CN1057868A - Barium metaborate (the constant level Czochralski grown of monocrystalline of β-BBO) - Google Patents
Barium metaborate (the constant level Czochralski grown of monocrystalline of β-BBO) Download PDFInfo
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- CN1057868A CN1057868A CN 90102894 CN90102894A CN1057868A CN 1057868 A CN1057868 A CN 1057868A CN 90102894 CN90102894 CN 90102894 CN 90102894 A CN90102894 A CN 90102894A CN 1057868 A CN1057868 A CN 1057868A
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- crucible
- growth
- bbo
- servo
- temperature
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Abstract
A kind of employing constant level method lifts β-BBO large single crystal continuously, carries out intermittence with servo crucible and feeds in raw material, and servo crucible is communicated with growth crucible, can realize that the limit is reinforced, the limit lifts.Because the temperature field is constant in the process of growth, perfection of crystal is good, transparency is high, inclusion is few.Advantages such as crystalline size is big can increase substantially yield rate.
Description
The present invention relates to field of crystal growth, particularly relate to and a kind ofly lift the barium metaborate (growth method of monocrystalline of β-BBO) with the solvent constant level method.
β-BBOJing Ti is a kind of ideal nonlinear optical material, use frequency multiplication widely at ultraviolet band, with practical value to laser freuqency doubling, this is because laser apparatus itself can only provide a high-intensity coherent source, desire to make light source to be widely used, must carry out frequency conversion phase modulation, technology such as tuningout.This just ideal modulation of β-BBOJing Ti material.Can think that nonlinear optical material will become a kind of base mateiral of new smooth industry.Therefore, the β-BBOJing Ti material has great practical value.
(1979) are found and succeeded in developing to existing β-BBOJing Ti by Chinese Academy of Sciences's Foochow thing structure.The main flux kyropoulos that adopts is grown.Also adopt Czochralski grown in recent years, but perfection of crystal is poor, defective is more, and is easy to crack, still do not have use value.This employed flux is BaB
2O
4-BaF
2, BaB
2O
4-BaCl
2, BaB
2O
4-Na
2O(whole nation crystal growth and material meeting paper summary compilation (A), Suzhou, 1979, P48) (artificial lens VOL.19.NO1 1990) is with aforementioned two kinds of methods, along with crystalline is grown up, the solute amount in the flux reduces gradually, is the comparison difficulty so desire to grow large single crystal.In addition, along with the carrying out of crystal growth, temperature descends, and the temperature field is stable inadequately, is prone to inclusion in the crystal.
The object of the present invention is to provide a kind of method that adopts the flux constant level to lift β-BBO large single crystal continuously, provide integrity good, yield rate height, the measured β of matter-BBO large single crystal.
Of the present invention theing contents are as follows:
1, prepare raw material:
(1) under 200-400 ℃, roasting solvent BaB in advance
3O
4;
(2) adopt flux than being Na
2O-BaB
2O
4%(20-30 by weight): (80-70);
(3) hydrostaticpressure moulding 10-50 pauses/cm
2;
2, use ball mill mixing through 48 hours.
3,2 °～4 ° of the errors directed C(0001 of seed crystal);
4, crucible is prepared:
Servo crucible is communicated with growth crucible, and the inclination angle is 30～50 degree, and the temperature difference is 50-120 ℃.
5, crystal growth condition:
(1) temperature is 910 ℃-925 ℃;
(2) pulling rate 0.8-1.0 millimeter/sky;
(3) rotating speed 5-15 rev/min;
(4) 20～50 ℃/cm of thermograde.
In process of growth, it is reinforced to have a rest with servo crucible consecutive hours space, but the limit is reinforced, and the limit lifts.β-BBO the large single crystal of growth reaches 82% in 220nm-230nm ultraviolet band transmitance; And can obtain different frequency-doubled effects.
Effect of the present invention: owing to adopt flux constant level crystal pulling method, and adopt servo crucible intermittently reinforced, can lift continuously, thus homo(io)thermism in the process of growth, thereby the temperature field is stable, causes the good transparency of the perfection of crystal of being grown good, inclusion is few, the yield rate height; And the flux nontoxicity, non-environmental-pollution.
The growth of example 1, β-BBO monocrystalline
(1) feedstock production
% takes by weighing Na at 20: 80 by weight
2O-BaB
2O
4Ball milling mixes to even; The following 20 tons/cm of hydrostaticpressure
2Moulding, the directed C(0001 of seed crystal) error is 2 °;
Prepare to do the servo crucible of intermittently reinforced usefulness:
In growth crucible one side, open a connecting pipe, its inclination angle is 30 °;
925 ℃ of growth conditionss;
Pulling rate 0.8mm/ days;
5 rev/mins of rotating speeds
20 ℃/cm of temperature ladder
Servo crucible is higher 50 ℃ than growth crucible temperature.
