CN103060891A - Device and method for directionally growing fluoride single crystal via lifting small-gradient thermal field - Google Patents
Device and method for directionally growing fluoride single crystal via lifting small-gradient thermal field Download PDFInfo
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- CN103060891A CN103060891A CN2013100392855A CN201310039285A CN103060891A CN 103060891 A CN103060891 A CN 103060891A CN 2013100392855 A CN2013100392855 A CN 2013100392855A CN 201310039285 A CN201310039285 A CN 201310039285A CN 103060891 A CN103060891 A CN 103060891A
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- 239000013078 crystal Substances 0.000 title claims abstract description 92
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000012010 growth Effects 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000009413 insulation Methods 0.000 claims abstract description 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 15
- 230000000630 rising effect Effects 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 3
- 239000000523 sample Substances 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 abstract description 13
- 229910001635 magnesium fluoride Inorganic materials 0.000 abstract description 13
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 230000007423 decrease Effects 0.000 description 10
- 239000000126 substance Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000002826 coolant Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
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Abstract
小梯度温场上升定向生长氟化物单晶的装置及方法属于晶体生长技术领域。现有技术成功率低、晶体质量差。本发明之装置其特征在于，坩埚经坩埚座安置在保温套底部上面；每个连接梁将两两相对的电极座连接起来，各个连接梁的中点相交于一点，各个连接梁在该点彼此连接成一体，提拉杆的下端在该点与各个连接梁相连；电极杆与密封圈动配合。本发明之方法其特征在于，由提拉杆通过连接梁、电极座、电极杆向上提拉加热体，温场随之上升，坩埚、仔晶筒、坩埚座、仔晶静止。依本发明生长氟化镁晶体成功率为95%以上，位错密度降低到10~30/cm2，在0.2~7.5μm波段的吸收系数小于2×10E-4/cm，晶体质量全面提高。
The device and method for directional growth of fluoride single crystal with small gradient temperature field increase belong to the technical field of crystal growth. The prior art has low success rate and poor crystal quality. The device of the present invention is characterized in that the crucible is placed on the bottom of the insulation cover through the crucible seat; each connecting beam connects two opposite electrode seats, and the midpoints of each connecting beam intersect at one point, and each connecting beam is connected to each other at this point. Connected into one body, the lower end of the lifting rod is connected with each connecting beam at this point; the electrode rod is dynamically matched with the sealing ring. The method of the present invention is characterized in that the heating body is pulled up by the lifting rod through the connecting beam, the electrode holder, and the electrode rod, and the temperature field rises accordingly, and the crucible, seed crystal tube, crucible seat, and seed crystal are stationary. According to the present invention, the success rate of growing magnesium fluoride crystals is over 95%, the dislocation density is reduced to 10-30/cm 2 , the absorption coefficient in the 0.2-7.5 μm band is less than 2×10E-4/cm, and the crystal quality is comprehensively improved.
Description
Technical field
The present invention relates to the device and method of a kind of little gradient temperature rising oriented growth fluoride single crystal, growth specific direction fluorochemical such as magnesium fluoride monocrystalline belong to the crystal technique field under vacuum condition.
Background technology
Fluoride single crystal is a kind of crystalline material with anisotropy and birefringent characteristic, is mainly used in the ultraviolet band polarization element.Because the requirement of birefringent characteristic aspect, cutting of crystal must be carried out according to specific direction, if crystal is failed according to the pre-determined direction growth, it is large then to cut loss, and utilization ratio is low.In order to increase operation rate, must the oriented growth crystal.The method of existing oriented growth fluoride single crystal is the brilliant descent method of a kind of son.The method is growing crystal under vacuum condition, take the magnesium fluoride monocrystalline as example, the magnesium fluoride seed crystal is placed in crucible bottom, and crucible is connected on the water-cooled decline bar.At the crystal early growth period, the accurately temperature of control seed crystal position and temperature make seed crystal melt approximately half, and then water-cooled decline bar slowly moves down, crucible thereupon in the stove hot-zone slowly mobile to the cold-zone, crystal is slowly grown according to the intrinsic direction of seed crystal.
