JPS6128639B2 - - Google Patents
Info
- Publication number
- JPS6128639B2 JPS6128639B2 JP11426878A JP11426878A JPS6128639B2 JP S6128639 B2 JPS6128639 B2 JP S6128639B2 JP 11426878 A JP11426878 A JP 11426878A JP 11426878 A JP11426878 A JP 11426878A JP S6128639 B2 JPS6128639 B2 JP S6128639B2
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- litao
- inert gas
- lithium tantalate
- cracks
- 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
Links
- 239000013078 crystal Substances 0.000 claims description 20
- 239000011261 inert gas Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 claims description 6
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 claims 1
- 239000012535 impurity Substances 0.000 description 5
- 229910000629 Rh alloy Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000012010 growth Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment 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
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 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
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
本発明はタンタル酸リチユームLiTaO3単結晶
の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing lithium tantalate LiTaO 3 single crystal.
LiTaO3単結晶はその融点が1650℃である為に
従来白金ロジユームの合金坩堝を用いて成長され
ていた。この単結晶の成長は大気中で行なう方
法と、不活性ガス雰囲気中にて行なう方法、の
２種類の方法が現存している。然し、上記・
の方法とも下記のような欠点を有している。 Since LiTaO 3 single crystal has a melting point of 1650°C, it has conventionally been grown using a platinum rhodium alloy crucible. There are currently two methods for growing this single crystal: one in the air and one in an inert gas atmosphere. However, the above
Both methods have the following drawbacks.
： 白金ロジユームの合金坩堝からロジユーム
等の不純物の混入が起り単結晶の割れやその他
の特性に劣化を招く。: Impurities such as rhodium enter the platinum rhodium alloy crucible, causing cracks in the single crystal and deterioration of other properties.
： ロジユーム等の不純物の混入は防げるが、
単結晶成長時に酸素O2分圧を下げるので
LiTaO3単結晶中に酸素欠陥が起り、クラツク
が単結晶中に発生する。: It can prevent contamination with impurities such as rhodium, but
Because it lowers the partial pressure of oxygen O2 during single crystal growth
Oxygen defects occur in the LiTaO 3 single crystal, and cracks occur in the single crystal.
従つて、この両者の方法に依つて成長される
LiTaO3単結晶の歩留りは向上せずコストアツプ
の原因となつていた。 Therefore, it is possible to grow by both methods.
The yield of LiTaO 3 single crystals did not improve, causing an increase in costs.
本発明は斯る点に鑑みて為されたものである。
即ち、LiTaO3単結晶中のクラツク発生を減少せ
しめ高品質の単結晶を提供せしめるものである。 The present invention has been made in view of this point.
That is, it is possible to reduce the occurrence of cracks in LiTaO 3 single crystals and provide high quality single crystals.
本発明者等は白金ロジユーム合金坩堝からの
LiTaO3単結晶への不純物の混入を防ぎ乍ら酸素
欠陥の発生を抑圧する為に窒素N2等の不活性ガ
ス中に少量O2を混入せしめる方法を見い出し
た。図は不活性ガスに対するO2の混入量と10回
のLiTaO3単結晶の成長に対するクラツクの発生
回数との相関関係を示すものである。この図から
も明らかな如くO2の含有量を0.2〜10％とした場
合クラツクの発生を極めて抑える事が出来ると共
に、白金ロジユーム坩堝からの不純物の混入も特
性の劣化を招かない程度にする事が出来る。 The present inventors have discovered that a platinum rhodium alloy crucible
We have found a method to mix a small amount of O 2 into an inert gas such as nitrogen N 2 in order to prevent impurities from entering the LiTaO 3 single crystal and suppress the generation of oxygen defects. The figure shows the correlation between the amount of O 2 mixed into the inert gas and the number of cracks generated for 10 LiTaO 3 single crystal growths. As is clear from this figure, when the O 2 content is set to 0.2 to 10%, the occurrence of cracks can be extremely suppressed, and the contamination of impurities from the platinum rhodium crucible can be kept to a level that does not cause deterioration of properties. I can do it.
次に具体的実施例を記す。 Next, specific examples will be described.
直径120mmφ高さ120mmの白金ロジユーム合金坩
堝にLiTaO3焼結体を入れ高周波加熱炉で該
LiTaO3を融解し、融解後LiTaO3のチツプ結晶を
回転せしめて直径60mmφ高さ100mmのLiTaO3単結
晶を引き上げた場合、N2雰囲気中では10回の引
き上げに対し平均的に３回のクラツクが発生した
が、N2に２％のO2を混入した混合ガス雰囲気中
に於いてはクラツクの発生を20回に対し１回に抑
える事が出来た。即ち２％のO2を混入せしめる
事に依つてクラツクの発生率を1/6に低下させる
事が出来る。 A LiTaO 3 sintered body was placed in a platinum rhodium alloy crucible with a diameter of 120 mm and a height of 120 mm and heated in a high-frequency heating furnace.
