CN102021647B - Method for rapid growth of centimeter magnitude ruby crystal - Google Patents
Method for rapid growth of centimeter magnitude ruby crystal Download PDFInfo
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- CN102021647B CN102021647B CN2010105224123A CN201010522412A CN102021647B CN 102021647 B CN102021647 B CN 102021647B CN 2010105224123 A CN2010105224123 A CN 2010105224123A CN 201010522412 A CN201010522412 A CN 201010522412A CN 102021647 B CN102021647 B CN 102021647B
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Abstract
The invention discloses a method for rapid growth of a centimeter magnitude ruby crystal, which belongs to the field of growth of the ruby crystals. The method comprises the following steps: preparing Al2O3 (aluminum oxide) and Cr2O3 (chromium oxide) powder into a biscuit rod; sintering material rods into polycrystalline material rods, wherein one polycrystalline material rod is fixed and used as a seed crystal, and the other one is hung and used as the material rod; enabling the tail ends of the two material rods to be in contact, enabling the contact place to be positioned on the same horizontal line with halogen lamps, and enabling the two material rods to form a straight line in the vertical direction; and enabling the four ellipsoidal halogen lamps to achieve the total power of 3360-3550W/h within 0.2-0.5h in air atmosphere, melting the contact place between the two material rods, keeping the power output, rotating the seed crystal and a raw material rod in reverse direction, enabling the raw material rod and the seed crystal rod to respectively move up and down and pass through a molten region, and reducing the output power to 0 within 1-2h after the growth of the crystal is completed. By adopting the method, the growth speed is fast, the preparation cycle is short, the efficiency is high, the length of a ruby can achieve 50-70mm, and the diameter can achieve 7-9mm.
Description
Technical field
The invention belongs to ruby crystal growth field, be specifically related to a kind of method of ruby crystal of quick growth centimetre magnitude.
Background technology
Crystalline material plays crucial effect in scientific technological advance, be the important foundation stone of information age, also is the basic substance of development hi-tech.Crystalline material mainly contains: semiconductor single crystal material, laser crystal material, scintillator crystal materials, non-linear optical crystal material, piezoelectric crystal material, ferroelectric crystal material, magneto-optical crystal material, superconduction crystalline material.Main single crystal preparation technology mainly contains: melt growth, solution growth, vapor phase growth, solid state growth.The optics float-zone method has the crucible of need not as a kind of novel crystal growth method, pollutes and lacks, and advantages such as fast growth are difficult to growth (comprising the crystal that crystal pulling method can not be grown), the easy crystal that pollutes for some, demonstrate very big meliority.Float-zone method belongs to a kind of method of melt growth, between crystal and the polycrystalline rod of growth, forms one section melting zone, and melting zone stable is that the balance of abutment surface tension force and gravity is kept.Perhaps move from top to bottom from bottom to top in the melting zone, to accomplish crystallisation process.The heating source of float-zone method growing crystal has the RF induction heating, discharge, and electric arc, resistive heating, light focuses on.The growing method that light focuses on as heating source is called the optics float-zone method, and it is the light that light source is sent, and through focusing on as thermal source, delivers on the heated polycrystalline sample, treats after the polycrystalline fusing growing crystal.The early stage light source that uses is the light that sends with carbon arc, but work-ing life is extremely short, after use incandescent light as light source again, but the tungsten filament of incandescent light highly volatile at high temperature, the work-ing life of lamp is still very short.At present, mostly the light source that infrared rays focuses on the process furnace use is tungsten-iodine lamp or xenon lamp, and its Heating temperature reaches 2100 ℃ or 2800 ℃ respectively.So the float-zone method Heating temperature is not limited by the crucible fusing point, the high material of fusing point of therefore can growing, and the speed of growth is very fast, is widely used in high temperature refractory oxide and intermetallic compound growth.
