JP2001345301A - How to clean electronic materials - Google Patents
How to clean electronic materialsInfo
- Publication number
- JP2001345301A JP2001345301A JP2000162206A JP2000162206A JP2001345301A JP 2001345301 A JP2001345301 A JP 2001345301A JP 2000162206 A JP2000162206 A JP 2000162206A JP 2000162206 A JP2000162206 A JP 2000162206A JP 2001345301 A JP2001345301 A JP 2001345301A
- Authority
- JP
- Japan
- Prior art keywords
- cleaning
- wafer
- hydrogen
- dissolved
- fine particles
- 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
Links
- 239000012776 electronic material Substances 0.000 title claims abstract description 30
- 238000004140 cleaning Methods 0.000 claims abstract description 84
- 239000001257 hydrogen Substances 0.000 claims abstract description 43
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 39
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 39
- 239000012498 ultrapure water Substances 0.000 claims abstract description 39
- 239000007789 gas Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000001301 oxygen Substances 0.000 claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 21
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 2
- 239000003513 alkali Substances 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 239000010419 fine particle Substances 0.000 abstract description 35
- 239000000126 substance Substances 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002923 metal particle Substances 0.000 abstract description 2
- 231100000167 toxic agent Toxicity 0.000 abstract description 2
- 239000003440 toxic substance Substances 0.000 abstract description 2
- 239000013317 conjugated microporous polymer Substances 0.000 abstract 1
- 235000012431 wafers Nutrition 0.000 description 52
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 28
- 239000011591 potassium Substances 0.000 description 28
- 229910052700 potassium Inorganic materials 0.000 description 28
- 125000004429 atom Chemical group 0.000 description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 22
- 150000002431 hydrogen Chemical class 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 17
- 238000005406 washing Methods 0.000 description 17
- 239000002245 particle Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 239000012528 membrane Substances 0.000 description 8
- 238000005498 polishing Methods 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 229910052756 noble gas Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000005380 borophosphosilicate glass Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Cleaning By Liquid Or Steam (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
(57)【要約】
【課題】ＣＭＰ後の洗浄工程において、濃厚な薬液や毒
物指定を受けている薬品を使うことなく、金属及び微粒
子を同時に、短時間で、安価に、効果的に被洗浄物から
除去することができる汎用性の高い電子材料の洗浄方法
を提供する。
【解決手段】ＣＭＰを行った後の電子材料の洗浄方法で
あって、水素、酸素又は希ガスを溶解した４５℃以上の
超純水を洗浄液とし、この洗浄液に１０kHz〜３MHzの超
音波を照射しながら洗浄することを特徴とする電子材料
の洗浄方法。(57) [Summary] In a cleaning process after CMP, metal and fine particles can be effectively and simultaneously cleaned in a short time, at a low cost, without using a concentrated chemical solution or a chemical designated as a toxicant. Provided is a highly versatile method for cleaning an electronic material that can be removed from an object. A method of cleaning an electronic material after performing CMP, wherein ultrapure water of 45 ° C. or higher in which hydrogen, oxygen, or a rare gas is dissolved is used as a cleaning liquid, and the cleaning liquid is irradiated with ultrasonic waves of 10 kHz to 3 MHz. A method for cleaning an electronic material, wherein the cleaning is performed while performing the cleaning.
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、電子材料の洗浄方
法に関する。さらに詳しくは、本発明は、ＣＭＰ（化学
機械研磨、Ｃｈｅｍｉｃａｌ Ｍｅｃｈａｎｉｃａｌ Ｐ
ｏｌｉｓｈｉｎｇ）後の電子材料の表面に付着した金属
不純物及び残留した研磨剤などの微粒子を、ウェット洗
浄により同時に、かつ、効果的に除去することができる
電子材料の洗浄方法に関する。The present invention relates to a method for cleaning electronic materials. More specifically, the present invention relates to CMP (Chemical Mechanical Polishing, Chemical Mechanical P
The present invention relates to a method for cleaning an electronic material, which can remove metal impurities and fine particles such as a residual abrasive adhered to the surface of the electronic material after the polishing simultaneously and effectively by wet cleaning.
