WO2013179926A1 - Polishing material slurry - Google Patents

Polishing material slurry Download PDF

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Publication number
WO2013179926A1
WO2013179926A1 PCT/JP2013/063902 JP2013063902W WO2013179926A1 WO 2013179926 A1 WO2013179926 A1 WO 2013179926A1 JP 2013063902 W JP2013063902 W JP 2013063902W WO 2013179926 A1 WO2013179926 A1 WO 2013179926A1
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Prior art keywords
polishing
oxide particles
iron oxide
abrasive slurry
substrate
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PCT/JP2013/063902
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French (fr)
Japanese (ja)
Inventor
龍一 佐藤
小池　淳
陽兵 丸山
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三井金属鉱業株式会社
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Publication of WO2013179926A1 publication Critical patent/WO2013179926A1/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02002—Preparing wafers
    • H01L21/02005—Preparing bulk and homogeneous wafers
    • H01L21/02008—Multistep processes
    • H01L21/0201—Specific process step
    • H01L21/02024—Mirror polishing
    • 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
    • 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
    • C09K3/1409—Abrasive particles per se
    • 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
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
    • H01L29/1608—Silicon carbide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/20—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only AIIIBV compounds
    • H01L29/2003—Nitride compounds

Definitions

  • the present invention relates to an abrasive slurry capable of polishing a high-hardness material such as silicon carbide at high speed and smoothly, and particularly to an abrasive slurry containing iron oxide particles.
  • silicon carbide, gallium nitride, or the like may be used in place of silicon conventionally used as a substrate for the purpose of increasing the breakdown voltage or increasing the current.
  • silicon carbide, gallium nitride, or the like have a large band gap as compared with the silicon substrate, they can withstand higher voltages.
  • the reason why the substrate made of silicon carbide, gallium nitride or the like has a high withstand voltage characteristic is considered to be derived from the fact that the atomic arrangement of atoms constituting silicon carbide or the like is denser than silicon.
  • a substrate made of a material such as silicon carbide has a particularly high hardness, it has a problem that it cannot be polished with a conventionally used polishing material.
  • Silicon carbide has a particularly high hardness because of its dense atomic arrangement.
  • a material having high hardness such as diamond or aluminum oxide has been used as the abrasive particles.
  • polishing is performed using diamond or the like, only mechanical polishing proceeds, and defects and distortion are likely to occur in the substrate due to this, which may impair device reliability.
  • transition metal fine particles such as Fe, Ni, Co, Cu, Cr, and Ti and oxidation such as SiO 2 , Al 2 O 3 , CeO 2 , Fe 2 O 3 , and TiO 2 are formed on an iron surface plate as a catalyst.
  • Carbonization is performed by bringing the workpiece into contact with a predetermined pressing force while supplying a blended polishing liquid based on hydrogen peroxide with at least one of the fine particles and moving the iron platen and the workpiece relative to each other.
  • a method for polishing a silicon substrate has been proposed (Patent Document 3).
  • the present invention provides an abrasive slurry that can be polished smoothly at a high polishing speed even with a substrate made of a hard material having a Mohs hardness of 8 or higher, which is a high hardness material.
  • the present invention for solving the above-mentioned problems relates to an abrasive slurry used for polishing difficult-to-cut materials having a Mohs hardness of 8 or more, characterized by containing iron oxide particles and manganate ions.
  • the abrasive slurry of the present invention is suitable for polishing a difficult-to-cut material having a Mohs hardness of 8 or more, for example, a substrate made of a high-hardness material such as silicon carbide. According to the present invention, a smooth surface can be easily formed. The polishing process can be performed quickly.
  • Mohs' hardness refers to a standard of hardness expressed as an index of the degree of scratching with reference to a standard material set in 10 levels from 1 to 10.
  • Examples of the high hardness material having a Mohs hardness of 8 or more include silicon carbide and gallium nitride.
  • the abrasive slurry of the present invention exhibits a high polishing power because the oxidizing particles of metal elements that can take various oxidation numbers and a solution containing ions with high oxidizing power coexist in the slurry. Changes in the oxidation number of metal atoms change the form between the oxidizable particles and ions in the solution to provide more suitable polishing characteristics for the microscopic / chemical surface condition of the material being polished. It is thought to do.
  • the present inventors have focused on iron as a metal element that causes this change in oxidation number, and found that when iron oxide particles and manganate ions are used at the same time, an abrasive slurry that exhibits particularly high polishing power is obtained.
  • the present invention has been conceived.
  • FeO, Fe 2 O 3 , Fe 3 O 4 and the like can be applied as iron oxide particles, and in particular, ⁇ -Fe 2 O 3 , ⁇ -Fe 2 O 3 , Fe 3 O 4 is preferred.
  • manganate ion MnO 4 ⁇ , MnO 4 2 ⁇ , MnO 4 3 ⁇ , MnO 4 6 ⁇ , and the like can be applied, and a permanganate ion (MnO 4 ⁇ ) having particularly high oxidation performance is used. Is preferred.
  • An abrasive slurry containing both iron oxide particles of ⁇ -Fe 2 O 3 or ⁇ -Fe 2 O 3 or Fe 3 O 4 and permanganate ions (MnO 4 ⁇ ) in the abrasive slurry is particularly preferred.
  • the average particle diameter DSEM of the iron oxide particles is preferably 0.4 ⁇ m or less, more preferably less than 0.3 ⁇ m, and particularly preferably 0.2 ⁇ m or less.
  • the average particle diameter D SEM exceeds 0.4 .mu.m, upon polishing treatment a substrate made of a material of high hardness such as silicon carbide, tend to have polishing rate becomes slow.
  • the thickness is 0.4 ⁇ m or less, a smooth surface can be easily realized, the polishing speed is high, and the polishing treatment can be continued stably for a long time.
