JP2929313B2 - Mirror finishing agent for polishing CdTe crystal and method for mirror finishing CdTe crystal - Google Patents

Mirror finishing agent for polishing CdTe crystal and method for mirror finishing CdTe crystal

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Publication number
JP2929313B2
JP2929313B2 JP2219483A JP21948390A JP2929313B2 JP 2929313 B2 JP2929313 B2 JP 2929313B2 JP 2219483 A JP2219483 A JP 2219483A JP 21948390 A JP21948390 A JP 21948390A JP 2929313 B2 JP2929313 B2 JP 2929313B2
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Japan
Prior art keywords
polishing
mirror finishing
aqueous solution
finishing agent
cdte
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JP2219483A
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Japanese (ja)
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JPH04101765A (en
Inventor
俊郎 土肥
敏雄 河西
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  • Mechanical Treatment Of Semiconductor (AREA)

Description

【発明の詳細な説明】 [産業上の利用分野] 本発明は、高硬度脆弱材料の機械化学的研摩技術に関
し、CdTe結晶研磨用の鏡面加工剤およびCdTe結晶の鏡面
加工方法に適用して好適な技術に関する。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a mechanochemical polishing technique for a high hardness brittle material, and is preferably applied to a mirror polishing agent for polishing CdTe crystal and a mirror polishing method for CdTe crystal. Technology.

[従来の技術] 従来、CdTeのような化合物半導体結晶基板の研摩に
は、高い研摩能率と加工表面の完全結晶性を得るため
に、化学的エッチング作用を有する臭素とメタノールの
混合溶液、あるいは臭素とメタノールとエチレングリコ
ールとの混合溶液、あるいは次亜塩素酸ナトリウム水溶
液などを研摩剤とするポリッシング方法が用いられてき
た。
[Prior art] Conventionally, in the polishing of a compound semiconductor crystal substrate such as CdTe, a mixed solution of bromine and methanol having a chemical etching action or a bromine in order to obtain high polishing efficiency and perfect crystallinity of a processed surface. A polishing method using a mixed solution of urea, methanol and ethylene glycol, or an aqueous solution of sodium hypochlorite as an abrasive has been used.

しかし、上記研摩方法をCdTe結晶の妙面加工に適用し
た場合、その表面粗さは良好とは言えず、ピット(突
起)やヘイズ(曇り)といった表面異常が発生し、エピ
タキシャル成長用基板として使用すると歩留りを低下さ
せるという問題点があった。
However, when the above polishing method is applied to the processing of a special surface of a CdTe crystal, the surface roughness cannot be said to be good, and surface abnormalities such as pits (projections) and haze (cloudiness) occur. There is a problem that the yield is reduced.

さらに、上記研摩方法において使用する臭素は、金属
を著しく腐蝕させるため、研摩装置を構成する材料が限
定される。その上、臭素は不快な刺激臭を有し、人体に
対して極めて有害な薬品であるため、取扱いには厳重な
注意が必要で、液の混合をはじめ、廃液処理、ガス排気
にあたり、研摩装置に種々の対策を施さねばならない。
その結果、大がかりな周辺装置が必要となって研摩装置
が高価格となり、安全上にも問題があるという欠点があ
る。
Further, bromine used in the above polishing method significantly corrodes metal, so that the material constituting the polishing apparatus is limited. In addition, bromine has an unpleasant irritating odor and is a chemical that is extremely harmful to the human body. Therefore, strict attention must be paid to its handling, including mixing of liquids, waste liquid treatment, gas exhaust, and polishing equipment. Various measures must be taken.
As a result, there is a disadvantage that a large-scale peripheral device is required, the polishing device becomes expensive, and there is a problem in safety.

しかも、臭素とメタノールの混合液は、混合してから
数十分足らずで分解してしまうため、使用するにしても
極めて扱いにくいため大量生産に不向きであった。
In addition, a mixed solution of bromine and methanol is decomposed in less than several tens of minutes after being mixed, so that even if used, it is extremely difficult to handle, and is not suitable for mass production.

本発明は上記の欠点を解決したもので、その目的とす
るところは、被加工物の表面うねりが小さくかつ表面異
常の少ない鏡面加工が可能で、安全上も問題がなく、し
かも大量生産に適した鏡面加工剤および鏡面加工方法を
提供することにある。
The present invention has solved the above-mentioned drawbacks. The object of the present invention is to provide a mirror-finished surface with a small surface waviness and a small surface abnormality on the workpiece, without any safety problems, and suitable for mass production. To provide a mirror finishing agent and a mirror finishing method.