The brilliant descent method of described son is very harsh to the requirement of crystal growth equipment and envrionment conditions, especially at the crystal early growth period, namely the magnesium fluoride seed crystal is melted the approximately critical stage of half, and this stage requires very accurately to control temperature.Seed crystal temperature of living in field is made of jointly heating element, crucible, water-cooled decline bar etc., the temperature of temperature of living in field, seed crystal middle part must be controlled at above 5 ~ 10 degree of young brilliant fusing point, the seed crystal first half is melted fully, and the seed crystal Lower Half is not melted, and crystal could normal growth like this.Adopt existing young brilliant descent method for growing magnesium fluoride monocrystalline, because seed crystal is connected in by crucible holder on the water-cooled decline bar in crucible bottom, the fluctuation of water coolant water temperature and flow can cause seed crystal temperature of living in field to depart from default temperature field, cause seed crystal to melt fully or melt insufficiently, both of these case all will cause crystal to be grown unsuccessfully.
Another shortcoming of existing young brilliant descent method is, because the existence of water coolant, the temperature of water-cooled decline bar is all the time less than 100 ℃, and the fusing point of crystal is far above this temperature, is 1255 ℃ such as the fusing point of magnesium fluoride crystal, this is just so that the warm field gradient of seed crystal position is very steep, make when seed crystal middle part temperature of living in to reach more than the crystalline melting point 5 ~ 10 when spending, in the crucible, the temperature on top will far above crystalline melting point, cause the volatilization of crystal raw material, even causing raw material excessive in a large number, crystal is grown unsuccessfully.
In a word, adopt the success ratio of existing young brilliant descent method oriented growth fluoride single crystal to only have 50 ~ 60%.Owing in crystal growing process, can't Real Time Observation melt situation to seed crystal, can't in time examine and know whether seed crystal melts according to predetermined requirement, until crystal growing process finishes just can know the crystal growth result fully, if failure certainly will cause the serious waste of starting material and electric energy.So low success ratio and so serious waste cause the magnesium fluoride monocrystalline blank price with specific direction on the market up to more than 10000 yuan/kilogram, have affected using in field widely of this material.
Although existing young brilliant descent method oriented growth crystal of fluoride still has 50 ~ 60% success ratio,, aspect crystal mass, also have problems.Because the existence of water-cooled decline bar, the phenomenons such as appearance temperature fluctuation, a temperature shakiness and thermograde are excessive, the negative results of these phenomenons is that to cause the shape of solid-liquid interface be not desirable smooth convex interface, and then causes matter crystal internal defect to form in a large number, and dislocation desity reaches 60 ~ 100/cm
2, uptake factor reaches 5 * 10E-4/cm, and such quality is difficult to satisfy the requirement of high-end ahrens prism.
Summary of the invention
The purpose of we's invention is, improves the success ratio of fluoride single crystal oriented growth, improves crystal mass, and for this reason, we have invented the device and method of a kind of little gradient temperature rising oriented growth fluoride single crystal.The core of its technical scheme is cancellation water-cooled decline bar, and the control heating element rises, brilliant covert decline of son, and the temperature field is stable, and thermograde reduces, and overcomes the problem that prior art exists comprehensively.
In the device of the present invention's a little gradient temperature rising oriented growth fluoride single crystal, be muff 2 in vacuum chamber 1 inner peripheral, crucible 3 is positioned at muff 2 center of inside, as shown in Figure 1; In crucible 3 bottom centre the brilliant cylinder 4 of son being arranged, is crucible holder 5 below young brilliant 4; Several heating member 6 contour being suspended on around crucible 3 sidewalls, heating member 6 upper ends connect water cooled electrode bar 7, and battery lead rod 7 passes first muff 2 tops and passes the sealing-ring 8 at vacuum chamber 2 tops again and be connected with electrode holder 9; Temperature-control heat couple 10 is positioned at young brilliant cylinder 4 sides 1/2 ~ 2/3 young brilliant cylinder At The Height; It is characterized in that crucible 3 is above crucible holder 5 is placed in muff 2 bottoms, as shown in Figure 2; Each tie-beam 11 couples together electrode holder 9 facing each other, and the mid point of each tie-beam 11 intersects at a point, and each tie-beam 11 is connected to each other at this point and is integral, and the lower end of lifting rod 12 links to each other with each tie-beam 11 at this point; Battery lead rod 7 and sealing-ring 8 are movingly.
