CN101717249A - Yttrium aluminum garnet transparent ceramic material of double-doped rare earth ions and preparation method thereof - Google Patents
Yttrium aluminum garnet transparent ceramic material of double-doped rare earth ions and preparation method thereof Download PDFInfo
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- CN101717249A CN101717249A CN200910263226A CN200910263226A CN101717249A CN 101717249 A CN101717249 A CN 101717249A CN 200910263226 A CN200910263226 A CN 200910263226A CN 200910263226 A CN200910263226 A CN 200910263226A CN 101717249 A CN101717249 A CN 101717249A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 15
- -1 rare earth ions Chemical class 0.000 title claims abstract description 14
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 40
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 235000015895 biscuits Nutrition 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 13
- 238000000465 moulding Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 abstract description 18
- 238000000137 annealing Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 abstract 1
- 239000011222 crystalline ceramic Substances 0.000 description 14
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 14
- 150000002500 ions Chemical class 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 6
- 239000004677 Nylon Substances 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229920001778 nylon Polymers 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010979 ruby Substances 0.000 description 1
- 229910001750 ruby Inorganic materials 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
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Abstract
The invention relates to an yttrium aluminum garnet transparent ceramic material of double-doped rare earth ions and a preparation method thereof. The invention is characterized in that the general expression of the chemical composition of the transparent ceramic material is (Y1-x-yYbxNdy)3Al5O12, wherein x is greater than or equal to 0.01 and less than or equal to 0.1, and y is greater than or equal to 0.005 and less than or equal to 0.05. The preparation method comprises the following steps: weighing and proportioning according to the general expression of the chemical composition; using commercial high-purity powder or nano powder prepared by the coprecipitation method as a raw material; and carrying out the processes of uniform ball milling, forming, vacuum sintering and annealing treatment on the raw material to obtain Yb, Nd: YAG transparent ceramics with good light transmission. The invention can achieve the purposes of improving the absorption efficiency of pump light and reducing the threshold value of laser oscillation by adopting double-doped Yb, Nd rare earth ions, and has very practical application value.
Description
Technical field
The present invention relates to a kind of yttrium aluminum garnet transparent ceramic material and preparation method of codope rare earth ion, belong to the advanced ceramics preparation field.
Background technology
Laser is one of human greatest invention of 20th century, and laser technology has been widely used in high-technology fields such as industrial and agricultural production, medical treatment, aerospace.Since nineteen sixty first ruby laser invention, a large amount of new pattern laser materials continue to bring out, and people begin working-laser material is carried out extensively and profoundly research and discovery.
Since 1964, the YAG crystalline of mixing Nd occurs, and is subjected to paying close attention to widely as the large power solid laser material.But mix the YAG crystal of Nd because shortcomings such as the growth cycle length of monocrystalline, crystal growth size, Nd ions dosage have restricted it uses widely.Along with improving constantly of great-power solid laser power, the wait in expectation appearance of new laserable material of people.Nineteen ninety-five, people such as Japanese A.Ikesue have made the polycrystalline Nd:YAG transparent ceramic material of complete densification and excellent optical performance, and obtain laser output.Coming years, especially after 2000, the Nd:YAG crystalline ceramics has obtained fast development, has realized the maximum power output of 67KW at present, has caused international extensive concern.Along with the continuous breakthrough of powder and ceramic preparation science and technology, polycrystalline transparent ceramic becomes the laserable material of the most competitive replacement monocrystalline.
