JP2621398B2 - Mirror polishing liquid for GaAs wafer and polishing method - Google Patents
Mirror polishing liquid for GaAs wafer and polishing methodInfo
- Publication number
- JP2621398B2 JP2621398B2 JP63198651A JP19865188A JP2621398B2 JP 2621398 B2 JP2621398 B2 JP 2621398B2 JP 63198651 A JP63198651 A JP 63198651A JP 19865188 A JP19865188 A JP 19865188A JP 2621398 B2 JP2621398 B2 JP 2621398B2
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- Japan
- Prior art keywords
- polishing
- polishing liquid
- wafer
- sodium
- mirror
- Prior art date
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- Expired - Lifetime
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- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Weting (AREA)
Description
【発明の詳細な説明】 「産業上の利用分野」 本発明は、例えばエピタキシャル成長用基板として使
用されるGaAsウェーハの鏡面研磨液および研磨方法に関
する。The present invention relates to a mirror polishing liquid and a polishing method for a GaAs wafer used as, for example, a substrate for epitaxial growth.
「従来の技術」 上記エピタキシャル成長用GaAs基板には、表面欠陥や
加工変質層のない無擾乱の平滑鏡面が要求され、製造時
の最終工程において化学研磨液および回転研磨盤を用い
た鏡面研磨が行なわれる。"Prior art" The above-mentioned GaAs substrate for epitaxial growth is required to have a smooth and non-disturbed mirror surface without surface defects or process-induced deterioration layers. It is.
従来より、この種の研磨液としては、特公昭55−2841
7号公報、および特開昭62−290136号公報に記載された
ものが周知である。前者は、次亜塩素酸塩および炭酸塩
の混合溶液であり、例えば、 GaAs＋4NaClO→GaAsO4＋4NaCl の反応によりウェーハ表面を酸化するとともに、 GaAsO4＋4Na2CO3＋4H2O →NaGa（OH）４＋Na3AsO4＋4NaHCO3 の反応により酸化膜を溶解し、回転研磨盤の研磨布によ
る摩擦作用と相まって研磨作用を得る。Conventionally, this type of polishing liquid has been disclosed in
No. 7 and JP-A-62-290136 are well known. The former is a mixed solution of hypochlorite and carbonate, for example, while oxidizing the wafer surface by a reaction of GaAs + 4NaClO → GaAsO 4 + 4NaCl, and GaAsO 4 + 4Na 2 CO 3 + 4H 2 O → NaGa (OH) 4 + Na The oxide film is dissolved by the reaction of 3AsO 4 + 4NaHCO 3 , and the polishing action is obtained in combination with the friction action by the polishing cloth of the rotary polishing machine.
一方、後者は、次亜塩素酸ナトリウムと炭酸水素ナト
リウムの混合溶液、またはこれに塩化ナトリウムを添加
したものであり、前者の研磨液よりもヘイズ、ピット等
の表面欠陥を低減しうるとしている。On the other hand, the latter is a mixed solution of sodium hypochlorite and sodium hydrogencarbonate or a solution obtained by adding sodium chloride to the mixed solution, and it is described that surface defects such as haze and pits can be reduced more than the former polishing liquid.
さらにこれらとは別に、NaClO溶液にコロイダルシリ
カ等の微細な砥粒を添加した研磨液も一部で用いられて
いる。Further, apart from these, a polishing liquid obtained by adding fine abrasive grains such as colloidal silica to a NaClO solution is also used in part.
「発明が解決しようとする課題」 しかし、上記研磨液のうち、砥粒を用いないものにお
いては、加工変質層の少ない鏡面は得られるものの、依
然としてヘイズやピット等の表面欠陥が発生しやすく、
表面粗さを小さくしにくいという問題があった。一方、
コロイダルシリカ等の砥粒を用いる方法では、表面粗さ
の小さな鏡面は得やすいが、ウェーハ表面に極薄く不均
質な加工変質層が生じ、微視的な局部的ダメージ（ある
種のエッチングを行なうとスクラッチが確認できる）が
発生し、エピタキシャル成長に悪影響を及ぼす欠点があ
った。"Problems to be Solved by the Invention" However, among the above polishing liquids, those which do not use abrasive grains, although a mirror surface with a less work-affected layer can be obtained, surface defects such as haze and pits still easily occur,
There is a problem that it is difficult to reduce the surface roughness. on the other hand,
In a method using abrasive grains such as colloidal silica, a mirror surface having a small surface roughness can be easily obtained, but an extremely thin and non-uniformly altered layer is formed on the wafer surface, and microscopic local damage (performs some kind of etching). Scratches can be confirmed), which has the disadvantage of adversely affecting the epitaxial growth.