【０００２】[0002]
【従来の技術】従来は、半導体産業の洗浄工程において
は、ＲＣＡ洗浄と呼ばれるウェット洗浄が主流であっ
た。ＲＣＡ洗浄は、硫酸と過酸化水素水の混合液（ＳＰ
Ｍ）を１２０〜１５０℃に加熱して用いたり、アンモニ
アと過酸化水素水の混合液（ＡＰＭ）を６０〜８０℃に
加温して用いたり、あるいは、塩酸と過酸化水素水の混
合液（ＨＰＭ）を６０〜８０℃に加温して用いたりする
洗浄方法である。この洗浄方法を採用した場合の多大な
薬液コスト、リンス用の超純水のコスト、廃液処理コス
ト、薬品蒸気を排気し新たに清浄空気を作る空調コスト
などを低減し、さらに水の大量使用、薬品の大量廃棄、
排ガスの放出などの環境への負荷を低減するために、近
年ウェット洗浄工程の見直しが進められている。また、
近年の半導体産業では、集積度の向上のためにウェハ上
に配線を集積させることが行われている。多層配線を行
うために酸化膜（絶縁膜）を平坦化する必要があり、そ
のための手法としてＣＭＰが半導体デバイス製造工程に
採用されてきている。このＣＭＰ工程では、水酸化カリ
ウム（ＫＯＨ）水溶液などのカリウムを含む溶液に、シ
リカ（ＳｉＯ2）などの研磨粒子を分散させた研磨液を
用いて研磨する。ところが、化学気相堆積法（ＣＶＤ、
Ｃｈｅｍｉｃａｌ Ｖａｐｏｒ Ｄｅｐｏｓｉｔｉｏｎ）
などで堆積した酸化膜を、前述の研磨液を用いて研磨す
ると、カリウム（Ｋ）がウェハ上に残留しやすいという
問題が明らかになってきた。カリウムがウェハ上に残留
すると、デバイス特性に影響を与えるために、洗浄で取
り除く必要がある。また、研磨剤の微粒子もウェハ上に
残留するために、洗浄により除去する必要がある。これ
までのＣＭＰ後の洗浄では、カリウムなどの金属除去と
微粒子除去を行うために、複数の洗浄工程を経るのが一
般的であった。例を挙げると、(１)超純水リンス → ブ
ラシスクラブ洗浄 → ＡＰＭ＋超音波 → 超純水リンス
→ ＨＦ → 超純水リンス → 乾燥、(２)温超純水 →
ＡＰＭ＋超音波 → 第一超純水リンス → 第二超純水リ
ンス→ 乾燥、(３)ブラシスクラブ洗浄 → ＨＦ → 超
純水リンス → 乾燥などの洗浄工程である。(１)、(２)
の方法では、大量の薬液を使用すること、薬品蒸気が出
ること、すすぐために大量の超純水を使用すること、生
産性が低いこと、洗浄工程が多いことなどの問題があ
る。また、(１)、(３)の方法では、毒物取締法で規制さ
れているフッ酸廃液が発生するために、廃液処理に莫大
なコストがかかるなどの問題がある。2. Description of the Related Art Conventionally, in the cleaning process of the semiconductor industry, wet cleaning called RCA cleaning has been mainly used. RCA cleaning is performed using a mixture of sulfuric acid and hydrogen peroxide (SP
M) is heated to 120 to 150 ° C., a mixture of ammonia and hydrogen peroxide (APM) is heated to 60 to 80 ° C., or a mixture of hydrochloric acid and hydrogen peroxide is used. This is a cleaning method in which (HPM) is heated to 60 to 80 ° C. and used. If this cleaning method is adopted, the cost of chemicals, the cost of ultrapure water for rinsing, the cost of waste liquid treatment, the cost of air conditioning that exhausts chemical vapors and creates clean air, etc. are reduced, and the use of large amounts of water is reduced. Mass disposal of chemicals,
In order to reduce the load on the environment such as emission of exhaust gas, the wet cleaning process has recently been reviewed. Also,
In recent years, in the semiconductor industry, wiring is integrated on a wafer in order to improve the degree of integration. It is necessary to planarize an oxide film (insulating film) in order to perform multilayer wiring, and CMP has been adopted in a semiconductor device manufacturing process as a technique for that. In this CMP step, polishing is performed using a polishing liquid in which polishing particles such as silica (SiO 2 ) are dispersed in a solution containing potassium such as an aqueous potassium hydroxide (KOH) solution. However, chemical vapor deposition (CVD,
Chemical Vapor Deposition
When the oxide film deposited by the above method is polished using the above-mentioned polishing liquid, the problem that potassium (K) tends to remain on the wafer has become apparent. If potassium remains on the wafer, it must be removed by cleaning because it affects device characteristics. Further, since fine particles of the abrasive remain on the wafer, they need to be removed by cleaning. Conventional cleaning after CMP generally involves a plurality of cleaning steps in order to remove metals such as potassium and fine particles. For example, (1) ultrapure water rinse → brush scrub cleaning → APM + ultrasonic → ultrapure water rinse → HF → ultrapure water rinse → drying, (2) warm ultrapure water →
APM + ultrasonic wave → first ultrapure water rinse → second ultrapure water rinse → drying, (3) brush scrub cleaning → HF → ultrapure water rinse → drying etc. (1), (2)
The method of (1) has a problem that a large amount of a chemical solution is used, a large amount of chemical vapor is generated, a large amount of ultrapure water is used for rinsing, productivity is low, and a number of cleaning steps are required. Further, the methods (1) and (3) have a problem that a huge cost is required for waste liquid treatment because a hydrofluoric acid waste liquid regulated by the Poison Control Law is generated.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、ＣＭＰ後の
洗浄工程において、濃厚な薬液や毒物指定を受けている
薬品を使うことなく、金属及び微粒子を同時に、短時間
で、安価に、効果的に被洗浄物から除去することができ
る汎用性の高い電子材料の洗浄方法を提供することを目