[課題を解決するための手段] 本発明者らは、人体に有害な臭素等を用いずにCdTeの
ような脆弱な化合物半導体結晶を高精度に研摩できる鏡
面加工剤について鋭意研究した。その結果、次亜塩素酸
カルシウムを含む薬剤として、一般に漂白剤として用い
られているさらし粉を水に溶かした水溶液を鏡面加工剤
として用いると、高精度の鏡面研摩が可能になることを
見出した。
Means for Solving the Problems The present inventors have intensively studied a mirror finishing agent that can polish a fragile compound semiconductor crystal such as CdTe with high precision without using bromine or the like harmful to the human body. As a result, it has been found that high precision mirror polishing can be achieved by using an aqueous solution obtained by dissolving bleaching powder generally used as a bleaching agent in water as a chemical containing calcium hypochlorite as a mirror finishing agent.

この発明は、上記知見に基づいてなされたもので、有
効塩素量が60%以上である高度さらし粉を主成分とする
水溶液、望ましくは該水溶液にこれに溶解しないSiO2
ような微粒子を混入したもの、もしくは上記水溶液に界
面活性剤あるいはNaClを添加したものを主剤とした鏡面
加工剤を提案するものである。
The present invention has been made based on the above findings, and contains an aqueous solution mainly composed of highly bleached powder having an effective chlorine amount of 60% or more, preferably mixed with fine particles such as SiO 2 which does not dissolve in the aqueous solution. The present invention proposes a mirror finishing agent whose main component is one obtained by adding a surfactant or NaCl to the above aqueous solution.

[作用] 上記した鏡面加工剤にあっては、従来の研摩剤と同様
の方法で使用でき、かつ人体に与える害が極めて少ない
とともに、従来の臭素−メタノール系研摩剤に比べて混
合液の安全性が良いため工業的な使用すなわち大量生産
に適している。
[Effect] The above-mentioned mirror finishing agent can be used in the same manner as a conventional abrasive, causes very little harm to the human body, and is safer than a conventional bromine-methanol abrasive. Because of its good properties, it is suitable for industrial use, that is, mass production.

また、高度さらし粉水溶液を主成分とする水溶液中に
界面活性剤、NaClを添加した場合には加工速度を向上さ
せ、かつ良好な表面状態を得ることができる。特に高度
さらし粉水溶液中に砥粒を添加した場合には、さらし粉
の水溶液中に含まれるClO-イオンの酸化作用によって被
加工物表面に形成された酸化物が、砥粒の機械的研摩作
用によって効果的に削られるため、加工速度の飛躍的な
向上が可能であるとともに、良好な表面状態を得ること
ができる。
In addition, when a surfactant and NaCl are added to an aqueous solution mainly composed of a highly bleached powder aqueous solution, the processing speed can be improved and a good surface state can be obtained. In particular, when the addition of the abrasive grains in high bleaching powder in an aqueous solution, ClO contained in an aqueous solution of bleaching powder - oxide formed on the surface of the workpiece by the oxidative action of ions, effective by mechanical abrasive action of abrasive grains As a result, the processing speed can be drastically improved, and a good surface condition can be obtained.

[実施例] 有効塩素量が60%以上である高度さらし粉水溶液を純
水に添加して溶解させ、濃度が10重量%以下の水溶液を
作る。この水溶液はそのまま鏡面加工剤として用いても
効果を奏するが、この高度さらし粉水溶液をベースとし
て、これに添加剤を加えることにより更に鏡面加工剤と
しての性能も向上させることができる。
[Example] A highly bleached powder aqueous solution having an effective chlorine amount of 60% or more is added to pure water and dissolved to prepare an aqueous solution having a concentration of 10% by weight or less. Although this aqueous solution is effective even when used as a mirror finishing agent as it is, the performance as a mirror finishing agent can be further improved by adding an additive to this highly bleached powder aqueous solution as a base.

上記添加剤としては、高度さらし粉水溶液に溶解しな
い微粒子(例えばSiO2)や界面活性剤、NaCl等がある。
このうち、難溶性微粒子は鏡面加工剤のもつ機械的研摩
作用を向上させ、界面活性剤やNaClは鏡面加工剤のもつ
化学的研摩作用を向上させるのに役立つ。これらの添加
物は、被加工物の高度、靱性、酸化性などの物性を考慮
して適当なものを選択すればよい。例えばCdTe結晶の研
摩においては難溶性微粒子としてSiO2の他、Cr2O3,Al2
O3,ZnO2,SiC,CeO2,Fe2O3やダイヤモンド等の微粒子を
用いることが可能である。
Examples of the additive include fine particles (for example, SiO 2 ) that are not dissolved in the highly exposed bleaching powder aqueous solution, a surfactant, and NaCl.
Among them, the hardly soluble fine particles improve the mechanical polishing action of the mirror finishing agent, and the surfactant and NaCl help to improve the chemical polishing action of the mirror finishing agent. These additives may be appropriately selected in consideration of physical properties such as the height, toughness, and oxidizing property of the workpiece. For example, in polishing CdTe crystal, in addition to SiO 2 , Cr 2 O 3 , Al 2
Fine particles such as O 3 , ZnO 2 , SiC, CeO 2 , Fe 2 O 3 and diamond can be used.

