CN85107803A - The growing technology of tellurium dioxide single crystal - Google Patents
The growing technology of tellurium dioxide single crystal Download PDFInfo
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- CN85107803A CN85107803A CN85107803.6A CN85107803A CN85107803A CN 85107803 A CN85107803 A CN 85107803A CN 85107803 A CN85107803 A CN 85107803A CN 85107803 A CN85107803 A CN 85107803A
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Abstract
A kind of tellurium dioxide (TeO that belongs to crystal technique
2) single crystal growth.It is characterized in that with can the grow single crystal of multiple tangential and shape of falling crucible method.Utilize the present technique can be along [100] [001] [110] direction and can be along the growth of either direction wherein square rod, ellipse, rhombus, tabular and cylindrical crystal.Institute's growing crystal can reach (70～80) mm * (20～30) mm * 100mm.
Advantages such as it is simple that present method and general crystal pulling method ratio have equipment, is not subjected to dip direction and cuts shape to limit, pollution-free substantially, and the crystal utilization ratio can corresponding improve 30～100%.
Description
The present invention is a kind of tellurium dioxide (TeO with the multiple tangential and shape of Bridgman-Stockbarge method for growing
2) technology of single crystal, belong to the crystal technique field.
TeO
2Crystal is a kind of acousto-material with high-quality-factor, has double refraction and opticity, and specific rotation is 87/mm, and the velocity of sound of propagating along (110) direction is 616 meter per seconds, slow 5～6 times than the velocity of sound of common acousto-optic medium.If under identical clear aperature, use TeO
2The acousto-optical device that monocrystalline is manufactured, its resolving power can have the raising of the order of magnitude.So this crystal is an ideal material of manufacturing acousto-optic deflection device, modulator, resonator, spectral filter etc.
Along with the widespread use of acoustooptic technique, to TeO
2The crystalline requirement, not only more and more higher qualitatively in quantity, and on tangential and geomery, also have higher requirement.
At present, growth TeO
2The method of monocrystalline is crystal pulling method normally.Because TeO
2733 ℃ of fusings, volatility is stronger, and its volatile matter is deleterious.Need add atmospheric rare gas element more than 10 in the process of lifting, could suppress or reduce volatilization, this just need lift with the pressurization single crystal growing furnace; In addition, this crystal has a plurality of cleavage surfaces, generally can only lift the garden styloid along (110) and (100) direction with crystal pulling method.So Czochralski grown TeO
2Single crystal is not only to the having relatively high expectations of equipment, and is subjected to dip direction and cuts shape to limit, and the crystal utilization ratio of growth is low, and the cost height is difficult to satisfy the acousto-optical device that develops rapidly to TeO
2The crystalline requirement.
In order to overcome with Czochralski grown tellurium dioxide crystalline shortcoming, adopt the falling crucible method technology, can produce multiple tangentially and the tellurium dioxide crystal of shape.The invention provides a kind of TeO of can growth multiple tangential and shape
2The technology of monocrystalline, specifically, the present invention can provide according to the requirement of acousto-optical device along (110), (001), (100) etc. directions and with the TeO of the square rod of the inclined to one side unspecified angle of these directions, ellipse garden shape, rhombus, multiple tangential and multiple shape such as tabular
2Single crystal.
Fig. 1 is a main technique schematic flow sheet of the present invention.1. raw material pre-burnings among the figure; 2. crystalline form is prepared; 3. charging; 4. stove is gone in tubulature; 5. heat up; 6. degrowth; 7. cooling; 8. the processing of coming out of the stove; 9. platinum is handled; 10. platinum melting; 11. platinum forging rolling processing weldering system crucible; 12. airtight inspection of platinum crucible and acid treatment; 13. crystal annealing is handled; 14. crystal processing; 15. performance test; 16. finished product.
Main technical process of the present invention is:
(1) raw material pre-burning: the TeO that the present invention uses
2Raw material is a specpure reagent.The high-content of impurity is silicon (Si) 0.001-0.003%, iron (Fe) 0.001-0.003%, magnesium (Mg) 0.003%, aluminium (Al) 0.001%, calcium (Ca) 0.001-0.003%.With above-mentioned spectroscopically pure TeO
2The powder alumina crucible of packing into is handled in the stove of uniformity of temperature profile, in 700 ℃ of insulations 12～15 hours, drops to room temperature more fast.Because growth TeO provided by the invention
2Single crystal technology is that the processing intent of carrying out in the sealing platinum crucible is to remove volatile matter under raw material planar water and the low temperature.
