JPH03279298A - Growth of beta-bab2o4 single crystal using nacl as flux - Google Patents
Growth of beta-bab2o4 single crystal using nacl as fluxInfo
- Publication number
- JPH03279298A JPH03279298A JP8200090A JP8200090A JPH03279298A JP H03279298 A JPH03279298 A JP H03279298A JP 8200090 A JP8200090 A JP 8200090A JP 8200090 A JP8200090 A JP 8200090A JP H03279298 A JPH03279298 A JP H03279298A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- bab2o4
- beta
- crystal
- nacl
- 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
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 37
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 22
- 230000004907 flux Effects 0.000 title claims abstract description 11
- 239000011780 sodium chloride Substances 0.000 claims abstract description 11
- 230000007704 transition Effects 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052697 platinum Inorganic materials 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 abstract 1
- 229910001626 barium chloride Inorganic materials 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000011369 resultant mixture Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910003252 NaBO2 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
（イ）産業上の利用分野
β−ＢａＢ２Ｏ４（以後β−ＢＢＯと呼ぶ）は非線形光
学結晶で特に紫外域まで透明であり、赤外域におけるレ
ーザ光を短波長側に１長変換する際有用な結晶である９
本発明はこの単結晶を育成する除用いる融剤に関する。Detailed Description of the Invention (a) Industrial Application Field β-BaB2O4 (hereinafter referred to as β-BBO) is a nonlinear optical crystal that is transparent especially up to the ultraviolet region, and it converts laser light in the infrared region to the shorter wavelength side. 9 is a useful crystal for long conversion
The present invention relates to a flux used to grow this single crystal.
（ロ）従来の技術
Ｂ Ｂ Ｏ＋；ｔ １０９５℃に融点を持つ、ＢＢＯ単
結晶は９２５℃に相転移点をもち、９２５℃以上てはα
相、 ９２５℃以下でβ相であることが知られている。(b) Conventional technology B B O+; t BBO single crystal has a melting point at 1095°C, and a phase transition point at 925°C, and above 925°C, α
phase, it is known to be a β phase at temperatures below 925°C.
非線形光学特性を有するのはβ相であるので、単結晶を
育成する場合は融剤を用いて９２５℃以下の温度で育成
することによりβ相のＢＢＯを得なければならない、従
来、この融剤について検討されてきてＢ ａ Ｃ１２、
Ｂ ａ Ｆ’ ２およびＢａＢ、０４・Ｎａ２Ｏが報告
されている。Since it is the β phase that has nonlinear optical properties, when growing a single crystal, it is necessary to obtain BBO of the β phase by growing a single crystal at a temperature of 925°C or lower using a flux. B a C12,
B a F' 2 and BaB,04.Na2O have been reported.
（ハ）発明が解決しようとする問題点
従来開発されてきた融剤も良質な単結晶が得られず、わ
ずかにＢａＢ２Ｏ４・Ｎａ２Ｏにおいて比較的良質な結
晶が得られた報告がある。 しかし。(c) Problems to be Solved by the Invention The fluxes developed in the past have not been able to provide good quality single crystals, and there are reports of relatively good quality crystals being obtained in BaB2O4.Na2O. but.
融剤を用いる育成の特徴である結晶の外形の明確な晶−
を示さないので、Ｓ結晶の利用のＬ Ｘ線等により方
位を求めなければならず不便であるなど満足できるもの
ではなかった９
本発明は良質な結晶が得られ、明確な晶癖を示しかつ収
率のよい優れた融剤を提供することを目的としている。A crystal with a clear external shape is a characteristic of growth using a flux.
Therefore, the use of S crystals is inconvenient and unsatisfactory because the orientation must be determined using L The purpose is to provide an excellent flux with good yield.
（ニ）間組点を解決するための手段 本発明は良質な単結晶を育成するため融剤に着目した。(d) Means for solving inter-set points The present invention focuses on a flux in order to grow high-quality single crystals.
ＢＢＯは次式により合成できる。BBO can be synthesized using the following formula.
ＢａＣ１，＋ ２ＮａＢ○２−２Ｈ２０４ＢａＢ２Ｏ
４＋ ２ＮａＣｌ＋ ４Ｈ２０（１）
この度広の結果得られるＮａＣｌが単結晶育成の際の融
剤となりうることを見いだしたことによる。BaC1, + 2NaB○2-2H204BaB2O
4+ 2NaCl+ 4H20 (1) This is based on the discovery that NaCl obtained as a result of this multiplication can serve as a flux during single crystal growth.
（ホ）作用と実施例
（１）式により合成した結晶のＸ線粉末回折によりβ−
ＢＢＯであることを確認した。得られたβ−ＢＢＯとＮ
ａＣｌを用いて相平衡状態図を作成した。これが第１図
である。この結果９モル比てＮ ａ Ｃｉ： β−Ｂ
ＢＯ＝ｌ： １−３： １の間てβ−ＢＢＯを育成
可能であることが分かる。そこで、既知量のＭａｉｌと
β−ＢＢＯにより溶解度曲線を求めると第２図のように
なった。８５０℃から７９５℃まで温度降下法で育成す
ることにより１００ｇのＮａＣｌより１１８．５７ｇの
β−ＢＢＯが得られ極めて収率が高いことがわかる。(e) Effects and Examples β-
I confirmed that it was BBO. The obtained β-BBO and N
A phase diagram was created using aCl. This is Figure 1. As a result, the 9 molar ratio was N a Ci: β-B
It can be seen that β-BBO can be grown between BO=l: 1-3:1. Therefore, a solubility curve was determined using known amounts of Mail and β-BBO, and the result was as shown in FIG. It can be seen that by growing from 850°C to 795°C by the temperature drop method, 118.57g of β-BBO was obtained from 100g of NaCl, indicating an extremely high yield.