  • the lower limit value of the average particle diameter DSEM of the iron oxide particles is preferably 0.01 ⁇ m, more preferably 0.03 ⁇ m or more, and particularly preferably 0.05 ⁇ m or more.
  • the average particle size is less than 0.01 ⁇ m, self-aggregation tends to occur, and it becomes difficult to obtain a high polishing rate.
  • the manganate ion is preferably 0.5% by mass or more, more preferably 1.0% by mass or more, and even more preferably 2.0% by mass or more. If it is less than 0.5% by mass, the oxidizing power of manganate ions becomes insufficient, and the polishing rate tends to be slow. Further, the higher the manganate ion concentration, the higher the polishing force can be. However, in order to ensure the safety in handling the abrasive slurry, it is preferably 40% by mass or less, more preferably 20% by mass or less. Furthermore, 10 mass% or less is especially preferable.
  • the content of manganate ions in the abrasive slurry can be measured by analyzing the filtrate obtained by filtering the slurry by ion chromatography or absorptiometry.
  • the iron oxide particles are preferably 35% by mass or less, and particularly preferably 10% by mass or less.
  • the iron oxide particles are preferably 0.5% by mass or more, and particularly preferably 1% by mass or more. If it is less than 0.5% by mass, the polishing force of the iron oxide particles tends to decrease.
  • the content in the abrasive slurry in the case of the iron oxide particles can be measured, for example, by filtering the abrasive slurry, drying the filtered particles, and weighing them.
  • the pH of the slurry is preferably weakly acidic to weakly alkaline, that is, the pH of the slurry is preferably pH 5 to pH 10.
  • manganate ions contained in the abrasive slurry of the present invention are generally known to exhibit high oxidation performance in acidic solutions, iron oxide particles coexisting with manganate ions maintain a dispersed state when strongly acidic. This is because it tends to be difficult to aggregate and tends to be scratched.
  • the abrasive slurry of the present invention is suitable for polishing a hard material having a Mohs hardness value of 8 or more, for example, difficult-to-cut materials such as silicon carbide and gallium nitride, and is particularly suitable for polishing silicon carbide.
  • a hard material with high hardness such as silicon carbide can be smoothly polished at high speed.
  • Fe 3 O 4 , ⁇ -Fe 2 O 3 , and ⁇ -Fe 2 O 3 were used as oxide particles to be abrasive grains, and these oxide particles were mixed with pure water, and this was used as an oxidizing agent.
  • KMnO 4 manufactured by Wako Pure Chemical Industries, Ltd.
  • ⁇ -Fe 2 O 3 was produced by firing the Fe 3 O 4 of Example 2 at 600 ° C. for 1 hour, and ⁇ -Fe 2 O 3 was obtained from Example 2.
  • Fe 3 O 4 is produced by baking at 300 ° C. for 1 hour.
  • SiO 2 is used as oxide particles to be abrasive grains, these oxide particles and pure water are mixed, KMnO 4 is added as an oxidant and stirred, and polishing of comparative examples shown in Table 1 is performed. A material slurry was prepared.
  • Table 1 shows the pH of each abrasive slurry, the average particle diameter D 50 of the oxide particles, the average particle diameter D SEM by a scanning electron microscope, the specific surface area (SSA), and the contents of the oxide particles and the oxidizing agent. Show.
  • the average particle diameters D 50 , D SEM and specific surface area (SSA) were measured as follows.
  • the average particle size D 50 is that a 50% diameter in cumulative fraction of the volume reference in the laser diffraction scattering method particle size distribution.
  • ultrasonic dispersion treatment was performed for 3 minutes, and measurement was performed using a laser diffraction / scattering particle size distribution measuring apparatus (Horiba, Ltd .: LA-920). .
  • Average particle diameter D SEM The particle diameter of 10 oxide particles in the field of view observed at an acceleration voltage of 5 kV and 20,000 times was measured using a scanning electron microscope (SEM), and the average value was determined as the average particle diameter D. SEM was used.
  • Specific surface area Based on the BET method, “6.2 Flow method (3.5) one-point method” in JIS R 1626-1996 (Method for measuring specific surface area by gas adsorption BET method of fine ceramic powder) Based on the above, the specific surface area of the oxide particles was measured. At that time, a mixed gas of helium as a carrier gas and nitrogen as an adsorbate gas was used.
  • each abrasive slurry was evaluated by conducting a polishing test.
  • the polishing characteristics were measured by measuring the polishing speed and the surface roughness after the polishing treatment.
  • Polishing test A lapping 4H—SiC substrate having a diameter of 2 inches was used as a polishing target. The polishing process was performed on the Si surface of the substrate.
  • a commercially available polishing apparatus manufactured by MG Corporation: single-sided grinder BC-15
  • a polishing pad Nita Haas: SUBA # 600
  • the rotation speed of the surface plate and the SiC substrate was set to 60 rpm.
  • the load during polishing was 200 gf / cm 2 .
  • the supply amount of the abrasive slurry was 200 mL / min.
  • the polishing time was 3 hours.
  • the surface roughness of the substrate was measured as a polishing characteristic.
  • the surface roughness Ra (JIS B0601) before and after polishing was measured by measuring the surface of the substrate with an atomic force microscope “Dimention 3100” (manufactured by Digital Instruments) and analyzing the measurement results using the software “Nanoscope V” of the company. I asked for it.
  • the surface roughness Ra of the substrate before polishing was 0.4 nm.
  • the results after the polishing treatment are shown in Table 2.
  • the polishing speed was measured as a polishing characteristic.
  • the polishing rate (nm / min) was calculated from the difference in mass of the substrate before and after polishing and the density of SiC (3.10 g / cm 3 ). The results are shown in Table 2.
  • the polishing slurry using the iron oxide of the example as an abrasive grain had a high polishing rate and a good surface roughness Ra after polishing.
  • the polishing characteristics of the abrasive slurry using the iron oxide particles of the present invention were good.