(2) according to required TeO
2Tangential and shape, cutting seed crystal and manufacture the crucible identical with the growing crystal desired shape for example need be given birth to the oval crystal and then be adopted the garden skittele pot, diameter generally only needs big 2～3mm to get final product than growing crystal, and is highly then different according to growing crystal height difference.
(3) pack into the platinum crucible of the required shape of growth and crucible is sealed of the spectroscopically pure powder (or briquetting) that required tangential seed crystal and pre-burning were handled with spot-welding technology.
(4) platinum crucible after will sealing is packed in the ceramic protecting pipe, therebetween the burnt Al in space
2O
3Powder fills up, yet protective tube is put into the stove preposition.
(5) with 80-100 ℃ of speed per hour furnace temperature is risen to 780-800 ℃ of insulation 1-4 hour, then with 0.2-0.8mm speed decline crucible per hour, the beginning crystal growth; Best lowering speed 0.4-0.6mm/ hour.
(6) descend to finish after, with 15～20 ℃ of speed per hour furnace temperature is dropped at leisure and to be lower than 100 ℃, cut off the electricity supply naturally cooling.
(7) crucible is taken out during near room temperature when crucible temperature, platinum crucible is cut open, take out crystal, put into the stove of uniformity of temperature profile then and anneal with point of a knife.Be raised to 680～700 ℃ with the speed about 70 ℃ per hour, be incubated 15～20 hours, again with cool to room temperature slowly.Have only crystal after heat treatment to use for manufacturing device.
(8) the exhausted platinum crucible need be used HNO
3Handle, in order to using again.
Growth TeO provided by the invention
2The crystalline technology is compared principal feature with common crystal pulling method:
1. the TeO of the multiple tangential and shape of can growing
2Crystal.The output height, cost is low.
2. can select the crystalline direction of growth, shape and size according to the requirement of manufacturing acousto-optical device.Present method be particularly useful for growing crystal of square rod, ellipse Cylinder, garden cylindricality, rhombus and shape such as tabular, can be along (001), (110), (100) face direction growth and can be along either direction growth (70～80) mm * (20～30) platelike crystal more than mm * 100mm wherein, and, can satisfy being of a size of 75mm (110) * 22mm (001) * 22mm (110) along (001) (110) direction rhombus monocrystalline; 60mm (001) * 50mm (110) * (10～20) mm (110), the requirement of the acousto-optical device of inclined to one side 18 ° 51 of inclined to one side 55 ° 36 of 53mm (110) ' * 37.5mm (001) ' * 30mm (110).These are and can't obtain with crystal pulling method at present.
3. because the crystalline growth is to carry out in the platinum crucible of sealing, therefore pollution-free substantially to environment, TeO in the crucible before and after the growth
2Loss all be lower than 1%.
As one of embodiments of the invention is along (110) direction, is of a size of the column single crystal growing of 50mm * 10mm * 100mm, at first handles raw material by above-mentioned raw material pre-burning, and 700 ℃ of insulations 15 hours, it was stand-by to reduce to room temperature.Secondly, along (110) face cut lengths is the seed crystal of mm of (52-54) mm * (12-14), put into corresponding column platinum crucible as crystal seed, the height of platinum crucible is slightly larger than 100mm, and basal cross section is the rectangle of mm of (52-54) mm * (12-14), packs into by the TeO of the required processing of theoretical density calculation
2, spot welding makes platinum crucible sealing, the whole platinum crucible Al that packs into
2O
3The burnt Al of crucible, intermediate gaps
2O
3The powder filling is raised to 780-800 ℃ in optimum temps district with 90 ℃ of speed per hour with furnace temperature, is incubated after 2 hours, descends with 0.5mm speed per hour, needs degrowth in about 200 hours, the growth back that finishes to cool to room temperature with 15 ℃ of speed per hour and take out annealing approximately.
As two of embodiments of the invention is along (001) face inclined to one side 19 with along the inclined to one side 56 topic rhombus TeO of (110) face
2Single crystal growing, basic technology is identical with above-mentioned example 1, different just seed crystal differences, this routine seed crystal cutting can be along (001) inclined to one side 19 °, cut for inclined to one side 56 ° along (110) face, just the diagonal lines of rhombus seed crystal than the big 2mm of required size about, about the used also corresponding big 2mm of rhombus platinum crucible diagonal lines, can grow along inclined to one side 19 ° of (001) face, along the inclined to one side 56 ° rhomboidan of (110) face.In fact can be along (001), any partially angle growing crystal of (110) or (100) face.