Ruby is a kind of corundum, is the important materials of wrist-watch gemstone element.Stone bearing in the wrist-watch, the redness decoration of pallet stone, dial plate etc. all is to be processed by ruby.In addition, ruby is as gain medium, and output light is in visible-range, and live width is narrower, and fluorescence lifetime is long, and quantum yield is high, and pump absorption bandwidth and position are superior.Ruby also has good physical and chemical performances such as high temperature resistant, hard, that the life-span is long, thermal conductivity good, chemical property is stable.Therefore ruby is being brought into play important effect as a kind of important crystalline material in national economy and military industry field.At present Growth of Ruby crystalline method mainly contains: flame melt method, fusing assistant melting method, lift send out, hydrothermal method.But above method, because its condition limitation, growth cycle is long, cost is high.
1985, Journal of Crystal Growth reported that M.SAITO has prepared through NEC two ellipsoid 3.5KW halogen lamp optics float-zone method single crystal growing furnaces and has mixed Cr
2O
3Be the ruby crystal of 2.0wt%, its sintering condition is 1450 ℃/10h, and 1700 ℃/10h, the actual crystal size is not quite clear, but contains more bubble in the crystal, and crystal mass is not high.(Saito，M.，Gas-bubble?formation?of?ruby?single?crystalsby?floating?zone?method?with?an?infrared?radiation?convergence?typeheater.Journal?of?Crystal?Growth?1985，71(3)，664-672)。
Tairus company of siberian branch of Russian NAS utilized temperature difference hydrothermal method successfully to grow ruby and batch process in the world first in 1993.Guangxi China jewel institute began to carry out the technical study of temperature difference Hydrothermal Growth jewel in 1991, and in 1998 can be stable the large-scale production ruby.The equipment of its Hydrothermal Growth ruby crystal mainly is made up of autoclave, temperature difference well formula resistance furnace, precious metal protection against corrosion lining pipe, platinum rhodium thermocouple and microcomputerized control precision temperature unit etc.Autoclave is made up of extraordinary high-temperature alloy steel, and its reaction chamber volume is about 900ml, can bear 650 ℃, the experiment condition of 250Mpa, and the temperature difference of fusion district and vitellarium is controlled between 30～100 ℃ in the autoclave, and pressure is 150～200MPa.Raw materials used is analytically pure corundum crystal fragment, Al (OH)
3, causing toner is Cr
2O
3Or K
2CrO
4(pressing massfraction 1% adds), mineralizer is KHCO
3And Na
2CO
3Formulated, concentration is respectively 1.0mol/l.Used seed crystal is the colourless corundum crystal of crystal pulling method synthetic; And form, and be suspended on the seed crystal frame that precious metal makes by
or
direction cutting.The mineralizer solution of filling about 60% is warming up to 500～620 ℃ in the autoclave reaction chamber, makes the pressure that produces 150～200MPa in the reaction chamber, and constant temperature is about 10 days.With this understanding, the ruby crystal growth velocity is 0.3～0.6mm/d.(Qi sword; Lin Hao Shan, TIROS hydrothermal synthetic ruby. Chinese Gem 1998,7 (001) ,122-124).
Temperature gradient method Growth of Ruby crystal unit mainly is made up of the crucible and the heating element that are placed in the simple bell-jar resistance furnace.During preparation, at first with raw material A l
2O
3And Cr
2O
31300 ℃ of left and right sides calcinations, press Cr again
2O
30.5%～3% atomic fraction of content carries out batch mixes, puts into the V-arrangement whisking appliance and mixes, and binder at 1400 ℃ of left and right sides sintering, is put into the crucible that (0001) direction is placed seed crystal then, and shove charge is in order to growth again.With being evacuated to 1.33 * 10 in the stove
-3Pa will expect fusion again, at 2050 ℃ of constant temperature numbers hour, slowly cool off with 0.5～2.5 ℃/h then, and crystal growth is accomplished in crystallization.(the such poems of the Song Dynasty; Zhou Shengming; It is good etc. that department continues, the research of temperature gradient method large size ruby. artificial lens journal 2003,32 (5), 423-426).
