JP2000169233A - Wet cleaning of silicon carbide sintered product - Google Patents

Wet cleaning of silicon carbide sintered product

Info

Publication number
JP2000169233A
JP2000169233A JP10348701A JP34870198A JP2000169233A JP 2000169233 A JP2000169233 A JP 2000169233A JP 10348701 A JP10348701 A JP 10348701A JP 34870198 A JP34870198 A JP 34870198A JP 2000169233 A JP2000169233 A JP 2000169233A
Authority
JP
Japan
Prior art keywords
silicon carbide
carbide sintered
aqueous solution
sintered body
aqueous
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP10348701A
Other languages
Japanese (ja)
Other versions
JP4188473B2 (en
Inventor
Masami Ootsuki
正珠 大月
Hiroaki Wada
宏明 和田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bridgestone Corp
Original Assignee
Bridgestone Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bridgestone Corp filed Critical Bridgestone Corp
Priority to JP34870198A priority Critical patent/JP4188473B2/en
Priority to US09/449,764 priority patent/US6419757B2/en
Publication of JP2000169233A publication Critical patent/JP2000169233A/en
Application granted granted Critical
Publication of JP4188473B2 publication Critical patent/JP4188473B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
    • C04B41/5315—Cleaning compositions, e.g. for removing hardened cement from ceramic tiles

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

PROBLEM TO BE SOLVED: To simply and easily remove organic impurities and inorganic ones both existing on the surface of and near the surface of a silicon carbide sintered product by washing it through the sequential immersion treatment of the sintered product in a quasi-aqueous organic solvent, an aqueous ammonium solution, an aqueous inorganic acid solution and deionized water. SOLUTION: This method for the wet cleaning of a silicon carbide sintered product is to sequentially subject the sintered product to the following treatment so as to wash it and to make the washing degree on its surface become the level of <1×1011 atoms/cm2: (1) removing organic impurities adhered to the surface of and near the surface of the sintered product by soaking it in a quasi-aqueous organic solution for 2-60 min; (2) soaking it in an aqueous ammonium solution having 25-35 dynes/cm surface tension for 5-120 min; (3) removing metallic impurities on its surface of and near its surface by soaking it in an aqueous inorganic acid solution having 0. 3-68 wt.% concentration for 5-120 min; (4) soaking it in deionized water having <=100 ppt impurity and 16-18 MΩ resistivity for 2-60 min in an overflowing state. At least one of the processes preferably is conducted in a state that ultrasonic vibration is applied to the aqueous solution and the aqueous solution of at least one of the processes preferably shows >=30 deg.C.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明は、半導体各種部材及
び電子部品用途向け炭化ケイ素焼結体の湿式洗浄方法に
関する。詳しくは、高純度が要求されるダミーウエハ、
ターゲット、発熱体等に関する半導体製造用途炭化ケイ
素焼結体の有機物汚染、金属元素汚染、及ぴパーティク
ル汚染の除去方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for wet-cleaning a silicon carbide sintered body for various semiconductor members and electronic parts. Specifically, dummy wafers that require high purity,
The present invention relates to a method for removing organic substance contamination, metal element contamination, and particle contamination of a silicon carbide sintered body for use in semiconductor production with respect to a target, a heating element, and the like.

【０００２】[0002]

【従来の技術】炭化ケイ素は、共有結合性の強い物質で
あり、従来より高温強度性。耐熱性、耐摩耗性。耐薬品
性等の優れた特性を生かして多くの用途で用いられてき
た。それらの利点が着目され、最近では電子分野、情報
分野、半導体分野への応用が期待されている。2. Description of the Related Art Silicon carbide is a substance having a strong covalent bond and has higher strength at high temperatures than before. Heat resistance, wear resistance. It has been used in many applications by taking advantage of its excellent properties such as chemical resistance. These advantages have attracted attention, and application to the fields of electronics, information, and semiconductors has recently been expected.

【０００３】半導体シリコン集積回路の高集積化、及び
それに付随した細線化に伴って、これらの分野で用いら
れる半導体各種部材及び電子部品は、高純度化、高密度
化が要求されるため、非金属系焼結助剤を用いたホット
プレス焼結法や反応焼結法が鋭意研究されている。しか
しながら、これらの焼結法で得られた炭化ケイ素焼結体
は、高純度化、高密度化でありながら製造前後のプロセ
ス（焼結、加工、及びハンドリング等）で、表面及び表
面近傍に汚染を受けているのが現状である。As semiconductor silicon integrated circuits become more highly integrated and thinner, the various semiconductor members and electronic components used in these fields are required to have higher purity and higher density. A hot press sintering method and a reaction sintering method using a metal-based sintering agent have been studied intensively. However, the silicon carbide sintered body obtained by these sintering methods has high purity and high density, but contaminates the surface and the vicinity of the surface during the pre- and post-production processes (sintering, processing, handling, etc.). It is the current situation.

【０００４】このため、炭化ケイ素焼結体を半導体各種
部材及び電子部品に応用するためには、即ちコンタミネ
ーション、パーティクル等の汚染を防ぐためには、表面
洗浄によるシリコンウエハ並みの表面純度の達成が必要
不可欠である。[0004] Therefore, in order to apply the silicon carbide sintered body to various semiconductor members and electronic components, that is, to prevent contamination and particles from contaminating, it is necessary to achieve a surface purity equivalent to that of a silicon wafer by surface cleaning. Indispensable.

【０００５】炭化ケイ素焼結体の洗浄方法に関する報告
としては、（１）登録１８１８４１号では、酸洗浄後、
１２００℃以上の温度で酸化処理し、その後窒素雰囲気
で表面処理する方法が、（２）特開平５−１７２２９号
ではシリカ砥粒でブラスト洗浄した後に、フッ酸及び硝
酸の混酸で湿式洗浄する方法が、（３）特開平６−７７
３１０号では、フッ酸水溶液に浸清洗浄した後、超純水
で濯ぎ、更に酸素・ハロゲンガスで乾式洗浄した後に、
酸素処理する方法が、（４）焼結後の、高純度化は非常
に困難なことから、多孔質炭化珪素成形時にハロゲン化
水素ガス及び無機酸洗浄処理をして一旦高純度化した
後、二次焼結する方法（特開昭５５−１５８６２２号、
特開昭６０−１３８９１３号、特開昭６４−７２９６４
号）等が報告されている。As a report on a method for cleaning a silicon carbide sintered body, (1) Registration No. 181841 discloses that after acid cleaning,
The method of oxidizing at a temperature of 1200 ° C. or more and then performing a surface treatment in a nitrogen atmosphere is described in (2) Japanese Patent Application Laid-Open No. 5-17229: a method of blast cleaning with silica abrasive grains and then wet cleaning with a mixed acid of hydrofluoric acid and nitric acid. However, (3) JP-A-6-77
In No. 310, after rinsing and washing in hydrofluoric acid aqueous solution, rinsing with ultrapure water and further dry-cleaning with oxygen and halogen gas,
The method of oxygen treatment is as follows: (4) Since it is very difficult to achieve high purity after sintering, once the porous silicon carbide is subjected to a hydrogen halide gas and inorganic acid cleaning treatment at the time of high purity purification, Secondary sintering method (JP-A-55-158622,
JP-A-60-138913, JP-A-64-72964
No.) have been reported.

