JPS63180466A - Polishing liquid - Google Patents

Polishing liquid

Info

Publication number
JPS63180466A
JPS63180466A JP62009993A JP999387A JPS63180466A JP S63180466 A JPS63180466 A JP S63180466A JP 62009993 A JP62009993 A JP 62009993A JP 999387 A JP999387 A JP 999387A JP S63180466 A JPS63180466 A JP S63180466A
Authority
JP
Japan
Prior art keywords
polishing
gallium arsenide
mirror
polishing liquid
reaction product
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.)
Pending
Application number
JP62009993A
Other languages
Japanese (ja)
Inventor
Katsutoshi Higuchi
勝敏 樋口
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.)
Toshiba Corp
Original Assignee
Toshiba 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 Toshiba Corp filed Critical Toshiba Corp
Priority to JP62009993A priority Critical patent/JPS63180466A/en
Publication of JPS63180466A publication Critical patent/JPS63180466A/en
Pending legal-status Critical Current

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  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

PURPOSE:To prevent a workpiece from being subjected to any damage by mix ing at least bleaching power, sodium tripolyphosphate and sodium sulfate into water, in the case of a polishing liquid used for polishing the mirror-like surface of a substrate made of monocrystal of gallium arsenide. CONSTITUTION:The mirror-like surface of a substrate 3 made of monocrystal of gallium arsenide is polished by means of polishing liquid formed by mixing about 0.4-4.4g of strong bleaching powder mainly consisting of calcium hypochlorite into a solution consisting of about 6.4g of sodium tripolyphosphate, about 7.2g of sodium sulfate and about 500ml of pure water. In this case, Ga2O3 and As2O3 are formed as a reaction product 4 on the surface of gallium arsenide 3 by aid of ClO<-> generated through dissociation of strong bleaching powder in pure water, the protruding portions of the reaction product 4 are swept off by polishing cloth 5 to get the surface of gallium arsenide 3 exposed, and a reaction product 6 is formed again. These processes are repeated alternately to form a flat and smooth mirror-like surface polishing state. A mirror-like surface polishing process of high accuracy can be carried out in this way, without giving any damage to a workpiece.

Description

【発明の詳細な説明】 〔発明の目的〕 (産業上の利用分野) 本発明は、化合物半導体、特に砒化ガリウム単結晶基板
の鏡面研磨に使用する研磨液に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Application Field) The present invention relates to a polishing liquid used for mirror polishing a compound semiconductor, particularly a gallium arsenide single crystal substrate.

(従来の技術) 砒化ガリウム(Ga As )単結晶基板の研磨加工に
用いる研磨液としては種々のものがあるが、従来より多
く用いられている研磨液には、ダイヤモンドの微細砥粒
を含む鉱物油と、臭素(Br )をメチルアルコールに
溶解させたBrメタノール溶液がある。このうち、ダイ
ヤモンドの微細砥粒を含む鉱物油を用いて、砒化ガリウ
ム単結晶基板を研磨する場合は、ダイヤモンドの微細砥
粒が砒化ガリウム単結晶基板の表面を少しずつ除去する
過程が繰り返し進行することによって、平滑な表面が作
製される。また、Brメタノール溶液を用いて、砒化ガ
リウム単結晶基板を研磨する場合は、Brメタノール溶
液が砒化ガリウムと化学反応を起こし、即ち砒化ガリウ
ムの構成成分であるGaと胎とを溶液中に溶かし込むい
わゆるエツチング反応を起こし、離合ガリウムを化学的
に溶解することによってしだいに平滑な表面が作製され
る。
(Prior Art) There are various polishing liquids used for polishing gallium arsenide (GaAs) single crystal substrates, but the polishing liquid that has been commonly used conventionally uses minerals containing fine diamond abrasive grains. There is an oil and a Br methanol solution in which bromine (Br) is dissolved in methyl alcohol. Among these, when polishing a gallium arsenide single crystal substrate using mineral oil containing fine diamond abrasive grains, the process in which the diamond fine abrasive grains gradually remove the surface of the gallium arsenide single crystal substrate progresses repeatedly. This creates a smooth surface. In addition, when polishing a gallium arsenide single crystal substrate using a Br methanol solution, the Br methanol solution causes a chemical reaction with gallium arsenide, that is, Ga and nitride, which are constituent components of gallium arsenide, are dissolved in the solution. By causing a so-called etching reaction and chemically dissolving the separated gallium, a smooth surface is gradually created.