2010; American Mineralogist report; People such as C.Guguschev adopt the optics floating region of four ellipsoids of CrystalSystems Incoporation production to send out the ruby crystal that crystal growing furnace prepares the doping different concns, and its crystal furnace model is FZ-T-10000-H-VI-FAS.Its processing condition are: adopt the ruby crystal of Czochralski grown, 60 ° on C axle is as seed crystal partially; The used polycrystalline rod of growing crystal is at 1500 ℃ of following sintering 24h; Growth velocity is 5.0～10.0mm/h; Growth atmosphere is the Ar gas of P=1.0bar, and gas velocity is 3.0l/h.Crystal shape is irregular, resembles a pear in shape mostly, and length is the longest is about 30mm, the minimum 10mm that is about.(Guguschev，C.；Gotze，J.；Gobbels，M.，Cathodoluminescencemicroscopy?and?spectroscopy?of?synthetic?ruby?crystals?grown?by?theoptical?floating?zone?technique.American?Mineralogist?2010，95(4)，449-455)。
Summary of the invention
But the object of the present invention is to provide a kind of ruby crystal preparation technology with the optics float-zone method, simple to operate, preparation cycle weak point, large size, high quality repetitive operation.
The present invention may further comprise the steps through scheme realization once:
(1) with Al
2O
3Powder and Cr
2O
3Powder places ball grinder, ball milling, and oven dry is sieved.
(2), the rubber sphere that powder is housed placed etc. under the static pressure process the biscuit rod with making the powder compacting in the rectangular rubber balloon of packing in (1).
(3) obtain the polycrystalline charge bar with making charge bar in (2) at 1300-1450 ℃ of following sintering 4h.
(4) one of polycrystalline charge bar is fixed on the seed rod of single crystal growing furnace as seed crystal, one hangs on the charge bar bar as charge bar.Regulate seed rod, charge bar bar position, make the terminal contact of two charge bars, and contact position and halogen lamp be on the same sea line, two charge bar in the vertical directions are in alignment.
(5) in air atmosphere, the halogen lamp of four ellipsoids melts two charge bar contact positions in 0.2-0.5h reaches 3360-3550W/h in the time total power output; Form the melting zone, keep this power output, seed crystal and fuel rod are respectively with the 15-20rpm retrograde rotation; Fuel rod and seed crystal rod respectively with the speed of 3-5mm/h to the upper and lower melting zone that moves through; Carry out crystal growth, crystal growth reduces to 0 with output rating at 1-2h in the time after accomplishing.
The Cr of above-mentioned steps (1)
2O
3The not concrete restriction of doping, but be preferably 0.1wt%-1.5wt%.
Compare the obvious advantage of technology of the present invention with existing technology:
(1) the ruby crystal uniform doping of this prepared, size is bigger, defectives such as flawless, bubble, inclusion.The ESEM shape appearance figure, powder x x ray diffration pattern x, polarizing microscope shows the sample inclusion-free, and is mutually pure, is monocrystalline.
(2) this raw materials technology is the general industry powder, and is loose to ingredient requirement, do not need seed crystal, need not crucible, reduces preparation cost greatly.
(3) required instrument is simple, only needs ball mill, sintering oven, crystal growing furnace.
(4) it is simple to use this technology institute Growth of Ruby crystal operation, only needs before crystal growth begins, regulate the position of seed crystal rod and fuel rod, regulates SR, the speed of growth in the process of growth, single crystal growing furnace halogen lamp output rating.
(5) do not need special atmosphere, pressure environment, only need to divide atmosphere can accomplish crystal growth, work simplification at normal pressure, air.
(6) this technology has uniform doping with respect to existing technology, fast growth (3-5mm/h), and preparation cycle is short, the advantage that preparation efficiency is high.
(7) this technology only needs the charge bar that crystal growth is required with respect to existing technology, and once sintered through 1300-1450 ℃/4h, sintering time is short, and temperature is low, cuts down the consumption of energy greatly.
(8) the prepared ruby crystal length of the inventive method can reach 50-70mm, and diameter can reach 7-9mm.