As three of the embodiment of the invention are garden pillar-shaped crystal of growth φ 30 * 100mm, only need to put into the Cylinder platinum crucible of φ (32-34) mm then along required tangential cutting seed crystal.
Claims (7)
1, the tellurium dioxide (TeO of the multiple tangential and shape of a kind of growth that belongs to the crystal technique field
2) technology of single crystal, comprise aspects such as the raw material pre-burning is handled, cooling annealing, it is characterized in that with Bridgman-Stockbarge method for growing multiple tangentially and the TeO of shape
2Crystal.
2, by the described multiple tangential and shape TeO of claim 1
2Crystal is characterized in that multiple shape can be square rod, ellipse garden shape, rhombus, tabular, garden cylindricality etc.Multiple tangentially is that (110) (001) (100) face also can be along wherein either direction growth.
3, handle by the described raw material pre-burning of claim 1, it is characterized in that the spectroscopically pure powder that growing crystal is used, be rapidly heated 700 ℃, be incubated 12-15 hour, be quickly cooled to normal temperature again.
4, by the described Bridgman-stockbarger of claim 1, it is characterized in that earlier furnace temperature being raised to 780～800 ℃ of preset temperatures with 80～100 ℃ of speed per hour, be incubated 1-4 hour, then with 0.2-0.8mm speed decline crucible per hour, growing crystal.
5, by the described cooling of claim 1, it is characterized in that furnace temperature being dropped to below 100 ℃ with 15～20 ℃ of speed per hour, be cooled to room temperature subsequently.
6, by the described crystal annealing of claim 1, it is characterized in that being raised to 680～700 ℃ with 70-100 ℃ of speed per hour, be incubated 15～20 hours, again cool to room temperature slowly.
7, descend by the described crucible of claim 3, it is characterized in that best lowering speed is 0.4-0.6mm/ hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85107803.6A CN1005159B (en) | 1985-10-09 | 1985-10-09 | Technology of tellurium dioxide single crystal growth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85107803.6A CN1005159B (en) | 1985-10-09 | 1985-10-09 | Technology of tellurium dioxide single crystal growth |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85107803A true CN85107803A (en) | 1987-04-15 |
| CN1005159B CN1005159B (en) | 1989-09-13 |
Family
ID=4795786
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85107803.6A Expired CN1005159B (en) | 1985-10-09 | 1985-10-09 | Technology of tellurium dioxide single crystal growth |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1005159B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010111965A1 (en) * | 2009-04-03 | 2010-10-07 | 上海硅酸盐研究所中试基地 | High-purity tellurium dioxide single crystal and manufacturing method thereof |
| CN112725877A (en) * | 2020-12-18 | 2021-04-30 | 桂林百锐光电技术有限公司 | Preparation method of tellurium dioxide single crystal |
| CN116103746A (en) * | 2022-12-09 | 2023-05-12 | 中国科学院福建物质结构研究所 | Growth method and growth device of tellurium dioxide monocrystal |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109350C (en) * | 1999-01-22 | 2003-05-21 | 大庆石油管理局第四采油厂 | System for transportation and dividing package opevation of radio isotope |
| CN1306074C (en) * | 2003-08-01 | 2007-03-21 | 中国科学院上海硅酸盐研究所 | Crucible lowering growth technology of Teo2 monocrystal |
-
1985
- 1985-10-09 CN CN85107803.6A patent/CN1005159B/en not_active Expired
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010111965A1 (en) * | 2009-04-03 | 2010-10-07 | 上海硅酸盐研究所中试基地 | High-purity tellurium dioxide single crystal and manufacturing method thereof |
| CN101851783B (en) * | 2009-04-03 | 2012-08-08 | 上海硅酸盐研究所中试基地 | High-purity tellurium dioxide single crystal and preparation method |
| US8480996B2 (en) | 2009-04-03 | 2013-07-09 | Research And Development Center, Shanghai Institute Of Ceramics | High-purity tellurium dioxide single crystal and manufacturing method thereof |
| CN112725877A (en) * | 2020-12-18 | 2021-04-30 | 桂林百锐光电技术有限公司 | Preparation method of tellurium dioxide single crystal |
| CN116103746A (en) * | 2022-12-09 | 2023-05-12 | 中国科学院福建物质结构研究所 | Growth method and growth device of tellurium dioxide monocrystal |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1005159B (en) | 1989-09-13 |
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