ＢＢＯは石英ガラス等と反応するため高価な白金ルツボ
を用いて育成しなければならないので、このように収率
が高いことはＮａＣｌが融剤として非常に優れているこ
とを示すものである。Since BBO reacts with quartz glass and the like, it must be grown using an expensive platinum crucible, so such a high yield indicates that NaCl is very excellent as a fluxing agent.
つぎに、育成例を述べる。 Ｂ ａ Ｃ１２： ２
５゜００ｇとＮａＢＯ２・２Ｈ２０： ２４．４５ｇ
をよく混合し白金ルツボにいれ９２０℃に２４時間保ち
β−ＢＢＯを合成したのち、 ８５０℃で種子結晶を挿
入し８１０℃まで１．７℃／ｈの速度で温度降下させて
育成した。その結果、三方晶の特徴を示す六角柱状の晶
癖をもった１４．２２ｇの結晶が得られた。少量の融液
から大きな結晶がえられることが分かる。育成した結晶
はＸ＃回折および―光Ｉ！ｌ１ｌｌ＃ｌｌで単結晶であ
ることがＮ認された。Next, an example of training will be described. B a C12: 2
5゜00g and NaBO2・2H20: 24.45g
The mixture was thoroughly mixed and placed in a platinum crucible and kept at 920°C for 24 hours to synthesize β-BBO. Seed crystals were inserted at 850°C and the temperature was lowered to 810°C at a rate of 1.7°C/h to grow. As a result, 14.22 g of crystals having a hexagonal columnar crystal habit exhibiting trigonal characteristics were obtained. It can be seen that large crystals can be obtained from a small amount of melt. The grown crystal exhibits X# diffraction and - light I! N was confirmed to be a single crystal with l1ll#ll.
（へ）発明の効果
本発明のＮａＣｌを融剤とする育成法により明確な外形
を畷えた晶癖をもち、かつ少量の融液から大きなβ−Ｂ
ＢＯＪＩＬ結晶を育成することができるので有用である
。(F) Effects of the Invention The growth method of the present invention using NaCl as a flux allows crystal habit with a clearly defined rough shape, and large β-B crystals can be obtained from a small amount of melt.
This method is useful because BOJIL crystals can be grown.
第１図はＢＢＯ−ＮａＣｌ相平衡状態図である。
第２図はβ−ＥＢＯの融剤ＮａＣｌに対する溶解度であ
る。FIG. 1 is a BBO-NaCl phase equilibrium diagram. FIG. 2 shows the solubility of β-EBO in the fluxing agent NaCl.
Claims (1)
＿２Ｏ＿４単結晶の相転移点９２５℃以下の温度で、β
−ＢａＢ＿２Ｏ＿４単結晶を育成するためにＮａＣｌを
融剤として用いることを特徴とする育成法。 ２、前記育成法の融液の組成はモル比でＮａＣｌ：β−
ＢａＢ＿２Ｏ＿４＝１：１〜３：１の範囲、温度は８５
０℃〜７９５℃の範囲であることを特徴とする特許請求
範囲第１項記載のＮａＣｌを融剤とするβ−ＢａＢ＿２
Ｏ＿４単結晶の育成法。[Claims] 1. When growing β-BaB_2O_4 single crystal, BaB
At a temperature below 925°C, the phase transition point of the _2O_4 single crystal, β
- A growth method characterized in that NaCl is used as a flux to grow a BaB_2O_4 single crystal. 2. The composition of the melt in the above growth method is NaCl:β- in molar ratio.
BaB_2O_4=1:1~3:1 range, temperature is 85
β-BaB_2 using NaCl as a fluxing agent according to claim 1, characterized in that the temperature is in the range of 0°C to 795°C.
Growth method of O_4 single crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8200090A JPH03279298A (en) | 1990-03-29 | 1990-03-29 | Growth of beta-bab2o4 single crystal using nacl as flux |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8200090A JPH03279298A (en) | 1990-03-29 | 1990-03-29 | Growth of beta-bab2o4 single crystal using nacl as flux |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03279298A true JPH03279298A (en) | 1991-12-10 |
Family
ID=13762220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8200090A Pending JPH03279298A (en) | 1990-03-29 | 1990-03-29 | Growth of beta-bab2o4 single crystal using nacl as flux |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03279298A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5343827A (en) * | 1992-02-19 | 1994-09-06 | Crystal Technology, Inc. | Method for crystal growth of beta barium boratean |
| CN104651933A (en) * | 2013-11-21 | 2015-05-27 | 中国科学院新疆理化技术研究所 | Chlorine barium borate, chlorine barium borate nonlinear optical crystal, and preparation method and uses of chlorine barium borate nonlinear optical crystal |
| CN106978627A (en) * | 2017-03-29 | 2017-07-25 | 中国科学院新疆理化技术研究所 | Lithium borate zinc phase-change material and its production and use |
-
1990
- 1990-03-29 JP JP8200090A patent/JPH03279298A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5343827A (en) * | 1992-02-19 | 1994-09-06 | Crystal Technology, Inc. | Method for crystal growth of beta barium boratean |
| EP0573738A3 (en) * | 1992-02-19 | 1996-03-27 | Crystal Tech Inc | Method for crystal growth of beta barium borate |
| CN104651933A (en) * | 2013-11-21 | 2015-05-27 | 中国科学院新疆理化技术研究所 | Chlorine barium borate, chlorine barium borate nonlinear optical crystal, and preparation method and uses of chlorine barium borate nonlinear optical crystal |
| CN106978627A (en) * | 2017-03-29 | 2017-07-25 | 中国科学院新疆理化技术研究所 | Lithium borate zinc phase-change material and its production and use |
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