Description of drawings
Fig. 1 is embodiment 1 a ruby crystal powder x XRD X spectrogram;
Fig. 2 is embodiment 2 ruby crystal shape appearance figures;
Fig. 3 is embodiment 3 a ruby crystal transverse sections polishing back shape appearance figure;
Fig. 4 is embodiment 4 shape appearance figures of ruby crystal square section under polarizing microscope;
Fig. 5 is the microscopic appearance figures of embodiment 5 ruby crystals under ESEM.
Embodiment
Do below in conjunction with the accompanying drawing specific embodiments of the invention and to describe in further detail.The prepared microscopic appearance figure of ruby crystal square section under polarizing microscope of following examples is similar basically, available Fig. 4 representative.
Embodiment 1: crystal growing furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optics float-zone method crystal growing furnace that Japanese Crystal Systems Corporation produces.
(1) with Al
2O
3, Cr
2O
3Press 99.9: 0.1 batchings of mass ratio, place ball grinder, ball milling 24h, oven dry is sieved.
(2) with making the powder compacting in the rectangular rubber balloon of packing in (1), the rubber sphere that powder is housed placed etc. under the static pressure process the biscuit rod, will make charge bar and obtain the polycrystalline charge bar at 1300 ℃ of following sintering 4h.
(3) one of polycrystal is fixed on the seed rod of single crystal growing furnace as seed crystal, one hangs on the charge bar bar as charge bar.Regulate seed rod, charge bar bar position, make the terminal contact of two charge bars, and contact position and halogen lamp be in samely on sea line, two charge bar in the vertical directions are in alignment.
(4) in air atmosphere, the halogen lamp of four ellipsoids reaches the power output of 3360W/h in 0.2h, and heating is melted two charge bar contact positions, forms the melting zone.Seed crystal and fuel rod be with 15rpm contrary side rotation, fuel rod and seed crystal rod respectively with the speed of 5mm/h to the upper and lower melting zone that moves through, the completion crystal growth.Crystal growth reduces to 0 with output rating at 1h in the time after accomplishing.
From Fig. 4: characteristic peak is sharp-pointed shown in the ruby crystal powder x XRD X spectrogram, shows that prepared sample is pure phase, and inclusion-free is the phase structure of homogeneous.
Embodiment 2: crystal growing furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optics float-zone method crystal growing furnace that Japanese Crystal Systems Corporation produces.
(1) with Al
2O
3, Cr
2O
3Press 99.7: 0.3 batchings of mass ratio, place ball grinder, ball milling 24h, oven dry is sieved.
(2) with making the powder compacting in the rectangular rubber balloon of packing in (1), the rubber sphere that powder is housed placed etc. under the static pressure process the biscuit rod, will make charge bar and obtain the polycrystalline charge bar at 1350 ℃ of following sintering 4h.
(3) one of polycrystal is fixed on the seed rod of single crystal growing furnace as seed crystal, one hangs on the charge bar bar as charge bar.Regulate seed rod, charge bar bar position, make the terminal contact of two charge bars, and contact position and halogen lamp be in samely on sea line, two charge bar in the vertical directions are in alignment.
(4) in air atmosphere, the halogen lamp of four ellipsoids reaches the power output of 3400W/h in 0.2h, and heating is melted two charge bar contact positions, forms the melting zone.Seed crystal and fuel rod be respectively with 20rpm contrary side rotation, fuel rod and seed crystal rod respectively with the speed of 5mm/h to the upper and lower melting zone that moves through, carry out crystal growth.Crystal growth reduces to 0 with output rating at 1.5h in the time after accomplishing.
From Fig. 2: the ruby crystal shape appearance figure can find out that the ruby crystal diameter that makes is approximately 9～10mm, and length is 50mm, and the metalluster that takes on a red color has obvious striation, uniform doping, flawless, scattering particles, inclusion.
Embodiment 3: crystal growing furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optics float-zone method crystal growing furnace that Japanese Crystal Systems Corporation produces.
(1) with Al
2O
3, Cr
2O
3Press 99.5: 0.5 batchings of mass ratio, place ball grinder, ball milling 24h, oven dry is sieved.