【０００６】以上の方法は、簡易に湿式洗浄するだけで
はなく、酸化処理、ブラスト洗浄、二次焼結等の処理が
必要で工程が複雑になり、優れた洗浄法であるとは言い
難い。The above method requires not only simple wet cleaning, but also oxidation, blast cleaning, secondary sintering and the like, which complicates the process, and cannot be said to be an excellent cleaning method.

【０００７】[0007]

【発明が解決しようとする課題】本発明は、前記事実を
考慮してなされたものであり、本発明の目的は、半導体
各種部材及び電子部品に用いられるよう、炭化ケイ素焼
結体の表面及び表面近傍に存在する有機及び無機不純物
を、簡易に洗浄除去することができる炭化ケイ素焼結体
の湿式洗浄方法を提供することである。SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned facts, and an object of the present invention is to provide a method for manufacturing a surface of a silicon carbide sintered body so as to be used for various semiconductor members and electronic components. An object of the present invention is to provide a wet cleaning method for a silicon carbide sintered body that can easily remove organic and inorganic impurities present in the vicinity of a surface by cleaning.

【０００８】[0008]

【課題を解決するための手段】本発明者らは、鋭意検討
した結果、半導体各種部材及び電子部品に応用可能な高
密度、高純度の炭化ケイ素焼結体であっても、工程汚染
等で表面及び表面近傍の有機及び無機不純物濃度が著し
く上がり、半導体各種部材及び電子部品に応用し難いこ
とに着目し、簡易に有機及び無機不純物を洗浄除去する
方法を見出した。即ち、本発明は、Means for Solving the Problems As a result of intensive studies, the present inventors have found that even high-density, high-purity silicon carbide sintered bodies applicable to various semiconductor members and electronic components are subject to process contamination and the like. Focusing on the fact that the concentration of organic and inorganic impurities on the surface and in the vicinity of the surface is remarkably increased and it is difficult to apply it to various semiconductor members and electronic components, a method for easily removing organic and inorganic impurities by washing has been found. That is, the present invention

【０００９】＜１＞炭化ケイ素焼結体を、準水系有機溶
剤に浸漬する工程、無機酸水溶液に浸漬する工程、及び
純水に浸漬する工程、で順次処理することを特徴とする
炭化ケイ素焼結体の湿式洗浄方法。<1> A silicon carbide sintered body characterized by sequentially treating a silicon carbide sintered body in a step of dipping in a semi-aqueous organic solvent, a step of dipping in an inorganic acid aqueous solution, and a step of dipping in pure water. A wet cleaning method for the aggregate.

【００１０】＜２＞炭化ケイ素焼結体を、準水系有機溶
剤に浸漬する工程、アンモニウム水溶液に浸漬する工
程、無機酸水溶液に浸漬する工程、及び純水に浸漬する
工程、で順次処理することを特徴とする炭化ケイ素焼結
体の湿式洗浄方法。<2> The silicon carbide sintered body is sequentially treated in a step of dipping in a semi-aqueous organic solvent, a step of dipping in an ammonium aqueous solution, a step of dipping in an inorganic acid aqueous solution, and a step of dipping in pure water. A wet cleaning method for a silicon carbide sintered body, characterized in that:

【００１１】＜３＞炭化ケイ素焼結体を、準水系有機溶
剤に浸漬する工程、無機酸水溶液に浸漬する工程、アン
モニウム水溶液に浸漬する工程、及び純水に浸漬する工
程、で順次処理することを特徴とする炭化ケイ素焼結体
の湿式洗浄方法。<3> The silicon carbide sintered body is sequentially treated in a step of dipping in a semi-aqueous organic solvent, a step of dipping in an aqueous solution of inorganic acid, a step of dipping in an aqueous solution of ammonium, and a step of dipping in pure water. A wet cleaning method for a silicon carbide sintered body, characterized in that:

【００１２】＜４＞少なくとも１つの工程が、液に超音
波振動を加えながら行うことを特徴とする前記＜１＞〜
＜３＞のいずれかに記載の炭化ケイ素焼結体の湿式洗浄
方法。<4> At least one step is performed while applying ultrasonic vibration to the liquid.
The wet cleaning method for a silicon carbide sintered body according to any one of <3>.

【００１３】＜５＞少なくとも１つの工程の液の温度
が、３０℃以上であることを特徴とする前記＜１＞〜＜
４＞のいずれかに記載の炭化ケイ素焼結体の湿式洗浄方
法。<5> The temperature of the liquid in at least one of the steps is at least 30 ° C.
4) The wet cleaning method for a silicon carbide sintered body according to any one of the above items.

【００１４】＜６＞準水系有機溶剤が、石油系炭化水
素、有機酸エステル、及びグリコールエーテル、これら
の混合溶剤、又はこれら溶剤或いは混合溶剤と界面活性
剤との混合物であることを特徴とする前記＜１＞〜＜５
＞のいずれかに記載の炭化ケイ素焼結体の湿式洗浄方
法。<6> The quasi-aqueous organic solvent is a petroleum hydrocarbon, an organic acid ester, a glycol ether, a mixed solvent thereof, or a mixture of these solvents or a mixed solvent and a surfactant. <1> to <5 above
> The wet cleaning method for a silicon carbide sintered body according to any one of the above items.