  • FIG. 1 is a graph showing the relationship between the average particle diameter D SEM of Fe 3 O 4 of Examples 1 to 7 and the polishing rate.
  • the polishing rate tended to decrease as the average particle size DSEM increased. From the relationship obtained by a graph plot of the average particle diameter DSEM of iron oxide and the polishing rate, it was found that the polishing rate was about 2 nm / min or more when it was 0.4 ⁇ m or less.
  • the polishing test conditions were the same as described above. One substrate was polished for 2 hours, and a total of 5 substrates (10 hours in total) were polished continuously. In this continuous polishing test, the abrasive slurry was not changed or the abrasive grains were not replenished. The surface roughness Ra after polishing of each substrate and the polishing speed of each substrate were calculated. The results are shown in FIGS.
  • the horizontal axis in FIGS. 2 and 3 is the order of the polished substrates. From the results of FIG. 2, it was found that any of the polishing slurry of Examples 2, 9 and Comparative Example 3 can realize a stable surface roughness even when polishing is performed for a long time of 10 hours. In the case of the polishing speed shown in FIG. 3, in the polishing slurry of Comparative Example 3 using MnO 2 oxide particles as the abrasive grains, the polishing speed decreases from the third substrate. In contrast, the polishing slurry of Example 2 and Example 9 using iron oxide as abrasive grains was found to have a stable polishing rate even after 10 hours of polishing treatment.
  • a difficult-to-cut material having a Mohs hardness of 8 or more for example, a hard-hard material having a high hardness such as silicon carbide or gallium nitride can be smoothly polished at a high speed and a continuous polishing process can be performed.
  • the polishing treatment of the substrate made of the above difficult-to-cut material can be performed efficiently.

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Abstract

Provided is a polishing material slurry which is capable of smoothly polishing a substrate with high polishing rate even if the substrate is a high-hardness material having a Mohs hardness of 8 or more. The present invention is a polishing material slurry for polishing a hard-to-grind material that has a Mohs hardness of 8 or more, said polishing material slurry being characterized by containing iron oxide particles and manganate ions. It is preferable that the iron oxide particles have an average particle diameter DSEM of 0.4 μm or less. It is also preferable that the iron oxide particles contain at least one of FeO, Fe2O3 and Fe3O4.

Description

研摩材スラリーAbrasive slurry
　本発明は、炭化ケイ素のような高硬度材料を高速かつ平滑に研摩できる研摩材スラリーに関し、特に酸化鉄粒子を含む研摩材スラリーに関する。 The present invention relates to an abrasive slurry capable of polishing a high-hardness material such as silicon carbide at high speed and smoothly, and particularly to an abrasive slurry containing iron oxide particles.
　半導体デバイスのうち、いわゆるパワーデバイスと呼ばれる電力用半導体素子においては、高耐圧化や大電流化の目的で、基板として従来用いられてきたシリコンに代えて、炭化ケイ素、窒化ガリウム等を用いることが進んでいる。これら炭化ケイ素等からなる基板は、シリコン基板と比較して大きなバンドギャップを持つため、より高い電圧に耐えられるものとなる。炭化ケイ素や窒化ガリウム等からなる基板が高耐圧な特性を有するのは、炭化ケイ素等を構成する原子の原子配列が、シリコンに比べて密であることに由来すると考えられる。 Among semiconductor devices, in power semiconductor elements called so-called power devices, silicon carbide, gallium nitride, or the like may be used in place of silicon conventionally used as a substrate for the purpose of increasing the breakdown voltage or increasing the current. Progressing. Since these substrates made of silicon carbide or the like have a large band gap as compared with the silicon substrate, they can withstand higher voltages. The reason why the substrate made of silicon carbide, gallium nitride or the like has a high withstand voltage characteristic is considered to be derived from the fact that the atomic arrangement of atoms constituting silicon carbide or the like is denser than silicon.
　一方、炭化ケイ素のような材料からなる基板は、特に硬度が高いため、従来より用いられてきた研摩材では、ほとんど研摩できないという問題を有している。炭化ケイ素は、原子配列が密であることから、特に硬度が高い。このような高硬度材料からなる基板を研摩するには、研摩粒子としても、ダイヤモンド、酸化アルミニウム等、硬度の高い材料が用いられてきた。しかし、ダイヤモンド等を用いて研摩すると、メカニカルな研摩のみが進行し、そのことに起因して基板中に欠陥や歪みが生じやすくなり、デバイスの信頼性を損なうおそれがある。 On the other hand, since a substrate made of a material such as silicon carbide has a particularly high hardness, it has a problem that it cannot be polished with a conventionally used polishing material. Silicon carbide has a particularly high hardness because of its dense atomic arrangement. In order to polish a substrate made of such a high hardness material, a material having high hardness such as diamond or aluminum oxide has been used as the abrasive particles. However, if polishing is performed using diamond or the like, only mechanical polishing proceeds, and defects and distortion are likely to occur in the substrate due to this, which may impair device reliability.