Example 2: β-BBO single crystal growing
The growth flow process is with example 1.
Na
2O: BaB
2O
4Be 50: 50(weight %)
The moulding hydrostaticpressure is 30 tons/cm
2
The directed C(0001 of seed crystal) error: 3 °;
Servo crucible and growth crucible incline 40 the degree angles.
910 ℃ of growth conditionss
Pulling rate 1.0mm/ opens
10 rev/mins of rotating speeds
35 ℃/centimetre of thermogrades
Servo crucible temperature is higher 80 ℃ than growth crucible temperature.
Example 3, β-BBO single crystal growing
The growth flow process is with example 1:
Na
2O BaB
2O
4It is 30: 70
50 tons/cm of moulding hydrostaticpressure
2
The directed C(0001 of seed crystal) error is 4 °
Servo crucible and growth crucible inclination 50 the two temperature of degree angle differ 120 ℃.
Claims (2)
1, a kind ofly lifts the method for β-BBO large single crystal continuously, adopt Na with the flux constant level
2-BaB
2O
4Make flux, it is characterized in that:
Undertaken by following flow process:
(1) feedstock production:
Adopt Na
2-BaB
2O
4% is 20-30:80～70 preparations by weight, and ball mill mixing is to even;
Hydrostaticpressure 10-50 ton/cm
2Moulding;
(2) the directed C (0001) of seed crystal; Error 2-4;
(3) crucible is prepared: the servo crucible that is communicated with growth crucible, make reinforced crucible, and carry out continuous automatic control, intermittently reinforced;
(4) growth conditions:
910 ℃-925 ℃ of temperature;
Pulling rate 0.8-1.0 millimeter/sky;
Rotating speed 5-15 rev/min
20～50 ℃/centimetre of temperature ladders.
2, according to the β-BBO growth method of claim 1, it is characterized in that: described servo crucible (1) is communicated with growth crucible;
(2) inclination angle with growth crucible is 30～50 degree;
(3) than the high 50-120 of growth crucible temperature ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102894 CN1057868A (en) | 1990-07-06 | 1990-07-06 | Barium metaborate (the constant level Czochralski grown of monocrystalline of β-BBO) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102894 CN1057868A (en) | 1990-07-06 | 1990-07-06 | Barium metaborate (the constant level Czochralski grown of monocrystalline of β-BBO) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1057868A true CN1057868A (en) | 1992-01-15 |
Family
ID=4877772
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90102894 Pending CN1057868A (en) | 1990-07-06 | 1990-07-06 | Barium metaborate (the constant level Czochralski grown of monocrystalline of β-BBO) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1057868A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046005C (en) * | 1994-08-30 | 1999-10-27 | 中国科学院上海硅酸盐研究所 | Method for pulling growth of beta-barium metaborate from solvent constant level |
| CN103225108A (en) * | 2013-04-07 | 2013-07-31 | 福建福晶科技股份有限公司 | Method for rapid growth of large-size BBO crystal |
| CN102076892B (en) * | 2008-07-25 | 2014-08-27 | 中国科学院福建物质结构研究所 | Doped low temperature phase BaB204 single crystal, the manufacturing method thereof and wave changing elements therefrom |
| CN106757341A (en) * | 2017-01-05 | 2017-05-31 | 福建福晶科技股份有限公司 | A kind of special growth technique for reducing bbo crystal envelope |
| CN107475772A (en) * | 2017-08-30 | 2017-12-15 | 福建福晶科技股份有限公司 | A kind of bbo crystal method for fast growing |
-
1990
- 1990-07-06 CN CN 90102894 patent/CN1057868A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046005C (en) * | 1994-08-30 | 1999-10-27 | 中国科学院上海硅酸盐研究所 | Method for pulling growth of beta-barium metaborate from solvent constant level |
| CN102076892B (en) * | 2008-07-25 | 2014-08-27 | 中国科学院福建物质结构研究所 | Doped low temperature phase BaB204 single crystal, the manufacturing method thereof and wave changing elements therefrom |
| CN103225108A (en) * | 2013-04-07 | 2013-07-31 | 福建福晶科技股份有限公司 | Method for rapid growth of large-size BBO crystal |
| CN103225108B (en) * | 2013-04-07 | 2016-04-06 | 福建福晶科技股份有限公司 | A kind of method of rapid growth of large-size BBO crystal |
| CN106757341A (en) * | 2017-01-05 | 2017-05-31 | 福建福晶科技股份有限公司 | A kind of special growth technique for reducing bbo crystal envelope |
| CN107475772A (en) * | 2017-08-30 | 2017-12-15 | 福建福晶科技股份有限公司 | A kind of bbo crystal method for fast growing |
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