JP3260039B2 - Manufacturing method of ferroelectric wafer - Google Patents

Manufacturing method of ferroelectric wafer

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Publication number
JP3260039B2
JP3260039B2 JP14896894A JP14896894A JP3260039B2 JP 3260039 B2 JP3260039 B2 JP 3260039B2 JP 14896894 A JP14896894 A JP 14896894A JP 14896894 A JP14896894 A JP 14896894A JP 3260039 B2 JP3260039 B2 JP 3260039B2
Authority
JP
Japan
Prior art keywords
wafer
ferroelectric
etching
tank
single crystal
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.)
Expired - Fee Related
Application number
JP14896894A
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Japanese (ja)
Other versions
JPH0813163A (en
Inventor
邦宏 伊藤
俊彦 流王
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.)
Shin Etsu Chemical Co Ltd
Original Assignee
Shin Etsu Chemical Co Ltd
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Priority to JP14896894A priority Critical patent/JP3260039B2/en
Publication of JPH0813163A publication Critical patent/JPH0813163A/en
Application granted granted Critical
Publication of JP3260039B2 publication Critical patent/JP3260039B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Description

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

【0001】[0001]

【産業上の利用分野】本発明は強誘電体ウエーハの製造
方法、特には弾性表面波素子の基板として有用とされる
タンタル酸リチウムおよびニオブ酸リチウムの単結晶か
らなる強誘電体ウエーハの製造方法に関するものであ
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a ferroelectric wafer, and more particularly to a method for manufacturing a ferroelectric wafer comprising a single crystal of lithium tantalate and lithium niobate which is useful as a substrate for a surface acoustic wave device. It is about.

【0002】[0002]

【従来の技術】タンタル酸リチウム単結晶、ニオブ酸リ
チウム単結晶などの強誘電体ウエーハは弾性表面波素子
用の基板として用いられているが、これらのウエーハは
表面波の伝搬する面を鏡面研磨し、裏面側はバルク波の
反射によるスプリアスを防止するために粗面加工して仕
上げられるのが一般的とされている。しかし、このよう
に表面側と裏面側の仕上げが異なる場合には、残留する
加工歪の差によりウエーハが大きく反ってしまうので、
裏面側の粗面加工による歪を低減してウエーハの反りを
改善するために、粗面加工後にフッ硝酸などの溶液を用
いてエッチング処理する方法が知られている(特公昭56
-36808号公報参照)。
2. Description of the Related Art Ferroelectric wafers such as lithium tantalate single crystal and lithium niobate single crystal are used as substrates for surface acoustic wave devices, but these wafers have mirror-polished surfaces on which surface waves propagate. However, it is generally considered that the back side is finished by roughening to prevent spurious due to reflection of bulk waves. However, when the finish on the front side and the back side is different as described above, the wafer is largely warped due to a difference in remaining processing strain.
In order to reduce the distortion due to the roughening of the back side and to improve the warpage of the wafer, there is known a method of performing an etching treatment using a solution such as hydrofluoric nitric acid after the roughening (Japanese Patent Publication No. Sho 56).
-36808).

【0003】ただし、タンタル酸リチウム、ニオブ酸リ
チウムなどの単結晶は化学的に安定であり、フッ硝酸の
ような強酸を用いてもエッチング速度が非常に遅いため
に、このエッチング処理はこの溶液を一般的に60〜 110
℃に加熱して行なわれている。
[0003] However, single crystals such as lithium tantalate and lithium niobate are chemically stable, and the etching rate is very low even with a strong acid such as hydrofluoric nitric acid. Generally 60 to 110
It is performed by heating to ° C.

【0004】[0004]

【発明が解決しようとする課題】しかしながら、これら
の単結晶ウエーハは熱膨張率の異方性や強誘電体として
の特性である圧電性、焦電性および粗面加工による加工
歪層の影響で非常に割れ易く、常温から加熱したエッチ
ング溶液に入れるときや、エッチング溶液から取り出し
て常温で水洗するときに、その温度差によって多数のウ
エーハが割れてしまい、歩留りが大幅に低下することが
問題となっている。したがって、これについてはエッチ
ング溶液にウエーハを入れたままで昇温、徐冷する方法
もあるが、これには時間がかかって効率的ではなく、量
産加工に不適当になるという不利がある。
However, these single crystal wafers are affected by the anisotropy of the coefficient of thermal expansion and the piezoelectricity, pyroelectricity, and ferroelectric properties of the ferroelectric material, and the effect of the strained layer due to roughening. The problem is that many wafers are cracked due to the temperature difference when they are easily broken and are put into an etching solution heated from room temperature or when they are taken out of the etching solution and washed with water at room temperature, and the yield is greatly reduced. Has become. Therefore, there is a method of raising the temperature and gradually cooling the wafer while the wafer remains in the etching solution. However, this method is disadvantageous in that it is time-consuming, inefficient, and unsuitable for mass production processing.