【００１５】＜７＞無機酸水溶液が、フッ酸水溶液、硝
酸水溶液、硫酸水溶液、塩酸水溶液、過酸化水素水、オ
ゾン水、又はこれらの混合酸水溶液であることを特徴と
する前記＜１＞〜＜６＞のいずれかに記載の炭化ケイ素
焼結体の湿式洗浄方法。<7> The above-mentioned <1> to <1>, wherein the inorganic acid aqueous solution is a hydrofluoric acid aqueous solution, a nitric acid aqueous solution, a sulfuric acid aqueous solution, a hydrochloric acid aqueous solution, a hydrogen peroxide solution, an ozone water, or a mixed acid aqueous solution thereof. <6> The wet cleaning method for a silicon carbide sintered body according to any one of <6>.

【００１６】＜８＞アンモニウム水溶液が、ハロゲン化
テトラアルキルアンモニウム水溶液、過塩素酸テトラア
ルキルアンモニウム水溶液、アンモニア水、又はこれら
と過酸化水素水との混合水溶液であること特徴とする前
記＜２＞〜＜７＞のいずれかに記載の炭化ケイ素焼結体
の湿式洗浄方法。<8> The above-mentioned <2> to <2>, wherein the aqueous ammonium solution is an aqueous solution of a tetraalkylammonium halide, an aqueous solution of a tetraalkylammonium perchlorate, aqueous ammonia, or a mixed aqueous solution of these and aqueous hydrogen peroxide. The wet cleaning method for a silicon carbide sintered body according to any one of <7>.

【００１７】本発明の炭化ケイ素焼結体の湿式洗浄方法
は、炭化ケイ素焼結体を、半導体各種部材及び電子部品
に応用可能な、表面洗浄度（不純物付着量）を１×１０
11ａｔｏｍｓ／ｃｍ2 未満のレベルまでにすることがで
きる。According to the wet cleaning method for a silicon carbide sintered body of the present invention, the silicon carbide sintered body can be applied to various semiconductor members and electronic parts.
It can be up to a level of less than 11 atoms / cm 2 .

【００１８】本発明の炭化ケイ素焼結体の湿式洗浄方法
は、全洗浄液が、水に可溶或いは濯ぎ可能な薬液により
構成されており、洗浄工程の途中で乾燥プロセス等が不
要であるため、全プロセスを簡略化できる利点がある。In the wet cleaning method for a silicon carbide sintered body according to the present invention, the entire cleaning liquid is constituted by a chemical solution that is soluble or rinsable in water, and a drying process or the like is not required during the cleaning step. There is an advantage that the entire process can be simplified.

【００１９】[0019]

【発明の実施の形態】本発明の炭化ケイ素焼結体の湿式
洗浄方法は、炭化ケイ素焼結体（以下、被洗浄体という
ことがある。）を、準水系有機溶剤に浸漬する工程と、
無機酸水溶液に浸漬する工程と、純水に浸漬する工程
と、で順次処理する方法である。これらの工程を、この
順番で行うことで、まず準水系有機溶剤により表面の有
機物（例えば油膜、指紋、ワックス）が除去され、その
上で無機酸水溶液による表面及び表面近傍の金属元素を
除去することが可能となる。また、アンモニウム水溶液
に浸漬する工程を、上記工程間に行うこと、用いた有機
溶剤及びパーティクルがより除去し易くなり好適であ
る。BEST MODE FOR CARRYING OUT THE INVENTION The wet cleaning method of a silicon carbide sintered body of the present invention comprises the steps of immersing a silicon carbide sintered body (hereinafter, sometimes referred to as a body to be cleaned) in a semi-aqueous organic solvent.
This is a method of sequentially performing a process of immersing in an inorganic acid aqueous solution and a process of immersing in pure water. By performing these steps in this order, first, organic substances (eg, oil films, fingerprints, and waxes) on the surface are removed by the quasi-aqueous organic solvent, and then the metal elements on the surface and near the surface by the aqueous inorganic acid solution are removed. It becomes possible. In addition, it is preferable that the step of immersing in an aqueous ammonium solution is performed between the above steps, and that the used organic solvent and particles are more easily removed.

【００２０】前記準水系有機溶剤に浸漬する工程は、炭
化ケイ素焼結体の表面及び表面近傍に付着した有機物を
除去する工程である。The step of immersing in the semi-aqueous organic solvent is a step of removing organic substances adhering to the surface and near the surface of the silicon carbide sintered body.

【００２１】前記準水系有機溶剤とは、水に可溶な有機
溶剤及びそれ自体が水に不溶であるが水による洗浄で容
易に除去できるものを示す。即ち、本発明において、準
水系有機溶剤とは、水に可溶なものの他、水不溶性溶剤
に親水性基を部分的に導入したもの、或いは予め界面活
性剤を添加したものも含む。前記準水系有機溶剤として
具体的には、石油系炭化水素、有機酸エステル、グリコ
ールエーテル、これらの混合溶剤、及びこれら溶剤或い
は混合溶剤と界面活性剤との混合物等が挙げられる。該
混合溶剤及び混合物としては、石油系炭化水素と有機酸
エステル又はグリコールエーテルとの混合溶剤、石油系
炭化水素と有機酸エステル又はグリコールエーテルと界
面活性剤との混合物、石油系炭化水素と界面活性剤との
混合物、有機エステルと界面活性剤との混合物等が挙げ
られる。The quasi-aqueous organic solvent refers to an organic solvent soluble in water and a solvent which is insoluble in water but can be easily removed by washing with water. That is, in the present invention, the quasi-aqueous organic solvent includes those which are soluble in water, those in which a hydrophilic group is partially introduced into a water-insoluble solvent, and those in which a surfactant is added in advance. Specific examples of the quasi-aqueous organic solvent include petroleum hydrocarbons, organic acid esters, glycol ethers, mixed solvents thereof, and mixtures of these solvents or mixed solvents with surfactants. As the mixed solvent and the mixture, a mixed solvent of a petroleum hydrocarbon and an organic acid ester or glycol ether, a mixture of a petroleum hydrocarbon and an organic acid ester or glycol ether and a surfactant, a petroleum hydrocarbon and a surfactant And a mixture of an organic ester and a surfactant.

【００２２】前記石油系炭化水素としては、ナフテンや
ヘキサンに代表される脂肪族炭化水素等が挙げられる。Examples of the petroleum hydrocarbon include aliphatic hydrocarbons represented by naphthene and hexane.