一方、界面活性剤としては、非イオン系溶剤を用いる
と良い。非イオン系溶剤としては、ポリオキシエチレン
ノニルフェノールエーテル、ポリオキシエチレンオレオ
イルエーテル、ポリオキシエチレンモノオレート、ソル
ビタンモノオレエート、ポリオキシエチレンソルビタン
モノオレエートなどがある。界面活性剤の濃度は、使用
する溶剤の種類、被加工物の物性等に応じて実験的に定
めてやればよい。例えば、非イオン系溶剤を高度さらし
粉水溶液に添加してCdTe結晶を鏡面加工する場合には、
非イオン系溶剤の濃度が5容量%程度に達すると加工速
度が飽和するからである。
On the other hand, a nonionic solvent is preferably used as the surfactant. Examples of the nonionic solvent include polyoxyethylene nonylphenol ether, polyoxyethylene oleoyl ether, polyoxyethylene monooleate, sorbitan monooleate, and polyoxyethylene sorbitan monooleate. The concentration of the surfactant may be determined experimentally according to the type of the solvent used, the physical properties of the workpiece, and the like. For example, when a nonionic solvent is added to a highly exposed powder aqueous solution to mirror-process a CdTe crystal,
This is because the processing speed is saturated when the concentration of the nonionic solvent reaches about 5% by volume.

また、高度さらし粉水溶液にNaClを添加する場合に
は、その濃度が10重量%以下となるように添加量を決定
してやればよい。それ以上、添加しても加工速度が向上
しないからである。
In addition, when NaCl is added to the highly exposed bleaching powder aqueous solution, the amount of addition may be determined so that the concentration becomes 10% by weight or less. This is because the processing speed is not improved even if it is added more.

上記高度さらし粉水溶液を主成分とする鏡面加工剤を
用いて、第1図に示すような構造の鏡面加工装置により
CdTe単結晶の加工を行なった。以下、その結果について
述べる。なお、ここで第1図の鏡面加工装置の構成を簡
単に説明しておく。
Using a mirror finishing agent having a structure as shown in FIG.
CdTe single crystal was processed. Hereinafter, the results will be described. Here, the configuration of the mirror finishing apparatus of FIG. 1 will be briefly described.

第1図の鏡面加工装置は、回転軸1の上端に固着され
た研摩盤2の表面に、ポリウレタン含浸ポリエステル不
織布や人口皮革等がポリシャ3として貼付されている。
そして、試料4をワックス等にてステンレス製接着プレ
ート治具5に接着させたものを下向きにして上記ポリシ
ャ3上に載置し、その上に重錘6を載せて適当な加工圧
力を与える。
In the mirror finishing apparatus shown in FIG. 1, a non-woven fabric of polyurethane impregnated polyester or artificial leather is adhered as a polisher 3 on the surface of a polishing plate 2 fixed to the upper end of a rotating shaft 1.
Then, the sample 4 attached to the stainless steel adhesive plate jig 5 with wax or the like is placed on the polisher 3 with the surface facing downward, and the weight 6 is placed thereon to apply an appropriate processing pressure.

また、ポリシャ3の上方には下部にノズル7aを有する
鏡面加工剤収納容器7が配置され、ノズル7aに設けられ
た流量調節用コック8を開いて容器7内の鏡面加工剤9
をポリシャ3の表面上へ滴下できるように構成されてい
る。上記接着プレート治具5は、所定の位置において研
摩盤2の回転に伴って自転する構造を有する。なお、上
記接着プレート治具5は、図示しない機構により、自転
しながら研摩盤2と異なる回転速度で公転する運動を与
えるようにしてもよい。
Above the polisher 3, a mirror finishing agent storage container 7 having a nozzle 7a at a lower portion is disposed, and a cock 8 for flow rate adjustment provided on the nozzle 7a is opened to open the mirror finishing agent 9 in the container 7.
Can be dropped onto the surface of the polisher 3. The adhesive plate jig 5 has a structure that rotates at a predetermined position as the polishing plate 2 rotates. In addition, the bonding plate jig 5 may give a motion of revolving at a rotation speed different from that of the polishing plate 2 while rotating by a mechanism not shown.