　上記問題に対応すべく、炭化ケイ素のような高硬度材料からなる基板の研摩手法として、酸化クロムや酸化セリウム、或いは酸化鉄などの砥粒を樹脂に分散させた研摩板を用いて乾式研摩を行う方法が提案されている（特許文献１）。また、酸化ケイ素や酸化アルミニウム等の研摩粒子に、過酸化水素、オゾン、過マンガン酸等の酸化性溶液を添加したものが提案されている（特許文献２）。そして、触媒としての鉄定盤上に、Ｆｅ、Ｎｉ、Ｃｏ、Ｃｕ、Ｃｒ、Ｔｉなどの遷移金属微粒子と、ＳｉＯ2、Ａｌ2Ｏ3、ＣｅＯ2、Ｆｅ2Ｏ3、ＴｉＯ2などの酸化物微粒子の少なくとも一方と過酸化水素水をベースとした配合研摩液を供給しながら被加工物を所定の押圧力で接触させ、鉄定盤と被加工物を相対的に移動させて研摩する炭化ケイ素基板の研摩方法が提案されている（特許文献３）。 In order to cope with the above problems, as a polishing method for a substrate made of a high hardness material such as silicon carbide, dry polishing is performed using a polishing plate in which abrasive grains such as chromium oxide, cerium oxide, or iron oxide are dispersed in a resin. A method of performing this has been proposed (Patent Document 1). Moreover, what added oxidizing solutions, such as hydrogen peroxide, ozone, permanganic acid, to abrasive particles, such as a silicon oxide and an aluminum oxide, is proposed (patent document 2). Then, transition metal fine particles such as Fe, Ni, Co, Cu, Cr, and Ti and oxidation such as SiO 2 , Al 2 O 3 , CeO 2 , Fe 2 O 3 , and TiO 2 are formed on an iron surface plate as a catalyst. Carbonization is performed by bringing the workpiece into contact with a predetermined pressing force while supplying a blended polishing liquid based on hydrogen peroxide with at least one of the fine particles and moving the iron platen and the workpiece relative to each other. A method for polishing a silicon substrate has been proposed (Patent Document 3).
特開平０６－３３３８９２号公報Japanese Patent Application Laid-Open No. 06-333892 特開２０１０－１８２７８２号公報JP 2010-182782 A 特表２０１０－１８８４８７号公報Special table 2010-188487
　上記のように、炭化ケイ素のような高硬度材料の基板に対する研摩手法は多数提案されている。しかし、炭化ケイ素は極めて難削であるため、これらの先行技術によっても、ある程度の時間を要すれば平滑な表面を実現できるものの、研摩速度が十分でなく、生産性に劣る点が指摘されている。そのため、平滑な表面を、容易に且つ素早く実現できる、優れた研摩特性を実現可能な、新たな研摩技術が強く要求されていることが現状である。かかる背景のもと、本発明は、高硬度材料であるモース硬度８以上の難削材からなる基板であっても、高い研摩速度でかつ平滑に研摩可能な、研摩材スラリーを提供することを目的とする。 As described above, a number of polishing techniques have been proposed for substrates of high hardness materials such as silicon carbide. However, since silicon carbide is extremely difficult to cut, it is pointed out that even with these prior art techniques, a smooth surface can be realized if a certain amount of time is required, but the polishing speed is not sufficient and the productivity is poor. Yes. Therefore, the current situation is that there is a strong demand for a new polishing technique capable of realizing a smooth surface easily and quickly and capable of realizing excellent polishing characteristics. Under such background, the present invention provides an abrasive slurry that can be polished smoothly at a high polishing speed even with a substrate made of a hard material having a Mohs hardness of 8 or higher, which is a high hardness material. Objective.
　上記課題を解決する本発明は、酸化鉄粒子とマンガン酸イオンとを含有したことを特徴とする、モース硬度８以上の難削材の研摩に用いる研摩材スラリーに関する。本発明の研摩材スラリーは、モース硬度８以上の難削材、例えば炭化ケイ素のような高硬度材料からなる基板の研摩処理に好適なものであり、本発明によれば、平滑な表面を容易に実現でき、その研摩処理も素早く行うことが可能となる。さらに、本発明によれば、モース硬度８以上の難削材からなる基板を、長時間安定して研摩処理を行うことが可能となる。尚、本発明における「モース硬度」は、１～１０までの１０段階に設定された標準物質を基準とし、傷つきやすさの指標として表された硬さの基準をいう。モース硬度で硬度８以上の高硬度材料としては、炭化ケイ素、窒化ガリウム等が挙げられる。 The present invention for solving the above-mentioned problems relates to an abrasive slurry used for polishing difficult-to-cut materials having a Mohs hardness of 8 or more, characterized by containing iron oxide particles and manganate ions. The abrasive slurry of the present invention is suitable for polishing a difficult-to-cut material having a Mohs hardness of 8 or more, for example, a substrate made of a high-hardness material such as silicon carbide. According to the present invention, a smooth surface can be easily formed. The polishing process can be performed quickly. Furthermore, according to the present invention, it is possible to stably polish a substrate made of a difficult-to-cut material having a Mohs hardness of 8 or more for a long time. In the present invention, “Mohs' hardness” refers to a standard of hardness expressed as an index of the degree of scratching with reference to a standard material set in 10 levels from 1 to 10. Examples of the high hardness material having a Mohs hardness of 8 or more include silicon carbide and gallium nitride.
　本発明の研摩材スラリーが高い研摩力を発揮するのは、様々な酸化数を取り得る金属元素の酸化性粒子と、酸化力の高いイオンを含む溶液とがスラリー中に共存することで、その金属原子の酸化数の変化により、酸化性粒子と溶液中のイオンとの間で、研摩される物質の微視的・化学的な表面状態に対してより好適な研摩特性を発揮する形態に変化するためと考えられる。本発明者等は、この酸化数の変化を起こす金属元素として鉄に着目し、酸化鉄粒子とマンガン酸イオンとを同時に用いた場合、特に高い研摩力を発揮する研摩材スラリーになることを見出し、上記本発明に想到したものである。 The abrasive slurry of the present invention exhibits a high polishing power because the oxidizing particles of metal elements that can take various oxidation numbers and a solution containing ions with high oxidizing power coexist in the slurry. Changes in the oxidation number of metal atoms change the form between the oxidizable particles and ions in the solution to provide more suitable polishing characteristics for the microscopic / chemical surface condition of the material being polished. It is thought to do. The present inventors have focused on iron as a metal element that causes this change in oxidation number, and found that when iron oxide particles and manganate ions are used at the same time, an abrasive slurry that exhibits particularly high polishing power is obtained. The present invention has been conceived.