【００２３】前記有機酸エステルとしては、脂肪酸エス
テル（例えば、脂肪酸メチルエステル等）、グリセリン
エステル、ソルビタンエステル等が挙げられる。Examples of the organic acid esters include fatty acid esters (for example, fatty acid methyl esters), glycerin esters, sorbitan esters and the like.

【００２４】前記グリコールエーテルとしては、プロピ
レングリコールエーテル、プロピレングリコールメチル
エーテル、ジエチレングリコールジメチルエーテル等が
挙げられる。Examples of the glycol ether include propylene glycol ether, propylene glycol methyl ether, diethylene glycol dimethyl ether and the like.

【００２５】前記界面活性剤としては、所望の目的を果
たす界面活性剤ならば特に制限はないが、ポリオキシエ
チレン脂肪酸メチル、アルキルアミンオキサイド、ポリ
オキシアルキレングリコール、アルキルアミンのエチレ
ンオキシド或いはプロピレンオキシド付加体等のノニオ
ン系界面活性剤が好適である。The surfactant is not particularly limited as long as it fulfills the desired purpose, but may be polyoxyethylene fatty acid methyl, alkylamine oxide, polyoxyalkylene glycol, ethylene oxide or propylene oxide adduct of alkylamine. And the like are preferable.

【００２６】前記準水系有機溶剤に浸漬する工程におい
て、炭化ケイ素焼結体を浸漬する時間は、付着している
有機物の量や種類にもよるが、２分〜６０分が好まし
く、１０分〜３０分がより好ましく、１０分〜１５分が
さらに好ましい。In the step of immersing in the semi-aqueous organic solvent, the time for immersing the silicon carbide sintered body depends on the amount and type of the organic substances adhered thereto, but is preferably 2 minutes to 60 minutes, preferably 10 minutes to 10 minutes. 30 minutes is more preferable, and 10 minutes to 15 minutes is still more preferable.

【００２７】前記準水系有機溶剤に浸漬する工程におい
て、付着している有機物の溶解力を大きくする観点か
ら、５０〜７０℃に加熱して行うことが効果的である。In the step of immersion in the quasi-aqueous organic solvent, it is effective to heat to 50 to 70 ° C. from the viewpoint of increasing the dissolving power of the attached organic substance.

【００２８】前記無機酸水溶液に浸漬する工程は、炭化
ケイ素焼結体の表面及び表面近傍の金属不純物を除去す
る工程である。The step of immersing in the inorganic acid aqueous solution is a step of removing metal impurities on and near the surface of the silicon carbide sintered body.

【００２９】前記無機酸水溶液としては、フッ化水素酸
水溶液、硝酸水溶液、硫酸水溶液、塩酸水溶液、過酸化
水素水、オゾン水及びこれらの混合酸水溶液が挙げられ
る。前記混合酸水溶液としては、フッ硝酸水溶液、フッ
硝酸と硫酸との混合酸水溶液、フッ酸と塩酸との混合酸
水溶液等が挙げられる。Examples of the inorganic acid aqueous solution include a hydrofluoric acid aqueous solution, a nitric acid aqueous solution, a sulfuric acid aqueous solution, a hydrochloric acid aqueous solution, a hydrogen peroxide solution, an ozone water, and a mixed acid aqueous solution thereof. Examples of the mixed acid aqueous solution include a hydrofluoric nitric acid aqueous solution, a mixed acid aqueous solution of hydrofluoric nitric acid and sulfuric acid, and a mixed acid aqueous solution of hydrofluoric acid and hydrochloric acid.

【００３０】前記無機酸水溶液の濃度としては、０．３
〜６８重量％が好ましく、１〜４０重量％がより好まし
く、５〜１０重量％がさらに好ましい。この濃度が０．
３重量％未満であると、金属不純物除去効果が不十分と
なることがあり、６８重量％を超えると、被洗浄物表面
の粗度を低下させることがある。The concentration of the aqueous inorganic acid solution is 0.3
The content is preferably from 68 to 68% by weight, more preferably from 1 to 40% by weight, still more preferably from 5 to 10% by weight. This concentration is 0.
If it is less than 3% by weight, the effect of removing metal impurities may be insufficient. If it exceeds 68% by weight, the roughness of the surface of the object to be cleaned may be reduced.

【００３１】前記無機酸水溶液は、一旦溶出した金属イ
オンの再付着を防止する目的で、ノニオン系界面活性剤
を添加してもよい。該ノニオン系界面活性剤としては、
前記挙げたものと同様である。A nonionic surfactant may be added to the inorganic acid aqueous solution in order to prevent reattachment of the metal ions once eluted. As the nonionic surfactant,
The same is as described above.

【００３２】前記無機酸水溶液に浸漬する工程におい
て、炭化ケイ素焼結体を浸漬する時間は、５分〜１２０
分が好ましく、１０分〜６０分がより好ましく、２０分
〜３０分がさらに好ましい。In the step of dipping in the inorganic acid aqueous solution, the time for dipping the silicon carbide sintered body is from 5 minutes to 120 minutes.
Minutes, more preferably 10 minutes to 60 minutes, even more preferably 20 minutes to 30 minutes.

【００３３】前記純水に浸漬する工程は、前記各工程で
使用した溶剤、水溶液によって炭化ケイ素焼結体の表面
及び表面近傍に付着した残留成分を除去する工程であ
る。The step of immersing in the pure water is a step of removing residual components adhered to the surface and the vicinity of the surface of the silicon carbide sintered body by using the solvent and the aqueous solution used in each step.

【００３４】前記純水としては、純度が１００ｐｐｔ以
下のレベルで、且つ比抵抗が１６〜１８ＭΩのものが好
ましく、純度が１０ｐｐｔ未満のものであればより好ま
しい。The pure water preferably has a purity of 100 ppt or less and a specific resistance of 16 to 18 MΩ, and more preferably has a purity of less than 10 ppt.

【００３５】前記純水に浸漬する工程は、常に新液によ
って洗浄されるように、オーバーフロー方式で行うこと
が好適である。It is preferable that the step of immersing in the pure water is performed by an overflow method so that the step is always washed with a new solution.

【００３６】前記アンモニウム水溶液に浸漬する工程
は、炭化ケイ素焼結体の表面及び表面近傍に微量に付着
していると推測される前工程の有機溶剤をその界面活性
効果で除去する、及びパーティクルを除去する工程であ
る。In the step of immersing in the ammonium aqueous solution, the organic solvent in the preceding step, which is presumed to be attached in a minute amount on the surface of the silicon carbide sintered body and in the vicinity of the surface, is removed by a surface active effect, and particles are removed. This is the step of removing.