的としてなされたものである。DISCLOSURE OF THE INVENTION The present invention is an object of the present invention is to provide a method for cleaning metal and fine particles simultaneously, in a short time, at low cost, without using a concentrated chemical solution or a chemical which has been designated as a toxicant in a cleaning step after CMP. An object of the present invention is to provide a highly versatile method for cleaning electronic materials that can be removed from an object to be cleaned.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、上記の課
題を解決すべく鋭意研究を重ねた結果、４５℃以上に加
温した温超純水で洗浄することにより、ＣＶＤ酸化膜上
に付着したカリウムを容易に除去することができ、さら
に、超純水に水素などのガスを溶解することにより、カ
リウムなどの金属不純物と微粒子を同時に除去し得るこ
とを見いだし、この知見に基づいて本発明を完成するに
至った。すなわち、本発明は、（１）ＣＭＰを行った後
の電子材料の洗浄方法であって、水素、酸素又は希ガス
を溶解した４５℃以上の超純水を洗浄液とし、この洗浄
液に１０kHz〜３MHzの超音波を照射しながら洗浄するこ
とを特徴とする電子材料の洗浄方法、及び、（２）洗浄
液にアルカリが添加されている第１項記載の電子材料の
洗浄方法、を提供するものである。さらに、本発明の好
ましい態様として、（３）水素、酸素又は希ガスの溶存
ガス濃度が、飽和溶解度の５０％以上である第１項記載
の電子材料の洗浄方法、及び、（４）アルカリが、アン
モニア又は水酸化テトラメチルアンモニウムである第２
項記載の電子材料の洗浄方法、を挙げることができる。Means for Solving the Problems The inventors of the present invention have conducted intensive studies to solve the above-mentioned problems, and as a result, they have been found to adhere to the CVD oxide film by cleaning with warm ultrapure water heated to 45 ° C. or more. It has been found that potassium can be easily removed, and furthermore, by dissolving a gas such as hydrogen in ultrapure water, metal impurities such as potassium and fine particles can be removed at the same time. Was completed. That is, the present invention relates to (1) a method for cleaning an electronic material after performing CMP, wherein ultrapure water at 45 ° C. or higher in which hydrogen, oxygen, or a rare gas is dissolved is used as a cleaning liquid, and the cleaning liquid has a frequency of 10 kHz to 3 MHz. And (2) the method for cleaning an electronic material according to claim 1, wherein an alkali is added to the cleaning solution. . Further, as preferred embodiments of the present invention, (3) the method for cleaning an electronic material according to (1), wherein the dissolved gas concentration of hydrogen, oxygen, or a rare gas is 50% or more of the saturation solubility; , Ammonia or tetramethylammonium hydroxide
And a method for cleaning an electronic material described in the section.
【０００５】[0005]
【発明の実施の形態】本発明の電子材料の洗浄方法は、
ＣＭＰを行った後の電子材料の洗浄方法であって、水
素、酸素又は希ガスを溶解した４５℃以上の超純水を洗
浄液として洗浄する。この温度が４５℃未満では十分な
洗浄効果が得られない。洗浄効果の点から、６０℃以上
であることが好ましく、８０℃以上であることがより好
ましい。本発明方法は、ＣＶＤ酸化膜工程を経た後にＣ
ＭＰを行った半導体基板の洗浄に特に好適に適用するこ
とができる。ＣＶＤ酸化膜としては、例えば、Ｐ−ＴＥ
ＯＳ（Ｐｌａｓｍａ ｅｎｈａｎｃｅｄ ｔｅｔｒａｅｔ
ｈｙｌｏｒｔｈｏｓｌｉｃａｔｅ）酸化膜、ＢＰＳＧ
（Ｂｏｒｏｎ−ｄｏｐｅｄ ｐｈｏｓｐｈｏ−ｓｉｌｉ
ｃａｔｅ Ｇｌａｓｓ）酸化膜、ＮＳＧ（Ｎｏｎ−ｄｏ
ｐｅｄ ｓｉｌｉｃａｔｅ Ｇｌａｓｓ）酸化膜、ＴＭＳ
（Ｐｌａｓｍａ ｅｎｈａｎｃｅｄ ｔｅｔｒａｍｅｔｈ
ｏｘｙｓｉｌａｎｅ）酸化膜などを挙げることができ
る。電子材料のＣＭＰには、水酸化カリウムなどのアル
カリと、シリカ、セリア、アルミナなどの微粒子を含有
する研磨液が用いられるので、ＣＭＰ後の電子材料の表
面には、研磨液に由来するカリウムなどの金属不純物
と、シリカなどの微粒子が付着している。水素、酸素又
は希ガスを溶解した超純水の温度が４５℃以上である
と、電子材料の表面に付着した金属不純物を効果的に除
去することができる。BEST MODE FOR CARRYING OUT THE INVENTION A method for cleaning an electronic material according to the present invention comprises:
This is a method of cleaning an electronic material after performing CMP, in which ultrapure water at 45 ° C. or higher in which hydrogen, oxygen, or a rare gas is dissolved is used as a cleaning liquid. If the temperature is lower than 45 ° C., a sufficient cleaning effect cannot be obtained. From the viewpoint of the cleaning effect, the temperature is preferably 60 ° C. or higher, more preferably 80 ° C. or higher. According to the method of the present invention, the C
It can be particularly suitably applied to cleaning of a semiconductor substrate on which MP has been performed. As the CVD oxide film, for example, P-TE
OS (Plasma enhanced tetraet)
hyorthoslicate) oxide film, BPSG
(Boron-doped phospho-sili
Cat Glass (Oxide), NSG (Non-do)
ped silica glass) Oxide film, TMS
(Plasma enhanced tetrametry
oxysilane) oxide film and the like. Since a polishing liquid containing an alkali such as potassium hydroxide and fine particles such as silica, ceria, and alumina is used for the CMP of the electronic material, the surface of the electronic material after the CMP contains potassium derived from the polishing liquid. Metal impurities and fine particles such as silica. When the temperature of ultrapure water in which hydrogen, oxygen, or a rare gas is dissolved is 45 ° C. or higher, metal impurities attached to the surface of the electronic material can be effectively removed.