ところで、前記ダイヤモンドの微細砥粒を含む鉱物油を
用いて砒化ガリウム単結晶基板を研磨する場合には、ダ
イヤモンドの微細砥粒による引っかき傷を基板表面に作
り、研磨加工後の基板表面に引っかき傷からなる損傷を
残留するという欠点があった。また、Brメタノール溶
液を用いて砒化ガリウム単結晶基板を研磨する場合には
、Brメタノールが砒化ガリウムを溶かし込む化学反応
による研磨加工であるため、基板表面の形状精度(平面
変、平行度、表面粗さなど)が悪いという欠点があった
By the way, when polishing a gallium arsenide single crystal substrate using mineral oil containing the aforementioned fine diamond abrasive grains, scratches are created on the substrate surface by the diamond fine abrasive grains, and scratches are left on the substrate surface after polishing. The disadvantage was that it left behind some damage. In addition, when polishing a gallium arsenide single crystal substrate using a Br methanol solution, the polishing process is based on a chemical reaction in which Br methanol dissolves gallium arsenide. It had the disadvantage of poor roughness, etc.).

(@明が解決しようとする問題点) 本発明は、上記実情にかんがみてなされたもので、その
目的とするところは、研磨加工後の基板表面に引っかき
傷等の損傷を残留することなしに、また、研磨加工後の
基板表面の形状精度が良好となる化合物半導体材料用の
研磨液を提供することにある。
(Problems to be solved by @Ming) The present invention was made in view of the above-mentioned circumstances, and its purpose is to prevent damage such as scratches from remaining on the surface of the substrate after polishing. Another object of the present invention is to provide a polishing liquid for compound semiconductor materials that provides good shape accuracy on the surface of a substrate after polishing.

〔発明の構成〕[Structure of the invention]

(問題点を解決するための手段と作用)化合物半導体材
料の研磨液において、水に少なくともさらし粉(Ca 
(CAO)tを主成分とする。)、トリポリりん酸ナト
リウム(N”s PS 010 ) 、硫酸ナトリウム
(Na、 80.)を混合してなり、損傷を生じること
なく高精度研磨が可能となるものである。
(Means and effects for solving the problem) In the polishing solution for compound semiconductor materials, at least a powder (Ca
(CAO)t is the main component. ), sodium tripolyphosphate (N"s PS 010 ), and sodium sulfate (Na, 80.), and enables high-precision polishing without causing damage.

(実施例) 以下、本発明の一実施例を図面を参照して詳述する。(Example) Hereinafter, one embodiment of the present invention will be described in detail with reference to the drawings.

本発明の実施例として、トリポリりん酸ナトリウム(N
as Ps Olo ) 、硫酸ナトリfy A (N
a、 80.)、純水をそれぞれ6.4t、 7.2p
、 500−の割合で混合した溶液の中に、次亜塩素化
カルシウム(Ca (CtO)りを主成分(含有i16
5.1 vol lly )とする高度さらし粉の混合
量を0.4f4.4tの範囲で変化させて、研磨液とし
、試験的に砒化ガリウムの研磨を行った0第1表に研磨
条件を示す。
As an example of the present invention, sodium tripolyphosphate (N
as Ps Olo), sodium sulfate fy A (N
a.80. ), 6.4t and 7.2p of pure water, respectively.
Calcium hypochlorite (Ca (CtO)) as the main component (containing i16
Table 1 shows the polishing conditions in which gallium arsenide was polished experimentally using a polishing solution in which the mixed amount of high-level bleaching powder (5.1 vol lly) was varied within the range of 0.4f4.4t.

