CN105369352A - Carbon-copper double-doped sapphire crystal and preparing method thereof - Google Patents

Carbon-copper double-doped sapphire crystal and preparing method thereof Download PDF

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Publication number
CN105369352A
CN105369352A CN201510591533.6A CN201510591533A CN105369352A CN 105369352 A CN105369352 A CN 105369352A CN 201510591533 A CN201510591533 A CN 201510591533A CN 105369352 A CN105369352 A CN 105369352A
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crystal
crucible
sapphire
cuo
carbon copper
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徐民
杭寅
洪佳琪
王向永
陈喆
王亚琦
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Abstract

The invention relate to a carbon-copper double-doped sapphire crystal and a preparing method thereof. The chemical formula of the crystal can be expressed as Cx(CuO)y(Al2O3)1-x-y, wherein 0.01wt%<=x<=1wt%, 0.01wt%<=y<=0.5 wt%, and x and y represents weight percentages. A melt method is adopted in growth of the carbon-copper double-doped sapphire crystal. The carbon-copper double-doped sapphire crystal can emit various kinds of colored light within the range from near-infrared waveband to the purple light waveband under the action of ultraviolet band pumping light. The crystal can be used for the fields of thermoluminescence dose detection, colour-center lasers outputting laser (continuous laser, pulse laser and tuning laser) within the range from near-infrared waveband to the purple light waveband and light-emitting display of corresponding wavebands.

Description

Carbon copper is two mixes sapphire crystal and preparation method thereof
Technical field
The present invention relates to optical function material and field of crystal growth, particularly a kind of carbon copper is two mixes sapphire crystal (chemical formula C x(CuO) y(Al 2o 3) 1-x-y, referred to as C:Cu:Al 2o 3) and preparation method thereof.
Background technology
Sapphire crystal is base mateiral very important in current opto-electronics and microelectronic industry, and it is as the key part of semiconductor lighting industry, is the important substrate of blue light and white light LEDs.As light functional crystal, namely sapphire and doping sapphire were started relevant research work before over one hundred year, and industrialization crystal the earliest mixes chrome blue jewel exactly, i.e. ruby (Cr:Al 2o 3).The fifties in last century, sapphire is found to have thermoluminescence performance, has pulled open the applicable prelude of its light merit.Release optical property for what improve crystal, investigator have developed the Al of a series of doping vario-property 2o 3crystal, the most important thing is carbon-doped sapphire (i.e. C:Al 2o 3).The optical property of releasing of this crystal derives from the autotelic Lacking oxygen defect producing high density in crystalline structure, forms certain colour center.But owing to finding C:Al 2o 3be applied to and release Fluorescent Densitomet and there is thermal quenching effect and extremely sensitive to light, limit C:Al to a certain extent 2o 3range of application in posology.The sapphire of investigator's dual element doping in developed recently again, as C:Mg:Al 2o 3, and a new detector---the fluorescent core mark detector that used it to make.Due to one of raw material MgO can with base starting material Al 2o 3reaction forms other impurity crystalline phase, as magnesium-aluminium spinel (MgAl 2o 4) enter in sapphire, reduce the optical quality of crystal, therefore the doping of MgO can not too high (about tens of ppm).In addition on the one hand, the electronic structure of Mg element is [Ne] 3s 2, belong to stable electrical minor structure, be difficult to form multivalent state.Thus, cannot at C:Mg:Al 2o 3the colour center defects count that middle formation is very good and kind, this is difficult to meet the demands in colour center research and the application of light function.
Based on Al 2o 3development of new light functional crystal material, expands the large focus that its Application Areas becomes the research of current sapphire crystal.
Summary of the invention
For the deficiency of existing process for sapphire-based optical function material, the invention provides a kind of carbon copper pair and mix sapphire crystal and preparation method thereof.This crystal under the effect of ultraviolet band (190 ~ 300nm) pump light, can be launched near infrared to the multiple coloured light in purple light wavelength band, especially strengthen the transmitting of wave band near 429nm, and the peak width at half height of these emission bands reaches tens nanometer.This crystal can be applicable to release the aspects such as light dosage detection, colour-center laser and luminescence display.
