JPH06199598A - Method for producing lithium niobate single crystal - Google Patents
Method for producing lithium niobate single crystalInfo
- Publication number
- JPH06199598A JPH06199598A JP30311792A JP30311792A JPH06199598A JP H06199598 A JPH06199598 A JP H06199598A JP 30311792 A JP30311792 A JP 30311792A JP 30311792 A JP30311792 A JP 30311792A JP H06199598 A JPH06199598 A JP H06199598A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- lithium niobate
- crystal
- niobate single
- grown
- 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.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 59
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000000034 method Methods 0.000 claims abstract description 32
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 239000011777 magnesium Substances 0.000 claims abstract description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 5
- 230000008018 melting Effects 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 239000010955 niobium Substances 0.000 claims abstract description 4
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000001603 reducing effect Effects 0.000 claims abstract description 4
- 239000011701 zinc Substances 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000001257 hydrogen Substances 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000007789 gas Substances 0.000 abstract description 7
- 230000003287 optical effect Effects 0.000 abstract description 7
- 230000008832 photodamage Effects 0.000 abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 5
- 230000000996 additive effect Effects 0.000 abstract description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 229910052786 argon Inorganic materials 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 238000005231 Edge Defined Film Fed Growth Methods 0.000 abstract description 2
- 229910052734 helium Inorganic materials 0.000 abstract description 2
- 239000001307 helium Substances 0.000 abstract description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000155 melt Substances 0.000 description 14
- 238000007711 solidification Methods 0.000 description 10
- 230000008023 solidification Effects 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000009828 non-uniform distribution Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Optical Integrated Circuits (AREA)
Abstract
(57)【要約】
【目的】 割れやスパイラル状の曲がりがなく、サブグ
レイン密度の少ない高品質なニオブ酸リチウム単結晶を
高収率で製造し得る方法を提供する。
【構成】 少なくとも、リチウム、ニオブ及び酸素の３
元素を含むニオブ酸リチウム単結晶を溶融固化法により
育成するに際して、雰囲気を中性或いは還元性によって
育成することを特徴としている。雰囲気ガスを窒素、ヘ
リウム又はアルゴン等々の中性とし、或いは水素又は一
酸化炭素等若しくは水素又は一酸化炭素等を混入した中
性ガスにする。上記３元素の他に、マグネシウム或いは
亜鉛を添加すると、添加物が結晶全体に均一に分散し、
耐光損傷性の強い高品質なニオブ酸リチウム単結晶を育
成できる。溶融固化法としては、Ｃz法の他に、ＦＺ法
或いはＥＦＧ法等の溶融固化法も適用できる。このう
ち、結晶品質の管理及び大口径化の観点から、Ｃz法が
優れている。この単結晶は導波路型光デバイスやＳＨＧ
素子などの光学用材料に用いられる。(57) [Summary] [Object] To provide a method capable of producing a high-quality lithium niobate single crystal having a small subgrain density without cracks or spiral bends in a high yield. [Structure] At least three of lithium, niobium and oxygen
When growing a lithium niobate single crystal containing an element by a melting and solidifying method, it is characterized in that the atmosphere is grown to be neutral or reducing. The atmosphere gas is neutral such as nitrogen, helium or argon, or hydrogen or carbon monoxide or the like or neutral gas mixed with hydrogen or carbon monoxide or the like. When magnesium or zinc is added in addition to the above three elements, the additive is dispersed uniformly throughout the crystal,
A high quality lithium niobate single crystal having strong light damage resistance can be grown. As the melting and solidifying method, besides the Cz method, a melting and solidifying method such as an FZ method or an EFG method can be applied. Among them, the Cz method is superior from the viewpoint of controlling the crystal quality and increasing the diameter. This single crystal is a waveguide type optical device or SHG.
Used for optical materials such as elements.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、導波路型光デバイスや
ＳＨＧ素子などの光学用材料に用いられるニオブ酸リチ
ウム単結晶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 producing a lithium niobate single crystal used as an optical material such as a waveguide type optical device and an SHG element.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】ニオブ
酸リチウム単結晶は、非線形光学定数の大きさや光学的
特性から導波路型光デバイスやＳＨＧ素子として、近
年、大きな注目を集めている。上記素子として用いられ
るニオブ酸リチウム単結晶は、その結晶性や大口径化の
観点から、チョクラルスキー法(Ｃz法)に代表される溶
融固化法で育成されることが多い。2. Description of the Related Art Lithium niobate single crystal has recently attracted a great deal of attention as a waveguide type optical device or an SHG element because of its nonlinear optical constant and optical characteristics. The lithium niobate single crystal used as the element is often grown by a melting and solidifying method represented by the Czochralski method (Cz method) from the viewpoint of its crystallinity and large diameter.