研磨治具(1)に切削された100−の砒化ガリウム結
晶(2)を第1図の様に12枚対象にはりつけ、95t
f/c−の圧力をかけて研磨を行った。第2図に研磨液
分の高度さらし粉の分量と研磨速度との関係を示す。第
2図より、研磨速度は研磨液中の高度さら“し粉の分量
がtpまでは急激に増加し、その後、はぼ一定になって
いる。この結果、本発明における研磨液組成においては
、高度さらし粉の分量を増加させることによって研磨速
度を制御できるといえる。また、研磨速度を安定化させ
るためには、1を以上の高度さらし粉が必要である。
As shown in Figure 1, 12 gallium arsenide crystals (2) cut into a polishing jig (1) were attached to the target, and 95t.
Polishing was performed by applying a pressure of f/c-. FIG. 2 shows the relationship between the amount of highly bleached powder in the polishing liquid and the polishing speed. From FIG. 2, the polishing rate increases rapidly until the amount of highly exposed powder in the polishing solution reaches tp, and then becomes almost constant.As a result, in the polishing solution composition of the present invention, It can be said that the polishing rate can be controlled by increasing the amount of high-level bleaching powder.Also, in order to stabilize the polishing rate, a high-level bleaching powder of 1 or more is required.

次に、高度さらし粉、トリポリりん酸ナトリウム、硫酸
ナトリウム、−純水を4.4P、 6.4f、 7.2
f、 500−の割合で混合した溶液に、希H,80,
ならびに水酸化ナトリウムを加えて溶液中のpHを変化
させたものを研磨液とし、砒化ガリウム結晶の研磨を行
った。
Next, add highly bleached powder, sodium tripolyphosphate, sodium sulfate, and pure water to 4.4P, 6.4f, 7.2
f, diluted H, 80,
The pH of the solution was changed by adding sodium hydroxide as a polishing liquid, and gallium arsenide crystals were polished.

研磨条件は第1表に準じて行った。第3図に、前記研磨
液のpH値と研磨速度との関係を示す。第3図中の注釈
は螢光打丁での目視による研磨表面の状態である。第3
図より、研磨速度に対して研磨液のpH値は大きな影響
を及ぼし、pi−1値の増加に伴い研磨速度は指数関数
的に増加する。また、研磨後の砒化ガリウム結晶表面は
p H= l O,5以下ではA面であるが、pH=1
1.5以上では黒色膜が形成されている。この結果、高
度さらし粉を用いた研磨液の適正pH値はPH=8〜t
iの範囲であるといえる。第4図ないし第6図は、高度
さらし粉、トリポリりん酸ナトリウム、硫酸ナトリウム
、純水からなる本発明における研磨液を用いて砒化ガリ
ウムを研磨したときの研磨モデルである。すなわち、研
磨液成分中の高度さらし粉の主成分であルCa (C1
0)tは、純水中で解離してCa 、 C40−に分解
する。そしてCtO−によって砒化ガリウム(3)表面
に反応生成物(4)としてのGa、 o3.入S、0.
が形成される。次いで、研磨布(5)によって前記反応
生成物(4)の一部(他より凸状の部分)が、ぬぐい取
られる。すると、ぬぐい取られた部分は砒化ガリウム面
が露出するため、再度Ga、 0. 、入S、0.から
なる反応生成物(6)が形成され、次いで研磨布(5)
によってこの反応生成物(6)がぬぐい取られる。この
過程が繰り返されて行なわれることによって研磨が進行
し、平滑な鏡面状態が形成される。
The polishing conditions were as shown in Table 1. FIG. 3 shows the relationship between the pH value of the polishing liquid and the polishing rate. The annotations in FIG. 3 indicate the condition of the polished surface visually observed with a fluorescent knife. Third
From the figure, the pH value of the polishing liquid has a large effect on the polishing rate, and the polishing rate increases exponentially as the pi-1 value increases. Furthermore, the surface of the gallium arsenide crystal after polishing is A-plane at pH=lO,5 or less, but when pH=1
If it is 1.5 or more, a black film is formed. As a result, the appropriate pH value of polishing liquid using high-level bleaching powder is PH = 8 ~ t
It can be said that it is within the range of i. FIGS. 4 to 6 are polishing models for polishing gallium arsenide using the polishing liquid of the present invention comprising high-grade bleaching powder, sodium tripolyphosphate, sodium sulfate, and pure water. In other words, Ca (C1
0) t dissociates in pure water and decomposes into Ca and C40-. Then, by CtO-, Ga as a reaction product (4) is formed on the surface of gallium arsenide (3), o3. Enter S, 0.
is formed. Next, a part of the reaction product (4) (a part that is more convex than the rest) is wiped off with a polishing cloth (5). Then, the gallium arsenide surface of the wiped off area is exposed, so Ga, 0. , Enter S, 0. A reaction product (6) consisting of
This reaction product (6) is wiped off. By repeating this process, polishing progresses and a smooth mirror surface is formed.

