JP2007005562A - Wafer polishing solution composition and wafer polishing method - Google Patents
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Abstract
Description
本発明は、ウェーハ研磨液組成物及びウェーハ研磨方法に関する。 The present invention relates to a wafer polishing liquid composition and a wafer polishing method.
従来より、ウェーハ研磨液組成物が種々知られている。例えば、特許文献１の実施例１には、コロイダルシリカ７．０重量％、３５％過酸化水素を純分で１重量％、１−ヒドロキシエチリデン−１，１−ジホスホン酸（＝ヒドロキシエタンジホスホン酸）０．４５重量％、残りを水として１００重量％としたｐＨ２の研磨液組成物が提案されている。また、半導体ウェーハ等の研磨に用いられる場合、研磨速度と表面品質の向上の観点からはｐＨ７〜１２が好ましいと記載され、ｐＨは水酸化カリウム、水酸化ナトリウム、アミン等の塩基性物質により調製することができると記載されている。
しかしながら、特許文献１では、ゲルマニウムウェーハを研磨する点については記載されておらず、どのような組成やｐＨであればゲルマニウムウェーハの研磨に適するのかは不明である。また、ゲルマニウムウェーハとシリコンウェーハとを同じ研磨液組成物で研磨することが要望されているが、両ウェーハの化学的性質の相違や物理的性質の相違から、これまでそのような研磨液組成物は知られていない。 However, Patent Document 1 does not describe the point of polishing a germanium wafer, and it is unclear what composition and pH are suitable for polishing a germanium wafer. Further, it is demanded to polish a germanium wafer and a silicon wafer with the same polishing liquid composition. However, due to the difference in chemical properties and physical properties of both wafers, such a polishing liquid composition has hitherto been used. Is not known.
本発明は、このような課題に鑑みなされたものであり、ゲルマニウムウェーハを研磨するのに好適なウェーハ研磨液組成物を提供することを目的の一つとする。また、ゲルマニウムウェーハとシリコンウェーハの両方を良好に研磨することができるウェーハ研磨液組成物及びウェーハ研磨方法を提供することを目的の一つとする。 The present invention has been made in view of such problems, and an object of the present invention is to provide a wafer polishing liquid composition suitable for polishing a germanium wafer. Another object of the present invention is to provide a wafer polishing composition and a wafer polishing method capable of satisfactorily polishing both germanium wafers and silicon wafers.
本発明は、上述の目的の少なくとも一部を達成するために以下の手段を採った。 The present invention employs the following means in order to achieve at least a part of the above-described object.
すなわち、本発明のウェーハ研磨液組成物は、ゲルマニウムウェーハを研磨するときに使用するウェーハ研磨液組成物であって、研磨材、酸化剤、有機ホスホン酸、アルカリ成分及び水を含有しｐＨが９〜１１のものである。このウェーハ研磨液組成物によれば、研磨後のゲルマニウムウェーハの表面を円滑に仕上げることができると共にスクラッチや傷が全くないか又はほとんどない状態に仕上げることができる。 That is, the wafer polishing liquid composition of the present invention is a wafer polishing liquid composition used when polishing a germanium wafer, and contains an abrasive, an oxidizing agent, an organic phosphonic acid, an alkali component and water, and has a pH of 9 ~ 11. According to this wafer polishing liquid composition, the surface of the polished germanium wafer can be finished smoothly and finished with no or almost no scratches or scratches.
また、本発明のウェーハ研磨方法は、ゲルマニウムウェーハとシリコンウェーハとを同じ組成の研磨液組成物で研磨するウェーハ研磨方法であって、（１）ゲルマニウムウェーハの研磨工程で上述した本発明のウェーハ研磨液組成物が供給される研磨パッドをゲルマニウムウェーハに押し当てるときの加圧圧力を、シリコンウェーハの研磨工程で上述した本発明のウェーハ研磨液組成物が供給される研磨パッドをシリコンウェーハに押し当てるときの加圧圧力の３〜５倍に設定するか、あるいは、（２）ゲルマニウムウェーハの研磨工程で上述した本発明のウェーハ研磨液組成物が供給される研磨パッドをゲルマニウムウェーハに押し当てるときの加圧圧力を３０〜３５ｋＰａに設定し、シリコンウェーハの研磨工程で上述した本発明のウェーハ研磨液組成物が供給される研磨パッドをシリコンウェーハに押し当てるときの加圧圧力を６〜１０ｋＰａに設定するものである。このウェーハ研磨方法によれば、同じ組成の研磨液組成物でもってゲルマニウムウェーハもシリコンウェーハも良好に研磨することができる。 The wafer polishing method of the present invention is a wafer polishing method for polishing a germanium wafer and a silicon wafer with a polishing composition having the same composition, and (1) the wafer polishing of the present invention described above in the polishing process of the germanium wafer. The pressure applied when the polishing pad supplied with the liquid composition is pressed against the germanium wafer is pressed against the silicon wafer with the polishing pad supplied with the wafer polishing liquid composition of the present invention described above in the polishing step of the silicon wafer. Or (2) when the polishing pad to which the wafer polishing composition of the present invention described above is supplied in the polishing process of the germanium wafer is pressed against the germanium wafer. The pressurizing pressure is set to 30 to 35 kPa, and the wafer of the present invention described above in the silicon wafer polishing step is used. The polishing pad C polishing composition is supplied is for setting the pressurizing pressure when pressed against the silicon wafer 6～10KPa. According to this wafer polishing method, both a germanium wafer and a silicon wafer can be satisfactorily polished with a polishing composition having the same composition.