【０００３】しかし、溶融固化法で育成されたニオブ酸
リチウム単結晶は、結晶内に熱歪に起因する割れが発生
し易いという欠点を有していた。そのため、融液直上の
温度勾配を緩くすることによって結晶の割れを回避する
方法が検討されたが、この方法では、安定な育成を持続
させることが困難で、結晶がスパイラル状に曲がった
り、サブグレイン密度が上がるなど、高品質なニオブ酸
リチウムを得ることができなかった。また、ニオブ酸リ
チウム結晶は耐光損傷性が低いという欠点も有してお
り、数mol％の酸化マグネシウム或いは酸化亜鉛を添加
することによって、耐光損傷性の改善を図る方法も検討
されたが、添加物の不均一分散の問題が新たに起こり、
満足な結果が得られていなかった。However, the lithium niobate single crystal grown by the melt solidification method has a drawback that cracks due to thermal strain are likely to occur in the crystal. Therefore, a method of avoiding cracking of the crystal by grading the temperature gradient directly above the melt was investigated, but with this method, it is difficult to maintain stable growth, and the crystal bends spirally or It was not possible to obtain high-quality lithium niobate, such as an increase in grain density. In addition, lithium niobate crystals also have the drawback of low light damage resistance, and a method of improving light damage resistance by adding a few mol% of magnesium oxide or zinc oxide was also investigated. A new problem of non-uniform distribution of materials,
The result was not satisfactory.
【０００４】本発明は、上記従来技術の欠点を解消し
て、割れやスパイラル状の曲がりがなく、サブグレイン
密度の少ない高品質なニオブ酸リチウム単結晶を高収率
で製造し得る方法を提供することを目的としている。The present invention solves the above-mentioned drawbacks of the prior art and provides a method capable of producing a high-quality lithium niobate single crystal having a small subgrain density without cracks or spiral bends in a high yield. The purpose is to do.
【０００５】[0005]
【課題を解決するための手段】本発明者らは、前述の目
的を達成すべく鋭意研究を重ねた結果、溶融固化法によ
るニオブ酸リチウム単結晶の育成において、育成雰囲気
によって融液の対流を制御できることを見い出した。こ
の融液対流制御は、原料融液が少なくなっても持続させ
ることができるので、高い固化率で結晶を育成すること
が可能となった。また、制御された融液対流は、添加物
を加えたニオブ酸リチウム単結晶の育成において、添加
物の不均一分散の抑制に有効であることを見い出した。Means for Solving the Problems As a result of intensive studies to achieve the above-mentioned object, the present inventors have found that in the growth of lithium niobate single crystal by the melt solidification method, the convection of the melt is caused by the growth atmosphere. I found that I could control it. Since this melt convection control can be continued even when the raw material melt becomes low, it has become possible to grow crystals with a high solidification rate. It was also found that the controlled melt convection is effective in suppressing the non-uniform dispersion of the additive in growing the lithium niobate single crystal containing the additive.
【０００６】すなわち、本発明は、少なくとも、リチウ
ム、ニオブ及び酸素の３元素を含むニオブ酸リチウム単
結晶を溶融固化法により育成するに際して、雰囲気を中
性或いは還元性によって育成することを特徴とするニオ
ブ酸リチウム単結晶の製造方法を要旨とするものであ
る。That is, the present invention is characterized in that, when a lithium niobate single crystal containing at least three elements of lithium, niobium and oxygen is grown by the melt solidification method, the atmosphere is grown by neutrality or reducibility. The gist is a method for producing a lithium niobate single crystal.
【０００７】以下に本発明を更に詳細に説明する。The present invention will be described in more detail below.
【０００８】[0008]
【０００９】前述のとおり、本発明は、少なくとも、リ
チウム、ニオブ及び酸素の３元素を含むニオブ酸リチウ
ム単結晶を溶融固化法により育成する方法に関するもの
であり、溶融固化法としては、Ｃz法の他に、ＦＺ法或
いはＥＦＧ法等の溶融固化法も適用できる。このうち、
結晶品質の管理及び大口径化の観点から、Ｃz法が優れ
ている。As described above, the present invention relates to a method for growing a lithium niobate single crystal containing at least three elements of lithium, niobium and oxygen by the melt solidification method, and the melt solidification method is the Cz method. Besides, a melt solidification method such as an FZ method or an EFG method can also be applied. this house,
The Cz method is superior from the viewpoint of controlling the crystal quality and increasing the diameter.