実施例に使用した鏡面加工装置は、研摩盤2の直径が
300mmで、これを40r.p.mの回転数で回転させた。また、
実施例1と4ではポリシャとして人口皮革を使用して加
圧圧力を230g/cm2とし、実施例2と3ではポリシャとし
てポリウレタン含浸ポリエステル不織布を用い、加圧圧
力を240g/cm2とした。
In the mirror finishing apparatus used in the embodiment, the diameter of the polishing
At 300 mm, this was rotated at a speed of 40 rpm. Also,
In Examples 1 and 4, artificial leather was used as the polisher and the pressure was 230 g / cm 2, and in Examples 2 and 3, a polyurethane impregnated polyester nonwoven fabric was used as the polisher and the pressure was 240 g / cm 2 .

さらに、試料4としては、すべての実施例において、
加工面が(100)面となるように切断された1辺の長さ1
0mm、厚さ0.7mmの正方形のCdTe単結晶基板を用いた。
Further, as Sample 4, in all Examples,
Length of one side cut so that the processing surface becomes (100) plane 1
A square CdTe single crystal substrate having a thickness of 0 mm and a thickness of 0.7 mm was used.

[実施例1] 鏡面加工剤として、有効塩素量65%の高度さらし粉
を、純水中に0.5重量%,1重量%,5重量%,7重量%,10重
量%の濃度となるように溶解したものに界面活性剤とし
て非イオン系溶剤を、1容量%の濃度となるように添加
したものを用意した。
[Example 1] As a mirror finishing agent, a highly bleached powder having an effective chlorine content of 65% was dissolved in pure water to a concentration of 0.5% by weight, 1% by weight, 5% by weight, 7% by weight, and 10% by weight. A nonionic solvent was added as a surfactant to the resulting mixture so as to have a concentration of 1% by volume.

第1図の鏡面加工装置でポリシャとして人口皮革を用
い、上記混合液を鏡面加工剤として、回転数40r.p.m、
加圧圧力230g/cm2の条件の下でCdTe単結晶の鏡面加工を
行なった。
Using artificial leather as a polisher in the mirror finishing apparatus of FIG. 1, the above mixture was used as a mirror finishing agent, and the number of revolutions was 40 rpm.
CdTe single crystal was mirror-finished under the condition of a pressure of 230 g / cm 2 .

その結果、高度さらし粉の濃度によって加工速度が異
なることを見出した。第2図に高度さらし粉の濃度と加
工速度との関係を示す。同図より、高度さらし粉水溶液
の濃度が高いほど加工速度が向上するとともに、濃度が
5重量%程度で加工速度が飽和することが分かる。
As a result, they found that the processing speed was different depending on the concentration of the highly exposed bleaching powder. FIG. 2 shows the relationship between the concentration of highly exposed powder and the processing speed. From the figure, it is understood that the processing speed is improved as the concentration of the highly bleached powder aqueous solution is higher, and the processing speed is saturated when the concentration is about 5% by weight.

[実施例2] 鏡面加工剤として、有効塩素量65%の高度さらし粉
を、純水中に0.5重量%の濃度となるように溶解したも
のと、これに界面活性剤として非イオン系溶剤を、0.5
容積%,1容積%,5容積%の濃度となるように添加したも
のを用意した。
Example 2 As a mirror finishing agent, a highly bleached powder having an effective chlorine amount of 65% was dissolved in pure water to a concentration of 0.5% by weight, and a nonionic solvent as a surfactant was added thereto. 0.5
What was added so that it might become the density | concentration of 1 volume%, 1 volume%, and 5 volume% was prepared.

第1図の鏡面加工装置でポリシャとしてポリウレタン
含浸ポリエステル不織布を用い、上記混合液を鏡面加工
剤として、回転数40r.p.m、加圧圧力240g/cm2の条件の
下でCdTe単結晶の鏡面加工を行なった。
Using a polyurethane impregnated polyester nonwoven as a polisher in mirror finishing device of FIG. 1, the liquid mixture as a mirror finishing agent, the rotational speed 40R.Pm, mirror finishing of the CdTe single crystal under the conditions of applied pressure 240 g / cm 2 Was performed.

その結果、非イオン系溶剤の濃度によって加工速度が
異なることを見出した。第3図に非イオン系溶剤の濃度
と加工速度との関係を示す。
As a result, they found that the processing speed was different depending on the concentration of the nonionic solvent. FIG. 3 shows the relationship between the concentration of the nonionic solvent and the processing speed.