【００３７】前記アンモニウム水溶液としては、アルキ
ルアミンオキサイドやアルキルアミン等のエチレンオキ
シド或いはプロピレンオキシド付加重合体の水溶液、ハ
ロゲン化テトラアルキルアンモニウム（例えば、ハロゲ
ン化テトラメチルアンモニウム等）や過塩素酸テトラア
ルキルアンモニウム等の４級アンモニウム塩の水溶液、
アンモニア水、及びこれらと過酸化水素水との混合水溶
液等が挙げられる。これらの中でもハロゲン化テトラア
ルキルアンモニウムや過塩素酸テトラアルキルアンモニ
ウム等の４級アンモニウム塩水溶液、アンモニア水が好
ましい。Examples of the aqueous ammonium solution include aqueous solutions of ethylene oxide or propylene oxide addition polymers such as alkylamine oxides and alkylamines, tetraalkylammonium halides (eg, tetramethylammonium halide) and tetraalkylammonium perchlorates. An aqueous solution of a quaternary ammonium salt of
Ammonia water, and a mixed aqueous solution of these and hydrogen peroxide water, and the like can be given. Of these, aqueous quaternary ammonium salts such as tetraalkylammonium halides and tetraalkylammonium perchlorates, and aqueous ammonia are preferred.

【００３８】前記アンモニウム水溶液は、種類等によっ
て異なるが、通常は表面張力が２５〜３５ｄｙｎｅ／ｃ
ｍのものを用いるのが好適である。The aqueous ammonium solution varies depending on the type and the like, but usually has a surface tension of 25 to 35 dyne / c.
It is preferable to use m.

【００３９】前記アンモニウム水溶液は、１種単独で用
いてもよいし、２種以上併用してもよい。The aqueous ammonium solution may be used alone or in combination of two or more.

【００４０】前記アンモニウム水溶液に浸漬する工程に
おいて、炭化ケイ素焼結体を浸漬する時間は、５分〜１
２０分が好ましく、１０分〜６０分がより好ましく、２
０分〜３０分がさらに好ましい。In the step of dipping in the aqueous ammonium solution, the time for dipping the silicon carbide sintered body is from 5 minutes to 1 minute.
20 minutes are preferable, 10 minutes to 60 minutes are more preferable, and 2 minutes
0 to 30 minutes is more preferable.

【００４１】本発明の炭化ケイ素焼結体の湿式洗浄方法
において、被洗浄物に物理的な振動を与えることでの表
面及び表面近傍に存在する不純物がより溶解し易くなる
観点から、前記各工程の少なくとも１つの工程は、水溶
液に超音波振動を照射しながら行うことが好適であり、
被洗浄物を振動させながら或いは超音波周波数をスイー
プさせながら行ってもよい。これは、特に無機酸水溶液
に浸漬する工程で行うと効果的である。In the wet cleaning method of the silicon carbide sintered body according to the present invention, from the viewpoint that impurities present on the surface and near the surface are more easily dissolved by applying physical vibration to the object to be cleaned, Preferably, at least one step of is performed while irradiating the aqueous solution with ultrasonic vibrations,
The cleaning may be performed while vibrating the object to be cleaned or sweeping the ultrasonic frequency. This is particularly effective when performed in a step of dipping in an aqueous solution of an inorganic acid.

【００４２】本発明の炭化ケイ素焼結体の湿式洗浄方法
は、各種不純物、付着物の溶解能を向上させるため、前
記各工程の少なくとも１つの工程の溶剤又は水溶液の温
度を、好ましくは３０℃以上、さらに好ましくは４０℃
以上、特に好ましくは５０℃以上にして行うことが好適
である。この温度の上限は、用いる溶剤、水溶液の沸点
以下である。これは、特に準水系有機溶剤に浸漬する工
程で行うと効果的である。In the wet cleaning method of the silicon carbide sintered body of the present invention, the temperature of the solvent or the aqueous solution in at least one of the above steps is preferably set to 30 ° C. in order to improve the dissolving ability of various impurities and deposits. Above, more preferably 40 ° C
As described above, it is particularly preferable to carry out the reaction at 50 ° C. or higher. The upper limit of this temperature is equal to or lower than the boiling point of the solvent or aqueous solution used. This is particularly effective when performed in a step of immersion in a quasi-aqueous organic solvent.

【００４３】本発明の炭化ケイ素焼結体の湿式洗浄方法
は、前記各工程間に、洗浄水に浸漬する工程を行っても
よい。この洗浄水に浸漬する工程を行うと、例えば、準
水系有機溶剤に浸漬する工程を経た後、被洗浄体に付着
した溶剤を簡単に洗い流すこができるので、次に行う工
程の水溶液を汚染し難くなる。In the wet cleaning method of the silicon carbide sintered body of the present invention, a step of immersing the silicon carbide sintered body in cleaning water may be performed between the above steps. When the step of immersing in the washing water is performed, for example, after the step of immersing in the quasi-aqueous organic solvent, the solvent attached to the object to be cleaned can be easily washed off, so that the aqueous solution in the next step is contaminated. It becomes difficult.

【００４４】前記洗浄水としては、前記純水、蒸留水、
イオン交換水等挙げられるが、洗浄水に浸漬する工程に
よる被洗浄体の逆汚染を防止する観点から、前記純水が
好ましい。As the washing water, pure water, distilled water,
Ion-exchanged water and the like can be mentioned, but from the viewpoint of preventing reverse contamination of the object to be cleaned in the step of immersing in cleaning water, the pure water is preferable.

【００４５】前記洗浄水に浸漬する工程において、炭化
ケイ素焼結体を浸漬する時間は、２分〜６０分が好まし
く、５分〜３０分がより好ましく、１０分〜２０分がさ
らに好ましい。In the step of dipping in the washing water, the time for dipping the silicon carbide sintered body is preferably 2 minutes to 60 minutes, more preferably 5 minutes to 30 minutes, and further preferably 10 minutes to 20 minutes.

【００４６】前記洗浄水に浸漬する工程は、常に新液に
よって洗浄されるように、オーバーフロー方式で行って
もよい。The step of dipping in the washing water may be performed by an overflow method so that the washing is always performed with a new solution.