本発明のウェーハ研磨液組成物は、ゲルマニウムウェーハを研磨するときに使用するウェーハ研磨液組成物であって、研磨材、酸化剤、有機ホスホン酸、アルカリ成分及び水を含有しｐＨが９〜１１のものである。 The wafer polishing liquid composition of the present invention is a wafer polishing liquid composition used when polishing a germanium wafer, and contains an abrasive, an oxidizing agent, an organic phosphonic acid, an alkali component, and water, and has a pH of 9 to 11 belongs to.
ここで、研磨材としては、特に限定されるものではないが、例えばコロイダルシリカ、ヒュームドシリカ、湿式合成シリカからなる群より選ばれる１種又は２種以上が挙げられ、そのうちコロイダルシリカが好ましい。研磨材としてシリカを用いる場合、その平均粒径は１０ｎｍ未満では研磨速度が低下し２００ｎｍを超えると研磨される被研磨面の粗度が必ずしも良好でなくなることから、１０〜２００ｎｍの範囲であることが好ましく、４０〜１００ｎｍの範囲であることがより好ましい。また、ウェーハ研磨液組成物中の研磨材の含有量は、１重量％未満では研磨速度が低下することがあり５０重量％を超えると研磨速度は向上するが表面品質が低下することがあるから、１〜５０重量％の範囲であることが好ましく、１０〜４０重量％の範囲であることがより好ましい。なお、本明細書で平均粒径とは、コロイダルシリカの場合は、周知のシアーズ滴定法によって測定された値である。シアーズ滴定法とは、アナリティカル・ケミストリ（ANALYTICAL CHEMISTRY）第２８巻第１２号（１９５６年１２月）第１９８１頁に説明されているように水酸化ナトリウムを用いた滴定による比表面積から換算される粒子径の測定方法である。また、ヒュームドシリカや湿式合成シリカの平均粒子径（Ｄｐ）は、下記の換算式を用いて、ＢＥＴ法比表面積の値（Ｓａ）から算出する。
Ｄｐ＝６０００／ρ・Ｓａ
（但し、Ｄｐ：平均粒子径（ｎｍ）、Ｓａ：ＢＥＴ法比表面積値（ｍ2／ｇ）、ρ：比重（ｇ／ｃｍ3））
Here, the abrasive is not particularly limited, and examples thereof include one or more selected from the group consisting of colloidal silica, fumed silica, and wet synthetic silica. Of these, colloidal silica is preferable. When silica is used as the abrasive, the average particle size is in the range of 10 to 200 nm because the polishing rate decreases when the average particle size is less than 10 nm and the roughness of the surface to be polished is not necessarily good when the average particle size exceeds 200 nm. Is preferable, and the range of 40 to 100 nm is more preferable. In addition, if the content of the abrasive in the wafer polishing liquid composition is less than 1% by weight, the polishing rate may decrease, and if it exceeds 50% by weight, the polishing rate improves but the surface quality may decrease. 1 to 50% by weight, and more preferably 10 to 40% by weight. In the present specification, the average particle diameter is a value measured by a known Sears titration method in the case of colloidal silica. The Sears titration method is converted from the specific surface area by titration with sodium hydroxide as described in ANALYTICAL CHEMISTRY Vol. 28 No. 12 (December 1956), p. 1981. This is a method for measuring the particle diameter. Moreover, the average particle diameter (Dp) of fumed silica or wet synthetic silica is calculated from the value (Sa) of the BET method specific surface area using the following conversion formula.
Dp = 6000 / ρ · Sa
(However, Dp: average particle diameter (nm), Sa: BET specific surface area value (m 2 / g), ρ: specific gravity (g / cm 3 ))
酸化剤としては、特に限定されるものではないが、過酸化物、過マンガン酸又はその塩、クロム酸又はその塩、硝酸又はその塩、ペルオキソ酸又はその塩、酸素酸又はその塩、金属塩類、硫酸類等が挙げられる。具体的には、過酸化物としては、過酸化水素、過酸化ナトリウム、過酸化バリウム等；過マンガン酸又はその塩としては、過マンガン酸カリウム等；クロム酸又はその塩としては、クロム酸金属塩、重クロム酸金属塩等；硝酸塩としては、硝酸鉄（III)、硝酸アンモニウム等；ペルオキソ酸又はその塩としては、ペルオキソ二硫酸、ペルオキソ二硫酸アンモニウム、ペルオキソ二硫酸金属塩、ペルオキソリン酸、ペルオキソ硫酸、ペルオキソホウ酸ナトリウム、過ギ酸、過酢酸、過安息香酸、過フタル酸等；酸素酸又はその塩としては、次亜塩素酸、次亜臭素酸、次亜ヨウ素酸、塩素酸、臭素酸、ヨウ素酸、過塩素酸、次亜塩素酸ナトリウム、次亜塩素酸カルシウム等；金属塩類としては、塩化鉄（III)、硫酸鉄（III)、クエン酸鉄（III)、硫酸アンモニウム鉄（III)等が挙げられる。このうち、過酸化水素、過酢酸、酸素酸塩（特に次亜塩素酸塩）が好ましく、表面に金属イオンが付着せず汎用に使用され安価であるという観点から過酸化水素がより好ましい。これらの酸化物は、単独で又は２種以上を混合して使用してもよい。また、ウェーハ研磨液組成物中の酸化剤の含有量は、純分で０．０１重量％未満では研磨速度が低下することがあり５重量％を超えると研磨速度は向上するが被研磨面の品質が低下することがあるから、０．０１〜５重量％の範囲が好ましく、０．０３〜１重量％の範囲がより好ましい。 Although it does not specifically limit as an oxidizing agent, Peroxy acid or its salt, Chromic acid or its salt, Nitric acid or its salt, Peroxo acid or its salt, Oxyacid or its salt, Metal salts And sulfuric acids. Specifically, as peroxide, hydrogen peroxide, sodium peroxide, barium peroxide, etc .; as permanganic acid or its salt, as potassium permanganate; as chromic acid or its salt as metal chromate Salts, dichromate metal salts, etc .; as nitrates, iron (III) nitrate, ammonium nitrate, etc .; as peroxo acids or salts thereof, peroxodisulfuric acid, ammonium peroxodisulfate, peroxodisulfate metal salts, peroxophosphoric acid, peroxosulfuric acid Sodium peroxoborate, performic acid, peracetic acid, perbenzoic acid, perphthalic acid, etc .; oxygen acids or salts thereof include hypochlorous acid, hypobromous acid, hypoiodous acid, chloric acid, bromic acid, Iodic acid, perchloric acid, sodium hypochlorite, calcium hypochlorite, etc .; metal salts include iron (III) chloride, iron (III) sulfate, iron (III) citrate, sulfate And ammonium iron (III). Among these, hydrogen peroxide, peracetic acid, and oxyacid salt (especially hypochlorite) are preferable, and hydrogen peroxide is more preferable from the viewpoint that metal ions do not adhere to the surface and are generally used and inexpensive. These oxides may be used alone or in admixture of two or more. Further, if the content of the oxidizing agent in the wafer polishing liquid composition is less than 0.01% by weight as a pure component, the polishing rate may decrease. If it exceeds 5% by weight, the polishing rate is improved, but the surface of the surface to be polished is improved. Since quality may deteriorate, the range of 0.01 to 5% by weight is preferable, and the range of 0.03 to 1% by weight is more preferable.