【０００６】本発明方法において、水素、酸素又は希ガ
スを溶解した４５℃以上の超純水の製造方法に特に制限
はなく、例えば、４５℃以上に加温された温超純水に水
素、酸素又は希ガスを溶解することができ、あるいは、
水素、酸素又は希ガスを溶解した超純水を４５℃以上に
加温することもできる。本発明方法において、洗浄液中
における水素、酸素又は希ガスの濃度に特に制限はない
が、溶存ガス濃度が、洗浄液の温度における飽和溶解度
の５０％以上であることが好ましく、７５％以上である
ことがより好ましい。ちなみに、６０℃における水への
飽和溶解度は、水素１.４３mg／Ｌ、酸素２７.９mg／
Ｌ、ヘリウム１.５９mg／Ｌ、ネオン８.５１mg／Ｌ、ア
ルゴン３７.０mg／Ｌ、クリプトン１２３mg／Ｌ、キセ
ノン２９３mg／Ｌである。水素、酸素又は希ガスは、１
種を単独で超純水に溶解することができ、あるいは、２
種以上を組み合わせて超純水に溶解することもできる。
本発明方法に用いる水素、酸素又は希ガスを溶解した超
純水の製造方法に特に制限はないが、あらかじめ超純水
を脱気して溶存気体の飽和度を下げ、水中の気体溶解キ
ャパシティーに空きを作ったのち、水素、酸素又は希ガ
スを溶解することが好ましい。水素、酸素又は希ガスの
溶解に際しては、気体透過膜モジュールを多段に用いて
溶存気体の除去及び水素、酸素又は希ガスの溶解を行う
ことができる。例えば、気体透過膜モジュールを２段に
設け、前段の気体透過膜モジュールを用いて全溶存気体
を対象とする減圧膜脱気を行い、後段の気体透過膜モジ
ュールを用いて水素、酸素又は希ガスを溶解することが
できる。気体透過膜モジュールを２段に設けて、全溶存
気体を対象とする減圧膜脱気と水素、酸素又は希ガスの
溶解を２段に行うことにより、水素、酸素又は希ガスを
無駄に放出することなく、ほぼ定量的に超純水に溶解す
ることができる。In the method of the present invention, there is no particular limitation on the method for producing ultrapure water at 45 ° C. or higher in which hydrogen, oxygen or a rare gas is dissolved. For example, hydrogen, oxygen or Noble gas can be dissolved, or
Ultrapure water in which hydrogen, oxygen, or a rare gas is dissolved can be heated to 45 ° C. or higher. In the method of the present invention, the concentration of hydrogen, oxygen or a rare gas in the cleaning solution is not particularly limited, but the dissolved gas concentration is preferably 50% or more of the saturation solubility at the temperature of the cleaning solution, and is preferably 75% or more. Is more preferred. Incidentally, the saturated solubility in water at 60 ° C. was 1.43 mg / L for hydrogen and 27.9 mg / oxygen for oxygen.
L, helium 1.59 mg / L, neon 8.51 mg / L, argon 37.0 mg / L, krypton 123 mg / L, xenon 293 mg / L. Hydrogen, oxygen or noble gas is 1
The seed alone can be dissolved in ultrapure water, or
A combination of more than one species can be dissolved in ultrapure water.
There is no particular limitation on the method of producing ultrapure water in which hydrogen, oxygen or a rare gas is dissolved used in the method of the present invention, but the ultrapure water is degassed in advance to reduce the degree of saturation of the dissolved gas, and the gas dissolution capacity in water is reduced. It is preferable to dissolve hydrogen, oxygen or a rare gas after making an empty space. When dissolving hydrogen, oxygen, or a rare gas, gas-permeable membrane modules can be used in multiple stages to remove dissolved gas and dissolve hydrogen, oxygen, or a rare gas. For example, a gas permeable membrane module is provided in two stages, a reduced-pressure membrane degassing is performed on all dissolved gases using the gas permeable membrane module in the preceding stage, and hydrogen, oxygen or a rare gas is used in the gas permeable membrane module in the subsequent stage. Can be dissolved. A gas permeable membrane module is provided in two stages, and decompression membrane degassing for all dissolved gases and dissolution of hydrogen, oxygen, or a rare gas are performed in two stages, so that hydrogen, oxygen, or a rare gas is wastefully released. Without being dissolved, it can be almost quantitatively dissolved in ultrapure water.