【００４７】本発明の炭化ケイ素焼結体の湿式洗浄方法
おいて、被洗浄体としての炭化ケイ素焼結体は、半導体
各種部材及び電子部品に使用し得る高密度、高純度のも
のであれば、特に限定しないが、例えば、非金属助剤を
用いてホットプレス焼結した炭化ケイ素焼結体、本願出
願人が先に出願した特願平１０−６７５６５号に記載の
炭化ケイ素焼結体等が挙げられる。In the wet cleaning method of the silicon carbide sintered body of the present invention, the silicon carbide sintered body as the body to be cleaned is of high density and high purity which can be used for various semiconductor members and electronic parts. Although not particularly limited, for example, a silicon carbide sintered body obtained by hot press sintering using a non-metallic auxiliary agent, a silicon carbide sintered body described in Japanese Patent Application No. 10-67565 previously filed by the present applicant, etc. Is mentioned.

【００４８】本発明の炭化ケイ素焼結体の湿式洗浄方法
に用いられる装置及び器具としては、耐薬品性に優れる
塩化ビニル（ＰＶＣ）製が好適であり、特に高純度化処
理されたＰＶＣが好適である。超音波発生装置、及びヒ
ーター等は、その表面にテフロン加工を施したものが好
適である。As a device and a tool used in the wet cleaning method of the silicon carbide sintered body of the present invention, polyvinyl chloride (PVC) having excellent chemical resistance is preferable, and highly purified PVC is particularly preferable. It is. The ultrasonic generator, the heater, and the like are preferably those whose surfaces are subjected to Teflon processing.

【００４９】本発明の炭化ケイ素焼結体の湿式洗浄方法
によって得られた炭化ケイ素焼結体は、半導体各種部材
及び電子部品等に好適に使用することができるが、半導
体各種部材としては、ダミーウエハ、ヒーター、プラズ
マエッチング電極、イオン注入装置ターゲット等の高純
度及びパーティクルフリーが望まれる部材が挙げられ
る。The silicon carbide sintered body obtained by the wet cleaning method of the silicon carbide sintered body of the present invention can be suitably used for various semiconductor members and electronic parts. , A heater, a plasma etching electrode, an ion implantation target, etc., for which high purity and particle free are desired.

【００５０】[0050]

【実施例】以下に、本発明の実施例を示すが、本発明
は、これら実施例に何ら制限されない。（被洗浄体）以
下に示す実施例及びに用いた被洗浄体（炭化ケイ素焼結
体）は、全て同一の試料使用して評価した。この被洗浄
体は４０×４０×２ｔの平版である。この平版は片面は
粗研磨、もう一方の面は鏡面であり、洗浄前の表面清浄
度（不純物付着量）は、１×１０13〜１×１０16ａｔｏ
ｍｓ／ｃｍ2 であった。EXAMPLES Examples of the present invention will be described below, but the present invention is not limited to these examples. (Cleaning object) The cleaning object (silicon carbide sintered body) used in the following Examples and Examples was evaluated using the same sample. The object to be cleaned is a lithographic plate of 40 × 40 × 2t. This lithographic plate has one surface rough-polished and the other surface a mirror surface. The surface cleanliness (impurity adhesion amount) before cleaning is 1 × 10 13 to 1 × 10 16 at.
ms / cm 2 .

【００５１】（表面清浄度（不純物付着量）の測定）表
面清浄度（不純物付着量）の測定は、軽元素（Ｂ、Ｎ
ａ、Ａｌ）は、フッ硝酸及び硝酸を各１％含む水溶液を
用いて被洗浄体表面を洗い流して不純物を抽出し、この
水溶液をＩＣＰ−ＭＳ（「Ｉｎｄｕｃｔｉｖｅｌｙ Ｃ
ｏｕｐｌｅｄＰｌａｓｍａ Ｍａｓｓ Ｓｐｅｃｔｒｏ
ｍｅｔｅｒ（誘導結合プラズマ質量分析装置）」）で分
析した。その他の元素は、純水水溶液に浸漬、乾燥した
後、ＴＸＲＦ（「Ｔｏｔａｌ Ｒｅｆｌｅｃｔｉｏｎ
Ｘ−Ｒａｙ Ｆｌｕｏｒｅｓｃｅｎｃｅｍｅｔｅｒ（全
反射蛍光Ｘ線分析装置）」）で分析した。なお、ＴＸＲ
Ｆで分析する際、シリコンにおける相対感度係数を使用
した。また、ＩＣＰ−ＭＳ分析値とＴＸＲＦ分析値とが
ほぼ等しいことは、Ｋ、Ｃｒ、Ｆｅ、Ｎｉ、Ｃｕ、Ｚｎ
の分析値で確認している。(Measurement of Surface Cleanliness (Amount of Impurity)) The measurement of surface cleanliness (amount of impurities) was carried out using light elements (B, N).
a, Al) is obtained by rinsing the surface of an object to be cleaned by using an aqueous solution containing 1% each of hydrofluoric nitric acid and nitric acid to extract impurities, and extracting the aqueous solution by ICP-MS (“Inductively C”).
coupledPlasma Mass Spectro
meter (inductively coupled plasma mass spectrometer) "). Other elements are immersed in a pure water solution and dried, and then subjected to TXRF (“Total Reflection”).
X-Ray Fluorescence meter (total reflection X-ray fluorescence spectrometer) "). Note that TXR
When analyzing in F, the relative sensitivity coefficient in silicon was used. In addition, the fact that the ICP-MS analysis value and the TXRF analysis value are substantially equal indicates that K, Cr, Fe, Ni, Cu, Zn
Confirmed by the analysis value.