Technical solution of the present invention is as follows:
A kind of carbon copper is two mixes sapphire crystal, and its feature is that the chemical formula of this crystal is: C x(CuO) y(Al 2o 3) 1-x-y, described x, y are weight percentage, and span is: 0.01wt%≤x≤1wt% and 0.01wt%≤y≤0.5wt%.
The two preparation method mixing sapphire crystal of described carbon copper, its feature is that the method comprises the following steps:
1. composition of raw materials:
Carbon copper is two mixes sapphire crystal, i.e. C x(CuO) y(Al 2o 3) 1-x-ythe growth raw material of crystal adopts purity to be the C of 99.99%, the CuO of the 99.99% and Al of 99.999% 2o 3, selected x and y value, and x:y:(1-x-y by weight percentage) and carry out weigh batching;
2. melt method for growing carbon copper pair is adopted to mix sapphire crystal:
Adopt the standby long brilliant materials of substep imitation frosted glass legal system: first by C and Al 2o 3load in tungsten crucible or molybdenum crucible; put in the high temperature imitation frosted glass stove of inert atmosphere protection; adopt ramp to 2000 ~ 2050 DEG C of 100 ~ 300 DEG C/h, be incubated and be cooled to room temperature with the speed of 150 ~ 400 DEG C/h after 2 ~ 5 hours, then CuO is loaded above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process; Or first by CuO and Al 2o 3to load in tungsten crucible or molybdenum crucible sintering once, then insert C and repeat sintering, from crucible, finally take out the Al being mixed with C, Cu element 2o 3material;
3. melt method for crystal growth is adopted.
Adopt the standby long brilliant materials of substep imitation frosted glass legal system: first by C and Al 2o 3load in the crucible of tungsten or molybdenum matter; put in the high temperature imitation frosted glass stove of inert atmosphere protection; adopt ramp to 2000 ~ 2050 DEG C of 100 ~ 300 DEG C/h, be incubated and be cooled to room temperature with the speed of 150 ~ 400 DEG C/h after 2 ~ 5 hours, then CuO is loaded above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process; Or first by CuO and Al 2o 3in the crucible loading tungsten or molybdenum matter, sintering once, then insert C and repeat sintering, from crucible, finally take out the Al being mixed with C, Cu element 2o 3material, adopts melt method for crystal growth.
Described melting method is temperature gradient method, described long crystalline substance crucible is tungsten or molybdenum crucible, crucible bottom can put into the ethereal blue jewel seed crystal in <11-20> or <0001> direction, or do not put into seed crystal, crystal growth carries out in an ar atmosphere, raw material intensification melting rate 80 ~ 150 DEG C/h, melt decrease temperature crystalline speed 0.5 ~ 5 DEG C/h, crystal cooling down speed 10 ~ 50 DEG C/h.
Described melting method is crystal pulling method, described long crystalline substance crucible is iridium crucible, seed crystal is the ethereal blue jewel single crystal rod in <11-20> or <0001> direction, crystal growth carries out in an ar atmosphere, the crystal rate of pulling 0.5 ~ 3mm/h, rotating speed 10 ~ 30rpm.
Described melting method is falling crucible method, described long crystalline substance crucible is tungsten or molybdenum crucible, crucible bottom puts into the ethereal blue jewel seed crystal in <11-20> or <0001> direction, or do not put into seed crystal, crystal growth carries out in an ar atmosphere, crucible fall off rate 0.1 ~ 3mm/h.
Described melting method is heat-exchanging method, described long crystalline substance crucible is molybdenum crucible, crucible bottom is put into the ethereal blue jewel seed crystal in <11-20> or <0001> direction or is not put into seed crystal, crystal growth carries out in the He atmosphere of flowing, raw material intensification melting rate 60 ~ 150 DEG C/h, melt decrease temperature crystalline speed 0.2 ~ 2.5 DEG C/h, crystal cooling down speed 50 ~ 80 DEG C/h.
Described melting method is kyropoulos, and described long crystalline substance crucible is tungsten crucible, and seed crystal is the ethereal blue jewel single crystal rod in <11-20> or <0001> direction, and crystal growth is 1 × 10 -3~ 1 × 10 -4carry out under Pa vacuum environment, raw material intensification melting rate 50 ~ 150 DEG C/h, melt decrease temperature crystalline speed 0.1 ~ 3 DEG C/h, the crystal rate of pulling 0.05 ~ 3mm/h, crystal cooling down speed 30 ~ 80 DEG C/h.