【０００７】本発明方法においては、水素、酸素又は希
ガスを溶解した超純水に、アルカリを添加することによ
り、pHを７以上に調整して使用することができる。アル
カリを添加することにより、ウェハ表面に付着した研磨
剤などの微粒子の除去効果と再付着防止効果を高めるこ
とができる。pH調整に使用するアルカリには特に制限は
なく、例えば、アンモニア、水酸化ナトリウム、水酸化
カリウム、水酸化テトラメチルアンモニウム（ＴＭＡ
Ｈ）などを挙げることができる。これらの中で、高純度
アンモニア水及び水酸化テトラメチルアンモニウムを好
適に使用することができる。本発明方法において、ＣＭ
Ｐを行った後の電子材料を、水素、酸素又は希ガスを溶
解した超純水を洗浄液として洗浄する方法に特に制限は
なく、例えば、洗浄液を満たした水槽に電子材料を浸漬
してバッチ式処理を行うことができ、あるいは、電子材
料をスピンナーやローダー上に載せ、洗浄液を電子材料
の中心から半径方向に注いで処理する枚葉式洗浄を行う
こともできる。本発明方法においては、水素、酸素又は
希ガスを溶解した４５℃以上の超純水を洗浄液として電
子材料を洗浄する際に、超音波を照射することが必要で
ある。超音波を照射することにより、研磨剤などの微粒
子の除去効果を高めることができる。照射する超音波
は、周波数１０kHz〜３MHzであり、好ましくは、０.８M
Hz〜１.６MHzである。超音波の周波数が１０kHz未満で
あると、キャビテーション効果により、極めて微細な加
工が施された電子材料に損傷を与えるおそれがある。超
音波の周波数が３MHzを超えると、キャビテーションが
起きず、洗浄効果が認められない。本発明の電子材料の
洗浄方法によれば、ＣＭＰを行った後の電子材料の表面
に付着しているカリウムなどの金属不純物と残留研磨剤
などの微粒子を、１工程の洗浄により同時に短時間で除
去することができる。In the method of the present invention, the pH can be adjusted to 7 or more by adding an alkali to ultrapure water in which hydrogen, oxygen or a rare gas is dissolved. By adding the alkali, the effect of removing fine particles such as abrasives attached to the wafer surface and the effect of preventing re-adhesion can be enhanced. The alkali used for pH adjustment is not particularly limited. For example, ammonia, sodium hydroxide, potassium hydroxide, tetramethylammonium hydroxide (TMA
H) and the like. Among them, high-purity aqueous ammonia and tetramethylammonium hydroxide can be preferably used. In the method of the present invention, the CM
There is no particular limitation on the method of cleaning the electronic material after performing P with ultrapure water in which hydrogen, oxygen or a rare gas is dissolved as a cleaning liquid. For example, a method in which the electronic material is immersed in a water tank filled with the cleaning liquid and batch-cleaned. Processing can be performed, or single-wafer cleaning in which an electronic material is placed on a spinner or a loader and a cleaning liquid is poured in a radial direction from the center of the electronic material to perform the processing can be performed. In the method of the present invention, it is necessary to irradiate ultrasonic waves when cleaning an electronic material using ultrapure water at 45 ° C. or higher in which hydrogen, oxygen or a rare gas is dissolved as a cleaning liquid. Irradiation of ultrasonic waves can enhance the effect of removing fine particles such as abrasives. The ultrasonic wave to be irradiated has a frequency of 10 kHz to 3 MHz, preferably 0.8 M
Hz to 1.6 MHz. If the frequency of the ultrasonic wave is less than 10 kHz, there is a possibility that the cavitation effect may damage an extremely finely processed electronic material. When the frequency of the ultrasonic wave exceeds 3 MHz, cavitation does not occur and the cleaning effect is not recognized. According to the method for cleaning an electronic material of the present invention, metal impurities such as potassium and fine particles such as a residual abrasive adhered to the surface of the electronic material after the CMP are simultaneously performed in a short time by one-step cleaning. Can be removed.
【０００８】[0008]
【実施例】以下に、実施例を挙げて本発明をさらに詳細
に説明するが、本発明はこれらの実施例によりなんら限
定されるものではない。なお、実施例及び比較例におい
ては、ＣＶＤ酸化膜付きウェハとして、Ｐ−ＴＥＯＳ膜
付き６インチウェハを用いた。ＣＭＰ工程後及び洗浄後
のウェハ上のカリウム濃度は、全反射蛍光Ｘ線分析装置
［(株)リガク、ＴＸＲＦ３７５０］を用いて測定した。
微粒子数は、レーザー散乱異物検査装置［トプコン
(株)、ＷＭ−１５００］を用い、粒径０.２０μｍ以上
の微粒子を計数した。ウェハの洗浄には、スピン洗浄機
［(株)カナメックス、ＷＳＣ−２００ＭＳ］を用い、超
音波付与ノズル［本多電子(株)、パルスジェットＷ−３
５７Ｐ２５−ＡＨＰＦ］により１.０MHzの超音波を照射
した。 実施例１ 温超純水供給装置［栗田工業(株)］より供給された６０
℃の温超純水を原水として、膜溶解方式の水素水製造装
置［栗田工業(株)］で水素を溶解し、溶存水素濃度１.