有機ホスホン酸は、本発明のウェーハ研磨液組成物において研磨促進剤として使用される。かかる有機ホスホン酸を使用することで表面品質が向上する。有機ホスホン酸としては、特に限定されるものではないが、ジエチレントリアミンペンタメチレンホスホン酸、ホスホノブタントリカルボン酸、ホスホノヒドロキシ酢酸、ヒドロキシエチルジメチレンホスホン酸、アミノトリスメチレンホスホン酸、ヒドロキシエタンジホスホン酸、エチレンジアミンテトラメチレンホスホン酸、ヘキサメチレンジアミンテトラメチレンホスホン酸及びこれらの塩等から選ばれる１種又は２種が挙げられる。また、ウェーハ研磨液組成物中の有機ホスホン酸の含有量は、０．０１重量％未満では被研磨面の汚染低減効果が不十分なことがあり５重量％を超えても汚染低減の向上が認められないことから、０．０１〜５重量％の範囲が好ましく、０．０１〜１重量％の範囲がより好ましく、０．０４〜０．２重量％の範囲が更に好ましい。 The organic phosphonic acid is used as a polishing accelerator in the wafer polishing liquid composition of the present invention. By using such an organic phosphonic acid, the surface quality is improved. The organic phosphonic acid is not particularly limited, but diethylenetriaminepentamethylenephosphonic acid, phosphonobutanetricarboxylic acid, phosphonohydroxyacetic acid, hydroxyethyldimethylenephosphonic acid, aminotrismethylenephosphonic acid, hydroxyethanediphosphonic acid , Ethylenediaminetetramethylenephosphonic acid, hexamethylenediaminetetramethylenephosphonic acid, and one or two selected from salts thereof. Further, if the content of the organic phosphonic acid in the wafer polishing liquid composition is less than 0.01% by weight, the effect of reducing the contamination of the surface to be polished may be insufficient. Since it is not recognized, the range of 0.01 to 5% by weight is preferable, the range of 0.01 to 1% by weight is more preferable, and the range of 0.04 to 0.2% by weight is still more preferable.
アルカリ成分は、特に限定されるものではないが、例えば無機アルカリ成分についていえば、塩基性を示すアルカリ金属化合物、アルカリ土類金属化合物などが挙げられ、有機アルカリ成分についていえば、有機アミン化合物などが挙げられる。具体的には、アルカリ金属化合物としては、水酸化ナトリウム、炭酸ナトリウム、リン酸ナトリウム、ホウ酸ナトリウムなどのナトリウム化合物や、水酸化カリウム、炭酸カリウム、リン酸カリウム、ホウ酸カリウムなどのカリウム化合物等が挙げられ、有機アミン化合物としては、メチルアミン、エチルアミン、プロピルアミン、イソプロピルアミン、ブチルアミン、イソブチルアミン、アミルアミン、ヘキシルアミン、ヘプチルアミン、オクチルアミン、ジメチルアミン、ジエチルアミン、ジプロピルアミン、ジブチルアミン、トリメチルアミン、トリエチルアミン、トリブチルアミン、エタノールアミン、プロパノールアミン、ブタノールアミン、ジエタノールアミン、ジプロパノールアミン、ジブタノールアミン、トリエタノールアミン、トリプロパノールアミン、トリブタノールアミン、エチレンジアミン等が挙げられる。このうちコストや環境への影響を考慮すると無機アルカリ成分が好ましく、特に水酸化ナトリウムや水酸化カリウムが好ましい。 The alkali component is not particularly limited, but for example, an inorganic alkali component includes basic alkali metal compounds, alkaline earth metal compounds, etc., and an organic alkali component includes organic amine compounds, etc. Is mentioned. Specifically, examples of the alkali metal compound include sodium compounds such as sodium hydroxide, sodium carbonate, sodium phosphate, and sodium borate, and potassium compounds such as potassium hydroxide, potassium carbonate, potassium phosphate, and potassium borate. Examples of organic amine compounds include methylamine, ethylamine, propylamine, isopropylamine, butylamine, isobutylamine, amylamine, hexylamine, heptylamine, octylamine, dimethylamine, diethylamine, dipropylamine, dibutylamine, trimethylamine , Triethylamine, tributylamine, ethanolamine, propanolamine, butanolamine, diethanolamine, dipropanolamine, dibutanolamine, triethanolamine Emissions, tripropanolamine, tributanolamine, ethylenediamine, and the like. Of these, inorganic alkali components are preferred in view of cost and environmental impact, and sodium hydroxide and potassium hydroxide are particularly preferred.
