JP6846193B2 - Polishing slurry - Google Patents
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Description
本発明は、酸化ケイ素を含む被研磨物を研磨する研磨用スラリーに関する。 The present invention relates to a polishing slurry for polishing an object to be polished containing silicon oxide.
従来、酸化ケイ素を含む被研磨物を研磨する研磨用スラリーとして、砥粒と、該砥粒を分散させる分散媒とを含有する研磨用スラリーが用いられている（例えば、特許文献１）。 Conventionally, as a polishing slurry for polishing an object to be polished containing silicon oxide, a polishing slurry containing abrasive grains and a dispersion medium for dispersing the abrasive grains has been used (for example, Patent Document 1).
ここで、砥粒が大きいと酸化ケイ素を含む被研磨物に研磨傷が生じやすい傾向にあり、一方で、砥粒が小さいと研磨速度が低くなる傾向にあるが、研磨速度を高めつつ、研磨傷が生じ難い研磨用スラリーが求められ得る。 Here, if the abrasive grains are large, polishing scratches tend to occur on the object to be polished containing silicon oxide, while if the abrasive grains are small, the polishing speed tends to be low. A polishing slurry that is less likely to be scratched can be required.
そこで、本発明は、上記要望点に鑑み、研磨速度を高めつつ、研磨傷が生じ難い研磨用スラリーを提供することを課題とする。 Therefore, in view of the above requirements, it is an object of the present invention to provide a polishing slurry that is less likely to cause polishing scratches while increasing the polishing rate.
本発明に係る研磨用スラリーは、酸化ケイ素を含む被研磨物を研磨する研磨用スラリーであって、
砥粒と、該砥粒を分散させる分散媒とを含有し、
前記砥粒を１０〜４０質量％含有し、
前記砥粒のＢＥＴ比表面積が５５〜６１ｍ２／ｇであり、
前記砥粒は、１次粒子及び１次粒子が複数凝集した２次粒子となって前記分散媒に分散され、且つ、粒度分布曲線のピーク値が１１７ｎｍ以下となるように前記分散媒に分散されている。
The polishing slurry according to the present invention is a polishing slurry for polishing an object to be polished containing silicon oxide.
Containing abrasive grains and a dispersion medium for dispersing the abrasive grains,
The abrasive grains are contained in an amount of 10 to 40% by mass.
The BET specific surface area of the abrasive grains is 55 to 61 m 2 / g.
The abrasive grains are dispersed in the dispersion medium as secondary particles in which a plurality of primary particles and primary particles are aggregated, and are dispersed in the dispersion medium so that the peak value of the particle size distribution curve is 117 nm or less. ing.
本発明によれば、研磨速度を高めつつ、研磨傷が生じ難い研磨用スラリーを提供し得る。 According to the present invention, it is possible to provide a polishing slurry in which polishing scratches are less likely to occur while increasing the polishing rate.
以下、本発明の一実施形態について説明する。 Hereinafter, an embodiment of the present invention will be described.
本実施形態に係る研磨用スラリーは、酸化ケイ素を含む被研磨物を研磨する研磨用スラリーである。
また、本実施形態に係る研磨用スラリーは、砥粒と、該砥粒を分散させる分散媒とを含有する。
さらに、本実施形態に係る研磨用スラリーは、砥粒を１０〜４０質量％含有する。
The polishing slurry according to the present embodiment is a polishing slurry for polishing an object to be polished containing silicon oxide.
Further, the polishing slurry according to the present embodiment contains abrasive grains and a dispersion medium for dispersing the abrasive grains.
Further, the polishing slurry according to the present embodiment contains 10 to 40% by mass of abrasive grains.
前記被研磨物としては、テトラエトキシシラン（ＴＥＯＳ）を用いプラズマＣＶＤによって形成されたＳｉＯ２を含む被研磨物などが挙げられる。 Examples of the object to be polished include an object to be polished containing SiO 2 formed by plasma CVD using tetraethoxysilane (TEOS).
前記砥粒としては、シリカ、アルミナ、酸化セリウム、窒化珪素、酸化ジルコニウム等が挙げられ、シリカが好ましい。 Examples of the abrasive grains include silica, alumina, cerium oxide, silicon nitride, zirconium oxide and the like, and silica is preferable.
前記砥粒のＢＥＴ比表面積は、５５〜６１ｍ２／ｇであることが重要である。 It is important that the BET specific surface area of the abrasive grains is 55 to 61 m 2 / g.