【００１０】溶融固化法によってニオブ酸リチウム単結
晶を育成する際に、雰囲気ガスを窒素、ヘリウム又はア
ルゴン等々の中性とし、或いは水素又は一酸化炭素等若
しくは水素又は一酸化炭素等を混入した中性ガスにする
ことにより、割れやスパイラル状の曲がりがなく、サブ
グレイン密度の少ない高品質なニオブ酸リチウム単結晶
を高収率で育成できる。When a lithium niobate single crystal is grown by the melt solidification method, the atmosphere gas is made to be neutral such as nitrogen, helium or argon, or hydrogen or carbon monoxide or the like or hydrogen or carbon monoxide or the like is mixed. By using a neutral gas, it is possible to grow a high-quality lithium niobate single crystal with a small subgrain density without cracking or spiral bending at a high yield.
【００１１】これは、雰囲気ガスを中性或いは還元性に
し、酸素分圧を低下させることにより、融液対流が著し
く促進されるためである。融液対流の促進には、表面張
力或いは粘性係数の変化が関与していると考えられる。
融液対流が促進されると、温度勾配が緩い炉構成或いは
原料融液が少なくなる育成終期において、自然対流が優
勢な状態を育成全般にわたって維持するため、割れやス
パイラル状の曲がりがなく、サブグレイン密度の少ない
高品質なニオブ酸リチウム単結晶を高収率で育成するこ
とが可能となる。This is because the convection of the melt is remarkably promoted by making the atmospheric gas neutral or reducing and reducing the oxygen partial pressure. It is considered that changes in surface tension or viscosity coefficient are involved in promoting melt convection.
When melt convection is promoted, natural convection is maintained over the entire growth at the end of the growth where the temperature gradient is gentle in the furnace configuration or the raw material melt is reduced, so there is no cracking or spiral bending, It becomes possible to grow a high quality lithium niobate single crystal having a low grain density in a high yield.
【００１２】このような育成法において、上記３元素に
加えて、更にＭg或いはＺn等を、好ましくは酸化マグネ
シウム或いは酸化亜鉛の形で添加したニオブ酸リチウム
単結晶を育成すると、添加物が結晶全体に均一に分散
し、耐光損傷性の強い高品質なニオブ酸リチウム単結晶
を育成できる。上述の如く促進された融液対流は、強い
撹拌効果を伴うので、添加物分布が一様なニオブ酸リチ
ウム単結晶を育成することが可能となる。なお、酸化マ
グネシウム或いは酸化亜鉛の添加量は適宜決め得るが、
３元素に対して、０.５〜１０.０wt％の添加量が望まし
い。In such a growing method, when a lithium niobate single crystal in which Mg, Zn or the like is further added in the form of magnesium oxide or zinc oxide in addition to the above three elements is grown, the additive is added to the entire crystal. It is possible to grow a high-quality lithium niobate single crystal that is evenly dispersed in, and has high light damage resistance. Since the melt convection promoted as described above is accompanied by a strong stirring effect, it becomes possible to grow a lithium niobate single crystal having a uniform additive distribution. The addition amount of magnesium oxide or zinc oxide can be appropriately determined,
The addition amount of 0.5 to 10.0 wt% is desirable with respect to the three elements.
【００１３】なお、溶融固化法における上記以外の製造
条件(原料調整、育成条件等々)は、常法による場合と同
様でよく、特に限定されるものではない。The production conditions (material adjustment, growth conditions, etc.) other than the above in the melt solidification method may be the same as those in the conventional method, and are not particularly limited.
【００１４】次に本発明の代表的な実施例を示す。Next, a typical embodiment of the present invention will be shown.
【００１５】[0015]
【実施例１】[Example 1]
【００１６】結晶育成は、高周波誘導加熱によるＣz法
によって行った。原料として、純度４Ｎの炭酸リチウム
と五酸化ニオブを原子比で４８.６：５１.４になるよう
に混合し、成型、焼成をした後、白金るつぼに充填し
た。育成条件は、引き上げ速度３.０mm／h、結晶回転数
３rpm、育成方位ｃ軸とした。また、雰囲気として、窒
素に１０％の水素を混合したガスを２０００ml／minの
流速で流した。充填した原料の約７０％を引き上げて、
育成を終了した。Crystal growth was carried out by the Cz method using high frequency induction heating. As raw materials, lithium carbonate having a purity of 4N and niobium pentoxide were mixed at an atomic ratio of 48.6: 51.4, molded and fired, and then filled in a platinum crucible. The growth conditions were a pulling rate of 3.0 mm / h, a crystal rotation speed of 3 rpm, and a growth orientation c-axis. As an atmosphere, a gas in which 10% hydrogen was mixed with nitrogen was flown at a flow rate of 2000 ml / min. About 70% of the filled raw material is pulled up,
The training was completed.