【0005】[0005]

【課題を解決するための手段】本発明はこのような不
利、問題点を解決した強誘電体ウエーハの製造方法に関
するものであり、これは強誘電体ウエーハをエッチング
処理するにあたり、エッチング槽の前後に段階的に加温
または冷却した槽を設け、ウエーハをエッチング槽に出
し入れするときの温度差を35℃以内とすることを特徴と
するものである。
SUMMARY OF THE INVENTION The present invention relates to a method of manufacturing a ferroelectric wafer which solves such disadvantages and problems, and includes a method for etching a ferroelectric wafer before and after an etching tank. A stepwise heated or cooled tank is provided, and a temperature difference when the wafer is put in and taken out of the etching tank is set to 35 ° C. or less.

【0006】すなわち、本発明者らは強誘電体ウエーハ
のエッチング処理における割れを防止する方法について
種々検討し、タンタル酸リチウム、ニオブ酸リチウムな
どの単結晶ウエーハのエッチング工程における割れの発
生状況を詳細に観察したところ、この割れはウエーハを
加温したエッチング溶液に入れた直後、およびエッチン
グ溶液から取り出して水洗槽に入れた直後に発生してい
ること、また特にはウエーハの厚み方向にC軸成分を含
む回転Yカット板で割れが発生し易く、ウエーハ厚が薄
く、裏面粗さの大きいほど割れ易いということを見出
し、これについてはエッチング液槽の前後に段階的に加
温または冷却した槽を設けてウエーハをエッチング液に
出し入れするときの温度差を35℃以内とすればウエーハ
割れの低減に大きな効果の得られることを確認して本発
明を完成させた。以下にこれをさらに詳述する。
That is, the present inventors have studied various methods for preventing cracks in the etching treatment of ferroelectric wafers, and have described in detail the occurrence of cracks in the etching process of single crystal wafers such as lithium tantalate and lithium niobate. The cracks were observed immediately after the wafer was placed in the heated etching solution and immediately after the wafer was taken out of the etching solution and placed in the washing tank. In particular, the C-axis component was observed in the thickness direction of the wafer. It is found that cracks easily occur in the rotating Y-cut plate containing, and that the wafer is thinner and the back surface roughness is more easily cracked. For this, a tank heated or cooled stepwise before and after the etching solution tank is found. If the temperature difference between when the wafer is put in and out of the etching solution and the temperature difference is within 35 ° C Make sure that the obtained results of the present invention has been completed. This will be described in more detail below.

【0007】[0007]

【作用】本発明は強誘電体ウエーハの製造方法に関する
ものであり、これは前記したようにタンタル酸リチウ
ム、ニオブ酸リチウムなどの単結晶からなる強誘電体ウ
エーハをエッチング処理するときに、エッチング槽の前
後に段階的に加温または冷却した槽を設けてウエーハを
これらの槽に順次挿入し、ウエーハをエッチング液に出
し入れするときの温度差を35℃以内とするものである
が、これによれば強誘電体ウエーハのエッチング処理時
における割れの低減に大きな効果が得られるという有利
性が与えられる。
The present invention relates to a method for manufacturing a ferroelectric wafer, which is used for etching a ferroelectric wafer made of a single crystal such as lithium tantalate or lithium niobate as described above. Before and after, steps are provided for heating or cooling tanks, wafers are sequentially inserted into these tanks, and the temperature difference when the wafers are taken in and out of the etching solution is set to 35 ° C or less. For example, there is an advantage that a great effect is obtained in reducing cracks during the etching process of the ferroelectric wafer.