本発明のウェーハ研磨液組成物のｐＨは９〜１１の範囲に調整されるが、このｐＨの数値範囲は研磨されるゲルマニウムウェーハの研磨速度、被研磨面の特性のほか、研磨液組成物の安定性の観点から決定したものである。シリコンウェーハでは、ｐＨが酸性であっても塩基性であっても良好に研磨することができるが、ゲルマニウムウェーハではｐＨが酸性では良好に研磨することができない。なお、ｐＨの調整は例えばアルカリ成分の配合割合を変更することにより行う。 The pH of the wafer polishing liquid composition of the present invention is adjusted to a range of 9 to 11. This pH value range is determined by the polishing rate of the germanium wafer to be polished, the characteristics of the surface to be polished, and the polishing liquid composition. It was determined from the viewpoint of stability. A silicon wafer can be satisfactorily polished regardless of whether the pH is acidic or basic, but a germanium wafer cannot be satisfactorily polished if the pH is acidic. In addition, adjustment of pH is performed by changing the mixture ratio of an alkali component, for example.
本発明のウェーハ研磨液組成物をゲルマニウムウェーハとシリコンウェーハの両方の研磨に用いる場合において、酸化剤として過酸化水素を使用した場合には、研磨材の純分（例えばコロイダルシリカを用いた場合にはコロイダルシリカに含まれるシリカ）の重量を１００としたときの酸化剤の重量を０．２〜４．４となるように設定するのが好ましい。こうすれば、ゲルマニウムウェーハの被研磨面もシリコンウェーハの被研磨面もスクラッチ・傷の少ない状態となるし、表面粗さ（Ｒａ）も良好な値になる。 In the case where the wafer polishing composition of the present invention is used for polishing both germanium wafers and silicon wafers, when hydrogen peroxide is used as the oxidizing agent, the pure content of the abrasive (for example, when colloidal silica is used) Is preferably set so that the weight of the oxidizing agent is 0.2 to 4.4 when the weight of silica contained in colloidal silica is 100. By doing so, both the polished surface of the germanium wafer and the polished surface of the silicon wafer are in a state of few scratches and scratches, and the surface roughness (Ra) is also good.
本発明のウェーハ研磨液組成物をゲルマニウムウェーハとシリコンウェーハの両方の研磨に用いる場合において、酸化剤として過酸化水素を使用し、アルカリ成分として無機アルカリ成分を使用した場合には、研磨材の重量を１００としたときの酸化剤の重量が０．４〜２．７となるように設定するのが好ましい。こうすれば、ゲルマニウムウェーハの被研磨面もシリコンウェーハの被研磨面もスクラッチ・傷が一層少ない状態となる。特に、研磨材の重量を１００としたときの酸化剤の重量が０．４〜１．０となるように設定すると、表面粗さ（Ｒａ）の値を低く抑えることができるしスクラッチ・傷をより一層少なくすることができるため、より好ましい。 When the wafer polishing liquid composition of the present invention is used for polishing both germanium wafers and silicon wafers, when hydrogen peroxide is used as an oxidizing agent and inorganic alkali components are used as alkali components, the weight of the abrasive It is preferable to set so that the weight of the oxidant is 0.4 to 2.7, when 100 is 100. In this way, the surface to be polished of the germanium wafer and the surface to be polished of the silicon wafer are in a state where scratches and scratches are further reduced. In particular, when the weight of the oxidizer is set to 0.4 to 1.0 when the weight of the abrasive is 100, the surface roughness (Ra) can be kept low, and scratches and scratches can be prevented. This is more preferable because it can be further reduced.
本発明のウェーハ研磨液組成物中の水は、媒体として使用されるものであり、その含有量はウェーハを研磨するうえで各種の含有成分が適切な濃度になると共に適切な粘度となるよう適宜定めればよい。なお、本発明のウェーハ研磨液組成物は、ウェーハを研磨するのに適する濃度に調整したものを製造してもよいが、濃厚液として製造したものを使用時に適切な濃度に調整してもよい。 The water in the wafer polishing liquid composition of the present invention is used as a medium, and the content thereof is appropriately adjusted so that various components are at an appropriate concentration and have an appropriate viscosity when polishing the wafer. You just have to decide. In addition, the wafer polishing liquid composition of the present invention may be manufactured to a concentration adjusted to polish the wafer, but may be adjusted to an appropriate concentration when used as a concentrated liquid. .
本発明のウェーハ研磨液組成物は、必要に応じて、通常この種のウェーハ研磨液組成物に含まれる成分を含有していてもよい。そのような成分としては、例えば、界面活性剤、洗浄剤、防錆剤、表面改質剤、粘度調整剤、抗菌剤、分散剤などが挙げられる。 The wafer polishing liquid composition of this invention may contain the component normally contained in this kind of wafer polishing liquid composition as needed. Examples of such components include surfactants, detergents, rust inhibitors, surface modifiers, viscosity modifiers, antibacterial agents, and dispersants.