【００５２】〔実施例１〕被洗浄体を、準水系有機溶剤
（石油系炭化水素、有機酸エステル及びノニオン系界面
活性剤の混合溶剤）の原液に、５０℃で超音波（１００
Ｖ−２６±２ｋＨｚ）を照射しながら１５分浸漬し、水
濯ぎを行い、次にフッ硝酸水溶液（３８％フッ酸：６８
％硝酸：水＝１：１：２０）に３０分浸漬し、さらに純
水に浸漬した後、表面清浄度の測定を行った。被洗浄体
の表面清浄度は、８×１０9 〜１×１０11ａｔｏｍｓ／
ｃｍ2 であり、詳しくは表１に示す。また、上記各処理
は、準水系有機溶剤に浸漬する処理以外は、水溶液の温
度を、常温にして行った。Example 1 An object to be cleaned was placed in a stock solution of a quasi-aqueous organic solvent (a mixed solvent of petroleum hydrocarbons, organic acid esters and nonionic surfactants) at 50 ° C. with ultrasonic waves (100
(V-26 ± 2 kHz) for 15 minutes, rinsing with water, and then hydrofluoric / nitric acid aqueous solution (38% hydrofluoric acid: 68%).
% Nitric acid: water = 1: 1: 20) for 30 minutes, and further immersed in pure water, and then the surface cleanliness was measured. The surface cleanliness of the object to be cleaned is 8 × 10 9 to 1 × 10 11 atoms / s.
cm 2 , and details are shown in Table 1. In addition, each of the above treatments was carried out at a normal temperature of the aqueous solution except for the treatment of immersion in the semi-aqueous organic solvent.

【００５３】〔実施例２〕被洗浄体を、グリコールエー
テルに２０分浸漬し、４級アンモニウム塩水溶液に３０
分浸漬し、フッ硝酸水溶液（３８％フッ酸：６８％硝
酸：水＝１：１：２０）に３０分浸漬し、さらに純水に
浸漬した後、表面清浄度の測定を行った。被洗浄体の表
面清浄度は、８×１０9 〜９×１０10ａｔｏｍｓ／ｃｍ
2 であり、詳しくは表１に示す。また、上記各処理は、
溶剤、水溶液の温度を、常温にして行った。Example 2 A body to be cleaned was immersed in glycol ether for 20 minutes, and immersed in a quaternary ammonium salt aqueous solution for 30 minutes.
After immersion in a hydrofluoric / nitric acid aqueous solution (38% hydrofluoric acid: 68% nitric acid: water = 1: 1: 20) for 30 minutes, and further immersion in pure water, the surface cleanliness was measured. The surface cleanliness of the object to be cleaned is 8 × 10 9 to 9 × 10 10 atoms / cm.
2 and details are shown in Table 1. In addition, each of the above processes
The temperature of the solvent and the aqueous solution was set to normal temperature.

【００５４】〔実施例３〕実施例１において、各処理で
超音波（１００Ｖ−２６±２ｋＨｚ）を照射する以外
は、実施例１同様に処理した後、表面清浄度の測定を行
った。被洗浄体の表面清浄度は、８×１０9 〜９×１０
10ａｔｏｍｓ／ｃｍ2 であり、詳しくは表１に示す。Example 3 The procedure of Example 1 was repeated, except that ultrasonic waves (100 V-26 ± 2 kHz) were used for each treatment, and the surface cleanliness was measured. The surface cleanliness of the object to be cleaned is 8 × 10 9 to 9 × 10
It is 10 atoms / cm 2 , and details are shown in Table 1.

【００５５】〔実施例４〕実施例１において、各処理で
溶剤、水溶液の温度を、７０℃にした以外は、実施例１
同様に処理した後、表面清浄度の測定を行った。被洗浄
体の表面清浄度は、８×１０9 〜１×１０11ａｔｏｍｓ
／ｃｍ2 未満であり、詳しくは表１に示す。Example 4 Example 1 was repeated except that the temperature of the solvent and the aqueous solution was changed to 70 ° C. in each treatment.
After the same treatment, the surface cleanliness was measured. The surface cleanliness of the object to be cleaned is 8 × 10 9 to 1 × 10 11 atoms.
/ Cm 2 , and details are shown in Table 1.

【００５６】〔実施例５〕被洗浄体を、準水系有機溶剤
（石油系炭化水素、有機酸エステル及びノニオン系界面
活性剤の混合溶剤）の原液に、５０℃で超音波（１００
Ｖ−２６±２ｋＨｚ）を照射しながら１５分浸漬し、４
級アンモニウム塩水溶液に３０分浸漬し、フッ酸／硝酸
／硫酸水溶液（３８％フッ酸：６８％硝酸：９８％硫
酸：水＝１：１：１：２０）に３０分浸漬し、さらに純
水に浸漬した後、表面清浄度の測定を行った。被洗浄体
の表面清浄度は、４×１０9 〜９×１０10ａｔｏｍｓ／
ｃｍ2未満であり、ここで得られたＺｎ及びＣｒの分析
値はＴＸＲＦの検出下限値である。詳しくは表１に示
す。また、上記各処理は、準水系有機溶剤に浸漬する処
理以外は、水溶液の温度を、常温にして行った。Example 5 An object to be cleaned was placed in a stock solution of a quasi-aqueous organic solvent (mixed solvent of petroleum hydrocarbon, organic acid ester and nonionic surfactant) at 50 ° C. with ultrasonic waves (100
V-26 ± 2 kHz) for 15 minutes while irradiating
Immersion for 30 minutes in aqueous solution of quaternary ammonium salt, immersion for 30 minutes in aqueous solution of hydrofluoric acid / nitric acid / sulfuric acid (38% hydrofluoric acid: 68% nitric acid: 98% sulfuric acid: water = 1: 1: 1: 20), and further pure water After immersion, the surface cleanliness was measured. The surface cleanliness of the object to be cleaned is 4 × 10 9 to 9 × 10 10 atoms /
cm 2 , and the analysis values of Zn and Cr obtained here are the detection lower limit of TXRF. Details are shown in Table 1. In addition, each of the above treatments was carried out at a normal temperature of the aqueous solution except for the treatment of immersion in the semi-aqueous organic solvent.

【００５７】〔比較例１〕実施例１において、フッ硝酸
水溶液に浸漬しない以外は、実施例１同様に処理した
後、表面清浄度の測定を行った。被洗浄体の表面清浄度
は、１×１０11〜１×１０15ａｔｏｍｓ／ｃｍ2 未満で
あり、詳しくは表１に示す。Comparative Example 1 The procedure of Example 1 was repeated, except that the sample was not immersed in an aqueous solution of hydrofluoric / nitric acid. The surface cleanliness of the object to be cleaned is less than 1 × 10 11 to 1 × 10 15 atoms / cm 2 , and details are shown in Table 1.

【００５８】〔比較例２〕実施例１において、準水系有
機溶剤に浸漬しない以外は、実施例１同様に処理した
後、表面清浄度の測定を行った。被洗浄体の表面清浄度
は、１×１０10〜１×１０14ａｔｏｍｓ／ｃｍ2 未満で
あり、詳しくは表１に示す。Comparative Example 2 The same procedure as in Example 1 was carried out except that the substrate was not immersed in a quasi-aqueous organic solvent, and the surface cleanness was measured. The surface cleanliness of the object to be cleaned is less than 1 × 10 10 to 1 × 10 14 atoms / cm 2 , and details are shown in Table 1.