そこで本発明者らは、研磨液の組成を種々変更して実
際に研磨試験を行ない、加工変質層や表面欠陥を極力低
減しうる組成を検討した結果、従来から用いられている
NaClOとNa2CO3の他にNaOHを特定の濃度範囲で添加する
ことにより、ヘイズやピット等の表面欠陥を低減できる
ことを見出だした。また、この研磨液にNaClを添加すれ
ば、NaClの酸化作用を緩衝し、一層表面欠陥を低減でき
ることを見出だした。さらに、上記組成からなる研磨液
とともにコロイダルシリカを供給して研磨することによ
り、GaAsウェーハの表面粗さを向上できることを見出だ
した。Therefore, the present inventors have performed a polishing test by actually changing the composition of the polishing liquid in various ways, and as a result of examining a composition capable of minimizing a process-affected layer and a surface defect as a result, it has been conventionally used.
It has been found that by adding NaOH in a specific concentration range in addition to NaClO and Na 2 CO 3 , surface defects such as haze and pits can be reduced. It has also been found that the addition of NaCl to this polishing solution can buffer the oxidizing action of NaCl and further reduce surface defects. Further, it has been found that the surface roughness of a GaAs wafer can be improved by supplying and polishing colloidal silica together with a polishing liquid having the above composition.
「課題を解決するための手段」 本発明は上記課題を解決するためになされたもので、
本発明の研磨液は、次亜塩素酸ナトリウム、水酸化ナト
リウム、および炭酸ナトリウムを含有することを特徴と
する。さらに、塩化ナトリウムを添加してもよい。"Means for solving the problem" The present invention has been made to solve the above problems,
The polishing liquid of the present invention is characterized by containing sodium hypochlorite, sodium hydroxide, and sodium carbonate. Further, sodium chloride may be added.
各組成の望ましい濃度は、次亜塩素酸ナトリウム:0.0
01〜1wt％（有効塩素濃度）、水酸化ナトリウム:0.01〜
5wt％、炭酸ナトリウム:0.01〜5wt％であり、塩化ナト
リウムを添加する場合は1wt％以下とされる。The desired concentration of each composition is sodium hypochlorite: 0.0
01 to 1 wt% (effective chlorine concentration), sodium hydroxide: 0.01 to
5 wt%, sodium carbonate: 0.01 to 5 wt%, and 1 wt% or less when sodium chloride is added.
一方、本発明の研磨方法は、前記研磨液を用い、回転
研磨盤によりGaAsウェーハの研磨を行なうことを特徴と
する。また、本発明の他の研磨方法は、前記研磨液にコ
ロイダルシリカを同時供給して用いることを特徴とす
る。On the other hand, a polishing method of the present invention is characterized in that a GaAs wafer is polished by a rotary polishing machine using the polishing liquid. Another polishing method of the present invention is characterized in that colloidal silica is simultaneously supplied to the polishing liquid and used.
上記研磨液の作用を説明すると、 GaAs＋4NaClO→GaAsO4＋4NaCl の反応によりウェーハ表面を酸化するとともに、 GaAsO4＋4Na2CO3＋4H2O →NaGa（OH）４＋Na3AsO4＋4NaHCO3 および GaAsO4＋4HaOH→NaGa（OH）４＋Na3AsO4 の２種の反応により、この酸化物を溶解する。式の反
応は反応熱が大きいため、前記特公昭55−28417号公報
では、「NaOHはGaAsO4を溶解するが、高い反応熱でGaAs
ウェーハの表面粗さを致命的に低下する」旨が記載され
ている。ところが本発明者らの実験では、各組成を前記
濃度範囲に設定し、式と式の反応速度のバランスを
取ることにより、反応熱を抑えてNaClOの熱分解を防
ぎ、同時にGaAsウェーハの面粗さをNaOHを添加しない場
合に比して格段に向上しうることが確認できた。またNa
ClはNaClOの酸化作用を緩衝し、ウェーハ表面を緩やか
に酸化させることにより、表面粗さを向上する作用を果
たす。The operation of the above polishing liquid is described as follows. In addition to oxidizing the wafer surface by the reaction of GaAs + 4NaClO → GaAsO 4 + 4NaCl, GaAsO 4 + 4Na 2 CO 3 + 4H 2 O → NaGa (OH) 4 + Na 3 AsO 4 + 4NaHCO 3 and GaAsO 4 + 4HaOH → This oxide is dissolved by two reactions of NaGa (OH) 4 + Na 3 AsO 4 . Since the reaction of the formula has a large heat of reaction, in the Japanese Patent Publication 55-28417 discloses, "NaOH is dissolving GaAsO 4, GaAs at high reaction heat
The surface roughness of the wafer is fatally reduced ". However, in the experiments of the present inventors, each composition was set in the above-mentioned concentration range, and by balancing the reaction rates of the equations, the reaction heat was suppressed to prevent thermal decomposition of NaClO, and at the same time, the surface roughness of the GaAs wafer was reduced. It has been confirmed that the remarkable improvement can be achieved as compared with the case where NaOH is not added. Also Na
Cl acts to improve the surface roughness by buffering the oxidizing action of NaClO and gently oxidizing the wafer surface.