同図より、高度さらし粉水溶液に非イオン系溶剤を添
加することにより加工速度が向上するとともに、添加量
が5容積%程度で加工速度が飽和することが分かる。ま
た、上記鏡面加工剤を用いて鏡面加工されたCdTe単結晶
の表面を顕微鏡で観察したところ、スクラッチやピッ
ト、ヘイズなどがなく、極めて良好な表面状態になって
いることが確認された。ちなみに、高度さらし粉0.5重
量%水溶液に非イオン系溶剤を1容積%添加したものを
鏡面加工剤としたときの表面粗さRmaxは20〜30Åで、非
イオン系溶剤を添加しない高度さらし粉0.5重量%水溶
液のみの場合にも表面粗さは30〜40Åであり、従来の鏡
面加工剤による加工後の表面粗さは50〜100Åに比べて
大幅に表面粗さが良好となることが分かった(表1参
照)。
From the figure, it is understood that the processing speed is improved by adding the nonionic solvent to the highly bleached powder aqueous solution, and the processing speed is saturated when the added amount is about 5% by volume. In addition, when the surface of the CdTe single crystal mirror-finished using the mirror finishing agent was observed with a microscope, it was confirmed that there was no scratch, pit, haze, etc., and the surface state was extremely good. By the way, the surface roughness Rmax when a non-ionic solvent was added to a 0.5% by weight aqueous solution of a non-ionic solvent in a 1% by volume aqueous solution as a mirror finishing agent was 20-30 高度, and the high-grade bleaching powder without a non-ionic solvent was 0.5% by weight. The surface roughness was 30 to 40 mm even in the case of only the aqueous solution, and it was found that the surface roughness after processing with the conventional mirror finishing agent was significantly better than that of 50 to 100 mm (see Table 1). 1).

さらに参考のため、高度さらし粉0.5重量%水溶液に
非イオン系溶剤を添加し、それを濾過したものを鏡面加
工剤として同様の加工を行なって加工速度を調べた。そ
の結果、第3図に▲印で示す。同図より、濾過した高度
さらし粉水溶液を用いると加工速度がやや低下するもの
の非イオン系溶剤の濃度が高くなるほど加工速度が速く
なることがわかる。
For reference, a non-ionic solvent was added to a 0.5% by weight aqueous solution of high-grade bleaching powder, and the filtered product was subjected to the same processing as a mirror finishing agent to examine the processing speed. As a result, it is shown by a mark in FIG. From the figure, it can be seen that the processing speed is slightly reduced when the filtered aqueous bleaching powder aqueous solution is used, but the processing speed is increased as the concentration of the nonionic solvent is increased.

第4図には高度さらし粉水溶液を濾過した後の残渣を
X線回折で分析したときのデータを示す。
FIG. 4 shows data obtained by analyzing the residue after filtering the highly exposed bleaching powder aqueous solution by X-ray diffraction.

同図において、○印が付されているのは、CaCO3のス
ペクトル成分、△印で示されているのはCa(OH)2のスペ
クトル成分である。
In the figure, the circles indicate the spectral components of CaCO 3 , and the triangles indicate the spectral components of Ca (OH) 2 .

同図より高度さらし粉水溶液中にはCaCO3とCa(OH)2
固形物の形で含まれていることが分かる。
From the figure, it can be seen that CaCO 3 and Ca (OH) 2 are contained in the form of solid matter in the highly exposed flour solution.

このことより、濾過した水溶液を用いると加工速度が
低下するのは、高度さらし粉水溶液中に固形物が含まれ
ており、それが機械的に表面を削る砥粒として作用する
ためと考えられる。
From the above, it is considered that the reason why the processing speed is decreased when the filtered aqueous solution is used is that the solid matter is contained in the highly exposed bleaching powder aqueous solution, which acts as abrasive grains for mechanically shaving the surface.

[実施例3] 鏡面加工剤として、有効塩素量65%の高度さらし粉
を、純水中に0.5重量%の濃度となるように溶解したも
のと、これにNaClを、1重量%,5重量%,10重量%,20重
量%の濃度となるように添加したものを用意した。
[Example 3] As a mirror finishing agent, a highly bleached powder having an effective chlorine amount of 65% was dissolved in pure water to a concentration of 0.5% by weight, and NaCl was added thereto in an amount of 1% by weight and 5% by weight. , 10% by weight and 20% by weight were prepared.

第1図の鏡面加工装置でポリシャとしてポリウレタン
含浸ポリエステル不織布を用い、上記混合液を鏡面加工
剤として、回転数40r.p.m、加圧圧力240g/cm2の条件の
下でCdTe単結晶の鏡面加工を行なった。
Using a polyurethane impregnated polyester nonwoven as a polisher in mirror finishing device of FIG. 1, the liquid mixture as a mirror finishing agent, the rotational speed 40R.Pm, mirror finishing of the CdTe single crystal under the conditions of applied pressure 240 g / cm 2 Was performed.