【0008】本発明は強誘電体ウエーハの製造方法、し
たがってこれはタンタル酸リチウムまたはニオブ酸リチ
ウムなどの単結晶からなる強誘電体ウエーハの製造方法
に関するものであり、これは表面側が表面波を伝搬する
ために鏡面研磨され、裏面側がバルク波の反射によるス
プリアスを防止するために粗面加工されたものである
が、このウエーハについてはその反りを改善するために
フッ硝酸などによるエッチング処理が行なわれ、これは
60〜 110℃の加温下に行なわれるのであるが、これには
熱膨張率の異方性や粗面加工による加工歪層の影響でウ
エーハが非常に割れ易く、歩留りが大幅に低下するとい
う問題があった。
The present invention relates to a method for manufacturing a ferroelectric wafer, and thus to a method for manufacturing a ferroelectric wafer made of a single crystal such as lithium tantalate or lithium niobate, which transmits a surface wave on the surface side. The wafer is mirror-polished and the back side is roughened to prevent spurious emission due to reflection of bulk waves. This wafer is etched with hydrofluoric nitric acid or the like to improve its warpage. ,this is
It is performed under heating of 60-110 ° C. This is because the wafer is very susceptible to cracking due to the anisotropy of the coefficient of thermal expansion and the strained layer caused by roughening, and the yield is greatly reduced. There was a problem.

【0009】したがってこの割れについて調査したとこ
ろ、これについては前記したようにウエーハを加温した
エッチング溶液に入れた直後、およびエッチング溶液か
ら取り出して水洗槽に入れた直後に割れが発生している
こと、また特にウエーハの厚み方向にC軸成分を含む回
転Yカット板で割れが発生し易く、ウエーハの厚さが薄
く、裏面粗さの大きいほど割れ易いことが見出された
が、これは急激な温度変化によりウエーハの熱膨張率の
異方性や強誘電体としての特性である圧電性、焦電性お
よび粗面加工による加工歪層が影響して割れが多発して
いるものと考えられる。
Therefore, when the cracks were examined, it was found that the cracks occurred immediately after the wafer was put in the heated etching solution and immediately after the wafer was taken out of the etching solution and put in the washing tank. In particular, it has been found that cracks easily occur in a rotating Y-cut plate containing a C-axis component in the thickness direction of the wafer, and that the thinner the wafer and the larger the back surface roughness, the easier it is to crack. It is considered that many cracks occur due to the influence of the anisotropic thermal expansion coefficient of the wafer and the ferroelectric properties of piezoelectricity, pyroelectricity, and strain due to rough surface processing due to a large temperature change. .

【0010】そこで、これについてはエッチング槽の前
後に中間温度に加温または冷却した水槽を複数種用意
し、これらの水槽に順次ウエーハを浸していくと、これ
らの水槽が段階的に加温または冷却されており、これら
の間の温度差が小さくされているので、この割れを低減
させることができるが、この一段階の温度をどのように
すれば最もよい効果が得られるかということについてこ
の温度差を種々変更して検討を続けた結果、これは35℃
以内とすればウエーハの割れ低減に大きな効果の得られ
ることが判った。
Therefore, in this regard, a plurality of water tanks heated or cooled to an intermediate temperature are prepared before and after the etching tank, and when the wafers are sequentially immersed in these water tanks, these water tanks are heated or cooled stepwise. Although it is cooled and the temperature difference between them is reduced, this cracking can be reduced, but it is not clear how best to obtain this one-stage temperature. As a result of continuing to study with various changes in the temperature difference, this was 35 ° C.
It was found that a large effect can be obtained in reducing the cracking of the wafer.

【0011】なお、この本発明の実施においては昇温時
および冷却時の両方に適用することが最も望ましく、こ
れはそのいずれか一方でも効果は得ることができるが、
昇温時よりも冷却時に適用したほうがより大きな効果を
得ることができる。なお、このエッチング処理は通常裏
面の粗面加工をした後に行なわれるが、これは表面側を
鏡面研磨する前でも後でもよく、いずれの場合にも本発
明によれば同様の効果を得ることができる。また、この
強誘電体ウエーハについては36°Yカットタンタル酸リ
チウム単結晶ウエーハ、64°Yカットニオブ酸リチウム
単結晶ウエーハのようにウエーハの厚み方向にC軸成分
を含む回転Yカット板について適用した場合に、より大
きな効果が得られる。
In the practice of the present invention, it is most preferable to apply the present invention to both heating and cooling, and although it is possible to obtain the effect of either of them,
A greater effect can be obtained when applied during cooling than during heating. Note that this etching process is usually performed after roughening the back surface, but may be performed before or after the front surface is mirror-polished. In any case, the same effect can be obtained according to the present invention. it can. This ferroelectric wafer was applied to a rotating Y-cut plate containing a C-axis component in the thickness direction of the wafer, such as a 36 ° Y-cut lithium single crystal tantalate wafer and a 64 ° Y-cut lithium niobate single crystal wafer. In this case, a greater effect can be obtained.