(2) with making the powder compacting in the rectangular rubber balloon of packing in (1), the rubber sphere that powder is housed placed etc. under the static pressure process the biscuit rod, will make charge bar and obtain the polycrystalline charge bar at 1350 ℃ of following sintering 4h.
(3) one of polycrystal is fixed on the seed rod of single crystal growing furnace as seed crystal, one hangs on the charge bar bar as charge bar.Regulate seed rod, charge bar bar position, make the terminal contact of two charge bars, and contact position and halogen lamp be in samely on sea line, two charge bar in the vertical directions are in alignment.
(4) in air atmosphere, the halogen lamp of four ellipsoids reaches the power output of 3450W/h in 0.3h, and heating is melted two charge bar contact positions, forms the melting zone.Seed crystal and fuel rod be respectively with 20rpm contrary side rotation, fuel rod and seed crystal rod respectively with the speed of 5mm/h to the upper and lower melting zone that moves through, the completion crystal growth.Crystal growth reduces to 0 with output rating at 1.5h in the time after accomplishing.
From Fig. 3: polishing back, ruby square section shape appearance figure can find out that it is blood red that ruby crystal is, and color even is consistent, and flawless, bubble have good complete form property.
Embodiment 4: crystal growing furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optics float-zone method crystal growing furnace that Japanese Crystal Systems Corporat ion produces.
(1) with Al
2O
3, Cr
2O
3Press 99.0: 1.0 batchings of mass ratio, place ball grinder, ball milling 24h, oven dry is sieved.
(2) with making the powder compacting in the rectangular rubber balloon of packing in (1), the rubber sphere that powder is housed placed etc. under the static pressure process the biscuit rod, will make charge bar and obtain the polycrystalline charge bar at 1380 ℃ of following sintering 4h.
(3) one of polycrystal is fixed on the seed rod of single crystal growing furnace as seed crystal, one hangs on the charge bar bar as charge bar.Regulate seed rod, charge bar bar position, make the terminal contact of two charge bars, and contact position and halogen lamp be in samely on sea line, two charge bar in the vertical directions are in alignment.
(4) in air atmosphere, the halogen lamp of four ellipsoids reaches the power output of 3500W/h in 0.5h, and heating is melted two charge bar contact positions, forms the melting zone.Seed crystal and fuel rod be respectively with 15rpm contrary side rotation, fuel rod and seed crystal rod respectively with the speed of 4mm/h to the upper and lower melting zone that moves through, the completion crystal growth.Crystal growth reduces to 0 with output rating at 1.5h in the time after accomplishing.
From Fig. 4: the microscopic appearance figure of ruby crystal square section under polarizing microscope can find out that the ruby crystal low-angle boundary seldom shows higher crystal mass.
Embodiment 5: crystal growing furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optics float-zone method crystal growing furnace that Japanese Crystal Systems Corporation produces.
(1) with Al
2O
3, Cr
2O
3Press 98.5: 1.5 batchings of mass ratio, place ball grinder, ball milling 24h, oven dry is sieved.
(2) with making the powder compacting in the rectangular rubber balloon of packing in (1), the rubber sphere that powder is housed placed etc. under the static pressure processes the biscuit rod, will in make charge bar and obtain the polycrystalline charge bar at 1450 ℃ of following sintering 4h
(3) one of polycrystal is fixed on the pedestal of single crystal growing furnace as seed crystal, one hangs on the charge bar bar as charge bar.
(4) in air atmosphere, the halogen lamp of four ellipsoids reaches the power output of 3550W/h in 0.5h, and heating is melted two charge bar contact positions, forms the melting zone.Seed crystal and fuel rod be respectively with 18rpm contrary side rotation, fuel rod and seed crystal rod respectively with the speed of 3mm/h to the upper and lower melting zone that moves through, the completion crystal growth.Crystal growth reduces to 0 with output rating at 2h in the time after accomplishing.
From Fig. 4: the ruby crystal surface scan Electronic Speculum figure, have figure can find out that the ruby crystal surface is uniform and smooth, show that crystal has good integrity and homogeneity.