２mg／Ｌの水素水を製造し、スピン洗浄機へ送水して、
超音波を照射しながらウェハに噴射洗浄した。洗浄前の
ウェハ上のカリウム濃度は４３.２×１０10原子／cm2で
あり、微粒子数は測定上限値の５,５００個／ウェハを
超えていた。洗浄液流量１Ｌ／分、洗浄時間３０秒の洗
浄により、ウェハ上のカリウム濃度は７.２１×１０10
原子／cm2、微粒子数は５７個／ウェハとなった。 実施例２ 温度６０℃、溶存水素濃度１.２mg／Ｌの水素水に、ア
ンモニア１mg／Ｌを添加してpHを９.４に調整した洗浄
液を用い、実施例１と同様にして洗浄を行った。ウェハ
上のカリウム濃度は、４９.１×１０10原子／cm2から
９.３３×１０10原子／cm2に減少し、微粒子数は５,５
００個／ウェハ以上から３６個／ウェハに減少した。 実施例３ 洗浄時間を６０秒とした以外は、実施例１と同様にして
洗浄を行った。ウェハ上のカリウム濃度は、４０.２×
１０10原子／cm2から検出下限値の３.１１×１０10原子
／cm2以下に減少し、微粒子数は５,５００個／ウェハ以
上から２１個／ウェハに減少した。 実施例４ 洗浄時間を６０秒とした以外は、実施例２と同様にして
洗浄を行った。ウェハ上のカリウム濃度は、４１.３×１
０10原子／cm2から３.１１×１０10原子／cm2以下に減
少し、微粒子数は５,５００個／ウェハ以上から１７個
／ウェハに減少した。EXAMPLES The present invention will be described in more detail with reference to the following Examples, which should not be construed as limiting the present invention. In Examples and Comparative Examples, a 6-inch wafer with a P-TEOS film was used as the wafer with a CVD oxide film. The potassium concentration on the wafer after the CMP step and after the cleaning was measured using a total reflection X-ray fluorescence analyzer [Rigaku Corporation, TXRF3750].
The number of fine particles can be measured using a laser scattering particle inspection device [Topcon
Using WM-1500], the fine particles having a particle size of 0.20 μm or more were counted. For cleaning the wafer, a spin cleaning machine [Kanamex Corporation, WSC-200MS] was used, and an ultrasonic wave application nozzle [Honda Electronics Co., Ltd., Pulse Jet W-3]
57P25-AHPF] to irradiate an ultrasonic wave of 1.0 MHz. Example 1 60 supplied from a hot ultrapure water supply device [Kurita Kogyo Co., Ltd.]
Using ultra-pure water at a temperature of ℃ as raw water, hydrogen is dissolved in a hydrogen water production system using a membrane dissolution method [Kurita Kogyo Co., Ltd.], and the dissolved hydrogen concentration is 1.
Produce 2 mg / L hydrogen water, send it to the spin washer,
The wafer was spray-cleaned while being irradiated with ultrasonic waves. The potassium concentration on the wafer before cleaning was 43.2 × 10 10 atoms / cm 2 , and the number of fine particles exceeded the upper limit of measurement of 5,500 particles / wafer. By cleaning with a cleaning liquid flow rate of 1 L / min and a cleaning time of 30 seconds, the potassium concentration on the wafer is 7.21 × 10 10
The number of atoms / cm 2 and the number of fine particles were 57 / wafer. Example 2 Washing was carried out in the same manner as in Example 1 using a washing solution adjusted to pH 9.4 by adding 1 mg / L of ammonia to hydrogen water having a temperature of 60 ° C. and a dissolved hydrogen concentration of 1.2 mg / L. Was. The potassium concentration on the wafer was reduced from 49.1 × 10 10 atoms / cm 2 to 9.33 × 10 10 atoms / cm 2 and the number of fine particles was 5.5
It was reduced from more than 00 wafers / wafer to 36 wafers / wafer. Example 3 The cleaning was performed in the same manner as in Example 1 except that the cleaning time was set to 60 seconds. The potassium concentration on the wafer is 40.2 ×
The number of particles decreased from 10 10 atoms / cm 2 to the lower limit of detection of 3.11 × 10 10 atoms / cm 2 or less, and the number of fine particles decreased from 5,500 particles / wafer or more to 21 particles / wafer. Example 4 The cleaning was performed in the same manner as in Example 2 except that the cleaning time was changed to 60 seconds. The potassium concentration on the wafer was 41.3 × 1
The particle number was reduced from 0 10 atoms / cm 2 to 3.11 × 10 10 atoms / cm 2 or less, and the number of fine particles was reduced from 5,500 particles / wafer or more to 17 particles / wafer.
【０００９】実施例５ 温超純水の温度を８０℃とし、溶存水素濃度０.８mg／
Ｌの水素水を製造した以外は、実施例１と同様にして洗
浄を行った。ウェハ上のカリウム濃度は、４５.４×１
０10原子／cm2から検出下限値の３.１１×１０10原子／
cm2以下に減少し、微粒子数は測定上限値の５,５００個
／ウェハ以上から２９個／ウェハに減少した。 実施例６ 水素水に、アンモニア１mg／Ｌを添加してpHを９.４に
調整した以外は、実施例５と同様にして洗浄を行った。
ウェハ上のカリウム濃度は、４２.２×１０10原子／cm2
から３.１１×１０10原子／cm2以下に減少し、微粒子数
は５,５００個／ウェハ以上から９個／ウェハに減少し
た。 実施例７ 洗浄時間を６０秒とした以外は、実施例５と同様にして
洗浄を行った。ウェハ上のカリウム濃度は、４３.８×
１０10原子／cm2から３.１１×１０10原子／cm2以下に
減少し、微粒子数は５,５００個／ウェハ以上から１６
個／ウェハに減少した。 実施例８ 洗浄時間を６０秒とした以外は、実施例６と同様にして
洗浄を行った。ウェハ上のカリウム濃度は、４６.５×１
０10原子／cm2から３.１１×１０10原子／cm2以下に減
少し、微粒子数は５,５００個／ウェハ以上から５個／
ウェハに減少した。Example 5 The temperature of ultra pure water was set to 80 ° C., and the dissolved hydrogen concentration was 0.8 mg /
The cleaning was performed in the same manner as in Example 1 except that L hydrogen water was produced. The potassium concentration on the wafer was 45.4 × 1
From 0 10 atoms / cm 2 to the lower limit of detection, 3.11 × 10 10 atoms / cm 2
cm 2 or less, and the number of fine particles was reduced from the upper limit of measurement of 5,500 particles / wafer to 29 particles / wafer. Example 6 Washing was performed in the same manner as in Example 5 except that the pH was adjusted to 9.4 by adding 1 mg / L of ammonia to hydrogen water.