【0012】[0012]

【実施例】つぎに本発明の実施例、比較例をあげる。 実施例1〜3、比較例1〜3 通常のチョクラルスキー法により育成した直径3インチ
φの36°Y軸引上げタンタル酸リチウム単結晶をスライ
スし、この両面を#2,000 の炭化けい素質砥粒でラッピ
ング加工して厚さ 400μmの36°Yカットウエーハを作
った。ついで、このウエーハの裏面を#240 の炭化けい
素質砥粒でラッピングして粗面加工したところ、ウエー
ハ表裏の加工歪の差により、このものは90〜 120μmも
の反りを生じた。
Next, examples of the present invention and comparative examples will be described. Examples 1-3, Comparative Examples 1-3 A 36 ° Y-axis pulled lithium tantalate single crystal having a diameter of 3 inches and grown by the usual Czochralski method is sliced, and both surfaces thereof are # 2,000 silicon carbide abrasive grains. To form a 400-μm thick 36 ° Y-cut wafer. Then, when the back surface of the wafer was lapped with # 240 silicon carbide abrasive grains and roughened, the wafer was warped by 90 to 120 μm due to the difference in processing strain between the front and back surfaces of the wafer.

【0013】そこで、これについては市販の50%フッ化
水素酸と36%塩酸を容量比で2:1の割合で混合したフ
ッ塩酸を用いてエッチング処理することとし、温度80℃
で60分間エッチング処理することとしたが、これについ
ては加温したエッチング槽の前後に中間温度に加温また
は冷却した水槽を必要に応じて設置し、ウエーハを25枚
ずつテフロン製のバスケットに入れて各槽に浸し、中間
温度の水槽での保持時間を1分として、 100枚のウエー
ハをエッチング処理した。
[0013] In view of this, etching is performed using hydrofluoric acid, which is a commercially available mixture of 50% hydrofluoric acid and 36% hydrochloric acid at a volume ratio of 2: 1.
In this case, a water tank heated or cooled to an intermediate temperature was installed before and after the heated etching tank as needed, and 25 wafers were placed in a Teflon basket at a time. Then, the wafer was immersed in each tank, and the holding time in the water tank at the intermediate temperature was set to 1 minute, and 100 wafers were etched.

【0014】この場合、この処理条件を変更して表1に
示した6条件のものとしたところ、いずれの条件でもこ
のエッチング処理によりウエーハの反りは15μm以下と
なり、表面側を鏡面研磨したのちの反りも20μm以下
で、このエッチング処理により加工歪が除去され反りを
矯正する効果が与えられたが、ウエーハをエッチング液
に出し入れする際の温度差が35℃以内となるように加温
または冷却したもの(実施例1〜3)はウエーハの割れ
が大幅に減少し、歩留りも向上したが、これが35℃以上
である比較例1〜3のものはウエーハの割れが多く、歩
留りが低下した。
In this case, the processing conditions were changed to those of the six conditions shown in Table 1. Under any of the conditions, the warping of the wafer was reduced to 15 μm or less by this etching treatment, and the surface side was mirror-polished. The warpage was also 20 μm or less, and the effect of correcting the warpage by removing the processing strain by this etching treatment was given. In Examples (Examples 1 to 3), wafer cracking was significantly reduced and the yield was improved, but in Comparative Examples 1 to 3 where the temperature was 35 ° C. or higher, the wafer cracks were large and the yield was reduced.

【0015】[0015]

【表1】 [Table 1]

【0016】実施例4〜6、比較例4 通常のチョクラルスキー法により育成した直径3インチ
φの64°Y軸引上げニオブ酸リチウム単結晶をスライス
し、この両面を#2,000 の炭化けい素質砥粒でラッピン
グ加工して厚さ 400μmの64°Yカットウエーハを作っ
た。ついで、このウエーハの裏面を#240 の炭化けい素
質砥粒でラッピングして粗面加工したところ、ウエーハ
表裏の加工歪の差により80〜 110μmもの反りを生じ
た。
Examples 4 to 6 and Comparative Example 4 A 64 ° Y-axis pulled lithium niobate single crystal having a diameter of 3 inches and grown by the ordinary Czochralski method was sliced, and both surfaces thereof were polished with silicon carbide # 2,000. The grains were wrapped to produce a 400 μm thick 64 ° Y-cut wafer. Then, when the back surface of the wafer was lapped with # 240 silicon carbide abrasive grains and roughened, a warp of 80 to 110 μm was generated due to a difference in processing strain between the front and back surfaces of the wafer.