Except Nd doping YAG crystalline ceramics, Yb mixes and has also received concern.Yb
3+Has the simplest level structure, with Nd
3+Compare, intrinsic quantum defective is low, photon efficient height, and the life time of the level is long, and absorption and emmission spectrum are wide.The appearance of the LD pumping source little along with volume, that the life-span is long, efficient is high, Yb
3+As laser active ionic research fast development.Yb particularly
3+Main absorption peak be positioned at 0.9～1.0 μ m, can effectively be coupled with the InGaAs laser diode pumping source of high brightness, and not need strict temperature control.While Yb
3+It also is a kind of high efficiency sensitized ions, sensitized ions can absorb more optical pump energy, and be transferred to active ions, and enlarging and strengthen the absorption spectrum of active ions, the optical pump energy that makes the ionic absorption that originally is not activated obtains utilizing by the effect of sensitized ions.Yb
3+Can absorb sensitizing agent as multiple laser active ionic pump energy, as Nd
3+Deng.Because the LD about 980nm is very general, so use Yb
3+Carry out sensitization and have more practical meaning, can reach raising the assimilated efficiency of pump light and the purpose of reduction laser generation threshold value.Also there are not two mix Yb, the relevant report of the yttrium aluminum garnet transparent ceramic material of Nd rare earth ion at present.
Summary of the invention
This purpose is to provide a kind of codope Yb for the deficiency of the yttrium aluminum garnet transparent ceramic material that further remedies, improves single doping with rare-earth ions, the yttrium aluminum garnet transparent ceramic material of Nd rare earth ion, another object of the present invention provides the preparation method of above-mentioned materials, doping by rare earth ion Yb, can improve the assimilated efficiency of Nd:YAG crystalline ceramics to pump light, and can reduce the laser generation threshold value, have actual application value.
Technical scheme of the present invention is: the yttrium aluminum garnet transparent ceramic material of codope rare earth ion is characterized in that: described transparent ceramic material chemical constitution general formula is: (Y
1-x-yYb
xNd
y)
3Al
5O
12, 0.01≤x≤0.1,0.005≤y≤0.05 wherein.
The present invention also provides the method for above-mentioned yttrium aluminum garnet transparent ceramic material, and its concrete steps are as follows:
(1) according to the chemical constitution general formula with Y
2O
3, Al
2O
3, Yb
2O
3And Nd
2O
3Powder carries out the weighing proportioning, adds the sintering aid that accounts for total powder quality 0.5～0.8%, and ball milling mixes the back oven dry and sieves;
(2) powder adopts first dry-pressing isostatic cool pressing technological forming again, and wherein dry-pressing pressure is 10～20MPa, and isostatic cool pressing pressure is 200～300MPa;
(3) biscuit of moulding carries out sintering, and the control sintering temperature is 1700～1800 ℃, and soaking time is 5～50h;
(4) the sample anneal behind the sintering prepares the yttrium aluminum garnet transparent ceramic material of codope rare earth ion.Preferred described Y
2O
3, Al
2O
3, Yb
2O
3And Nd
2O
3The purity of powder is 99.9%～99.999%.Sieve order number is 160～200 orders in the above-mentioned step (1).
Described sintering aid is at least a kind of in tetraethoxy, magnesium oxide or the Calcium Fluoride (Fluorspan).
The biscuit of moulding is in hydrogen atmosphere or 10 in the preferred steps (3)
-3～10
-4Sintering in the vacuum of Pa; Sample 1300～1550 ℃ of following anneal 2～20h in air in the step (4) behind the sintering.
Beneficial effect:
(1) mixing codope Yb on the YAG crystalline ceramics basis of Nd, Nd rare earth element, Yb
3+Be a kind of high efficiency sensitized ions, sensitized ions can absorb more optical pump energy, and is transferred to active ions Nd
3+, enlarging and strengthen the absorption spectrum of active ions, the optical pump energy that makes the ionic absorption that originally is not activated obtains utilizing by the effect of sensitized ions.Laserable material is needed just for the assimilated efficiency of raising material, and this lays a good foundation for it becomes the large power solid laser material.
(2) technology by optimizing is prepared the YAG transparent ceramic material of the codope rare earth ion of high permeability, and its high permeability reaches 76%.Illustrate that method that this patent provides can prepare the transparent ceramic material of high permeability.The crystalline ceramics that has high permeability simultaneously can effectively reduce the optical loss.
Description of drawings
The Yb that Fig. 1 embodiment 3 is prepared, the surface corrosion electromicroscopic photograph of Nd:YAG crystalline ceramics.