【００１７】得られた結晶は、割れやスパイラル状の曲
がりがなく、サイズは直径２２mm×直胴部約１００mmで
あった。得られた結晶は、透明で茶褐色を呈していた。
この結晶を大気中１１００℃でアニールしたところ、わ
すがに黄色に着色した透明な結晶が得られた。The obtained crystal was free from cracks and spiral bends, and had a size of 22 mm in diameter and about 100 mm in the straight body portion. The obtained crystals were transparent and had a dark brown color.
When this crystal was annealed at 1100 ° C. in the atmosphere, a slightly yellow transparent crystal was obtained.
【００１８】比較のため、大気中で育成した以外は同じ
条件で育成した結晶は、直胴部５０mm付近からスパイラ
ル状の曲がりが有り、その付近から発生した割れが存在
していた。両結晶の直胴部最初の部分をウエハーに切断
し、サブグレイン密度と耐光損傷性を比較したところ、
水素を含む雰囲気で育成した前者の結晶の方が良好な結
果を示した。For comparison, the crystal grown under the same conditions except that it was grown in the atmosphere had a spiral bend from about 50 mm in the straight body portion, and had cracks generated from the vicinity. When the first part of the straight body part of both crystals was cut into wafers and the subgrain density and light damage resistance were compared,
The former crystal grown in an atmosphere containing hydrogen showed better results.
【００１９】[0019]
【実施例２】Example 2
【００２０】育成雰囲気を、アルゴンに５％の水素を混
合したガスを使用した以外、実施例１と同じ条件で育成
した。得られた結晶は、割れやスパイラル状の曲がりが
なく、サイズは直径２２mm×直胴部約１００mmであっ
た。得られた結晶は、透明で茶褐色を呈していた。この
結晶を大気中１１００℃でアニールしたところ、わずか
に黄色に着色した透明な結晶が得られた。The growth atmosphere was the same as in Example 1 except that a gas in which argon was mixed with 5% hydrogen was used. The obtained crystal did not have cracks or spiral bends, and had a size of 22 mm in diameter and about 100 mm in the straight body portion. The obtained crystals were transparent and had a dark brown color. When this crystal was annealed at 1100 ° C. in the atmosphere, a slightly yellow colored transparent crystal was obtained.
【００２１】比較のため、大気中で育成した以外は同じ
条件で育成した結晶は、直胴部５０mm付近からスパイラ
ル状の曲がりが有り、その付近から発生した割れが存在
していた。両結晶の直胴部最初の部分をウエハーに切断
し、サブグレイン密度と耐光損傷性を比較したところ、
水素を含む雰囲気で育成した前者の結晶の方が良好な結
果を示した。For comparison, the crystal grown under the same conditions except that it was grown in the atmosphere had a spiral bend from about 50 mm in the straight body portion, and had cracks generated from the vicinity. When the first part of the straight body part of both crystals was cut into wafers and the subgrain density and light damage resistance were compared,
The former crystal grown in an atmosphere containing hydrogen showed better results.
【００２２】[0022]
【実施例３】Example 3
【００２３】原料として、純度４Ｎの炭酸リチウム、五
酸化ニオブ及び酸化マグネシウムを原子比で４８.６：
５１.４：５.０になるように混合し、成型、焼成をした
後、白金るつぼに充填した。育成条件は実施例１と同様
である。得られた結晶は、割れやスパイラル状の曲がり
がなく、サイズは直径２２mm×直胴部約１００mmであっ
た。得られた結晶は、透明で茶褐色を呈していた。この
結晶を大気中１１００℃でアニールしたところ、わずか
に黄色に着色した透明な結晶が得られた。As raw materials, lithium carbonate having a purity of 4N, niobium pentoxide and magnesium oxide in an atomic ratio of 48.6:
The mixture was mixed at 51.4: 5.0, molded and fired, and then filled in a platinum crucible. The growing conditions are the same as in Example 1. The obtained crystal did not have cracks or spiral bends, and had a size of 22 mm in diameter and about 100 mm in the straight body portion. The obtained crystals were transparent and had a dark brown color. When this crystal was annealed at 1100 ° C. in the atmosphere, a slightly yellow colored transparent crystal was obtained.