なお、前記砥粒のＢＥＴ比表面積は、原料である砥粒について、ＪＩＳ Ｚ８８３０：２０１３（ガス吸着による粉体（固体）のＢＥＴ比表面積測定方法）に従って測定した値を意味する。
また、ＪＩＳ Ｚ８８３０：２０１３における吸着ガス量の測定は、静的容量法を用いる。
さらに、ＪＩＳ Ｚ８８３０：２０１３における吸着データの解析は、多点法を用いる。
The BET specific surface area of the abrasive grains means a value measured for the abrasive grains as a raw material according to JIS Z8830: 2013 (method for measuring the BET specific surface area of powder (solid) by gas adsorption).
Further, the static capacitance method is used for the measurement of the amount of adsorbed gas in JIS Z8830: 2013.
Furthermore, the multipoint method is used for the analysis of the adsorption data in JIS Z8830: 2013.
前記砥粒は、１次粒子及び１次粒子が複数凝集した２次粒子となって前記分散媒に分散され、且つ、粒度分布曲線のピーク値（粒径の最頻値）が１１７ｎｍ以下となるように前記分散媒に分散されている。
前記ピーク値は、１０５〜１１７ｎｍであることが好ましい。
The abrasive grains become secondary particles in which a plurality of primary particles and primary particles are aggregated and dispersed in the dispersion medium, and the peak value (the most frequent value of the particle size) of the particle size distribution curve is 117 nm or less. As described above, it is dispersed in the dispersion medium.
The peak value is preferably 105 to 117 nm.
なお、砥粒の粒度分布曲線は、砥粒及び分散媒を含有する研磨用スラリーについて、ディスク遠心沈降光透過法で測定した質量基準の粒度分布曲線を意味する。
例えば、砥粒の粒度分布曲線は、ディスク遠心式高分解能粒度分布測定装置（ＣＰＳ Ｉｎｓｔｒｕｍｅｎｔｓ社製）を用いて測定することができる。
なお、粒度分布曲線においてピークが複数存在する場合、本実施形態におけるピーク値は、粒度分布曲線において高さが最も大きいピークにおけるピーク値を意味する。
The particle size distribution curve of the abrasive grains means a mass-based particle size distribution curve measured by the disk centrifugal sedimentation light transmission method for the polishing slurry containing the abrasive grains and the dispersion medium.
For example, the particle size distribution curve of the abrasive grains can be measured using a disk centrifugal high-resolution particle size distribution measuring device (manufactured by CPS Instruments).
When there are a plurality of peaks on the particle size distribution curve, the peak value in the present embodiment means the peak value at the peak having the highest height on the particle size distribution curve.
前記分散媒は、アルカリを含有することが好ましい。
前記アルカリとしては、無機物である無機アルカリ剤、有機物である有機アルカリ剤が挙げられる。
無機アルカリ剤としては、水酸化カリウム、水酸化ナトリウム、アンモニア等が挙げられる。
有機アルカリ剤としては、モノメチルアミン、ジメチルアミン、モノエチルアミン、ジエチルアミン等が挙げられる。
The dispersion medium preferably contains an alkali.
Examples of the alkali include an inorganic alkali agent which is an inorganic substance and an organic alkaline agent which is an organic substance.
Examples of the inorganic alkaline agent include potassium hydroxide, sodium hydroxide, ammonia and the like.
Examples of the organic alkaline agent include monomethylamine, dimethylamine, monoethylamine, diethylamine and the like.
本実施形態に係る研磨用スラリーのｐＨは、好ましくは８〜１２、より好ましくは１０〜１２である。 The pH of the polishing slurry according to this embodiment is preferably 8 to 12, more preferably 10 to 12.
本実施形態に係る研磨用スラリーは、上記のように構成されているので、以下の利点を有するものである。 Since the polishing slurry according to the present embodiment is configured as described above, it has the following advantages.