　本発明の研摩材スラリーにおいて、酸化鉄粒子としては、ＦｅＯ、Ｆｅ２Ｏ３、Ｆｅ３Ｏ４等を適用することができ、特に、α－Ｆｅ２Ｏ３、γ－Ｆｅ２Ｏ３、Ｆｅ３Ｏ４が好適である。また、マンガン酸イオンとしては、ＭｎＯ４ －、ＭｎＯ４ ２－、ＭｎＯ４ ３－、ＭｎＯ４ ６－等を適用することができ、特に高い酸化性能を持つ過マンガン酸イオン(ＭｎＯ４ －)が好適である。研摩材スラリー中に、α－Ｆｅ２Ｏ３或いはγ－Ｆｅ２Ｏ３、Ｆｅ３Ｏ４の酸化鉄粒子と、過マンガン酸イオン(ＭｎＯ４ －)の両方を含む研摩材スラリーが特に好ましい。 In the abrasive slurry of the present invention, FeO, Fe 2 O 3 , Fe 3 O 4 and the like can be applied as iron oxide particles, and in particular, α-Fe 2 O 3 , γ-Fe 2 O 3 , Fe 3 O 4 is preferred. Further, as the manganate ion, MnO 4 − , MnO 4 2− , MnO 4 3− , MnO 4 6−, and the like can be applied, and a permanganate ion (MnO 4 − ) having particularly high oxidation performance is used. Is preferred. An abrasive slurry containing both iron oxide particles of α-Fe 2 O 3 or γ-Fe 2 O 3 or Fe 3 O 4 and permanganate ions (MnO 4 − ) in the abrasive slurry is particularly preferred.
　本発明の研摩材スラリーにおいて、酸化鉄粒子の平均粒径ＤＳＥＭが０．４μｍ以下であることが好ましく、さらには０．３μｍ未満が好ましく、特に好ましいのは０．２μｍ以下である。平均粒径ＤＳＥＭが０．４μｍを超えると、炭化ケイ素のような高硬度材料からなる基板を研摩処理した際に、研摩速度が遅くなる傾向となる。０．４μｍ以下であると、平滑な表面を容易に実現できかつ、その研摩速度も高く、さらに研摩処理を長時間安定して継続できるものとなる。この酸化鉄粒子の平均粒径ＤＳＥＭの下限値は、０．０１μｍであることが好ましく、より好ましくは０．０３μｍ以上で、特に好ましくは０．０５μｍ以上である。０．０１μｍ未満のような平均粒径であると、自己凝集が起こりやすくなり、高い研摩速度を得ることが困難となる。 In the abrasive slurry of the present invention, the average particle diameter DSEM of the iron oxide particles is preferably 0.4 μm or less, more preferably less than 0.3 μm, and particularly preferably 0.2 μm or less. When the average particle diameter D SEM exceeds 0.4 .mu.m, upon polishing treatment a substrate made of a material of high hardness such as silicon carbide, tend to have polishing rate becomes slow. When the thickness is 0.4 μm or less, a smooth surface can be easily realized, the polishing speed is high, and the polishing treatment can be continued stably for a long time. The lower limit value of the average particle diameter DSEM of the iron oxide particles is preferably 0.01 μm, more preferably 0.03 μm or more, and particularly preferably 0.05 μm or more. When the average particle size is less than 0.01 μm, self-aggregation tends to occur, and it becomes difficult to obtain a high polishing rate.
　本発明の研摩材スラリーにおいて、マンガン酸イオンは０．５質量％以上であることが好ましく、１．０質量％以上がより好ましく、さらには２．０質量％以上が特に好ましい。０．５質量％未満であると、マンガン酸イオンの酸化力が不十分となり、研摩速度が遅くなる傾向となる。また、マンガン酸イオンの濃度が高いほど、研摩力を高めることができるが、研摩材スラリーの取り扱い上の安全を確保するため、４０質量％以下であることが好ましく、２０質量％以下がより好ましく、さらには１０質量％以下が特に好ましい。ここで、研摩材スラリー中における、マンガン酸イオンの含有量は、イオンクロマトグラフ法や吸光光度分析法によりスラリーを濾過した濾液を分析することで測定できる。 In the abrasive slurry of the present invention, the manganate ion is preferably 0.5% by mass or more, more preferably 1.0% by mass or more, and even more preferably 2.0% by mass or more. If it is less than 0.5% by mass, the oxidizing power of manganate ions becomes insufficient, and the polishing rate tends to be slow. Further, the higher the manganate ion concentration, the higher the polishing force can be. However, in order to ensure the safety in handling the abrasive slurry, it is preferably 40% by mass or less, more preferably 20% by mass or less. Furthermore, 10 mass% or less is especially preferable. Here, the content of manganate ions in the abrasive slurry can be measured by analyzing the filtrate obtained by filtering the slurry by ion chromatography or absorptiometry.
　また、研摩材スラリーの取り扱い上、好適な流動性を確保するため、酸化鉄粒子は３５質量％以下であることが好ましく、１０質量％以下が特に好ましい。また、酸化鉄粒子は０．５質量％以上であることが好ましく、１質量％以上であることが特に好ましい。０．５質量％未満であると、酸化鉄粒子の研摩力が低下する傾向となる。この酸化鉄粒子の場合における、研摩材スラリーにおける含有量は、例えば、研摩材スラリーを濾過し、濾別した粒子を乾燥し秤量することにより測定することができる。 Further, in order to ensure suitable fluidity in handling the abrasive slurry, the iron oxide particles are preferably 35% by mass or less, and particularly preferably 10% by mass or less. The iron oxide particles are preferably 0.5% by mass or more, and particularly preferably 1% by mass or more. If it is less than 0.5% by mass, the polishing force of the iron oxide particles tends to decrease. The content in the abrasive slurry in the case of the iron oxide particles can be measured, for example, by filtering the abrasive slurry, drying the filtered particles, and weighing them.