Technique effect of the present invention:
The present invention utilizes electronic structure [Ar] 3d of transition metal Cu 104s 1can form the feature of multivalent state, and Cu element and Al, O element not easily form the advantage of compound crystal phase, mix in sapphire crystal using C, Cu as defect ion, to form the colour center defect of enough concentration and kind, and melt method for growing is adopted to go out high-quality C:Cu:Al 2o 3crystal.This crystal has two obvious absorption peaks at 190 ~ 300nm wave band of ultraviolet region, and this crystal under the effect of ultraviolet band pump light, can launch near infrared to the multiple coloured light in purple light wavelength band.Adopt the pumping of 205nm continuous light, emission center wavelength can be positioned at the fluorescence of 391nm and 781nm.Adopt the pumping of 250nm continuous light, emission center wavelength can be positioned at the fluorescence of 333nm and 647nm.Adopt the pumping of 300nm continuous light, emission center wavelength can be positioned at the fluorescence of 429nm and 503nm.The bandwidth of these fluorescence emission peaks is very wide, and peak width at half height generally reaches tens nanometer.The C:Al of Fluorescent Densitomet is released with light 2o 3crystal is compared, C:Cu:Al of the present invention 2o 3crystal especially obviously strengthens the transmitting of wave band near 429nm.These characteristics of luminescences show, C:Cu:Al of the present invention 2o 3crystal not only with C:Al 2o 3the same, can be applicable to release light dosage detection, also can be applicable to the colour-center laser of near infrared to purple light wavelength band Laser output (continuous laser, pulse laser and tuning laser) and the luminescence display field of corresponding wave band.
Accompanying drawing explanation
Fig. 1 is C:Cu:Al 2o 3the absorption spectrum of crystal;
Fig. 2 is under the pumping of 205nm continuous light, C:Cu:Al 2o 3the fluorescence emission spectrum of crystal;
Fig. 3 is under the pumping of 250nm continuous light, C:Cu:Al 2o 3the fluorescence emission spectrum of crystal;
Fig. 4 is under the pumping of 300nm continuous light, C:Cu:Al 2o 3the fluorescence emission spectrum of crystal (and attached C:Al 2o 3the fluorescence emission spectrum of the corresponding wave band of crystal).
Embodiment
Below by specific embodiment, the invention will be further described, but should be appreciated that following embodiment is only for illustration of the present invention, but not limit the scope of the invention.
Embodiment 1
C, CuO and Al is weighed by x=0.2wt%, y=0.025wt% 2o 3raw material 500g.By C and Al 2o 3load in the crucible of molybdenum matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2050 DEG C with 150 DEG C/h, be incubated and be cooled to room temperature with 200 DEG C/h after 2 hours.Again CuO is loaded and above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance tungsten matter crucible, adopt Growth by Temperature Gradient Technique C:Cu:Al 2o 3crystal.Crucible bottom puts into the sapphire seed crystal in <11-20> direction, and crystal growth carries out under Ar compression ring border.Raw material intensification melting rate 100 DEG C/h, melt decrease temperature crystalline speed 1 DEG C/h, crystal cooling down speed 30 DEG C/h.
Embodiment 1 grows the C:Cu:Al obtained 2o 3crystal is transparent, does not occur the macroscopic defectss such as cracking, bubble, wrap.10 × 10 × 2mm is cut into the crystal ingot of growth 3wafer, after polishing to sample carried out absorption spectrum, fluorescence spectrum test, result is as shown in Figure 1 to 4.
Fig. 1 is C:Cu:Al in the present embodiment 2o 3crystal is at the absorption spectrum of 190nm-2500nm wavelength band.C:Cu:Al in this wave band 2o 3there are two main absorption peaks in crystal, central position lays respectively at 204nm and 255nm place.