【0017】そこで、これについては市販の50%フッ化
水素酸と60%硝酸を容量比で2:1の割合で混合したフ
ッ硝酸を用いてエッチング処理することとし、温度60℃
で90分間エッチング処理することとしたが、これについ
ては加温したエッチング槽の前後に中間温度に加温また
は冷却した水槽を必要に応じて設置し、ウエーハを25枚
ずつテフロン製のバスケットに入れて各槽に浸し、中間
温度の水槽での保持時間を1分間として、 100枚のウエ
ーハをエッチング処理した。
In view of this, an etching process is performed using a commercially available 50% hydrofluoric acid and 60% nitric acid mixed at a volume ratio of 2: 1 with hydrofluoric nitric acid at a temperature of 60 ° C.
In this case, a water tank heated or cooled to an intermediate temperature was installed before and after the heated etching tank as needed, and 25 wafers were placed in a Teflon basket at a time. The wafers were immersed in each of the tanks, and the holding time in the water tank at the intermediate temperature was set to 1 minute, and 100 wafers were etched.

【0018】この場合、この処理条件を変更して表2に
示した4条件のものとしたところ、いずれの場合でもこ
のエッチング処理によりウエーハの反りは15μm以下と
なり、表面側を鏡面研磨したのちの反りも20μm以下
で、このエッチング処理により加工歪が除去され、反り
を矯正する効果が与えられたが、ウエーハをエッチング
液に出し入れする際の温度差が35℃以内となるように加
温または冷却したもの(実施例4、5、6)はウエーハ
の割れが大幅に減少し、歩留り向上したが、これが35℃
以上である比較例4のものはウエーハの割れが多く、歩
留りが低下した。
In this case, the processing conditions were changed to the four conditions shown in Table 2. In any case, the warpage of the wafer was reduced to 15 μm or less by this etching treatment, and the surface side was mirror-polished. The warpage is also 20 μm or less, and the processing distortion is removed by this etching treatment, and the effect of correcting the warp is given. In Examples (Examples 4, 5, and 6), wafer cracking was significantly reduced, and the yield was improved.
In the case of Comparative Example 4 described above, the wafer had many cracks, and the yield was reduced.

【0019】[0019]

【表2】 [Table 2]

【0020】[0020]

【発明の効果】本発明は強誘導体ウエーハの製造方法に
関するものであり、これは強誘電体ウエーハをエッチン
グ処理するときに、ウエーハ処理槽を段階的に加温また
は冷却するようにし、ウエーハをエッチング液に出し入
れする際の温度差を35℃以内とすることを特徴とするも
のであるが、これによればウエーハの反りを小さくする
と共に、このエッチング処理によるウエーハの割れを大
幅に低下させることができるという有利性が与えられ
る。
The present invention relates to a method of manufacturing a ferroelectric wafer, and more particularly to a method of etching a ferroelectric wafer by heating or cooling a wafer processing tank in a stepwise manner. It is characterized in that the temperature difference at the time of taking in and out of the liquid is within 35 ° C., according to which the warpage of the wafer is reduced and the cracking of the wafer due to this etching process is significantly reduced. The advantage of being able to do so is given.

───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) C23F 1/00 H01B 3/12 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. 7 , DB name) C23F 1/00 H01B 3/12

Claims (3)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 強誘電体ウエーハをエッチング処理する
にあたり、エッチング槽の前後に段階的に加温または冷
却した槽を設け、ウエーハをエッチング液に出し入れす
るときの温度差を35℃以内とすることを特徴とする強誘
電体ウエーハの製造方法。
1. When etching a ferroelectric wafer, a stepwise heated or cooled tank is provided before and after the etching tank, and the temperature difference when the wafer is taken in and out of the etching solution is within 35 ° C. A method for producing a ferroelectric wafer, comprising:
【請求項2】 強誘電体ウエーハがタンタル酸リチウム
またはニオブ酸リチウムの単結晶ウエーハである請求項
1に記載した強誘電体ウエーハの製造方法。
2. The method for producing a ferroelectric wafer according to claim 1, wherein the ferroelectric wafer is a single crystal wafer of lithium tantalate or lithium niobate.
【請求項3】 強誘電体ウエーハが36°Yカットタンタ
ル酸リチウムまたは64°Yカットニオブ酸リチウムの単
結晶ウエーハである請求項1に記載した強誘電体ウエー
ハの製造方法。
3. The method for producing a ferroelectric wafer according to claim 1, wherein the ferroelectric wafer is a single crystal wafer of 36 ° Y-cut lithium tantalate or 64 ° Y-cut lithium niobate.
JP14896894A 1994-06-30 1994-06-30 Manufacturing method of ferroelectric wafer Expired - Fee Related JP3260039B2 (en)

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JP3260039B2 true JP3260039B2 (en) 2002-02-25

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