【００５９】[0059]

【表１】 [Table 1]

【００６０】表１より、本発明の炭化ケイ素焼結体の湿
式洗浄処理を行ったものは、半導体各種部材及び電子部
材に応用可能な、１×１０11ａｔｏｍｓ／ｃｍ2 未満の
レベルの表面洗浄度であることがわかる。特に硫酸を併
用した実施例５は、特にＡｌの除去に効果が表れた。From Table 1, it can be seen that the silicon carbide sintered body of the present invention subjected to the wet cleaning treatment has a surface cleaning level of less than 1 × 10 11 atoms / cm 2 applicable to various semiconductor members and electronic members. It turns out that it is a degree. In particular, Example 5 using sulfuric acid was particularly effective for removing Al.

【００６１】[0061]

【発明の効果】以上により、本発明は、炭化ケイ素焼結
体の表面及び表面近傍に存在する有機及び無機不純物
を、簡易に洗浄除去することができる炭化ケイ素焼結体
の湿式洗浄方法を提供することができる。As described above, the present invention provides a method for wet-cleaning a silicon carbide sintered body which can easily clean and remove organic and inorganic impurities existing on and near the surface of the silicon carbide sintered body. can do.

Claims (8)

【特許請求の範囲】[Claims] 【請求項１】 炭化ケイ素焼結体を、準水系有機溶剤に
浸漬する工程、無機酸水溶液に浸漬する工程、及び純水
に浸漬する工程、で順次処理することを特徴とする炭化
ケイ素焼結体の湿式洗浄方法。1. A method of sintering a silicon carbide sintered body in a step of dipping in a semi-aqueous organic solvent, a step of dipping in an inorganic acid aqueous solution, and a step of dipping in pure water. How to wet clean the body. 【請求項２】 炭化ケイ素焼結体を、準水系有機溶剤に
浸漬する工程、アンモニウム水溶液に浸漬する工程、無
機酸水溶液に浸漬する工程、及び純水に浸漬する工程、
で順次処理することを特徴とする炭化ケイ素焼結体の湿
式洗浄方法。2. a step of immersing the silicon carbide sintered body in a quasi-aqueous organic solvent, a step of immersing it in an aqueous ammonium solution, a step of immersing it in an aqueous inorganic acid solution, and a step of immersing it in pure water.
Wet cleaning method for a silicon carbide sintered body, characterized by sequentially treating the silicon carbide sintered body. 【請求項３】炭化ケイ素焼結体を、準水系有機溶剤に浸
漬する工程、無機酸水溶液に浸漬する工程、アンモニウ
ム水溶液に浸漬する工程、及び純水に浸漬する工程、で
順次処理することを特徴とする炭化ケイ素焼結体の湿式
洗浄方法。3. A process of immersing a silicon carbide sintered body in a quasi-aqueous organic solvent, a step of immersing in an inorganic acid aqueous solution, a step of immersing in an ammonium aqueous solution, and a step of immersing in pure water sequentially. A wet cleaning method for a silicon carbide sintered body. 【請求項４】 少なくとも１つの工程が、液に超音波振
動を加えながら行うことを特徴とする請求項１〜３のい
ずれかに記載の炭化ケイ素焼結体の湿式洗浄方法。4. The wet cleaning method for a silicon carbide sintered body according to claim 1, wherein at least one step is performed while applying ultrasonic vibration to the liquid. 【請求項５】 少なくとも１つの工程の液の温度が、３
０℃以上であることを特徴とする請求項１〜４のいずれ
かに記載の炭化ケイ素焼結体の湿式洗浄方法。5. The method according to claim 1, wherein the temperature of the liquid in at least one step is 3
The method for wet-cleaning a silicon carbide sintered body according to claim 1, wherein the temperature is 0 ° C. or higher. 【請求項６】 準水系有機溶剤が、石油系炭化水素、有
機酸エステル、及びグリコールエーテル、これらの混合
溶剤、又はこれら溶剤或いは混合溶剤と界面活性剤との
混合物であることを特徴とする請求項１〜５のいずれか
に記載の炭化ケイ素焼結体の湿式洗浄方法。6. The quasi-aqueous organic solvent is a petroleum hydrocarbon, an organic acid ester, a glycol ether, a mixed solvent thereof, or a mixture of these solvents or a mixed solvent and a surfactant. Item 6. The wet cleaning method for a silicon carbide sintered body according to any one of Items 1 to 5. 【請求項７】 無機酸水溶液が、フッ酸水溶液、硝酸水
溶液、硫酸水溶液、塩酸、過酸化水素水、オゾン水、又
はこれらの混合酸水溶液であることを特徴とする請求項
１〜６のいずれかに記載の炭化ケイ素焼結体の湿式洗浄
方法。7. The method according to claim 1, wherein the inorganic acid aqueous solution is a hydrofluoric acid aqueous solution, a nitric acid aqueous solution, a sulfuric acid aqueous solution, a hydrochloric acid, a hydrogen peroxide solution, an ozone water, or a mixed acid aqueous solution thereof. A wet cleaning method for a silicon carbide sintered body according to any one of the above. 【請求項８】 アンモニウム水溶液が、ハロゲン化テト
ラアルキルアンモニウム水溶液、過塩素酸テトラアルキ
ルアンモニウム水溶液、アンモニア水、又はこれらと過
酸化水素水との混合水溶液であること特徴とする請求項
２〜７のいずれかに記載の炭化ケイ素焼結体の湿式洗浄
方法。8. The method according to claim 2, wherein the aqueous ammonium solution is an aqueous solution of a tetraalkylammonium halide, an aqueous solution of a tetraalkylammonium perchlorate, aqueous ammonia, or a mixed aqueous solution of these and an aqueous solution of hydrogen peroxide. The wet cleaning method for a silicon carbide sintered body according to any one of the above.
JP34870198A 1998-12-08 1998-12-08 Wet cleaning method for sintered silicon carbide Expired - Lifetime JP4188473B2 (en)

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US09/449,764 US6419757B2 (en) 1998-12-08 1999-11-26 Method for cleaning sintered silicon carbide in wet condition

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