本発明の研磨液組成物は、片面及び両面研磨機でウェーハを研磨する際に用いることができる。例えば、片面研磨機として、上面に研磨パッドを有し回転する定盤と、下面にウェーハを吸着保持して定盤の研磨面にそのウェーハを押し付けるよう定盤の上方に回転可能で且つ上下動可能に設けられた保持装置とを備えたものを使用する場合には、この研磨パッドに本発明の研磨液組成物を供給しながら保持装置に吸着保持されたウェーハを所定の加圧圧力で研磨パッドに押し付けて研磨を行う。研磨パッドは、スウェードタイプ、不織布タイプ、その他いずれのタイプも使用することができる。本発明の研磨液組成物は第１研磨（ラッピング）、第２研磨（仕上げ研磨、ポリシング）のいずれにも使用することができる。本発明の研磨液組成物は被研磨面のスクラッチ・傷等の発生が少ないため、仕上げの研磨に使用することができる。 The polishing composition of the present invention can be used when a wafer is polished with a single-sided or double-sided polishing machine. For example, as a single-side polishing machine, a rotating platen with a polishing pad on the upper surface, and a wafer that is held on the lower surface by suction and can be rotated above and below the platen to press the wafer against the polishing surface of the platen When using a device provided with a holding device provided as possible, the wafer adsorbed and held by the holding device is polished with a predetermined pressure while supplying the polishing composition of the present invention to the polishing pad. Polish against the pad. As the polishing pad, a suede type, a non-woven fabric type, or any other type can be used. The polishing composition of the present invention can be used for both the first polishing (lapping) and the second polishing (finish polishing, polishing). The polishing liquid composition of the present invention can be used for finishing polishing because scratches and scratches on the surface to be polished are small.
同じ組成のウェーハ研磨液組成物を用いてゲルマニウムウェーハとシリコンウェーハとを研磨する場合、ゲルマニウムウェーハの研磨工程で上述したウェーハ研磨液組成物が供給される研磨パッドをゲルマニウムウェーハに押し当てるときの加圧圧力を、シリコンウェーハの研磨工程で上述したウェーハ研磨液組成物が供給される研磨パッドをシリコンウェーハに押し当てるときの加圧圧力の３〜５倍に設定して研磨を行うようにしてもよい。あるいは、ゲルマニウムウェーハの研磨工程で上述したウェーハ研磨液組成物が供給される研磨パッドをゲルマニウムウェーハに押し当てるときの加圧圧力を３０〜３５ｋＰａに設定し、シリコンウェーハの研磨工程で上述したウェーハ研磨液組成物が供給される研磨パッドをシリコンウェーハに押し当てるときの加圧圧力を６〜１０ｋＰａに設定して研磨を行うようにしてもよい。このように加圧圧力を調整することにより、同じ組成のウェーハ研磨液組成物でもってゲルマニウムウェーハとシリコンウェーハの両方を良好に研磨することができる。 When polishing a germanium wafer and a silicon wafer using a wafer polishing liquid composition having the same composition, it is added when the polishing pad to which the wafer polishing liquid composition is supplied is pressed against the germanium wafer in the germanium wafer polishing process. Polishing may be performed by setting the pressure to 3 to 5 times the pressure applied when the polishing pad supplied with the above-described wafer polishing liquid composition is pressed against the silicon wafer in the polishing process of the silicon wafer. Good. Alternatively, the pressure applied when the polishing pad to which the above-described wafer polishing composition is supplied in the germanium wafer polishing step is pressed against the germanium wafer is set to 30 to 35 kPa, and the above-described wafer polishing is performed in the silicon wafer polishing step. Polishing may be performed by setting the pressure applied when the polishing pad supplied with the liquid composition is pressed against the silicon wafer to 6 to 10 kPa. Thus, by adjusting the pressure, both the germanium wafer and the silicon wafer can be satisfactorily polished with the wafer polishing liquid composition having the same composition.
次に、本発明のウェーハ研磨液組成物を、実施例を用いて具体的に説明する。なお、本発明は以下の実施例に何ら限定されるものではなく、本発明の技術的範囲に属する限り、種々の態様で実施できることはいうまでもない。 Next, the wafer polishing liquid composition of this invention is demonstrated concretely using an Example. In addition, this invention is not limited to the following Examples at all, and as long as it belongs to the technical scope of this invention, it cannot be overemphasized that it can implement with a various aspect.
［実施例１］
５０％コロイダルシリカ（触媒化成工業（株）のカタロイドＳi−５０）８０重量部、３５％過酸化水素水５．０重量部、６０％ヒドロキシエチルジホスホン酸０．５重量部、１０％水酸化カリウム３．４０重量部、水１１．１重量部を混合し、濃厚液を調製した。ｐＨは、Ｄ−１３ガラス電極式水素イオン濃度計（株式会社堀場製作所）により測定したところ、１０．１１であった。この濃厚液１００重量部に対し、純水１００重量部を添加し混合することによりウェーハ研磨液組成物とした。得られたウェーハ研磨液組成物には、コロイダルシリカが２０重量％、過酸化水素水が０．８７５重量％、ヒドロキシエチルジホスホン酸が０．１５重量％、水酸化カリウムが０．１７重量％含まれている。
[Example 1]
80 parts by weight of 50% colloidal silica (Cataloid Si-50 from Catalytic Chemical Industry Co., Ltd.), 5.0 parts by weight of 35% hydrogen peroxide, 0.5 parts by weight of 60% hydroxyethyl diphosphonic acid, 10% hydroxylation A concentrated solution was prepared by mixing 3.40 parts by weight of potassium and 11.1 parts by weight of water. The pH was 10.11 as measured by a D-13 glass electrode type hydrogen ion concentration meter (Horiba, Ltd.). To 100 parts by weight of this concentrated liquid, 100 parts by weight of pure water was added and mixed to obtain a wafer polishing liquid composition. The resulting wafer polishing liquid composition contained 20% by weight of colloidal silica, 0.875% by weight of hydrogen peroxide, 0.15% by weight of hydroxyethyl diphosphonic acid, and 0.17% by weight of potassium hydroxide. include.