このようにして研磨が進行するため、本発明における研
磨液を用いての研磨の場合には前記ダイヤモンドの微細
砥粒を含む鉱物油を用いての研磨において問題となる基
板表面に残留する引っかき傷などの損傷を生ずることな
しに研磨が可能であり、また、前記Brメタノール溶液
を用いての研磨において問題となる基板表面の形状精度
の悪化なしに研磨が可能である。また、研磨液成分とし
てのトリポリりん酸ナトリウムは、反応生成物を生成さ
せる前記次亜塩素酸((、tO″″)が研磨液中で分解
し、さらに純水中の水素イオンと反応して、Ct、。
Because polishing proceeds in this manner, when polishing using the polishing liquid of the present invention, scratches remain on the substrate surface, which is a problem when polishing using mineral oil containing fine diamond abrasive grains. Polishing is possible without causing damage such as, and polishing is also possible without deteriorating the shape accuracy of the substrate surface, which is a problem in polishing using the Br methanol solution. In addition, in sodium tripolyphosphate as a polishing liquid component, the above-mentioned hypochlorous acid ((, tO''), which generates a reaction product, decomposes in the polishing liquid and further reacts with hydrogen ions in pure water. , Ct.

HClが生成されて研磨速度が不安定になる過程を妨げ
る作用をし、安定した研磨作用をさせるために、必要不
可欠な成分である。また、硫酸ナトリウムについては含
まない場合、即ち、高度さらし粉、トリポリりん酸ナト
リウム、純水からなる場合においても研磨可能であるが
、硫酸ナトリウムは純水に容易にNa+とSOニーに解
離し、他の化学反応を容易にする作用があるため、混合
させた方が良い。また、純水については、研磨液の溶液
となるため、これも必要不可欠な成分である。
It acts to prevent the process in which HCl is generated and the polishing rate becomes unstable, and is an essential component for stable polishing action. In addition, polishing is possible even when it does not contain sodium sulfate, that is, when it consists of highly bleached powder, sodium tripolyphosphate, and pure water, but sodium sulfate easily dissociates into Na + and SO knee in pure water, and other It is better to mix them because they have the effect of facilitating chemical reactions. Further, pure water is also an essential component since it becomes a solution of the polishing liquid.