Fig. 2 is C:Cu:Al in the present embodiment 2o 3crystal under the pumping of 205nm continuous light, the fluorescence emission spectrum of 260nm-850nm wavelength band.C:Cu:Al in this wave band 2o 3there is a very strong purple light fluorescence peak (central position is positioned at 391nm) and a more weak near-infrared fluorescent peak (central position is positioned at 781nm) in crystal.
Fig. 3 is C:Cu:Al in the present embodiment 2o 3crystal under the pumping of 250nm continuous light, 260nm-480nm and 530nm-850nm two wavelength band fluorescence emission spectrums.C:Cu:Al in this wave band 2o 3there is a central position respectively and be positioned at the ruddiness fluorescence peak that the Ultraluminescence peak of 333nm and central position are positioned at 647nm in crystal.
Fig. 4 (solid line) is C:Cu:Al in the present embodiment 2o 3crystal under the pumping of 300nm continuous light, the fluorescence emission spectrum of 400nm-750nm wavelength band.C:Cu:Al in this wave band 2o 3there are two fluorescence peaks in crystal, central position is positioned at 429nm and 503nm, respectively corresponding royal purple light emission and green emission.With C:Al 2o 3the fluorescent emission contrast of crystal, the C:Cu:Al in the present embodiment 2o 3crystal clearly enhances the transmitting near 429nm, shows that micro Cu element enters Al effectively 2o 3lattice, and define a certain amount of colour center defect center, under the effect of useful photon, there is energy level transition.
The C:Cu:Al prepared in the present embodiment 2o 3the spectrum test display of crystal, not only with C:Al 2o 3the same, can be applicable to release light dosage detection, also can be applicable to the colour-center laser of near infrared to purple light wavelength band Laser output (continuous laser, pulse laser and tuning laser) and the luminescence display field of corresponding wave band.
Embodiment 2
C, CuO and Al is weighed by x=0.25wt%, y=0.05wt% 2o 3raw material 600g.By C and Al 2o 3load in the crucible of molybdenum matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2050 DEG C with 180 DEG C/h, be incubated and be cooled to room temperature with 200 DEG C/h after 2 hours.Again CuO is loaded and above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance tungsten matter crucible, adopt Growth by Temperature Gradient Technique C:Cu:Al 2o 3crystal.Crucible bottom puts into the sapphire seed crystal in <0001> direction, and crystal growth carries out under Ar compression ring border.Raw material intensification melting rate 120 DEG C/h, melt decrease temperature crystalline speed 1.5 DEG C/h, crystal cooling down speed 25 DEG C/h.
Embodiment 3
C, CuO and Al is weighed by x=0.5wt%, y=0.08wt% 2o 3raw material 500g.By C and Al 2o 3load in the crucible of tungsten matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2030 DEG C with 200 DEG C/h, be incubated and be cooled to room temperature with 200 DEG C/h after 2 hours.Again CuO is loaded and above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance Iridium Crucible, adopt Czochralski grown C:Cu:Al 2o 3crystal.Select the sapphire ingot in <11-20> direction to make seed crystal, crystal growth carries out under Ar compression ring border.Crystal pull rate is 1.2mm/h, rotating speed 15rpm, controls the growth of crystal Raised key axis, through shove charge → vacuumize → fill Ar gas → temperature increasing for melting materials → sow → necking down → shouldering → isodiametric growth → carry the stages such as de-cooling, obtains high-quality C:Cu:Al 2o 3crystal.
Embodiment 4
C, CuO and Al is weighed by x=0.3wt%, y=0.1wt% 2o 3raw material 600g.By C and Al 2o 3load in the crucible of tungsten matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2020 DEG C with 160 DEG C/h, be incubated and be cooled to room temperature with 250 DEG C/h after 3 hours.Again CuO is loaded and above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance Iridium Crucible, adopt Czochralski grown C:Cu:Al 2o 3crystal.Select the sapphire ingot in <0001> direction to make seed crystal, crystal growth carries out under Ar compression ring border.Crystal pull rate is 2mm/h, rotating speed 10rpm, controls the growth of crystal Raised key axis and prepares C:Cu:Al 2o 3crystal.