その結果、NaClを高度さらし粉水溶液に添加すること
により加工速度が向上することが分かった。第5図にNa
Cl添加量と加工速度との関係を示す。同図より、NaClの
濃度が高くなるほど加工速度か速くなるが、およそ10重
量%で飽和することが分かる。
As a result, it was found that the processing speed was improved by adding NaCl to the highly bleached powder aqueous solution. Fig. 5 shows Na
The relationship between the amount of Cl added and the processing speed is shown. The figure shows that the processing speed increases as the concentration of NaCl increases, but it saturates at about 10% by weight.

また、研摩後の試料の表面を観察したところ、ピット
が少なく表面状態は良好であった。
When the surface of the sample after polishing was observed, the surface state was good with few pits.

[実施例4] 鏡面加工剤として、有効塩素量65%の高度さらし粉
を、純水中に5重量%と濃度となるように溶解したもの
に界面活性剤として非イオン系溶剤を、1容積%の濃度
となるように添加し、さらに、平均粒径0.04μmのSiO2
微粒子を2重量%の含有率となるように混合したものを
用意した。
[Example 4] A non-ionic solvent as a surfactant was dissolved in pure water at a concentration of 5% by weight as a non-ionic solvent in a solution prepared by dissolving a highly bleached powder having an effective chlorine amount of 65% as a mirror finishing agent in an amount of 1% by volume. Of SiO 2 having an average particle size of 0.04 μm.
A mixture in which the fine particles were mixed so as to have a content of 2% by weight was prepared.

第1図の鏡面加工装置でポリシャとして人口皮革を用
い、上記混合液を虚面加工剤として、回転数40r.p.m、
加圧圧力233g/cm2の条件の下でCdTe単結晶の鏡面加工を
行なった。
Using artificial leather as a polisher in the mirror finishing device of FIG.
CdTe single crystal was mirror-finished under the condition of a pressure of 233 g / cm 2 .

その結果、SiO2微粒子を添加すると、加工速度は50〜
60μm/時間となり、無添加の場合の5〜6倍の速さにな
ることが分かった。これは、SiO2微粒子が砥粒として機
械的研摩作用をなすとともに、試料表面を活性化させ化
学的エッチング作用を活発化させるためと考えられる。
As a result, when SiO 2 fine particles are added, the processing speed becomes 50-
It was found that the speed was 60 μm / hour, which was 5 to 6 times faster than the case without addition. This is considered to be because the SiO 2 fine particles perform mechanical polishing as abrasive grains and activate the sample surface to activate the chemical etching.

また、加工後の試料表面を観察したところ、表面粗さ
Rmaxは20Å以下であり、表面状態は極めて良好でエピタ
キシャル成長用基板として充分に満足できるものであっ
た。
When the sample surface after processing was observed, the surface roughness was
Rmax was 20 ° or less, the surface condition was extremely good, and the substrate was sufficiently satisfactory as a substrate for epitaxial growth.

なお、SiO2粒径を変えた場合平均粒径の大きい粒子を
用いると加工速度は速くなる反面、加工面の表面粗さが
若干劣る傾向を示した。また、逆に、より細かい微粒子
を用いると加工速度が劣るものの加工面の表面粗さは均
一で良好なものであった。
When the SiO 2 particle size was changed, the use of particles having a large average particle size increased the processing speed, but showed a tendency that the surface roughness of the processed surface was slightly inferior. Conversely, when finer fine particles were used, the processing speed was inferior, but the surface roughness of the processed surface was uniform and good.

[比較例] 従来よりCdTe単結晶の研摩剤として用いられていた0.
05〜0.25容量%の臭素−メタノール混合液および次亜塩
素酸ナトリウム水溶液を用いて、上記実施例と同様の条
件下でCdTe単結晶の研摩を行なった。その結果、加工速
度は、臭素−メタノール使用時に20〜40μm/時間、次亜
塩素酸ナトリウム水溶液使用時に3〜7μm/時で、研摩
後の表面粗さRmaxはいずれも50〜100Åであった。上記
比較例の結果を、本発明の実施例の代表的なものによる
結果とともに表1に示す。
[Comparative Example] Conventionally used as an abrasive for CdTe single crystals.
A CdTe single crystal was polished under the same conditions as in the above example using a bromine-methanol mixed solution of 05 to 0.25% by volume and an aqueous solution of sodium hypochlorite. As a result, the processing speed was 20 to 40 μm / hour when using bromine-methanol, 3 to 7 μm / hour when using an aqueous solution of sodium hypochlorite, and the surface roughness Rmax after polishing was 50 to 100 °. The results of the above comparative examples are shown in Table 1 together with the results of typical examples of the present invention.

表1より、本発明の実施例はいずれも従来の研摩剤に
比べて表面粗さが小さくなり、加工面にピットやヘイズ
が見られなく、表面状態が良好になることが分かる。ま
た、本発明は実施例4を除き、加工速度は2つの比較例
の中間程度であるが、実施例4は加工速度においても従
来例に比べて優れていることが分かる。
Table 1 shows that the examples of the present invention all have a smaller surface roughness than conventional abrasives, have no pits or haze on the processed surface, and have a good surface condition. In addition, the working speed of the present invention is intermediate between the two comparative examples except for the working example 4, but it can be seen that the working speed of the working example 4 is superior to that of the conventional example.