本実施形態に係る研磨用スラリーは、酸化ケイ素を含む被研磨物を研磨する研磨用スラリーである。また、本実施形態に係る研磨用スラリーは、砥粒と、該砥粒を分散させる分散媒とを含有する。さらに、本実施形態に係る研磨用スラリーは、前記砥粒を１０〜４０質量％含有する。また、前記砥粒のＢＥＴ比表面積は５５〜６１ｍ２／ｇである。前記砥粒は、１次粒子及び１次粒子が複数凝集した２次粒子となって前記分散媒に分散され、且つ、粒度分布曲線のピーク値が１１７ｎｍ以下となるように前記分散媒に分散されている。 The polishing slurry according to the present embodiment is a polishing slurry for polishing an object to be polished containing silicon oxide. Further, the polishing slurry according to the present embodiment contains abrasive grains and a dispersion medium for dispersing the abrasive grains. Further, the polishing slurry according to the present embodiment contains 10 to 40% by mass of the abrasive grains. The BET specific surface area of the abrasive grains is 55 to 61 m 2 / g. The abrasive grains are dispersed in the dispersion medium as secondary particles in which a plurality of primary particles and primary particles are aggregated, and are dispersed in the dispersion medium so that the peak value of the particle size distribution curve is 117 nm or less. ing.
斯かる研磨用スラリーは、前記砥粒のＢＥＴ比表面積が５５〜６１ｍ２／ｇであり、前記砥粒の粒度分布曲線のピーク値が１１７ｎｍ以下となるように前記砥粒が前記分散媒に分散されていることにより、研磨速度を高めつつ、研磨傷が生じ難くなるという利点を有する。 In such a polishing slurry, the abrasive grains are dispersed in the dispersion medium so that the BET specific surface area of the abrasive grains is 55 to 61 m 2 / g and the peak value of the particle size distribution curve of the abrasive grains is 117 nm or less. This has the advantage that polishing scratches are less likely to occur while increasing the polishing speed.
なお、本発明に係る研磨用スラリーは、上記実施形態に限定されるものではない。また、本発明に係る研磨用スラリーは、上記した作用効果に限定されるものでもない。本発明に係る研磨用スラリーは、本発明の要旨を逸脱しない範囲で種々の変更が可能である。 The polishing slurry according to the present invention is not limited to the above embodiment. Further, the polishing slurry according to the present invention is not limited to the above-mentioned effects. The polishing slurry according to the present invention can be variously modified without departing from the gist of the present invention.
次に、試験例を挙げて本発明についてさらに具体的に説明する。 Next, the present invention will be described in more detail with reference to test examples.
ＢＥＴ比表面積が下記表１に示す値となっている試験例１〜７の砥粒（シリカ）を用意した。
なお、砥粒のＢＥＴ比表面積は、上述した方法で測定した。
次に、砥粒とアルカリ水溶液（水酸化カリウム水溶液）とイオン交換水とを混合することにより、試験例１〜７の研磨用スラリー（砥粒の含有割合：１０．５質量％、ｐＨ：１１）を作製した。
そして、試験例１〜７の研磨用スラリーを用いて、前記砥粒の粒度分布曲線のピーク値（以下、単に「粒度分布曲線のピーク値」ともいう。）を測定した。前記粒度分布曲線は、上述した方法において遠心沈降法を用いＭｉｅ散乱理論に基づいて測定した。そして、前記粒度分布曲線のピーク値を求めた。
また、試験例１〜７の研磨用スラリーを用いて、下記研磨条件で下記被研磨物を研磨した。
次に、試験例１〜７の研磨速度と、研磨傷の数を求めた。
Abrasive grains (silica) of Test Examples 1 to 7 having a BET specific surface area of the values shown in Table 1 below were prepared.
The BET specific surface area of the abrasive grains was measured by the method described above.
Next, by mixing the abrasive grains, the alkaline aqueous solution (potassium hydroxide aqueous solution), and the ion-exchanged water, the polishing slurry of Test Examples 1 to 7 (abrasive grain content: 10.5% by mass, pH: 11). ) Was prepared.
Then, using the polishing slurry of Test Examples 1 to 7, the peak value of the particle size distribution curve of the abrasive grains (hereinafter, also simply referred to as “peak value of the particle size distribution curve”) was measured. The particle size distribution curve was measured based on the Mie scattering theory using the centrifugal sedimentation method in the above method. Then, the peak value of the particle size distribution curve was obtained.
In addition, the following objects to be polished were polished under the following polishing conditions using the polishing slurries of Test Examples 1 to 7.
Next, the polishing speed of Test Examples 1 to 7 and the number of polishing scratches were determined.