　本発明の研摩材スラリーは、スラリーのｐＨが弱酸性から弱アルカリ性、すなわち、スラリーのｐＨがｐＨ５～ｐＨ１０であることが好ましい。本発明の研摩材スラリーに含まれるマンガン酸イオンは、一般に酸性溶液で高い酸化性能を発揮することが知られているが、マンガン酸イオンと共存する酸化鉄粒子は強酸性では分散状態を維持しにくく凝集し易い傾向となり、研摩対象にキズを付けることもあるためである。 In the abrasive slurry of the present invention, the pH of the slurry is preferably weakly acidic to weakly alkaline, that is, the pH of the slurry is preferably pH 5 to pH 10. Although manganate ions contained in the abrasive slurry of the present invention are generally known to exhibit high oxidation performance in acidic solutions, iron oxide particles coexisting with manganate ions maintain a dispersed state when strongly acidic. This is because it tends to be difficult to aggregate and tends to be scratched.
　本発明の研摩材スラリーは、モース硬度で８以上の値を有する高硬度材料、例えば、炭化ケイ素、窒化ガリウムなどの難削材の研摩に好適であり、特に炭化ケイ素の研摩に最適である。 The abrasive slurry of the present invention is suitable for polishing a hard material having a Mohs hardness value of 8 or more, for example, difficult-to-cut materials such as silicon carbide and gallium nitride, and is particularly suitable for polishing silicon carbide.
　本発明の研摩材スラリーによれば、炭化ケイ素のような高硬度の難削材も、高速に平滑研摩が可能となる。 According to the abrasive slurry of the present invention, even a hard material with high hardness such as silicon carbide can be smoothly polished at high speed.
酸化鉄粒子の平均粒径ＤＳＥＭと研摩速度との関係グラフGraph of the relationship between the average particle diameter D SEM of iron oxide particles and the polishing speed 繰り返し使用試験における表面粗度変化のグラフGraph of surface roughness change in repeated use test 繰り返し使用試験における研摩速度変化のグラフGraph of polishing speed change in repeated use test
　以下、本発明における実施形態について、実施例及び比較例を参照しながら説明する。 Hereinafter, embodiments of the present invention will be described with reference to examples and comparative examples.
　実施例は、砥粒となる酸化物粒子としてＦｅ３Ｏ４、α－Ｆｅ２Ｏ３、γ－Ｆｅ２Ｏ３を用い、これら酸化物粒子と純水とを混合し、これに酸化剤としてＫＭｎＯ４(和光純薬社製)を加えて撹拌し、表１に示す各研摩材スラリーを作製した。表１に示すようにＦｅ３Ｏ４については粒径が異なるものを市販の酸化鉄より選別して準備した。また、α－Ｆｅ２Ｏ３については、実施例２のＦｅ３Ｏ４を６００℃、１時間、焼成処理をして生成したものであり、γ－Ｆｅ２Ｏ３については、実施例２のＦｅ３Ｏ４を３００℃、１時間、焼成処理をして生成したものである。 In this example, Fe 3 O 4 , α-Fe 2 O 3 , and γ-Fe 2 O 3 were used as oxide particles to be abrasive grains, and these oxide particles were mixed with pure water, and this was used as an oxidizing agent. KMnO 4 (manufactured by Wako Pure Chemical Industries, Ltd.) was added and stirred to prepare each abrasive slurry shown in Table 1. As shown in Table 1, for Fe 3 O 4 , those having different particle diameters were prepared from commercially available iron oxides. In addition, α-Fe 2 O 3 was produced by firing the Fe 3 O 4 of Example 2 at 600 ° C. for 1 hour, and γ-Fe 2 O 3 was obtained from Example 2. Fe 3 O 4 is produced by baking at 300 ° C. for 1 hour.
　また比較として、砥粒となる酸化物粒子としてＳｉＯ２を用い、これら酸化物粒子と純水とを混合し、これに酸化剤としてＫＭｎＯ４を加えて撹拌し、表１に示す比較例の研摩材スラリーを作製した。 As a comparison, SiO 2 is used as oxide particles to be abrasive grains, these oxide particles and pure water are mixed, KMnO 4 is added as an oxidant and stirred, and polishing of comparative examples shown in Table 1 is performed. A material slurry was prepared.
　表１には、各研摩材スラリーのｐＨ、酸化物粒子の平均粒径Ｄ５０、走査型電子顕微鏡による平均粒径ＤＳＥＭ、比表面積（ＳＳＡ）、及び酸化物粒子と酸化剤の含有量を示している。平均粒径Ｄ５０、ＤＳＥＭ、比表面積（ＳＳＡ）の測定は次のようにして行った。 Table 1 shows the pH of each abrasive slurry, the average particle diameter D 50 of the oxide particles, the average particle diameter D SEM by a scanning electron microscope, the specific surface area (SSA), and the contents of the oxide particles and the oxidizing agent. Show. The average particle diameters D 50 , D SEM and specific surface area (SSA) were measured as follows.
　平均粒径Ｄ５０：ここでいう平均粒径Ｄ５０はレーザー回折・散乱法粒子径分布における体積基準の積算分率における５０％径のことである。測定前に酸化物粒子の分散を行うために超音波分散処理を３分間実施し、レーザ回折・散乱法粒子径分布測定装置（（株）堀場製作所製：ＬＡ－９２０）を使用して測定した。 The average particle size D 50: average particle diameter D 50 here is that a 50% diameter in cumulative fraction of the volume reference in the laser diffraction scattering method particle size distribution. In order to disperse oxide particles before measurement, ultrasonic dispersion treatment was performed for 3 minutes, and measurement was performed using a laser diffraction / scattering particle size distribution measuring apparatus (Horiba, Ltd .: LA-920). .