［実施例２〜９，比較例１〜５］
実施例２〜９，比較例１〜５では、濃縮液の各成分の種類や配合量、ｐＨを表１に示すように変更した以外は、実施例１に準じて濃厚液を調製した。各実施例では、濃厚液全体で１００重量部となるように水を加えた。調製した濃厚液１００重量部に対し、純水１００重量部を添加し混合することによりウェーハ研磨液組成物とした。得られたウェーハ研磨液組成物に含まれる各成分の純分の重量％を表２に示す。なお、コロイダルシリカは、実施例３ではデュポン社製のサイトンＨＴ−５０を使用したが、その他は実施例１と同様、触媒化成工業（株）のカタロイドＳｉ−５０を使用した。これらのコロイダルシリカの平均粒径は２０〜７０ｎｍである。
[Examples 2 to 9, Comparative Examples 1 to 5]
In Examples 2 to 9 and Comparative Examples 1 to 5, concentrated solutions were prepared according to Example 1 except that the types, blending amounts, and pH of each component of the concentrate were changed as shown in Table 1. In each Example, water was added so that it might be 100 weight part in the whole concentrated liquid. To 100 parts by weight of the prepared concentrated liquid, 100 parts by weight of pure water was added and mixed to obtain a wafer polishing liquid composition. Table 2 shows the pure weight% of each component contained in the obtained wafer polishing liquid composition. The colloidal silica used was Cyton HT-50 manufactured by DuPont in Example 3, but Cataloid Si-50 from Catalyst Kasei Kogyo Co., Ltd. was used in the same manner as in Example 1. These colloidal silicas have an average particle size of 20 to 70 nm.
［比較例６］
特開２００２−３２７１７０の実施例１に準じて調製した。すなわち、４０％コロイダルシリカ１７．５重量部（純分で７重量％）、３５％過酸化水素２．８６重量部（純分で１重量％）、１−ヒドロキシエチリデン−１，１−ジホスホン酸（ヒドロキシエタンジホスホン酸）０．４５重量部を混合し、残りを水として、合計１００重量部とした。
[Comparative Example 6]
Prepared according to Example 1 of JP-A-2002-327170. That is, 17.5 parts by weight of 40% colloidal silica (7% by weight in pure content), 2.86 parts by weight of 35% hydrogen peroxide (1% by weight in pure content), 1-hydroxyethylidene-1,1-diphosphonic acid (Hydroxyethanediphosphonic acid) 0.45 parts by weight was mixed, and the rest was water to make a total of 100 parts by weight.
［研磨試験］
シリコンウェーハとしてディスクの直径が４インチのものを使用し、ゲルマニウムウェーハとしてディスクの直径が１インチのものを使用した。また、研磨試験機として片面ラッピングマシンＳＬＭ−１００（不二越機械工業社）、研磨パッドとしてスウェード状のポリウレタン（ローデル社）を使用し、研磨パッドへのウェーハ研磨液の供給量を２００ｍＬ／ｍｉｎとし、１回の研磨時間を６０分として、ラッピング（研磨加工）を行ったあとのディスクにつきポリシング（鏡面加工）を行い、ウェーハを洗浄、乾燥後に被研磨面の特性評価に供した。ポリシングは同じ条件で３回実施し、各データ値は３回の平均値とした。なお、ポリシング時の加圧圧力は、ゲルマニウムウェーハの場合３３３ｇ／ｃｍ2（３２．７ｋＰａ）とし、シリコンウェーハの場合８２ｇ／ｃｍ2（８．０ｋＰａ）とした。また、ポリシングの前段階のラッピングについては、ポリシング時と同じウェーハ研磨液を用いて３０分間１次ラップを行った。
[Polishing test]
A silicon wafer having a disk diameter of 4 inches was used, and a germanium wafer having a disk diameter of 1 inch was used. Moreover, a single-sided lapping machine SLM-100 (Fujikoshi Machine Industry Co., Ltd.) is used as a polishing test machine, a suede-like polyurethane (Rodel) is used as a polishing pad, and the amount of wafer polishing liquid supplied to the polishing pad is 200 mL / min. Polishing (mirror finishing) was performed on the disk after lapping (polishing) with a polishing time of 60 minutes, and the wafer was cleaned and dried, and then subjected to characteristic evaluation of the surface to be polished. Polishing was performed three times under the same conditions, and each data value was an average of three times. Incidentally, the applied pressure at the time of polishing in the case of germanium wafer and 333g / cm 2 (32.7kPa), and in the case of silicon wafers 82g / cm 2 (8.0kPa). For lapping in the previous stage of polishing, primary lapping was performed for 30 minutes using the same wafer polishing liquid as that used during polishing.
［被研磨面の特性評価］
被研磨面の特性評価は、研磨速度、表面粗さ（Ｒａ）、スクラッチ・傷の有無の３つの項目について行った。研磨速度は、下記数１式により求めた。また、表面粗さ（Ｒａ）は、算術平均粗さであり、光干渉式非接触３次元表面形状計測装置であるＺＹＧＯ Ｎｅｗ Ｖｉｅｗ５０００（ザイゴ社）を用いて測定した。この測定は、０．０８ｍｍ以上の周波数をカットして行った。スクラッチ・傷の有無は、光学顕微鏡を用い、倍率１００倍でウェーハ表面を９０度おきに１箇所の測定面積を５．０００ｍｍ×２．０００ｍｍとして４箇所測定し、スクラッチ・傷の個数を調べ、スクラッチ・傷が認められなかったものを評価Ｓとし、スクラッチ・傷が５個未満だったものを評価Ａとし、スクラッチ・傷が５個以上１０個未満だったものを評価Ｂとし、スクラッチ・傷が１０個以上だったものを評価Ｃとした。各実施例、各比較例の評価結果を表３に示す。
[Characteristic evaluation of polished surface]
The characteristics of the surface to be polished were evaluated for three items: polishing rate, surface roughness (Ra), and presence / absence of scratches / scratches. The polishing rate was determined by the following equation (1). Moreover, surface roughness (Ra) is arithmetic mean roughness, and was measured using ZYGO New View5000 (Zygo) which is an optical interference type non-contact three-dimensional surface shape measuring apparatus. This measurement was performed by cutting a frequency of 0.08 mm or more. Presence / absence of scratches / scratches was measured using an optical microscope at a magnification of 100 ×, measuring the number of scratches / scratches at four locations with a measurement area of 5.000 mm × 2.000 mm every 90 degrees on the wafer surface. Scratch / scratch was evaluated as S, Scratch / scratch was less than 5 evaluation A, Scratch / scratch was 5 or more but less than 10 evaluation B, scratch / scratch Was rated C. Table 3 shows the evaluation results of each example and each comparative example.