The potassium concentration on the wafer is 42.2 × 10 10 atoms / cm 2
From 3.11 × 10 10 atoms / cm 2 or less, and the number of fine particles decreased from more than 5,500 / wafer to 9 / wafer. Example 7 The cleaning was performed in the same manner as in Example 5, except that the cleaning time was changed to 60 seconds. The potassium concentration on the wafer was 43.8 ×
It is reduced from 10 10 atoms / cm 2 to 3.11 × 10 10 atoms / cm 2 or less, and the number of fine particles is increased from 5,500 particles / wafer or more to 16
Reduced to pieces / wafer. Example 8 The cleaning was performed in the same manner as in Example 6, except that the cleaning time was 60 seconds. The potassium concentration on the wafer was 46.5 × 1
From 0 10 atoms / cm 2 to 3.11 × 10 10 atoms / cm 2 or less, and the number of fine particles is from 5,500 / wafer or more to 5 /
Reduced to wafer.
【００１０】比較例１ 超純水製造装置［栗田工業(株)］より供給された２５℃
の超純水を原水として、膜溶解方式の水素水製造装置
［栗田工業(株)］で水素を溶解し、溶存水素濃度１.２m
g／Ｌの水素水を製造し、スピン洗浄機へ送水して、超
音波を照射しながらウェハに流量１Ｌ／分で噴射し、６
０秒間洗浄した。ウェハ上のカリウム濃度は４６.７×
１０10原子／cm2から３８.１×１０10原子／cm2に減少
し、微粒子数は測定上限値の５,５００個／ウェハ以上
から７７個／ウェハに減少した。 比較例２ 温度２５℃、溶存水素濃度１.２mg／Ｌの水素水に、ア
ンモニア１mg／Ｌを添加してpHを９.４に調整した洗浄
液を用い、比較例１と同様にして洗浄を行った。ウェハ
上のカリウム濃度は、４４.１×１０10原子／cm2から３
７.５×１０10原子／cm2に減少し、微粒子数は５,５０
０個／ウェハ以上から４５個／ウェハに減少した。 比較例３ 温超純水供給装置［栗田工業(株)］より供給された８０
℃の温超純水をスピン洗浄機へ送水し、超音波を照射し
ながらウェハに流量１Ｌ／分で噴射し、６０秒間洗浄し
た。ウェハ上のカリウム濃度は４１.２×１０10原子／c
m2から検出下限値の３.１１×１０10原子／cm2以下に減
少したが、微粒子数は洗浄前後ともに測定上限値の５,
５００個／ウェハ以上であった。 比較例４ ８０℃の温超純水にアンモニア１mg／Ｌを添加してpHを
９.４に調整した以外は、比較例３と同様にして洗浄を
行った。ウェハ上のカリウム濃度は４５.７×１０10原
子／cm2から３.１１×１０10原子／cm2以下に減少した
が、微粒子数は洗浄前後ともに測定上限値の５,５００
個／ウェハ以上であった。実施例１〜８及び比較例１〜
４の結果を、第１表に示す。Comparative Example 1 25 ° C. supplied from an ultrapure water production system [Kurita Kogyo Co., Ltd.]
Hydrogen is dissolved in ultra-pure water as raw water using a membrane-dissolved hydrogen water production system [Kurita Kogyo Co., Ltd.], and the dissolved hydrogen concentration is 1.2 m.
g / L of hydrogen water is produced, fed to a spin washer, and sprayed onto the wafer at a flow rate of 1 L / min while irradiating ultrasonic waves.
Washed for 0 seconds. Potassium concentration on wafer is 46.7x
The particle number was reduced from 10 10 atoms / cm 2 to 38.1 × 10 10 atoms / cm 2 , and the number of fine particles was reduced from the measurement upper limit of 5,500 or more / wafer to 77 / wafer. Comparative Example 2 Washing was carried out in the same manner as in Comparative Example 1 using a cleaning solution adjusted to pH 9.4 by adding ammonia 1 mg / L to hydrogen water having a temperature of 25 ° C. and a dissolved hydrogen concentration of 1.2 mg / L. Was. The potassium concentration on the wafer should be between 44.1 × 10 10 atoms / cm 2 and 3
7.5 × 10 10 atoms / cm 2 and the number of fine particles is 5,50
The number decreased from 0 / wafer to 45 / wafer. Comparative Example 3 80 supplied from a hot ultrapure water supply device [Kurita Kogyo Co., Ltd.]