　平均粒径ＤＳＥＭ：走査型電子顕微鏡(ＳＥＭ)を用いて加速電圧５ｋＶ、２万倍で観察した視野内の１０個の酸化物粒子について粒径を測定し、その平均値を平均粒径ＤＳＥＭとした。 Average particle diameter D SEM : The particle diameter of 10 oxide particles in the field of view observed at an acceleration voltage of 5 kV and 20,000 times was measured using a scanning electron microscope (SEM), and the average value was determined as the average particle diameter D. SEM was used.
　比表面積（ＳＳＡ）：ＢＥＴ法によるもので、ＪＩＳ　Ｒ　１６２６-1996（ファインセラミックス粉体の気体吸着ＢＥＴ法による比表面積の測定方法）の「６．２　流動法　の（３．５）一点法」に準拠して、酸化物粒子の比表面積の測定を行った。その際、キャリアガスであるヘリウムと、吸着質ガスである窒素の混合ガスを使用した。 Specific surface area (SSA): Based on the BET method, “6.2 Flow method (3.5) one-point method” in JIS R 1626-1996 (Method for measuring specific surface area by gas adsorption BET method of fine ceramic powder) Based on the above, the specific surface area of the oxide particles was measured. At that time, a mixed gas of helium as a carrier gas and nitrogen as an adsorbate gas was used.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　また、各研摩材スラリーについて研摩試験を行って評価した。研摩特性は、研摩速度と研摩処理後の表面粗度を測定することにより行った。 Also, each abrasive slurry was evaluated by conducting a polishing test. The polishing characteristics were measured by measuring the polishing speed and the surface roughness after the polishing treatment.
研摩試験：研摩対象は直径２インチのラッピングされた４Ｈ－ＳｉＣ基板を用いた。研摩処理は基板のＳｉ面に対して行った。市販の研摩装置（エム・エー・ティー社製：片面研摩機ＢＣ－１５）を用い、定盤には研摩パッド（ニッタ・ハース社製：ＳＵＢＡ＃６００）を取り付けた。定盤及びＳｉＣ基板の回転数は６０ｒｐｍに設定した。また、研摩時の荷重は２００ｇｆ／ｃｍ２とした。研摩材スラリーの供給量は２００ｍＬ／ｍｉｎとした。なお、研摩処理時間は３時間とした。 Polishing test: A lapping 4H—SiC substrate having a diameter of 2 inches was used as a polishing target. The polishing process was performed on the Si surface of the substrate. A commercially available polishing apparatus (manufactured by MG Corporation: single-sided grinder BC-15) was used, and a polishing pad (Nitta Haas: SUBA # 600) was attached to the surface plate. The rotation speed of the surface plate and the SiC substrate was set to 60 rpm. The load during polishing was 200 gf / cm 2 . The supply amount of the abrasive slurry was 200 mL / min. The polishing time was 3 hours.
また、研摩特性として、基板の表面粗度を測定した。研摩前後の表面粗さＲａ（ＪＩＳ　Ｂ０６０１）は、原子間力顕微鏡「Ｄｉｍｅｎｔｉｏｎ３１００」（Ｄｉｇｉｔａｌ　Ｉｎｓｔｒｕｍｅｎｔｓ社製）により該基板の表面を測定し、同社のソフトウエア「Ｎａｎｏｓｃｏｐｅ　Ｖ」を用いて測定結果を解析することで求めた。測定条件は、測定範囲＝１０μｍ×１０μｍ、測定点５１２×５１２ポイント、スキャンレート＝1Ｈｚとした。尚、研摩前の基板における表面粗さＲａは０．４ｎｍであった。研摩処理後の結果は表２に示す。 Further, the surface roughness of the substrate was measured as a polishing characteristic. The surface roughness Ra (JIS B0601) before and after polishing was measured by measuring the surface of the substrate with an atomic force microscope “Dimention 3100” (manufactured by Digital Instruments) and analyzing the measurement results using the software “Nanoscope V” of the company. I asked for it. The measurement conditions were measurement range = 10 μm × 10 μm, measurement point 512 × 512 point, and scan rate = 1 Hz. The surface roughness Ra of the substrate before polishing was 0.4 nm. The results after the polishing treatment are shown in Table 2.
　そして、研摩特性として研摩速度を測定した。また、研摩速度（ｎｍ／ｍｉｎ）は、研摩前後の基板の質量差とＳｉＣの密度（３．１０ｇ／ｃｍ３とした）とから算出した。その結果を表２示す。 Then, the polishing speed was measured as a polishing characteristic. The polishing rate (nm / min) was calculated from the difference in mass of the substrate before and after polishing and the density of SiC (3.10 g / cm 3 ). The results are shown in Table 2.
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
　表２に示すように、比較例１、２のＳｉＯ２を砥粒とした研摩材スラリーでは、研摩速度が遅く、ごく表層のみが研摩されるのみであった。そのため、原子間力顕微鏡（ＡＦＭ）で確認した際にも、研摩後の表面にはキズが確認された。このため、デバイスなどに使用できる程度の研摩処理が行えていないと判断した。比較例１の場合の表面粗さＲａは０．４ｎｍであったが、比較例２の場合は表面にキズが多く発生していて表面粗さを測定できなかった。これに対して、実施例の酸化鉄を砥粒とした研摩材スラリーでは研摩速度も大きく、研摩後の表面粗さＲａも良好な結果となった。特に、実施例２、実施例８及び９に示すように、本発明の酸化鉄粒子を用いた研摩材スラリーでは、その研摩特性が良好であることが判明した。 As shown in Table 2, in the abrasive slurry using the SiO 2 abrasive grains of Comparative Examples 1 and 2 , the polishing rate was slow and only the surface layer was polished. For this reason, scratches were confirmed on the surface after polishing even when confirmed with an atomic force microscope (AFM). For this reason, it was judged that the grinding | polishing process of the grade which can be used for a device etc. was not performed. In the case of Comparative Example 1, the surface roughness Ra was 0.4 nm, but in the case of Comparative Example 2, many scratches were generated on the surface, and the surface roughness could not be measured. On the other hand, the polishing slurry using the iron oxide of the example as an abrasive grain had a high polishing rate and a good surface roughness Ra after polishing. In particular, as shown in Example 2 and Examples 8 and 9, it was found that the polishing characteristics of the abrasive slurry using the iron oxide particles of the present invention were good.