When LiTaO 3 is melted and a LiTaO 3 single crystal with a diameter of 60 mm and a height of 100 mm is pulled by rotating the LiTaO 3 chip crystal after melting, in an N 2 atmosphere, there will be an average of 3 cracks for every 10 pulls. However, in a mixed gas atmosphere containing 2% O 2 in N 2 , the occurrence of cracks could be suppressed to 1 out of 20. That is, by mixing 2% O 2 , the crack occurrence rate can be reduced to 1/6.
尚、不活性ガスとしてN2の他にアルゴンAr、
ヘリウムHe、ネオンNe及びクリプトンKr等のガ
スを用いても上記したと同様の結果が得られた。
更に、上記実施例のLiTaO3単結晶としてはLi／
Taの比の変つたタンタル酸リチユームであつて
もよい。又、ニオブNbを添加したLiTaO3やそれ
等の混晶体であるLiTaxNbi−xO3及び不純物添加
LiTaO3単結晶であつても同様の効果が得られ
る。 In addition to N2 , argon, Ar, etc. are used as inert gases.
Similar results were obtained using gases such as helium He, neon Ne, and krypton Kr.
Furthermore, the LiTaO 3 single crystal in the above example is Li/
It may also be lithium tantalate with a different Ta ratio. In addition, LiTaO 3 doped with niobium Nb, LiTaxNbi− x O 3 which is a mixed crystal thereof, and impurity addition
A similar effect can be obtained even with LiTaO 3 single crystal.
本発明は以上の説明から明らかな如く、少量の
酸素を不活性ガスに混入せしめた混合ガス雰囲気
中でタンタル酸リチユームを成長せしめたので、
不活性ガス雰囲気中にて成長せしめた場合に比べ
特性を害なう事なくクラツクの発生率を低下させ
る事が出来る。従つて、歩留りが向上するので製
造コストの低減化が図れる。 As is clear from the above description, the present invention grows lithium tantalate in a mixed gas atmosphere in which a small amount of oxygen is mixed with an inert gas.
Compared to the case of growth in an inert gas atmosphere, the occurrence rate of cracks can be reduced without impairing the characteristics. Therefore, since the yield is improved, manufacturing costs can be reduced.
図は不活性ガス中の酸素の含有量とクラツクの
発生回数との関係を示す曲線図である。
The figure is a curve diagram showing the relationship between the oxygen content in the inert gas and the number of crack occurrences.
Claims (1)
タル酸リチユーム単結晶を成長せしめるに際し、
不活性ガスに0.2〜10％の酸素を含ませた混合ガ
ス雰囲気中にて成長せしめる事を特徴としたタン
タル酸リチユーム単結晶の製造方法。 ２ 上記不活性ガスに対する酸素の含有量を0.2
〜10％とした事を特徴とする特許請求の範囲第１
項記載のタンタル酸リチユーム単結晶の製造方
法。[Claims] 1. When growing a lithium tantalate single crystal using an alloy crucible containing platinum rhodium,
A method for producing a lithium tantalate single crystal characterized by growing it in a mixed gas atmosphere containing an inert gas containing 0.2 to 10% oxygen. 2 Oxygen content for the above inert gas is 0.2
Claim 1 characterized in that the percentage is 10%.
A method for producing a lithium tantalate single crystal as described in .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11426878A JPS5542238A (en) | 1978-09-14 | 1978-09-14 | Production of lithium tantalate single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11426878A JPS5542238A (en) | 1978-09-14 | 1978-09-14 | Production of lithium tantalate single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5542238A JPS5542238A (en) | 1980-03-25 |
| JPS6128639B2 true JPS6128639B2 (en) | 1986-07-01 |
Family
ID=14633545
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11426878A Granted JPS5542238A (en) | 1978-09-14 | 1978-09-14 | Production of lithium tantalate single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5542238A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4439265A (en) * | 1981-07-17 | 1984-03-27 | Bell Telephone Laboratories, Incorporated | Fabrication method for LiNbO3 and LiTaO3 integrated optics devices |
| JPS5969490A (en) * | 1982-10-14 | 1984-04-19 | Sumitomo Metal Mining Co Ltd | Manufacture of lithium tantalate single crystal |
| US4724038A (en) * | 1986-06-02 | 1988-02-09 | Hughes Aircraft Company | Process for preparing single crystal binary metal oxides of improved purity |
-
1978
- 1978-09-14 JP JP11426878A patent/JPS5542238A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5542238A (en) | 1980-03-25 |
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