次に、各組成の濃度設定の理由を述べる。 Next, the reason for setting the concentration of each composition will be described.
NaClO:前記よりも高濃度であるとヘイズ発生傾向が増
し、面粗さが低下する。また前記よりも低濃度では前述
の局部的ダメージが発生する。NaClO: If the concentration is higher than the above, the tendency of haze generation increases, and the surface roughness decreases. If the concentration is lower than the above, the above-mentioned local damage occurs.
Na2CO3:前記より高濃度では面粗さが増し、低濃度では
前記局部的ダメージが増す。Na 2 CO 3 : At higher concentrations, the surface roughness increases, and at lower concentrations, the local damage increases.
NaOH:前記より高濃度ではNaClOの熱分解を促進するとと
もに、ウェーハ表面にうねりが生じる。逆に低濃度では
面粗さが低下する。NaOH: If the concentration is higher than the above, the thermal decomposition of NaClO is promoted and undulation is generated on the wafer surface. Conversely, when the concentration is low, the surface roughness decreases.
NaCl:前記より高濃度ではNaClOの酸化力を低減しすぎ、
ヘイズや面荒れのおそれが生じる。NaCl: At higher concentrations, the oxidizing power of NaClO is excessively reduced,
Haze and surface roughening may occur.
一方、前記研磨液を用いて回転研磨盤で研磨を行え
ば、前記研磨液の作用と、研磨パッドの摩擦作用とが相
まって、ヘイズやピット等の表面欠陥が少なく、面粗さ
が良好で、加工変質層の少ない鏡面が得られる。On the other hand, if the polishing is performed on a rotary polishing machine using the polishing liquid, the action of the polishing liquid and the frictional action of the polishing pad are combined to reduce surface defects such as haze and pits, and the surface roughness is good. A mirror surface with a less work-affected layer is obtained.
また、研磨液とコロイダルシリカとを、いわゆる共流
しにより使用直前に混合して回転研磨盤に供給し、研磨
を行なった場合には、コロイダルシリカを加えない場合
に比してウェーハの面粗さを向上することができる。本
発明者らの実験ではコロイダルシリカの混合量を変更し
てもウェーハの研磨率には変化が見られず、面粗さにの
み影響することが判明した。この事実から、コロイダル
シリカは砥粒としてウェーハを研磨するのではなく、研
磨パッドとウェーハとの摩擦作用を均一化する作用を果
たしているものと推測される。なお、共流ししてコロイ
ダルシリカを混合するのは、事前に混合しておくと、Na
OHとコロイダルシリカが反応するためである。Further, the polishing liquid and colloidal silica are mixed immediately before use by so-called co-flow and supplied to a rotary polishing machine, and when the polishing is performed, the surface roughness of the wafer is smaller than when no colloidal silica is added. Can be improved. The experiments of the present inventors revealed that even if the amount of colloidal silica was changed, the polishing rate of the wafer did not change, and only the surface roughness was affected. From this fact, it is presumed that the colloidal silica does not polish the wafer as abrasive grains, but plays an action of equalizing the frictional action between the polishing pad and the wafer. It should be noted that the colloidal silica is mixed by co-flowing if Na is mixed in advance.
This is because OH and colloidal silica react.
付言すると、研磨時の研磨液温度は０〜50℃程度、コ
ロイダルシリカの粒径は20〜200nm程度、コロイダルシ
リカの混合量は５〜25wt％程度であることが望ましい。
研磨液温度は０℃以下では研磨性が低下し、50℃以上で
はNaClOが分解するおそれがある。また前記粒径および
混合量の範囲は、良好な研磨性が得られる範囲である。
他の研磨条件等は、従来と同様でよい。In addition, it is desirable that the polishing liquid temperature during polishing is about 0 to 50 ° C., the particle size of colloidal silica is about 20 to 200 nm, and the mixing amount of colloidal silica is about 5 to 25 wt%.
If the polishing liquid temperature is 0 ° C. or lower, the polishing property is reduced, and if the polishing liquid temperature is 50 ° C. or higher, NaClO may be decomposed. The ranges of the particle size and the mixing amount are ranges in which good polishing properties can be obtained.