The Yb that Fig. 2 embodiment 3 is prepared, the cross-section morphology of Nd:YAG crystalline ceramics.
The Yb that Fig. 3 embodiment 5 is prepared, Nd:YAG pottery XRD figure spectrum.
Embodiment
Embodiment 1
Take by weighing 10.1961g purity and be α-Al of 99.99%
2O
3Powder, 13.2099g purity are 99.99% Y
2O
3Powder, 0.4729g purity are 99.99% Yb
2O
3Powder and 0.1009g purity are 99.99% Nd
2O
3Powder is put into nylon ball grinder with powder, and adds 100gAl
2O
3Abrading-ball, the analytically pure dehydrated alcohol of 12g, the analytically pure TEOS of 0.19g, ball milling is 12 hours then.To grind 200 mesh sieves after the oven dry of the slurry behind the ball milling.With above-mentioned powder earlier in stainless steel mould with the first one-step forming of 15MPa pressure, be pressed into biscuit through the 200MPa isostatic cool pressing then.Biscuit is placed vacuum tightness 10
-3～10
-4In the vacuum oven of Pa in 1700 ℃ of sintering 6 hours, the 1450 ℃ of anneal 20 hours in air of the sample behind the sintering.The two-sided sanding and polishing of sample after will annealing at last is thick to 1mm.Sintering obtains codope Yb, (the Y of Nd
0.975Yb
0.02Nd
0.005)
3Al
5O
12Crystalline ceramics, the relative density of sample are greater than 99%, and transmitance is 76%.
Embodiment 2
Take by weighing 10.1961g purity and be α-Al of 99.99%
2O
3Powder, 12.7357g purity are 99.99% Y
2O
3Powder, 1.1822g purity are 99.99% Yb
2O
3Powder and 0.2019g purity are 99.99% Nd
2O
3Powder is put into nylon ball grinder with powder, and adds 100gAl
2O
3Abrading-ball, the analytically pure dehydrated alcohol of 12g, the analytically pure TEOS of 0.2g, ball milling is 12 hours then.To grind 200 mesh sieves after the oven dry of the slurry behind the ball milling.With above-mentioned powder earlier in stainless steel mould with the first one-step forming of 15MPa pressure, be pressed into biscuit through the 200MPa isostatic cool pressing then.Biscuit is placed vacuum tightness 10
-3～10
-4In the vacuum oven of Pa in 1720 ℃ of sintering 12 hours, the 1450 ℃ of anneal 10 hours in air of the sample behind the sintering.The two-sided sanding and polishing of sample after will annealing at last is thick to 1mm.Sintering obtains codope Yb, (the Y of Nd
0.94Yb
0.05Nd
0.01)
3Al
5O
12Crystalline ceramics, sample relative density are greater than 99%, and transmitance is 75%, and average grain size is 20 μ m.
Embodiment 3
Take by weighing 10.1961g purity and be α-Al of 99.99%
2O
3Powder, 11.5163g purity are 99.99% Y
2O
3Powder, 2.3645g purity are 99.99% Yb
2O
3Powder and 1.0094g purity are 99.99% Nd
2O
3Powder is put into nylon ball grinder with powder, and adds 100gAl
2O
3Abrading-ball, the analytically pure dehydrated alcohol of 12g, the analytically pure TEOS of 0.2g, ball milling is 12 hours then.To grind 200 mesh sieves after the oven dry of the slurry behind the ball milling.With above-mentioned powder earlier in stainless steel mould with the first one-step forming of 15MPa pressure, be pressed into biscuit through the 200MPa isostatic cool pressing then.Biscuit is placed vacuum tightness 10
-3～10
-4In the vacuum oven of Pa in 1750 ℃ of sintering 6 hours, the 1450 ℃ of anneal 10 hours in air of the sample behind the sintering.The two-sided sanding and polishing of sample after will annealing at last is thick to 1mm.Sintering obtains codope Yb, (the Y of Nd
0.85Yb
0.1Nd
0.05)
3Al
5O
12Crystalline ceramics, sample relative density are greater than 99%, and transmitance is 76%.The Yb that the present invention is prepared, the surface corrosion electromicroscopic photograph of Nd:YAG crystalline ceramics as shown in Figure 1, the Yb that the present invention is prepared, Nd:YAG crystalline ceramics cross-section morphology as shown in Figure 2.Can see that sample does not have tangible pore basically on scheming, ceramic section all is transgranular fractures, and crystal boundary is clean, no crystal boundary phase.