表３に示すように、比較例１〜６ではゲルマニウムウェーハの被研磨面はスクラッチ・傷が多く表面粗さ（Ｒａ）が測定不能だったのに対して、実施例１〜９ではゲルマニウムウェーハの被研磨面はスクラッチ・傷がほとんどなく表面粗さ（Ｒａ）も良好な値が得られた。また、比較例５，６では、シリコンウェーハの被研磨面はスクラッチ・傷がほとんどなく表面粗さ（Ｒａ）も良好な値が得られたものの、ゲルマニウムウェーハの被研磨面はスクラッチ・傷が多く表面粗さ（Ｒａ）が測定不能だったのに対して、実施例１〜７では、シリコンウェーハ及びゲルマニウムウェーハの両方の被研磨面ともスクラッチ・傷がほとんどなく表面粗さ（Ｒａ）も良好な値が得られた。特に実施例３〜６，８〜９では、両方の被研磨面ともスクラッチ・傷が全く見られなかった。 As shown in Table 3, in Comparative Examples 1 to 6, the polished surface of the germanium wafer had many scratches and scratches, and the surface roughness (Ra) could not be measured. The polished surface was almost free from scratches and scratches, and the surface roughness (Ra) was good. In Comparative Examples 5 and 6, the polished surface of the silicon wafer was almost free from scratches and scratches, and the surface roughness (Ra) was good, but the polished surface of the germanium wafer was scratched and scratched frequently. Whereas the surface roughness (Ra) was not measurable, in Examples 1 to 7, both the polished surfaces of the silicon wafer and the germanium wafer had almost no scratches or scratches, and the surface roughness (Ra) was also good. A value was obtained. In particular, in Examples 3 to 6 and 8 to 9, no scratches or scratches were observed on both polished surfaces.
なお、実施例６〜９ではアルカリ成分として有機アミンを用いているが、環境面を考慮すれば、無機アルカリ成分を用いる実施例１〜５の方が好ましい。 In Examples 6 to 9, an organic amine is used as the alkali component. However, in consideration of the environment, Examples 1 to 5 using an inorganic alkali component are preferable.
Claims (8)
研磨材、酸化剤、有機ホスホン酸、アルカリ成分及び水を含有しｐＨが９〜１１である、ウェーハ研磨液組成物。 A wafer polishing liquid composition used when polishing a germanium wafer,
A wafer polishing liquid composition comprising an abrasive, an oxidizing agent, an organic phosphonic acid, an alkali component and water and having a pH of 9 to 11.
前記酸化剤は過酸化水素、次亜塩素酸塩及び過酢酸からなる群より選ばれる少なくとも１種であり、
前記有機ホスホン酸はジエチレントリアミンペンタメチレンホスホン酸、ホスホノブタントリカルボン酸、ホスホノヒドロキシ酢酸、ヒドロキシエチルジメチレンホスホン酸、アミノトリメチレンホスホン酸、ヒドロキシエタンジホスホン酸、エチレンジアミンテトラメチレンホスホン酸、ヘキサメチレンジアミンテトラメチレンホスホン酸及びこれらの塩からなる群より選ばれる少なくとも１種である、
請求項１又は２に記載のウェーハ研磨液組成物。 The abrasive is at least one selected from the group consisting of colloidal silica, fumed silica and wet synthetic silica,
The oxidizing agent is at least one selected from the group consisting of hydrogen peroxide, hypochlorite and peracetic acid,
The organic phosphonic acid is diethylenetriaminepentamethylenephosphonic acid, phosphonobutanetricarboxylic acid, phosphonohydroxyacetic acid, hydroxyethyldimethylenephosphonic acid, aminotrimethylenephosphonic acid, hydroxyethanediphosphonic acid, ethylenediaminetetramethylenephosphonic acid, hexamethylenediamine Is at least one selected from the group consisting of tetramethylenephosphonic acid and salts thereof,
The wafer polishing liquid composition according to claim 1 or 2.
前記研磨材の純分の重量を１００としたときの前記酸化剤の重量が０．２〜４．４である、
請求項３に記載のウェーハ研磨液組成物。 The oxidizing agent is hydrogen peroxide;
The weight of the oxidizing agent when the weight of the pure part of the abrasive is 100 is 0.2 to 4.4.
The wafer polishing liquid composition according to claim 3.
前記アルカリ成分は無機アルカリ成分であり、
前記研磨材の重量を１００としたときの前記酸化剤の重量が０．４〜２．７である、
請求項３に記載のウェーハ研磨液組成物。 The oxidizing agent is hydrogen peroxide;
The alkali component is an inorganic alkali component,
The weight of the oxidizing agent when the weight of the abrasive is 100 is 0.4 to 2.7,
The wafer polishing liquid composition according to claim 3.