Claims (1)
1. the method for centimetre magnitude ruby crystal of growing fast is characterized in that, may further comprise the steps:
(1) with Al
2O
3Powder and Cr
2O
3Powder places ball grinder, ball milling, and oven dry is sieved;
(2), the rubber sphere that powder is housed placed etc. under the static pressure process the biscuit rod with making the powder compacting in the rectangular rubber balloon of packing in (1);
(3) obtain the polycrystalline charge bar with making charge bar in (2) at 1300-1450 ℃ of following sintering 4h;
(4) one of polycrystalline charge bar is fixed on the seed rod of single crystal growing furnace as seed crystal, one hangs on the charge bar bar as charge bar; Regulate seed rod, charge bar bar position, make the terminal contact of two charge bars, and contact position and halogen lamp be on the same sea line, two charge bar in the vertical directions are in alignment;
(5) in air atmosphere; The halogen lamp of four ellipsoids melts two charge bar contact positions, the formation melting zone in 0.2-0.5h reaches 3360-3550W/h in the time total power output; Keep this power output; Seed crystal and fuel rod be respectively with the 15-20rpm retrograde rotation, fuel rod and seed crystal rod respectively with the speed of 3-5mm/h to the upper and lower melting zone that moves through, carry out crystal growth; Crystal growth reduces to 0 with output rating at 1-2h in the time after accomplishing;
Above-mentioned Cr
2O
3Doping is 0.1wt%-1.5wt%.
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| CN103160911B (en) * | 2013-03-03 | 2015-08-26 | 北京工业大学 | A kind of grow BiFe1 the method of xCoxO3 serial crystal |
| CN103882521A (en) * | 2014-04-04 | 2014-06-25 | 玉溪市明珠晶体材料有限公司 | Method for growing jewelry-grade ruby monocrystal |
| CN105239161B (en) * | 2015-10-19 | 2018-06-26 | 中国科学院青海盐湖研究所 | The preparation method of ruby crystal |
| CN106544730A (en) * | 2017-01-22 | 2017-03-29 | 四川省久宝晶体科技有限公司 | A kind of ruby preparation method of synthetic major diameter |
Citations (4)
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|---|---|---|---|---|
| CN1103680A (en) * | 1993-09-24 | 1995-06-14 | 通用电气公司 | Solid state thermal conversion of polycrystalline alumina to sapphire using a seed crystal |
| CN1167842A (en) * | 1996-03-22 | 1997-12-17 | 株式会社村田制作所 | Cerium-containing magnetic garnet single crystal and production method therefor |
| CN1831084A (en) * | 2006-02-23 | 2006-09-13 | 中国科学院上海光学精密机械研究所 | Doped rare earth element gallium oxide type fluorescent substrate material and its prepn. method |
| CN101255602A (en) * | 2007-12-03 | 2008-09-03 | 中国科学院上海硅酸盐研究所 | Non-crucible growing method for magneto-optic rear earth ferrite crystal |
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| US6689293B2 (en) * | 2002-05-31 | 2004-02-10 | The Regents Of The University Of California | Crystalline rare-earth activated oxyorthosilicate phosphor |
| CH696907A5 (en) * | 2003-02-18 | 2008-01-31 | Schott Ag | A process for the manufacture of hexagonal monocrystals and their use as a substrate for semiconductor devices. |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103680A (en) * | 1993-09-24 | 1995-06-14 | 通用电气公司 | Solid state thermal conversion of polycrystalline alumina to sapphire using a seed crystal |
| CN1167842A (en) * | 1996-03-22 | 1997-12-17 | 株式会社村田制作所 | Cerium-containing magnetic garnet single crystal and production method therefor |
| CN1831084A (en) * | 2006-02-23 | 2006-09-13 | 中国科学院上海光学精密机械研究所 | Doped rare earth element gallium oxide type fluorescent substrate material and its prepn. method |
| CN101255602A (en) * | 2007-12-03 | 2008-09-03 | 中国科学院上海硅酸盐研究所 | Non-crucible growing method for magneto-optic rear earth ferrite crystal |
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