Method according to the present invention's a little gradient temperature rising oriented growth fluoride single crystal, as shown in Figure 3, son brilliant 13 is inserted young brilliant cylinder 4, young brilliant 13 upper end probes into crucible 3, with growth material 14 crucible 3 of packing into, produce growth temperature field by heating member 6, be the temperature that is higher than 5 ~ 10 ℃ of the fluoride single crystal fusing points of growing by young brilliant 13 first halves of temperature-control heat couple 10 control temperature of living in field temperature, after brilliant 13 first halves of son melt, young crystalline substance 13 and a temperature up and down relative movement, solid-liquid interface is shifted to the cold-zone from the hot-zone of temperature field, until the crystal growth is complete; It is characterized in that, upwards lift heating member 6 by lifting rod 12 by tie-beam 11, electrode holder 9, battery lead rod 7, rises in temperature field thereupon, crucible 3, young brilliant cylinder 4, crucible holder 5, young brilliant 13 static.
Its technique effect of the present invention is, because crucible 3 is above crucible holder 5 is placed in muff 2 bottoms, cancelled the water-cooled decline bar below the crucible holder of the prior art 5, crucible 3, young brilliant cylinder 4, crucible holder 5, young brilliant 13 keep static in crystal growing process, up and down relative movement between young crystalline substance 13 and the temperature field, shift to the cold-zone from the hot-zone of temperature be rise to realize that these technical measures can be brought many-sided technique effect by temperature to solid-liquid interface in other words.For example, the gradient of the temperature field around the young crystalline substance 13 diminishes, and young brilliant 13 first halves temperature of living in is easy to control, and avoids to a great extent occurring young brilliant 13 first halves and does not have thawing or young crystalline substance 13 full situations of melting; Can normally keep young brilliant 13 first halves temperature of living in field temperature is the temperature that is higher than 5 ~ 10 ℃ of the fluoride single crystal fusing points of growing, need not to bring up to more than the fluoride single crystal fusing point growth material melt temperature a lot, thereby the volatilization that can alleviate crystal raw material, avoid raw material excessive in a large number.Therefore the success ratio of final crystal growth can be brought up to more than 95%.For another example, steady, the warm field gradient of growth temperature is close to constant, the shape of solid-liquid interface presents desirable smooth convex interface substantially, significantly reduce matter crystal internal defect, adopt X-ray orientation device directed, orientation accuracy is 30 "; directional precision is for reaching 2 °; at the magnesium fluoride monocrystalline crystal ingot diameter of C direction growth maximum 100mm, length 200mm, the availability of C direction is greater than 90%, and dislocation desity is reduced to 10 ~ 30/cm
2, less than 2 * 10E-4/cm, crystal mass improves comprehensively at the uptake factor of 0.2 ~ 7.5 mu m waveband.The present invention also has a subsidiary effect, and along with the cancellation of original water-cooled decline bar, cooling structure is simplified.
Description of drawings
Fig. 1 is the device one-piece construction synoptic diagram of the present invention's a little gradient temperature rising oriented growth fluoride single crystal.Fig. 2 is device lower part structure enlarged diagram of the present invention's a little gradient temperature rising oriented growth fluoride single crystal.Fig. 3 is the method synoptic diagram of the present invention's a little gradient temperature rising oriented growth fluoride single crystal, and this figure is simultaneously as Figure of abstract.
Embodiment
In the device of the present invention's a little gradient temperature rising oriented growth fluoride single crystal, muff 2 in vacuum chamber 1 inner peripheral, muff 2 materials are carbon fiber reinforce plastic, crucible 3 is positioned at muff 2 center of inside, add graphite material crucible cover 15 on the crucible 3, prevent growth material melt heat loss and stop the growth material volatilization, as shown in Figure 1; In crucible 3 bottom centre the brilliant cylinder 4 of son being arranged, is crucible holder 5 below young brilliant 4, and crucible holder 5 is graphite material; Several heating member 6 contour being suspended on around crucible 3 sidewalls, heating member 6 upper ends connect water cooled electrode bar 7, and battery lead rod 7 passes first muff 2 tops and passes the sealing-ring 8 at vacuum chamber 2 tops again and be connected with electrode holder 9; Temperature-control heat couple 10 is positioned at young brilliant cylinder 4 sides 1/2 ~ 2/3 young brilliant cylinder At The Height; Crucible 3 is above crucible holder 5 is placed in muff 2 bottoms, as shown in Figure 2; Each tie-beam 11 couples together electrode holder 9 facing each other, tie-beam 11 and electrode holder 9 insulation, supply lead receiving electrode seat 9; The mid point of each tie-beam 11 intersects at a point, and each tie-beam 11 is connected to each other at this point and is integral, and the lower end of lifting rod 12 links to each other with each tie-beam 11 at this point; Battery lead rod 7 and sealing-ring 8 movingly, battery lead rod 7 be the red copper material, hollow water flowing cooling keeps the interior vacuum tightness of vacuum chambers 1 by sealing-ring 8.Battery lead rod 7 is connected with the graphite terminal of heating member 6 by bolt and nut.