請求項５に記載のウェーハ研磨液組成物。 The weight of the oxidant when the weight of the abrasive is 100 is 0.4 to 1.0.
The wafer polishing liquid composition according to claim 5.
ゲルマニウムウェーハの研磨工程で請求項１〜６のいずれかに記載のウェーハ研磨液組成物が供給される研磨パッドをゲルマニウムウェーハに押し当てるときの加圧圧力を、シリコンウェーハの研磨工程で請求項１〜５のいずれかに記載のウェーハ研磨液組成物が供給される研磨パッドをシリコンウェーハに押し当てるときの加圧圧力の３〜５倍に設定する、
ウェーハ研磨方法。 A wafer polishing method for polishing a germanium wafer and a silicon wafer with a polishing composition having the same composition,
The pressure applied when the polishing pad supplied with the wafer polishing composition according to any one of claims 1 to 6 is pressed against the germanium wafer in the germanium wafer polishing step is determined in the silicon wafer polishing step. To 3 to 5 times the pressure applied when pressing the polishing pad to which the wafer polishing composition according to any one of 5 to 5 is pressed against a silicon wafer,
Wafer polishing method.
ゲルマニウムウェーハの研磨工程で請求項１〜６のいずれかに記載のウェーハ研磨液組成物が供給される研磨パッドをゲルマニウムウェーハに押し当てるときの加圧圧力を３０〜３５ｋＰａに設定し、シリコンウェーハの研磨工程で請求項１〜５のいずれかに記載のウェーハ研磨液組成物が供給される研磨パッドをシリコンウェーハに押し当てるときの加圧圧力を６〜１０ｋＰａに設定する、
ウェーハ研磨方法。 A wafer polishing method for polishing a germanium wafer and a silicon wafer with a polishing composition having the same composition,
The pressure for pressing the polishing pad to which the wafer polishing composition according to any one of claims 1 to 6 is pressed against the germanium wafer in the polishing process of the germanium wafer is set to 30 to 35 kPa, The pressing pressure when pressing the polishing pad supplied with the wafer polishing composition according to any one of claims 1 to 5 to the silicon wafer in the polishing step is set to 6 to 10 kPa,
Wafer polishing method.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013018015A3 (en) * | 2011-08-01 | 2013-03-28 | Basf Se | A PROCESS FOR THE MANUFACTURE OF SEMICONDUCTOR DEVICES COMPRISING THE CHEMICAL MECHANICAL POLISHING OF ELEMENTAL GERMANIUM AND/OR Si1-XGeX MATERIAL IN THE PRESENCE OF A CMP COMPOSITION COMPRISING A SPECIFIC ORGANIC COMPOUND |
| JP2013197212A (en) * | 2012-03-16 | 2013-09-30 | Fujimi Inc | Polishing composition |
| JP2013254777A (en) * | 2012-06-05 | 2013-12-19 | Fujikura Ltd | Polishing method |
| KR20170038809A (en) | 2014-07-28 | 2017-04-07 | 신에쯔 한도타이 가부시키가이샤 | Method for polishing germanium wafer |
| US9688884B2 (en) | 2011-11-25 | 2017-06-27 | Fujimi Incorporated | Polishing composition |
| CN114605922A (en) * | 2022-03-18 | 2022-06-10 | 北京通美晶体技术股份有限公司 | Chemical polishing solution for rapid polishing and preparation method thereof |
| RU2809530C1 (en) * | 2022-06-27 | 2023-12-12 | Акционерное общество "Новосибирский приборостроительный завод" | Suspension for polishing germanium crystals |
| JP7409899B2 (en) | 2020-02-18 | 2024-01-09 | 株式会社フジミインコーポレーテッド | Polishing composition, polishing method, and semiconductor substrate manufacturing method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013018015A3 (en) * | 2011-08-01 | 2013-03-28 | Basf Se | A PROCESS FOR THE MANUFACTURE OF SEMICONDUCTOR DEVICES COMPRISING THE CHEMICAL MECHANICAL POLISHING OF ELEMENTAL GERMANIUM AND/OR Si1-XGeX MATERIAL IN THE PRESENCE OF A CMP COMPOSITION COMPRISING A SPECIFIC ORGANIC COMPOUND |
| RU2605941C2 (en) * | 2011-08-01 | 2016-12-27 | Басф Се | PROCESS FOR MANUFACTURE OF SEMICONDUCTOR DEVICES COMPRISING CHEMICAL MECHANICAL POLISHING OF ELEMENTAL GERMANIUM AND/OR Si1-x Gex MATERIAL IN PRESENCE OF CMP (CHEMICAL MECHANICAL POLISHING) COMPOSITION COMPRISING A SPECIFIC ORGANIC COMPOUND |
| US9688884B2 (en) | 2011-11-25 | 2017-06-27 | Fujimi Incorporated | Polishing composition |
| JP2013197212A (en) * | 2012-03-16 | 2013-09-30 | Fujimi Inc | Polishing composition |
| JP2013254777A (en) * | 2012-06-05 | 2013-12-19 | Fujikura Ltd | Polishing method |
| KR20170038809A (en) | 2014-07-28 | 2017-04-07 | 신에쯔 한도타이 가부시키가이샤 | Method for polishing germanium wafer |
| JP7409899B2 (en) | 2020-02-18 | 2024-01-09 | 株式会社フジミインコーポレーテッド | Polishing composition, polishing method, and semiconductor substrate manufacturing method |
| CN114605922A (en) * | 2022-03-18 | 2022-06-10 | 北京通美晶体技术股份有限公司 | Chemical polishing solution for rapid polishing and preparation method thereof |
| RU2809530C1 (en) * | 2022-06-27 | 2023-12-12 | Акционерное общество "Новосибирский приборостроительный завод" | Suspension for polishing germanium crystals |
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