なお、本発明での研磨液の一成分である高度さらし粉は
、Ca(CAO)、 (次亜塩素化カルシウム)を主成
分(含有量65.1vo1%)  とする白色粉状の薬
品でのCa (CtO)を濃度が73.6wtチと高度
さらし粉よりも高い、トヨクロンPTG(商品名;製造
元、東洋曹達工業株式会社) なる白色顆粒状の薬品を
用いても研磨液の一成分として満足する。さらに、以上
の実施例は化合物半導体の1種である砒化ガリウムの研
磨についてであるが、燐化ガリウム、燐化インジウムな
どの化合物半導体の研磨における研磨液として使用可能
である。
In addition, the highly bleached powder, which is one component of the polishing liquid in the present invention, is a white powder chemical containing Ca (CAO), (calcium hypochlorite) as its main component (content 65.1 vol%). Even if a white granular chemical called Toyoclone PTG (trade name; manufacturer, Toyo Soda Kogyo Co., Ltd.), which has a concentration of (CtO) of 73.6 wt, which is higher than that of high-level bleaching powder, is used, it is satisfactory as a component of the polishing liquid. Furthermore, although the above embodiments are about polishing gallium arsenide, which is a type of compound semiconductor, it can be used as a polishing liquid for polishing compound semiconductors such as gallium phosphide and indium phosphide.

〔発明の効果〕〔Effect of the invention〕

本発明の研磨液は、被加工物に損傷を与えることなく、
高精度の研磨加工を可能とする。ことに、砒化ガリウム
、燐化ガリウム、燐化インジウムなどの化合物半導体用
のメカニカル・ケミカルボリジング用の研磨液として格
別の効果を奏する。
The polishing liquid of the present invention does not damage the workpiece.
Enables high-precision polishing. In particular, it is particularly effective as a polishing liquid for mechanical/chemical boriding of compound semiconductors such as gallium arsenide, gallium phosphide, and indium phosphide.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明の一実施例の研磨液による研磨の説明図
、第2図は同じく研磨液中の高度さらし粉の分量と研磨
速度との関係を示すグラフ、第3図は同じく研磨液のp
H値と研磨速度との関係を示すグラフ、第4図ないし第
6図は同じく研磨モデルの説明図である。 (1):研磨治具。 (2):砒化ガリウム結晶。 (4)、 t6) :反応生成物。 (5):研磨布。 代理人 弁理士 則 近 憲 佑 同    竹 花 喜久男 第 1 図 高度ごらし#っ扮−1(?) 第2図 高度さらし衿系縛磨旋nPHイ直 gs4図 第5図
FIG. 1 is an explanatory diagram of polishing using a polishing liquid according to an embodiment of the present invention, FIG. 2 is a graph showing the relationship between the amount of high-level bleaching powder in the polishing liquid and the polishing speed, and FIG. p
Graphs showing the relationship between the H value and the polishing rate, FIGS. 4 to 6, are also explanatory diagrams of the polishing model. (1): Polishing jig. (2): Gallium arsenide crystal. (4), t6): reaction product. (5): Polishing cloth. Agent Patent Attorney Nori Ken Yudo Takehana Kikuo No. 1 Figure Altitude View #pp-1 (?) Figure 2 Altitude Exposed Collar System Tied-up Rotation nPH Straight Gs4 Figure Figure 5

Claims (1)

【特許請求の範囲】[Claims] 水に少なくともさらし粉とトリポリりん酸ナトリウムと
硫酸ナトリウムとを混合してなることを特徴とする研磨
液。
A polishing liquid comprising a mixture of at least bleaching powder, sodium tripolyphosphate, and sodium sulfate in water.
JP62009993A 1987-01-21 1987-01-21 Polishing liquid Pending JPS63180466A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62009993A JPS63180466A (en) 1987-01-21 1987-01-21 Polishing liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62009993A JPS63180466A (en) 1987-01-21 1987-01-21 Polishing liquid

Publications (1)

Publication Number Publication Date
JPS63180466A true JPS63180466A (en) 1988-07-25

Family

ID=11735381

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62009993A Pending JPS63180466A (en) 1987-01-21 1987-01-21 Polishing liquid

Country Status (1)

Country Link
JP (1) JPS63180466A (en)

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