【００２４】比較のため、大気中で育成した以外は同じ
条件で育成した結晶は、直胴部５０mm付近からスパイラ
ル状の曲がりが有り、その付近から発生した割れが存在
していた。両結晶の直胴部最初の部分をウエハーに切断
し、サブグレイン密度と耐光損傷性を比較したところ、
水素を含む雰囲気で育成した前者の結晶の方が良好な結
果を示した。また、残りの直胴部を育成方向と平行に切
断し、マグネシウムの分布状態をＥＰＭＡを用いて比較
したところ、大気中で育成した後者の結晶では、マグネ
シウムが不均一に存在していたのに対して、水素を含む
雰囲気で育成した前者の結晶では、マグネシウムがほぼ
均一に存在していた。For comparison, the crystal grown under the same conditions except that it was grown in the atmosphere had a spiral bend from about 50 mm in the straight body portion, and had cracks generated from the vicinity. When the first part of the straight body part of both crystals was cut into wafers and the subgrain density and light damage resistance were compared,
The former crystal grown in an atmosphere containing hydrogen showed better results. Further, when the remaining straight body was cut in parallel with the growing direction and the distribution state of magnesium was compared using EPMA, it was found that magnesium was nonuniformly present in the latter crystal grown in the atmosphere. On the other hand, in the former crystal grown in an atmosphere containing hydrogen, magnesium was present almost uniformly.
【００２５】[0025]
【発明の効果】以上詳述したように、本発明によれば、
ニオブ酸リチウム単結晶を溶融固化法により育成するに
際して、育成雰囲気を調整することにより、融液の対流
を制御できるので、割れやスパイラル状の曲がりがな
く、サブグレイン密度の少ない高品質なニオブ酸リチウ
ムを高収率で製造できる。特にチョクラルスキー法に適
用することにより、高品質で大口径の結晶を安定して供
給することが可能である。As described in detail above, according to the present invention,
When growing a lithium niobate single crystal by the melt-solidification method, the convection of the melt can be controlled by adjusting the growth atmosphere, so there is no cracking or spiral bending, and high quality niobate with a small subgrain density. Lithium can be produced in high yield. In particular, by applying it to the Czochralski method, it is possible to stably supply high-quality crystals with a large diameter.
Claims (2)
の３元素を含むニオブ酸リチウム単結晶を溶融固化法に
より育成するに際して、雰囲気を中性或いは還元性によ
って育成することを特徴とするニオブ酸リチウム単結晶
の製造方法。1. When growing a lithium niobate single crystal containing at least three elements of lithium, niobium and oxygen by a melting and solidifying method, the atmosphere is grown by a neutral or reducing property. Crystal manufacturing method.
亜鉛を添加する請求項１に記載の方法。2. The method according to claim 1, wherein magnesium or zinc is added in addition to the three elements.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4303117A JPH0774119B2 (en) | 1992-10-15 | 1992-10-15 | Method for producing lithium niobate single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4303117A JPH0774119B2 (en) | 1992-10-15 | 1992-10-15 | Method for producing lithium niobate single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06199598A true JPH06199598A (en) | 1994-07-19 |
| JPH0774119B2 JPH0774119B2 (en) | 1995-08-09 |
Family
ID=17917091
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4303117A Expired - Lifetime JPH0774119B2 (en) | 1992-10-15 | 1992-10-15 | Method for producing lithium niobate single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0774119B2 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5460300A (en) * | 1977-10-21 | 1979-05-15 | Sumitomo Metal Mining Co | Process for producing lithium niobate single crystal and apparatus therefor |
| JPH01281407A (en) * | 1988-05-09 | 1989-11-13 | Nippon Telegr & Teleph Corp <Ntt> | Method and apparatus for producing single crystal fiber |
| JPH03218997A (en) * | 1989-09-20 | 1991-09-26 | Ibiden Co Ltd | Production of thin film of lithium niobate single crystal |
| JPH0437697A (en) * | 1990-05-30 | 1992-02-07 | Ibiden Co Ltd | Thin film of lithium niobate single crystal |
-
1992
- 1992-10-15 JP JP4303117A patent/JPH0774119B2/en not_active Expired - Lifetime
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5460300A (en) * | 1977-10-21 | 1979-05-15 | Sumitomo Metal Mining Co | Process for producing lithium niobate single crystal and apparatus therefor |
| JPH01281407A (en) * | 1988-05-09 | 1989-11-13 | Nippon Telegr & Teleph Corp <Ntt> | Method and apparatus for producing single crystal fiber |
| JPH03218997A (en) * | 1989-09-20 | 1991-09-26 | Ibiden Co Ltd | Production of thin film of lithium niobate single crystal |
| JPH0437697A (en) * | 1990-05-30 | 1992-02-07 | Ibiden Co Ltd | Thin film of lithium niobate single crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0774119B2 (en) | 1995-08-09 |
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