Method according to the present invention's a little gradient temperature rising oriented growth fluoride single crystal, as shown in Figure 3, fritter magnesium fluoride monocrystalline is processed into cylindric as young brilliant 13, seed crystal 13 diameter 15mm, length 65mm, cylinder axially be monocrystalline C to, the utilization ratio of the fluoride single crystal crystal ingot of growing along this direction is the highest; Son brilliant 13 is inserted young brilliant cylinder 4, and seed crystal cylinder 13 internal diameters match with seed crystal 13 external diameters, keep the vertical state of seed crystal 13; Young brilliant 13 upper end probes into crucible 3.With magnesium fluoride particle growth material 14 crucible 3 of packing into.Open successively rotary-vane vaccum pump and oil diffusion pump, vacuum chamber 1 is evacuated to the vacuum of 2 * 10E-3 torr.Produce growth temperature field by heating member 6, furnace temperature rises to more than the magnesium fluoride crystal fusing point 5 ~ 10 ℃ of i.e. certain temperature between 1260 ~ 1265 ℃ by room temperature by 25 ℃/hour of temperature rise rates, such as 1263 ℃, growth material 14 slowly is fused into melt, control afterwards constant temperature, in period, melt is fully got rid of gas and other impurity at constant temperature.Control young brilliant 13 a first halves temperature of living in temperature on this temperature value by temperature-control heat couple 10.Behind the constant temperature 5 hours, young brilliant 13 first halves melt, pass through tie-beam 11 by lifting rod 12, electrode holder 9, battery lead rod 7 upwards lifts heating member 6 with speed such as the 1mm/h of 1 ~ 3mm/h, rise in the temperature field thereupon, crucible 3, young brilliant cylinder 4, crucible holder 5, young brilliant 13 is static, young crystalline substance 13 and a temperature up and down relative movement, the bottom of crucible 3, young brilliant cylinder 4 places suitable for reading take the lead in becoming away from heating member 6 the Wen Chang cold-zone, solid-liquid interface is also shifted to the cold-zone with the speed of 1mm/h from the hot-zone of temperature field simultaneously, by the mass transport in the melt, crystal in crucible 3 interior growths will constantly grow according to seed crystal 13 intrinsic directions fully, the crystal growth is complete after 200 hours, by temperature-control heat couple 10 control automatic coolings, cooling rate is 30 ℃/h, and temperature stops to be heating member 6 power supplies when being down to 150 ℃, naturally cool to room temperature, obtain the complete magnesium fluoride monocrystalline consistent with seed crystal 13 directions, crystal ingot diameter 58mm, length 160mm, crystal ingot cylinder axis and crystal C are to parallel.Described fluoride single crystal also comprises CaF
2, BaF
2, the LiF crystal.
Claims (4)
1. the device of one a kind little gradient temperature rising oriented growth fluoride single crystal is muff (2) in vacuum chamber (1) inner peripheral, and crucible (3) is positioned at muff (2) center of inside; In crucible (3) bottom centre the brilliant cylinder of son (4) being arranged, is crucible holder (5) below young brilliant tin (4); Several heating members (6) are contour to be suspended on around crucible (3) sidewall, heating member (6) upper end connects water cooled electrode bar (7), and battery lead rod (7) passes first muff (2) top and passes the sealing-ring (8) at vacuum chamber (2) top again and be connected with electrode holder (9); Temperature-control heat couple (10) is positioned at young brilliant cylinder (4) side 1/2 ~ 2/3 young brilliant cylinder At The Height; It is characterized in that crucible (3) is above crucible holder (5) is placed in muff (2) bottom; Each tie-beam (11) couples together electrode holder facing each other (9), the mid point of each tie-beam (11) intersects at a point, each tie-beam (11) is connected to each other at this point and is integral, and the lower end of lifting rod (12) links to each other with each tie-beam (11) at this point; Battery lead rod (7) and sealing-ring (8) are movingly.