Ultra-pure water at a temperature of 0 ° C. was fed to a spin washer, and was sprayed onto the wafer at a flow rate of 1 L / min while irradiating ultrasonic waves to wash for 60 seconds. Potassium concentration on wafer is 41.2 × 10 10 atoms / c
was reduced from m 2 to 3.11 × 10 10 atoms / cm 2 or less of the detection limit, 5 of both the measurement upper limit number of fine particles before and after washing,
More than 500 wafers / wafer. Comparative Example 4 Washing was performed in the same manner as in Comparative Example 3 except that the pH was adjusted to 9.4 by adding 1 mg / L of ammonia to 80 ° C. ultrapure water. Although the potassium concentration on the wafer was reduced from 45.7 × 10 10 atoms / cm 2 to 3.11 × 10 10 atoms / cm 2 or less, the number of fine particles before and after cleaning was 5,500, which is the upper limit of the measurement.
Pcs / wafer or more. Examples 1 to 8 and Comparative Examples 1 to
Table 1 shows the results of No. 4.
【００１１】[0011]
【表１】 [Table 1]
【００１２】第１表に見られるように、水素を溶解した
６０℃又は８０℃の温超純水を洗浄液として洗浄した実
施例１〜８においては、ウェハ上のカリウムと微粒子が
ともに除去されているのに対して、水素を溶解した２５
℃の超純水を洗浄液とした比較例１〜２では、微粒子は
除去されているがカリウムの除去率が極めて低く、水素
を溶解していない８０℃の温超純水を洗浄液とした比較
例３〜４では、カリウムは除去されているが、微粒子が
除去されていない。また、実施例１〜８の結果から、洗
浄時に超音波を照射することにより、微粒子の除去率が
向上すること、アンモニアを添加してpHを９.４に調整
することによっても、微粒子の除去率が向上すること、
洗浄時間を３０秒から６０秒に延長することによって
も、微粒子の除去率が向上すること、水温を高めること
により、カリウムの除去率と微粒子の除去率がともに向
上することが分かる。比較例１〜４の結果から、温超純
水を洗浄液として洗浄したのち水素水を洗浄液として洗
浄する、あるいは、水素水を洗浄液として洗浄したのち
温超純水を洗浄液として洗浄することにより、ウェハ上
のカリウムと微粒子の両方を除去し得ることが推定され
るが、このような洗浄方法によれば、本発明方法の２倍
の水量と２倍の洗浄時間を必要とするので得策ではな
い。As shown in Table 1, in Examples 1 to 8 in which hot ultrapure water at 60 ° C. or 80 ° C. in which hydrogen was dissolved was used as a cleaning liquid, potassium and fine particles on the wafer were both removed. To which hydrogen was dissolved
In Comparative Examples 1 and 2 using ultrapure water at a temperature of 80 ° C. as cleaning liquids, fine particles were removed but the removal rate of potassium was extremely low, and Comparative Examples 3 and 4 using warm ultrapure water at 80 ° C. in which hydrogen was not dissolved were used. In No. 4, potassium was removed, but fine particles were not removed. Further, from the results of Examples 1 to 8, it is found that the removal rate of fine particles can be improved by irradiating ultrasonic waves during cleaning, and the removal of fine particles can also be achieved by adjusting the pH to 9.4 by adding ammonia. Rate is improved,
It can be seen that extending the washing time from 30 seconds to 60 seconds also improves the removal rate of fine particles, and increasing the water temperature improves both the removal rate of potassium and the removal rate of fine particles. From the results of Comparative Examples 1 to 4, by washing with hot ultrapure water as a washing liquid and then washing with hydrogen water as a washing liquid, or washing with hydrogen water as a washing liquid and washing with hot ultrapure water as a washing liquid, potassium on the wafer was removed. It is presumed that both of the fine particles can be removed, but such a washing method is not advantageous because it requires twice the amount of water and twice the washing time as the method of the present invention.
【００１３】[0013]
【発明の効果】本発明の電子材料の洗浄方法によれば、
ＣＭＰを行った後の電子材料の表面に付着しているカリ
ウムなどの金属不純物と残留する研磨剤などの微粒子
を、１工程の洗浄により同時に短時間で除去することが
できる。According to the method for cleaning an electronic material of the present invention,
Metal impurities such as potassium and fine particles such as abrasive remaining on the surface of the electronic material after the CMP can be simultaneously removed in a short time by one-step cleaning.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｂ０８Ｂ 3/12 Ｂ０８Ｂ 3/12 Ａ ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) B08B 3/12 B08B 3/12 A
Claims (2)
あって、水素、酸素又は希ガスを溶解した４５℃以上の
超純水を洗浄液とし、この洗浄液に１０kHz〜３MHzの超
音波を照射しながら洗浄することを特徴とする電子材料
の洗浄方法。1. A method of cleaning an electronic material after performing CMP, wherein ultrapure water of 45 ° C. or higher in which hydrogen, oxygen or a rare gas is dissolved is used as a cleaning liquid, and ultrasonic waves of 10 kHz to 3 MHz are applied to the cleaning liquid. A method for cleaning electronic materials, wherein the cleaning is performed while irradiating.
１記載の電子材料の洗浄方法。2. The method for cleaning an electronic material according to claim 1, wherein an alkali is added to the cleaning liquid.
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| JP2000162206A JP4482844B2 (en) | 2000-05-31 | 2000-05-31 | Wafer cleaning method |
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| JP2000162206A JP4482844B2 (en) | 2000-05-31 | 2000-05-31 | Wafer cleaning method |
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| JP2000162206A Expired - Lifetime JP4482844B2 (en) | 2000-05-31 | 2000-05-31 | Wafer cleaning method |
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