　図１に、実施例１～７のＦｅ３Ｏ４の平均粒径ＤＳＥＭと研摩速度との関係を調べたグラフを示す。酸化鉄を砥粒とする場合、平均粒径ＤＳＥＭが大きくなると、研摩速度が遅くなる傾向となった。酸化鉄の平均粒径ＤＳＥＭと研摩速度についてのグラフプロットにより得られた関係から、０．４μｍ以下であると、研摩速度が２ｎｍ／ｍｉｎ程度以上となることが判った。 FIG. 1 is a graph showing the relationship between the average particle diameter D SEM of Fe 3 O 4 of Examples 1 to 7 and the polishing rate. When iron oxide was used as the abrasive grains, the polishing rate tended to decrease as the average particle size DSEM increased. From the relationship obtained by a graph plot of the average particle diameter DSEM of iron oxide and the polishing rate, it was found that the polishing rate was about 2 nm / min or more when it was 0.4 μm or less.
　次に、研摩材スラリーの繰り返し使用に関する評価を行った結果について説明する。この繰り返し使用試験は次のようにして行った。研摩材スラリーとしては実施例２、実施例９を用いた。また、比較例３として、電解ＭｎＯ２(三井金属鉱業社製)の酸化物粒子(Ｄ５０＝０．３μｍ、ＤＳＥＭ＝０．２μｍ、比表面積４８．７ｍ２／ｇ）と、酸化剤としてＫＭｎＯ４を用いて研摩材スラリーを作製して使用した。 Next, the results of evaluation regarding repeated use of the abrasive slurry will be described. This repeated use test was conducted as follows. Examples 2 and 9 were used as the abrasive slurry. Moreover, as Comparative Example 3, oxide particles of electrolytic MnO 2 (Mitsui Metal Mining Co., Ltd.) (D 50 = 0.3 μm, D SEM = 0.2 μm, specific surface area 48.7 m 2 / g) and an oxidizing agent An abrasive slurry was prepared using KMnO 4 and used.
　研摩試験条件は、上記と同様にして行い、一枚の基板を２時間の研摩をし、合計５枚（合計１０時間）の基板を連続して研摩処理した。なお、この連続研摩試験では、途中で研摩材スラリーの交換や砥粒の補充はしていない。各基板の研摩後の表面粗度Ｒａと、各基板における研摩速度を算出した。その結果を図２及び図３に示す。 The polishing test conditions were the same as described above. One substrate was polished for 2 hours, and a total of 5 substrates (10 hours in total) were polished continuously. In this continuous polishing test, the abrasive slurry was not changed or the abrasive grains were not replenished. The surface roughness Ra after polishing of each substrate and the polishing speed of each substrate were calculated. The results are shown in FIGS.
　図２及び図３の横軸は研摩処理した基板の順番とした。図２の結果から、実施例２、実施例９、比較例３のいずれの研摩材スラリーも、１０時間という長時間の研摩処理であっても安定した表面粗度を実現できることが判明した。そして、図３に示す研摩速度の場合、砥粒としてＭｎＯ２の酸化物粒子を用いた比較例３の研摩材スラリーでは３枚目の基板から研摩速度が低下している。これに対して、酸化鉄を砥粒とした実施例２、実施例９の研摩材スラリーでは１０時間の研摩処理を連続して行っても、安定した研摩速度であることが判明した。 The horizontal axis in FIGS. 2 and 3 is the order of the polished substrates. From the results of FIG. 2, it was found that any of the polishing slurry of Examples 2, 9 and Comparative Example 3 can realize a stable surface roughness even when polishing is performed for a long time of 10 hours. In the case of the polishing speed shown in FIG. 3, in the polishing slurry of Comparative Example 3 using MnO 2 oxide particles as the abrasive grains, the polishing speed decreases from the third substrate. In contrast, the polishing slurry of Example 2 and Example 9 using iron oxide as abrasive grains was found to have a stable polishing rate even after 10 hours of polishing treatment.
　本発明によれば、モース硬度８以上の難削材、例えば炭化ケイ素、窒化ガリウムのような高硬度の難削材を高速に平滑研摩でき、連続した研摩処理も可能となるので、モース硬度８以上の難削材からなる基板の研摩処理を効率的に行うことができる。 According to the present invention, a difficult-to-cut material having a Mohs hardness of 8 or more, for example, a hard-hard material having a high hardness such as silicon carbide or gallium nitride can be smoothly polished at a high speed and a continuous polishing process can be performed. The polishing treatment of the substrate made of the above difficult-to-cut material can be performed efficiently.

Claims (3)

  1. 　酸化鉄粒子とマンガン酸イオンとを含有したことを特徴とするモース硬度８以上の難削材の研摩に用いる研摩材スラリー。 An abrasive slurry used for polishing difficult-to-cut materials having a Mohs hardness of 8 or more, characterized by containing iron oxide particles and manganate ions.
  2. 　酸化鉄粒子の平均粒径ＤＳＥＭが０．４μｍ以下である請求項１記載の研摩材スラリー。 The abrasive slurry according to claim 1, wherein the average particle diameter DSEM of the iron oxide particles is 0.4 µm or less.
  3. 　酸化鉄粒子は、ＦｅＯ、Ｆｅ２Ｏ３、Ｆｅ３Ｏ４のうち少なくともいずれか１種を含む請求項１または請求項２に記載の研摩材スラリー。 The abrasive slurry according to claim 1 or 2 , wherein the iron oxide particles include at least one of FeO, Fe 2 O 3 , and Fe 3 O 4 .
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