐｍ、１５分間）することによって、固液分離を施して液体と共に金属不純物を除去し、固形分１．２重量％になるように７．４ｋｇの純水を加え超音波洗浄器（シャープマニュファクチャリングシステム製ＵＴ２０５、出力２００Ｗ）にかけて分散処理を行い、９０分おきに２０ｃｃ程度サンプリングを行い、粒径の変化を光子相関法（マルバーン製、ゼータサイザ）にて測定する。
(Example 3)
0.11 kg of Ce (NH 4 ) 2 (NO 3 ) 6 is mixed with 9.46 kg of pure water to prepare an aqueous solution of a metal salt. Next, while confirming the pH value using a glass electrode-type hydrogen ion concentration meter (manufactured by Horiba, Ltd., trade name D-21), an aqueous ammonia solution (2.5 wt% aqueous solution) as an alkali solution while confirming the pH value. ) Is mixed and stirred. When the value of the pH meter reaches 5.0, mixing of aqueous ammonia is once completed and stirring is performed. When the pH value decreased, ammonia water was further added to obtain a cerium hydroxide particle-containing suspension in which metal hydroxide particles (cerium hydroxide particles) having a final pH value of 5.05 were deposited. The obtained cerium hydroxide particle-containing suspension is centrifuged (using Hitachi, Ltd., HIMAC CENTRIFUGE CT5DL, conditions: 3000 rpm, 15 minutes) to perform solid-liquid separation to remove metal impurities along with the liquid. 7.4 kg of pure water was added so that the solid content was 1.2% by weight, and dispersion treatment was performed using an ultrasonic cleaner (UT205 manufactured by Sharp Manufacturing System, output 200 W), and about 20 cc was sampled every 90 minutes. The change in particle size is measured by the photon correlation method (Malvern, Zetasizer).
粒径が２００ｎｍ以下になったら超音波洗浄器を停止し、研磨剤を得た。この時の研磨剤中の水酸化セリウム粒子の平均粒径は、１４３．２ｎｍであった。また、研磨剤のｐＨ値は３．８１であった。研磨剤を容器に密封して静置しておき、１日おきに、研磨剤中の水酸化セリウム粒子の粒径と研磨剤のｐＨを測定した。粒径は光子相関法を用いて測定を行った。また、ｐＨに関してはガラス電極式水素イオン濃度計を用いて測定した。研磨剤を静置して７日後の水酸化セリウム粒子の平均粒径は１４６．４ｎｍ（変化率２．２％）、研磨剤のｐＨは３．７７（変化率１％）であった。 When the particle size became 200 nm or less, the ultrasonic cleaner was stopped to obtain an abrasive. At this time, the average particle size of the cerium hydroxide particles in the abrasive was 143.2 nm. The pH value of the abrasive was 3.81. The abrasive was sealed in a container and allowed to stand, and the particle size of the cerium hydroxide particles in the abrasive and the pH of the abrasive were measured every other day. The particle size was measured using the photon correlation method. The pH was measured using a glass electrode type hydrogen ion concentration meter. The average particle diameter of the cerium hydroxide particles after 7 days from the standing of the abrasive was 146.4 nm (change rate: 2.2%), and the pH of the abrasive was 3.77 (change rate: 1%).
実施例１〜３に示したように、金属水酸化物粒子の析出時のｐＨを制御することにより、研磨剤製造７日後でも、研磨剤中に含まれる金属水酸化物粒子の粒径の変化率は、０．６から４．１％であり、また研磨剤のｐＨの変化率は、０．５から１％と安定していた。以上、経時的に安定な研磨剤の製造方法及び研磨剤を提供することができた。
As shown in Examples 1 to 3, by controlling the pH at the time of precipitation of the metal hydroxide particles, the change in the particle size of the metal hydroxide particles contained in the abrasive even after 7 days of production of the abrasive The rate was 0.6 to 4.1%, and the change rate of the pH of the abrasive was stable from 0.5 to 1%. As mentioned above, the manufacturing method of an abrasive | polishing agent and abrasive | polishing agent which were stable over time were able to be provided.
Claims (11)
The abrasive according to claim 9 or 10, wherein the pH change rate after 7 days of production is 10% or less.
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