Embodiment 5
C, CuO and Al is weighed by x=0.6wt%, y=0.15wt% 2o 3raw material 700g.By CuO and Al 2o 3load in the crucible of molybdenum matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2010 DEG C with 250 DEG C/h, be incubated and be cooled to room temperature with 250 DEG C/h after 4 hours.Again C is loaded and above-mentionedly fill CuO and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance molybdenum crucible, adopt Bridgman-Stockbarge method for growing C:Cu:Al 2o 3crystal.Select the sapphire ingot in <0001> direction to make seed crystal, crystal growth carries out under Ar compression ring border, and crucible fall off rate is 0.3mm/h.
Embodiment 6
C, CuO and Al is weighed by x=0.8wt%, y=0.4wt% 2o 3raw material 3000g.By C and Al 2o 3load in the crucible of tungsten matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2030 DEG C with 200 DEG C/h, be incubated and be cooled to room temperature with 200 DEG C/h after 2 hours.Again CuO is loaded and above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance molybdenum crucible, adopt heat-exchanging method growth C:Cu:Al 2o 3crystal.Select the sapphire in <11-20> direction to make seed crystal, crystal growth carries out in the He atmosphere of flowing.Raw material intensification melting rate 70 DEG C/h, melt decrease temperature crystalline speed 1 DEG C/h, crystal cooling down speed 70 DEG C/h.
Embodiment 7
C, CuO and Al is weighed by x=0.7wt%, y=0.35wt% 2o 3raw material 5000g.By CuO and Al 2o 3load in the crucible of tungsten matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2010 DEG C with 130 DEG C/h, be incubated and be cooled to room temperature with 200 DEG C/h after 5 hours.Again C is loaded and above-mentionedly fill CuO and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance molybdenum crucible, adopt heat-exchanging method growth C:Cu:Al 2o 3crystal.Select the sapphire in <0001> direction to make seed crystal, crystal growth carries out in the He atmosphere of flowing.Raw material intensification melting rate 100 DEG C/h, melt decrease temperature crystalline speed 0.5 DEG C/h, crystal cooling down speed 50 DEG C/h.
Embodiment 8
C, CuO and Al is weighed by x=0.65wt%, y=0.45wt% 2o 3raw material 10000g.By CuO and Al 2o 3load in the crucible of tungsten matter, put in the high temperature imitation frosted glass stove of inert atmosphere protection, be warming up to 2010 DEG C with 120 DEG C/h, be incubated and be cooled to room temperature with 250 DEG C/h after 5 hours.Again C is loaded and above-mentionedly fill CuO and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process.From crucible, take out the material prepared, be placed in long crystalline substance tungsten crucible, adopt kyropoulos growth C:Cu:Al 2o 3crystal.Select the sapphire in <11-20> direction to make seed crystal, crystal growth is 6 × 10 -3carry out under Pa vacuum environment, raw material intensification melting rate 120 DEG C/h, melt decrease temperature crystalline speed 0.3 DEG C/h, crystal rate of pulling 0.1mm/h, crystal cooling down speed 40 DEG C/h.
C:Cu:Al prepared by above-described embodiment 2 ~ 8 2o 3the test of crystal has the result similar with embodiment 1.
Above specific embodiments of the invention have been described in detail, but just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should be covered by scope of the present invention.

Claims (7)

1. carbon copper is two mixes a sapphire crystal, it is characterized in that the chemical formula of this crystal is C x(CuO) y(Al 2o 3) 1-x-y, described x, y are weight percentage, and span is: 0.01wt%≤x≤1wt% and 0.01wt%≤y≤0.5wt%.
2. the two preparation method mixing sapphire crystal of carbon copper according to claim 1, is characterized in that the method comprises the following steps:
1. composition of raw materials:
Carbon copper is two mixes sapphire crystal, i.e. C x(CuO) y(Al 2o 3) 1-x-ythe growth raw material of crystal adopts purity to be the C of 99.99%, the CuO of the 99.99% and Al of 99.999% 2o 3, selected x and y value, and x:y:(1-x-y by weight percentage) and carry out weigh batching;
2. melt method for growing carbon copper pair is adopted to mix sapphire crystal:
Adopt the standby long brilliant materials of substep imitation frosted glass legal system: first by C and Al 2o 3load in tungsten crucible or molybdenum crucible; put in the high temperature imitation frosted glass stove of inert atmosphere protection; adopt ramp to 2000 ~ 2050 DEG C of 100 ~ 300 DEG C/h, be incubated and be cooled to room temperature with the speed of 150 ~ 400 DEG C/h after 2 ~ 5 hours, then CuO is loaded above-mentionedly fill C and Al 2o 3in the crucible of sintered material, repeat above-mentioned sintering process; Or first by CuO and Al 2o 3to load in tungsten crucible or molybdenum crucible sintering once, then insert C and repeat sintering, from crucible, finally take out the Al being mixed with C, Cu element 2o 3material;
3. melt method for crystal growth is adopted.