Embodiment 4
Y with rare earth oxide 12.7357g
2O
3Powder, the Yb of 1.1822g
2O
3The Nd of powder and 0.2019g
2O
3Powder is dissolved in the nitric acid, and adds the analytically pure Al (NO of 75.026g
3)
39H
2O, with the mixing salt solution thin up to 1333ml.Get the 80ml strong aqua and add 252.992g bicarbonate of ammonia and be made into compound precipitants, wherein bicarbonate of ammonia concentration is 2mol/L, and precipitation agent is diluted to 1600ml.The salts solution that the mixes speed with 3ml/min is added drop-wise in the precipitation agent of vigorous stirring, generates white gelatinous precipitate.Behind precipitate with deionized water, dehydrated alcohol and washing with acetone, dry 24h in 80 ℃ of baking ovens obtains presoma.Presoma was obtained rear-earth-doped YAG powder in 2 hours 1200 ℃ of calcinings.Burnt powder is put into nylon ball grinder, and add 100gAl
2O
3Abrading-ball, the analytically pure dehydrated alcohol of 16g, the analytically pure TEOS of 0.12g, ball milling is 12 hours then.To grind 200 mesh sieves after the oven dry of the slurry behind the ball milling.With above-mentioned powder earlier in stainless steel mould with the first one-step forming of 15MPa, be pressed into biscuit through the 200MPa isostatic cool pressing then.Biscuit is placed vacuum tightness 10
-3～10
-4In the vacuum oven of Pa in 1750 ℃ of sintering 6 hours, the 1550 ℃ of anneal 2 hours in air of the sample behind the sintering.The two-sided sanding and polishing of sample after will annealing at last is thick to 1mm.Sintering obtains codope Yb, (the Y of Nd
0.94Yb
0.05Nd
0.01)
3Al
5O
12Crystalline ceramics, sample relative density are greater than 99%, and transmitance is 73%.
Embodiment 5
Y with rare earth oxide 11.5163g
2O
3Powder, the Yb of 2.3645g
2O
3The Nd of powder and 1.0094g
2O
3Powder is dissolved in the nitric acid, and adds the analytically pure Al (NO of 75.026g
3)
39H
2O, with the mixing salt solution thin up to 1333ml.Get the 120ml strong aqua and add 252.992g bicarbonate of ammonia and be made into compound precipitants, wherein bicarbonate of ammonia concentration is 2mol/L, and precipitation agent is diluted to 1600ml.The salts solution that the mixes speed with 3ml/min is added drop-wise in the precipitation agent of vigorous stirring, generates white gelatinous precipitate.Behind precipitate with deionized water, dehydrated alcohol and washing with acetone, dry 24h in 80 ℃ of baking ovens obtains presoma.Presoma was obtained rear-earth-doped YAG powder in 2 hours 1200 ℃ of calcinings.Burnt powder is put into nylon ball grinder, and add 100gAl
2O
3Abrading-ball, the analytically pure dehydrated alcohol of 16g, the analytically pure TEOS of 0.12g, ball milling is 12 hours then.To grind 200 mesh sieves after the oven dry of the slurry behind the ball milling.With above-mentioned powder earlier in stainless steel mould with the first one-step forming of 15MPa, be pressed into biscuit through the 200MPa isostatic cool pressing then.Biscuit is placed vacuum tightness 10
-3～10
-4In the vacuum oven of Pa in 1780 ℃ of sintering 6 hours, the 1550 ℃ of anneal 2 hours in air of the sample behind the sintering.The two-sided sanding and polishing of sample after will annealing at last is thick to 1mm.Sintering obtains codope Yb, (the Y of Nd
0.85Yb
0.1Nd
0.05)
3Al
5O
12Crystalline ceramics, sample relative density are greater than 99%, and transmitance is 75%.The Yb that the present invention is prepared, Nd:YAG pottery XRD figure spectrum as shown in Figure 3.Sample is pure YAG phase from scheming as can be seen, does not have other dephasign peak.