なお、上記実施例では、CdTe単結晶に加工を例にとっ
て説明したが、本発明はそれに限定されるものでなく、
他の化合物半導体や、シリコン、サファイヤ、タンタル
酸リチウム、ガラス等、高硬度で脆弱な材料の加工に適
用することが可能である。
Note that, in the above embodiment, the processing of CdTe single crystal was described as an example, but the present invention is not limited to this.
The present invention can be applied to the processing of other hard and brittle materials such as other compound semiconductors, silicon, sapphire, lithium tantalate, and glass.

また、本発明では、加工剤の主成分として高度さらし
粉を使用した例について説明したが、さらし粉、さらし
液等の他の次亜塩素酸カルシウムを含む薬剤を主剤とし
て用いることも可能である。
Further, in the present invention, an example in which high-grade bleaching powder is used as a main component of the processing agent has been described. However, other agents containing calcium hypochlorite, such as bleaching powder and bleaching solution, can be used as the main agent.

[発明の効果] 以上説明したように本発明は、有効塩素量が60%以上
である高度さらし粉を主成分とする水溶液、望ましくは
該水溶液にこれに溶解しないSiO2のような微粒を混入し
たもの、もしくは上記水溶液に界面活性剤あるいはNaCl
を添加したものを鏡面加工剤としたので、従来の研摩剤
と同様の方法で使用でき、かつ人体に与える害が極めて
少ないという効果がある。
[Effects of the Invention] As described above, in the present invention, an aqueous solution mainly composed of highly exposed flour having an effective chlorine content of 60% or more, preferably, fine particles such as SiO 2 which is not dissolved in the aqueous solution are mixed in the aqueous solution. Or the above aqueous solution with a surfactant or NaCl
Is used as a mirror finishing agent, so that it can be used in the same manner as a conventional abrasive, and has the effect of extremely little harm to the human body.

また、高度さらし粉水溶液を主成分とする水溶液は従
来の臭素−メタノール系研摩剤に比べ混合液の安定性が
良いため工業的な使用すなわち大量生産に適している。
In addition, an aqueous solution mainly composed of a highly bleached powder aqueous solution is suitable for industrial use, that is, mass production, because the stability of the mixture is better than that of a conventional bromine-methanol abrasive.

さらに、高度さらし粉水溶液を主成分とする水溶液中
に砥粒や界面活性剤、NaClを添加した場合には良好な表
面状態を得ることができるとともに、加工速度が速くな
って、作業効率を向上させることができるという効果が
ある。
In addition, when abrasive grains, a surfactant, and NaCl are added to an aqueous solution mainly composed of a highly bleached powder aqueous solution, a good surface state can be obtained, and a processing speed is increased, thereby improving work efficiency. There is an effect that can be.

【図面の簡単な説明】[Brief description of the drawings]

第1図は本発明の実施例に使用した鏡面加工装置の構成
例を示す概略正面図、 第2図は実施例1で使用した鏡面加工剤の高度さらし粉
濃度と加工速度との関係を示すグラフ、 第3図は実施例2で使用した鏡面加工剤中の非イオン系
溶剤の濃度と加工速度との関係を示すグラフ、 第4図は高度さらし粉水溶液を濾過した後の残渣のX線
回折による分析結果を示す図、 第5図は実施例3で使用した鏡面加工剤のNaCl濃度と加
工速度との関係を示すグラフである。 1……回転軸、2……研摩盤、3……ポリシャ、4……
試料、5……接着プレート治具、6……重錘、7……鏡
面加工剤収納容器。
FIG. 1 is a schematic front view showing a configuration example of a mirror finishing apparatus used in an embodiment of the present invention, and FIG. 2 is a graph showing a relationship between a highly exposed powder concentration of a mirror finishing agent used in the embodiment 1 and a processing speed. Fig. 3 is a graph showing the relationship between the concentration of the nonionic solvent in the mirror finishing agent used in Example 2 and the processing speed, and Fig. 4 is obtained by X-ray diffraction of the residue after filtering the highly exposed bleaching powder aqueous solution. FIG. 5 is a graph showing the results of analysis. FIG. 5 is a graph showing the relationship between the NaCl concentration of the mirror finishing agent used in Example 3 and the processing speed. 1 ... rotating shaft 2 ... polishing machine 3 ... polisher 4 ...
Sample, 5: Adhesive plate jig, 6: Weight, 7: Mirror finishing agent storage container.