＜研磨条件＞
研磨機：Ｅｃｏｍｅｔ３
研磨時間：６０ｓｅｃ
加重：３５ｋＰａ
定番回転数：１２０ｍｉｎ−１
ヘッド回転数：６４ｍｉｎ−１
研磨用スラリーの流量：２６ｍＬ／ｍｉｎ
パッド：ＩＣ１４００ Ｋ−Ｇｒｖ Ａ２
被研磨物：テトラエトキシシラン（ＴＥＯＳ）を用いプラズマＣＶＤによって形成されたＳｉＯ２膜を有するブランケットウェハ（Ｐ−ＴＥＯＳブランケットウェハ）
<Polishing conditions>
Polishing machine: Ecomet3
Polishing time: 60 sec
Weight: 35kPa
Standard rotation speed: 120min -1
Head rotation speed: 64min -1
Flow rate of polishing slurry: 26 mL / min
Pad: IC1400 K-Grv A2
Object to be polished: Blanket wafer having SiO 2 film formed by plasma CVD using tetraethoxysilane (TEOS) (P-TEOS blanket wafer)
＜研磨速度比の算出＞
研磨速度は、研磨によって減少した厚み（研磨厚み）を研磨時間で割ることにより求めた。
なお、研磨厚みは、Ｎａｎｏ−ｍｅｔｒｉｃｓ社製のｎａｎｏｓｐｅｃＡＦＴ５１００で測定した。
そして、研磨速度比は下記式（１）によって求めた。
各試験例の研磨速度比 ＝ （ 各試験例の研磨速度 ／ 試験例３の研磨速度 ） × １００（％） （１）
結果を下記表１及び図１、３に示す。
<Calculation of polishing rate ratio>
The polishing rate was determined by dividing the thickness reduced by polishing (polishing thickness) by the polishing time.
The polishing thickness was measured with a nanospec AFT5100 manufactured by Nano-metrics.
Then, the polishing rate ratio was obtained by the following formula (1).
Polishing speed ratio of each test example = (polishing speed of each test example / polishing speed of test example 3) x 100 (%) (1)
The results are shown in Table 1 and FIGS. 1 and 3 below.
＜研磨傷の数＞
研磨によって被研磨物に生じた、直径８インチの円における０．２μｍ以上の研磨傷の数（以下、単に「研磨傷の数」ともいう。）は、日立ハイテクノロジーズ社製のＬＳ６６００により求めた。
結果を下記表１及び図２、４に示す。図２、４の研磨傷の数は、平均値を示す。
<Number of polishing scratches>
The number of polishing scratches of 0.2 μm or more in a circle having a diameter of 8 inches (hereinafter, also simply referred to as “the number of polishing scratches”) generated on the object to be polished by polishing was determined by LS6600 manufactured by Hitachi High-Technologies Corporation. ..
The results are shown in Table 1 and FIGS. 2 and 4 below. The numbers of polishing scratches in FIGS. 2 and 4 show average values.
表１、及び、図１〜４に示すように、本発明によれば、研磨速度を高めつつ、研磨傷が生じ難い研磨用スラリーを提供することができる。 As shown in Table 1 and FIGS. 1 to 4, according to the present invention, it is possible to provide a polishing slurry in which polishing scratches are less likely to occur while increasing the polishing rate.
Claims (5)
砥粒と、該砥粒を分散させる分散媒とを含有し、
前記砥粒を１０〜４０質量％含有し、
前記砥粒のＢＥＴ比表面積が５５〜６１ｍ２／ｇであり、
前記砥粒は、１次粒子及び１次粒子が複数凝集した２次粒子となって前記分散媒に分散され、且つ、粒度分布曲線のピーク値が１０５〜１１７ｎｍとなるように前記分散媒に分散されている、研磨用スラリー。 A polishing slurry that polishes an object to be polished containing silicon oxide.
Containing abrasive grains and a dispersion medium for dispersing the abrasive grains,
The abrasive grains are contained in an amount of 10 to 40% by mass.
The BET specific surface area of the abrasive grains is 55 to 61 m 2 / g.
The abrasive grains are dispersed in the dispersion medium as secondary particles in which a plurality of primary particles and primary particles are aggregated, and are dispersed in the dispersion medium so that the peak value of the particle size distribution curve is 105 to 117 nm. A polishing slurry.
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| JP2003342554A (en) * | 2002-05-24 | 2003-12-03 | Nippon Aerosil Co Ltd | Abrasive composition |
| JP2005286046A (en) * | 2004-03-29 | 2005-10-13 | Nitta Haas Inc | Abrasive composition for semiconductor |
| US20070034116A1 (en) * | 2005-08-10 | 2007-02-15 | Mac Donald Dennis L | Silica sols with controlled minimum particle size and preparation thereof |
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