3. the two preparation method mixing sapphire crystal of carbon copper according to claim 2, be characterised in that described melting method is temperature gradient method, described long crystalline substance crucible is tungsten crucible or molybdenum crucible, crucible bottom can put into the ethereal blue jewel seed crystal in <11-20> or <0001> direction, or do not put into seed crystal, crystal growth carries out in an ar atmosphere, raw material intensification melting rate 80 ~ 150 DEG C/h, melt decrease temperature crystalline speed 0.5 ~ 5 DEG C/h, crystal cooling down speed 10 ~ 50 DEG C/h.
4. the two preparation method mixing sapphire crystal of carbon copper according to claim 2, be characterised in that described melting method is crystal pulling method, described long crystalline substance crucible is iridium crucible, seed crystal is the ethereal blue jewel single crystal rod in <11-20> or <0001> direction, crystal growth carries out in an ar atmosphere, the crystal rate of pulling 0.5 ~ 3mm/h, rotating speed 10 ~ 30rpm.
5. the two preparation method mixing sapphire crystal of carbon copper according to claim 2, be characterised in that described melting method is falling crucible method, described long crystalline substance crucible is tungsten crucible or molybdenum crucible, crucible bottom puts into the ethereal blue jewel seed crystal in <11-20> or <0001> direction, or do not put into seed crystal, crystal growth carries out in an ar atmosphere, crucible fall off rate 0.1 ~ 3mm/h.
6. the two preparation method mixing sapphire crystal of carbon copper according to claim 2, be characterised in that described melting method is heat-exchanging method, described long crystalline substance crucible is molybdenum crucible, crucible bottom is put into the ethereal blue jewel seed crystal in <11-20> or <0001> direction or is not put into seed crystal, crystal growth carries out in the He atmosphere of flowing, raw material intensification melting rate 60 ~ 150 DEG C/h, melt decrease temperature crystalline speed 0.2 ~ 2.5 DEG C/h, crystal cooling down speed 50 ~ 80 DEG C/h.
7. the two preparation method mixing sapphire crystal of carbon copper according to claim 2, be characterised in that described melting method is kyropoulos, described long crystalline substance crucible is tungsten crucible, seed crystal is the ethereal blue jewel single crystal rod in <11-20> or <0001> direction, and crystal growth is 1 × 10 -3~ 1 × 10 -4carry out under Pa vacuum environment, raw material intensification melting rate 50 ~ 150 DEG C/h, melt decrease temperature crystalline speed 0.1 ~ 3 DEG C/h, the crystal rate of pulling 0.05 ~ 3mm/h, crystal cooling down speed 30 ~ 80 DEG C/h.
CN201510591533.6A 2015-09-17 2015-09-17 Carbon-copper double-doped sapphire crystal and preparing method thereof Pending CN105369352A (en)

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CN107937983A (en) * 2018-01-04 2018-04-20 河北工业大学 A kind of sapphire material of multicomponent doping and its preparation method and application
CN112453419A (en) * 2020-11-03 2021-03-09 中国地质大学（武汉） Method for growing copper nano material in feldspar crystal

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Publication number Priority date Publication date Assignee Title
CN107937983A (en) * 2018-01-04 2018-04-20 河北工业大学 A kind of sapphire material of multicomponent doping and its preparation method and application
CN112453419A (en) * 2020-11-03 2021-03-09 中国地质大学（武汉） Method for growing copper nano material in feldspar crystal
CN112453419B (en) * 2020-11-03 2021-08-31 中国地质大学（武汉） Method for growing copper nano material in feldspar crystal

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