Other polishing conditions and the like may be the same as those in the related art.
「実施例」 （実施例１） （100）面で切り出したGaAsウェーハに両面ラッピン
グを施し、さらに歪除去エッチングの後、コロイダルシ
リカ系研磨液による粗研磨を行なった。そして、NaClO:
0.5wt％（有効塩素濃度）、NaCl:0.1wt％、NaOH:1.5wt
％、Na2CO3:2.5wt％の組成からなる第１液と、粒径50〜
70nmのコロイダルシリカを10wt％含有する第２液を共流
しして鏡面研磨を行なった。研磨条件は次の通りであ
る。"Example" (Example 1) A GaAs wafer cut out on the (100) plane was subjected to double-sided lapping, and after strain removal etching, rough polishing was performed using a colloidal silica-based polishing liquid. And NaClO:
0.5wt% (effective chlorine concentration), NaCl: 0.1wt%, NaOH: 1.5wt
%, Na 2 CO 3 : 2.5wt% composition, the first liquid, particle size 50 ~
A second liquid containing 10 wt% of 70 nm colloidal silica was co-flowed to perform mirror polishing. The polishing conditions are as follows.
研磨定盤径:500mmφ 定盤回転数:100rpm 研磨布：スエードタイプポリッシャー 加工圧:34g/cm2 研磨液流量：第１液20ml/分 第２液10ml/分 研磨時間:10分 （実施例２） NaClを含まない他は実施例１と同じ研磨液を用い、同
様のウェーハを同一条件で研磨した。Polishing plate diameter: 500 mmφ Platen rotation speed: 100 rpm Polishing cloth: Suede type polisher Working pressure: 34 g / cm 2 Polishing liquid flow rate: First liquid 20 ml / min Second liquid 10 ml / min Polishing time: 10 minutes (Example 2) The same wafer was polished under the same conditions using the same polishing liquid as in Example 1 except that NaCl was not included.
（実施例３） コロイダルシリカを含まない他は実施例１と同じ研磨
液を用い、同じ条件で研磨を行なった。(Example 3) Polishing was performed under the same conditions using the same polishing liquid as in Example 1 except that colloidal silica was not included.
（比較例１） 特公昭55−28417号公報に記載の研磨液（NaClO:0.2g
mol/、Na2CO3:0.2g mol/）を用いて実施例１と同じ
条件で研磨を行なった。(Comparative Example 1) Polishing liquid described in JP-B-55-28417 (NaClO: 0.2 g)
mol /, Na 2 CO 3 : 0.2 g mol /), and polishing was performed under the same conditions as in Example 1.
（比較例２） 特開昭62−290136号公報に記載の研磨液（NaClO:0.25
wt％、NaHCO3:1wt％、NaCl:0.1wt％）を用いて実施例１
と同じ条件で研磨を行なった。Comparative Example 2 Polishing liquid described in JP-A-62-290136 (NaClO: 0.25
Example 1 using the following components (wt%, NaHCO 3 : 1 wt%, NaCl: 0.1 wt%).
Polishing was performed under the same conditions as described above.
（比較例３） NaClOとコロイダルシリカのみの研磨液（NaClO:0.004
wt％（有効塩素濃度）、コロイダルシリカ（50〜70nm
φ）:5wt％）を用いて実施例１と同一条件で研磨を行な
った。(Comparative Example 3) Polishing solution containing only NaClO and colloidal silica (NaClO: 0.004
wt% (effective chlorine concentration), colloidal silica (50-70nm
(φ): 5 wt%) and polished under the same conditions as in Example 1.
そして、以上で得られた実施例１〜３、比較例１〜３
のGaAsウェーハの表面粗さを測定し、集光燈および微分
干渉顕微鏡でヘイズ，キズ，ピット等の表面欠陥の有無
を確認した。その後さらにアンモニア系のエッチング液
にウェーハを浸して表面を約１μｍエッチングし、局部
的なダメージによるスクラッチ発生の有無を確認した。
その結果を次表に示す。Then, Examples 1 to 3 and Comparative Examples 1 to 3 obtained above are obtained.
The surface roughness of the GaAs wafer was measured, and the presence or absence of surface defects such as haze, scratches, and pits was confirmed using a condensing lamp and a differential interference microscope. Thereafter, the wafer was further immersed in an ammonia-based etching solution to etch the surface by about 1 μm, and it was confirmed whether scratches were generated due to local damage.
The results are shown in the following table.