───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6,DB名) B24B 37/00 H01L 21/304 622 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 6 , DB name) B24B 37/00 H01L 21/304 622

Claims (9)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】次亜塩素酸カルシウムを含む薬剤を水に溶
解させたことを特徴とするCdTe結晶研磨用の鏡面加工
剤。
1. A mirror finishing agent for polishing CdTe crystals, wherein a drug containing calcium hypochlorite is dissolved in water.
【請求項2】有効塩素量が60%以上の次亜塩素酸カルシ
ウムを主成分とする薬剤を水に溶解させ、濃度0.5〜10
重量%の水溶液としたことを特徴とするCdTe結晶研磨用
の鏡面加工剤。
2. A method comprising dissolving a drug mainly composed of calcium hypochlorite having an effective chlorine content of 60% or more in water, and dissolving the drug in a concentration of 0.5 to 10%.
A mirror finishing agent for polishing CdTe crystals, characterized in that it is an aqueous solution of weight%.
【請求項3】次亜塩素酸カルシウムを含む薬剤を水に溶
解させた水溶液に、界面活性剤を添加してなることを特
徴とするCdTe結晶研磨用の鏡面加工剤。
3. A mirror finishing agent for polishing a CdTe crystal, wherein a surfactant is added to an aqueous solution obtained by dissolving a drug containing calcium hypochlorite in water.
【請求項4】上記界面活性剤の濃度を5容積%以下とし
たことを特徴とする請求項3記載のCdTe結晶研磨用の鏡
面加工剤。
4. The mirror finishing agent for polishing a CdTe crystal according to claim 3, wherein the concentration of the surfactant is 5% by volume or less.
【請求項5】次亜塩素酸カルシウムを含む薬剤を水に溶
解させた水溶液に、NaClを添加してなることを特徴とす
るCdTe結晶研磨用の鏡面加工剤。
5. A mirror finishing agent for polishing CdTe crystals, wherein NaCl is added to an aqueous solution in which a drug containing calcium hypochlorite is dissolved in water.
【請求項6】NaClの濃度を10重量%以下としたことを特
徴とする請求項5記載のCdTe結晶研磨用の鏡面加工剤。
6. The mirror finishing agent for polishing a CdTe crystal according to claim 5, wherein the concentration of NaCl is 10% by weight or less.
【請求項7】次亜塩素酸カルシウムを含む薬剤を水に溶
解させた水溶液に、該水溶液に溶解しない粒子もしくは
難溶性の粒子を添加してなることを特徴とするCdTe結晶
研磨用の鏡面加工剤。
7. A mirror finishing for CdTe crystal polishing, characterized in that particles which are insoluble or hardly soluble in an aqueous solution are added to an aqueous solution in which a drug containing calcium hypochlorite is dissolved in water. Agent.
【請求項8】上記次亜塩素酸カルシウムを含む薬剤を水
に溶解させた水溶液に溶解しない粒子もしくは難溶性の
粒子が、SiO2,Cr2O3,Al2O3,ZnO2,SiC,CeO2,Fe2O3
たはダイアモンドであることを特徴とする請求項7に記
載のCdTe結晶研磨用の鏡面加工剤。
8. Particles which do not dissolve in an aqueous solution obtained by dissolving a drug containing calcium hypochlorite in water or particles which are hardly soluble are SiO 2 , Cr 2 O 3 , Al 2 O 3 , ZnO 2 , SiC, mirror finishing agent for CdTe crystal polishing according to claim 7, wherein the CeO 2, a Fe 2 O 3 or diamond.
【請求項9】請求項1〜請求項8の何れかに記載のCdTe
結晶研磨用の鏡面加工剤を使用して、ポリッシャを有す
る回転研摩盤において、鏡面加工を行なうことを特徴と
するCdTe結晶の鏡面加工方法。
9. The CdTe according to any one of claims 1 to 8,
A mirror polishing method for a CdTe crystal, wherein mirror polishing is performed on a rotary polishing machine having a polisher using a mirror polishing agent for crystal polishing.
JP2219483A 1990-08-21 1990-08-21 Mirror finishing agent for polishing CdTe crystal and method for mirror finishing CdTe crystal Expired - Fee Related JP2929313B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2219483A JP2929313B2 (en) 1990-08-21 1990-08-21 Mirror finishing agent for polishing CdTe crystal and method for mirror finishing CdTe crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2219483A JP2929313B2 (en) 1990-08-21 1990-08-21 Mirror finishing agent for polishing CdTe crystal and method for mirror finishing CdTe crystal

Publications (2)

Publication Number Publication Date
JPH04101765A JPH04101765A (en) 1992-04-03
JP2929313B2 true JP2929313B2 (en) 1999-08-03

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Country Link
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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