Claims (6)
1. the yttrium aluminum garnet transparent ceramic material of codope rare earth ion, it is characterized in that: described transparent ceramic material chemical constitution general formula is: (Y
1-x-yYb
xNd
y)
3Al
5O
12, 0.01≤x≤0.1,0.005≤y≤0.05 wherein.
2. method for preparing yttrium aluminum garnet transparent ceramic material as claimed in claim 1, its concrete steps are as follows:
(1) according to the chemical constitution general formula with Y
2O
3, Al
2O
3, Yb
2O
3And Nd
2O
3Powder carries out the weighing proportioning, adds the sintering aid that accounts for total powder quality 0.5～0.8%, and ball milling mixes the back oven dry and sieves;
(2) powder adopts first dry-pressing isostatic cool pressing technological forming again, and wherein dry-pressing pressure is 10～20MPa, and isostatic cool pressing pressure is 200～300MPa;
(3) biscuit of moulding carries out sintering, and the control sintering temperature is 1700～1800 ℃, and soaking time is 5～50h;
(4) the sample anneal behind the sintering prepares the yttrium aluminum garnet transparent ceramic material of codope rare earth ion.
3. method according to claim 2 is characterized in that in described Y
2O
3, Al
2O
3, Yb
2O
3And Nd
2O
3The purity of powder is 99.9%～99.999%.
4. method according to claim 2 is characterized in that sieve order number is 160～200 orders in the described step (1).
5. method according to claim 2 is characterized in that described sintering aid is at least a kind of in tetraethoxy, magnesium oxide or the Calcium Fluoride (Fluorspan).
6. method according to claim 2, the biscuit that it is characterized in that moulding in the step (3) is in hydrogen atmosphere or 10
-3～10
-4Sintering in the vacuum of pa; Sample 1300～1550 ℃ of following anneal 2～20h in air in the step (4) behind the sintering.
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| CN101891477A (en) * | 2010-07-23 | 2010-11-24 | 中国科学院上海硅酸盐研究所 | Method for preparing circular rod-shaped RE:YAG laser transparent ceramics |
| CN101891477B (en) * | 2010-07-23 | 2013-01-02 | 中国科学院上海硅酸盐研究所 | Method for preparing circular rod-shaped RE:YAG laser transparent ceramics |
| CN102581929A (en) * | 2012-02-16 | 2012-07-18 | 山东晶鑫晶体科技有限公司 | Cake forming method of high-purity alumina powder |
| CN102581929B (en) * | 2012-02-16 | 2014-03-05 | 山东晶鑫晶体科技有限公司 | Cake forming method of high-purity alumina powder |
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| CN104059635A (en) * | 2013-03-21 | 2014-09-24 | 海洋王照明科技股份有限公司 | Neodymium and ytterbium double doping alkali fluoborate up-conversion luminescent material, preparation method and application thereof |
| CN104099090A (en) * | 2013-04-09 | 2014-10-15 | 海洋王照明科技股份有限公司 | Dysprosium-doped alkali fluosilicic acid glass up-conversion luminescent material, and preparation method and application thereof |
| CN107253854A (en) * | 2017-05-18 | 2017-10-17 | 北京科技大学 | A kind of laser transparent ceramic of grade doping and preparation method thereof |
| CN107253854B (en) * | 2017-05-18 | 2020-10-02 | 北京科技大学 | Gradient doped laser transparent ceramic and preparation method thereof |
| CN108536993A (en) * | 2018-01-04 | 2018-09-14 | 广东工业大学 | A kind of determination method of raw material proportioning in optical ceramics preparation process |
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