2. the device of a little gradient temperature according to claim 1 rising oriented growth fluoride single crystal is characterized in that, tie-beam (11) and electrode holder (9) insulation, supply lead receiving electrode seat (9).
3. the method for one kind little gradient temperature rising oriented growth fluoride single crystal, son brilliant (13) is inserted young brilliant cylinder (4), the upper end of young brilliant (13) probes into crucible (3), with growth material (14) crucible (3) of packing into, produce growth temperature field by heating member (6), be the temperature that is higher than 5 ~ 10 ℃ of the fluoride single crystal fusing points of growing by young brilliant (13) first half of temperature-control heat couple (10) control temperature of living in field temperature, after young brilliant (13) first half melts, young brilliant (13) and a temperature up and down relative movement, solid-liquid interface is shifted to the cold-zone from the hot-zone of temperature field, until the crystal growth is complete; It is characterized in that, upwards lift heating member (6) by lifting rod (12) by tie-beam (11), electrode holder (9), battery lead rod (7), rises in temperature field thereupon, and crucible (3), young brilliant cylinder (4), crucible holder (5), young brilliant (13) are static.
4. the method for a little gradient temperature according to claim 3 rising oriented growth fluoride single crystal, it is characterized in that, upwards lift heating member (6) by tie-beam (11), electrode holder (9), battery lead rod (7) with the speed of 1 ~ 3mm/h by lifting rod (12).
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104790025A (en) * | 2015-04-14 | 2015-07-22 | 营口市荣兴达科技实业有限公司 | Preparation device and preparation technology for magnesium fluoride single crystal coating material |
| CN105112993A (en) * | 2015-10-12 | 2015-12-02 | 山东大学 | Device and method for regulating growth temperature gradients of mu-PD (micro-pulling-down) crystals |
| CN105133005A (en) * | 2014-06-03 | 2015-12-09 | 长春理工大学 | Crystal growth method for obtaining flat solid-liquid interface, and apparatus thereof |
| CN107287657A (en) * | 2017-06-26 | 2017-10-24 | 北京中材人工晶体研究院有限公司 | The growing method and gained crystal of a kind of lanthanum bromide scintillation crystal |
| CN108866619A (en) * | 2018-07-02 | 2018-11-23 | 南京光宝光电科技有限公司 | The oriented growth device and technique of large scale magnesium fluoride monocrystalline |
| CN116988155A (en) * | 2023-07-31 | 2023-11-03 | 上海芯飞睿科技有限公司 | Fluoride crystal and preparation method thereof |
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| CN1603475A (en) * | 2004-09-06 | 2005-04-06 | 周永宗 | Pure static state double heating apparatus for crystal growth by temperature gradient technique |
| CN102766901A (en) * | 2012-08-20 | 2012-11-07 | 元亮科技有限公司 | Device for growing large-size and high-temperature crystals with real-time adjustable temperature gradient method and method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105133005A (en) * | 2014-06-03 | 2015-12-09 | 长春理工大学 | Crystal growth method for obtaining flat solid-liquid interface, and apparatus thereof |
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| CN105112993A (en) * | 2015-10-12 | 2015-12-02 | 山东大学 | Device and method for regulating growth temperature gradients of mu-PD (micro-pulling-down) crystals |
| CN107287657A (en) * | 2017-06-26 | 2017-10-24 | 北京中材人工晶体研究院有限公司 | The growing method and gained crystal of a kind of lanthanum bromide scintillation crystal |
| CN107287657B (en) * | 2017-06-26 | 2019-10-08 | 北京中材人工晶体研究院有限公司 | A kind of growing method and gained crystal of lanthanum bromide scintillation crystal |
| CN108866619A (en) * | 2018-07-02 | 2018-11-23 | 南京光宝光电科技有限公司 | The oriented growth device and technique of large scale magnesium fluoride monocrystalline |
| CN116988155A (en) * | 2023-07-31 | 2023-11-03 | 上海芯飞睿科技有限公司 | Fluoride crystal and preparation method thereof |
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| CN103060891B (en) | 2015-04-29 |
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