「発明の効果」 以上説明したように、本発明に係わるGaAsウェーハの
鏡面研磨液および研磨方法によれば、従来の研磨液およ
び研磨方法に比して、ピットやヘイズ等の表面欠陥が少
なく、面粗さが良好で、しかも加工変質層の少ない鏡面
が得られる。 [Effects of the Invention] As described above, according to the mirror polishing solution and polishing method for a GaAs wafer according to the present invention, surface defects such as pits and haze are less than those of the conventional polishing solution and polishing method, A mirror surface having a good surface roughness and a small number of damaged layers can be obtained.
Claims (6)
ム、および炭酸ナトリウムを含有するGaAsウェーハの鏡
面研磨液。1. A mirror polishing liquid for GaAs wafers containing sodium hypochlorite, sodium hydroxide, and sodium carbonate.
水酸化ナトリウム、および炭酸ナトリウムを含有するGa
Asウェーハの鏡面研磨液。(2) sodium hypochlorite, sodium chloride,
Ga containing sodium hydroxide and sodium carbonate
Mirror polishing liquid for As wafer.
効塩素濃度）、水酸化ナトリウム:0.01〜5wt％、炭酸ナ
トリウム:0.01〜5wt％を含有するGaAsウェーハの鏡面研
磨液。3. A mirror polishing liquid for GaAs wafers containing sodium hypochlorite: 0.001 to 1 wt% (effective chlorine concentration), sodium hydroxide: 0.01 to 5 wt%, and sodium carbonate: 0.01 to 5 wt%.
効塩素濃度）、塩化ナトリウム:1wt％以下、水酸化ナト
リウム:0.01〜5wt％、炭酸ナトリウム:0.01〜5wt％を含
有するGaAsウェーハの鏡面研磨液。4. A GaAs wafer containing sodium hypochlorite: 0.001 to 1 wt% (effective chlorine concentration), sodium chloride: 1 wt% or less, sodium hydroxide: 0.01 to 5 wt%, and sodium carbonate: 0.01 to 5 wt%. Mirror polishing liquid.
は第４項記載の研磨液を用い、回転研磨盤によりGaAsウ
ェーハの研磨を行なうGaAsウェーハの研磨方法。5. A method for polishing a GaAs wafer, wherein the polishing liquid according to claim 1, 2, 3, or 4 is polished with a rotary polishing machine.
は第４項記載の研磨液にコロイダルシリカを添加した研
磨液を用い、回転研磨盤によりGaAsウェーハの研磨を行
なうGaAsウェーハの研磨方法。6. A polishing method for polishing a GaAs wafer by using a polishing liquid obtained by adding colloidal silica to the polishing liquid according to claim 1 or 2, and polishing the GaAs wafer with a rotary polishing machine. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63198651A JP2621398B2 (en) | 1988-08-09 | 1988-08-09 | Mirror polishing liquid for GaAs wafer and polishing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63198651A JP2621398B2 (en) | 1988-08-09 | 1988-08-09 | Mirror polishing liquid for GaAs wafer and polishing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0246729A JPH0246729A (en) | 1990-02-16 |
| JP2621398B2 true JP2621398B2 (en) | 1997-06-18 |
Family
ID=16394763
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63198651A Expired - Lifetime JP2621398B2 (en) | 1988-08-09 | 1988-08-09 | Mirror polishing liquid for GaAs wafer and polishing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2621398B2 (en) |
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| US11505743B2 (en) * | 2018-09-06 | 2022-11-22 | Fujifilm Corporation | Chemical solution and method for treating substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4759298B2 (en) * | 2005-03-30 | 2011-08-31 | 株式会社フジミインコーポレーテッド | Abrasive for single crystal surface and polishing method |
| JP5703133B2 (en) * | 2011-05-31 | 2015-04-15 | 京セラクリスタルデバイス株式会社 | Wafer polishing method and nanobubble circulation polishing apparatus |
| JP5742780B2 (en) * | 2012-05-17 | 2015-07-01 | 信越半導体株式会社 | Alkali etching solution and alkali etching method using the same |
| WO2016052408A1 (en) * | 2014-09-30 | 2016-04-07 | 株式会社フジミインコーポレーテッド | Polishing composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5212057B2 (en) | 2008-12-03 | 2013-06-19 | トヨタ自動車株式会社 | Abnormality diagnosis device for exhaust gas recirculation device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5212057B2 (en) | 2008-12-03 | 2013-06-19 | トヨタ自動車株式会社 | Abnormality diagnosis device for exhaust gas recirculation device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11505743B2 (en) * | 2018-09-06 | 2022-11-22 | Fujifilm Corporation | Chemical solution and method for treating substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0246729A (en) | 1990-02-16 |
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