CN1277000C - Preparation method of double tungstate crystal with stoichiometric ratio - Google Patents
Preparation method of double tungstate crystal with stoichiometric ratio Download PDFInfo
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- CN1277000C CN1277000C CN 200310109409 CN200310109409A CN1277000C CN 1277000 C CN1277000 C CN 1277000C CN 200310109409 CN200310109409 CN 200310109409 CN 200310109409 A CN200310109409 A CN 200310109409A CN 1277000 C CN1277000 C CN 1277000C
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- crystal
- tungstate
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- stoichiometric ratio
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- 239000013078 crystal Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title abstract 5
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 12
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 12
- 238000009792 diffusion process Methods 0.000 claims abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 18
- 229910052697 platinum Inorganic materials 0.000 claims description 16
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 13
- 229910052691 Erbium Inorganic materials 0.000 claims description 11
- 229910052779 Neodymium Inorganic materials 0.000 claims description 9
- 229910052700 potassium Chemical group 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 229910052693 Europium Inorganic materials 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 229910052727 yttrium Inorganic materials 0.000 claims description 7
- 238000007716 flux method Methods 0.000 claims description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 4
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 229910052765 Lutetium Inorganic materials 0.000 claims description 3
- 229910052728 basic metal Inorganic materials 0.000 claims description 3
- 150000003818 basic metals Chemical class 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims 1
- 229910052702 rhenium Inorganic materials 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
- 229910001413 alkali metal ion Inorganic materials 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 abstract 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 abstract 1
- 229910000027 potassium carbonate Inorganic materials 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000011067 equilibration Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006295 Si—Mo Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005466 cherenkov radiation Effects 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Stoichiometric ratio double tungstate crystal A (Re)xMe1-x)(WO4)2The preparation method mainly utilizes Na2CO3，K2CO3And the low melting point and the easy volatilization diffusion characteristic, the gas phase transmission balance is adopted, and the diffusion of alkali metal ions in the non-stoichiometric double tungstate crystal is controlled by adjusting the composition ratio, the temperature, the time and other parameters of the mixture in the atmosphere rich in alkali metal vapor, so that the stoichiometric double tungstate crystal is prepared. The invention greatly reduces the non-crystallization in the crystalThe defect of the stoichiometric ratio point can meet the requirements of the double tungstate crystal in the fields of laser, scintillation and other luminescence.
Description
Technical field
The present invention relates to double-tungstate crystal.Be particularly related to a kind of preparation stoichiometric ratio double-tungstate crystal, chemical general formula can be expressed as A (Re
xMe
1-x) (WO
4)
2, (wherein A represents alkali metal: K, Na; Re represents doped with rare-earth elements: Nd, Yb, Ho, Pr, Eu, Er; Me represents Y, Bi, Gd, La, Dy, elements such as Lu; 0≤x≤0.2) method is specifically related at rich alkali metal vapour (A=Na
+, K
+) in the atmosphere by the gas phase transmission with alkalimetal ion (A=Na
+, K
+) diffuse to non-metering than in the double-tungstate crystal to obtain the double-tungstate crystal of stoichiometric ratio.This serial crystal is with a wide range of applications in Solid State Laser field, scintillation crystal field and Raman shifting device.
Background technology
Double-tungstate crystal has A (Re
xMe
1-x) (WO
4)
2Chemical general formula, wherein A represents alkali metal: K, Na etc.; Re represents doped with rare-earth elements: Nd, Yb, Ho, Pr, Eu, Er etc.; Me represents Y, Bi, Gd, La, Dy, elements such as Lu; 0≤x≤0.2.They have two kinds of spacer structure: C
2/cAnd I
41/a, for example, β-KGd (WO commonly used
4)
2Crystal belongs to oblique system C
2/c, behind the rare earth ions such as this crystal doping Nd, Yb, be a kind of good laser crystal material with the big excitation-emission of low threshold value cross section; NaBi (WO commonly used
4)
2Belong to tetragonal system I in crystal
41/a, this crystal also is good laser host material, it has advantages such as the big emission of the wide absorption of low threshold value equally, in addition, pure NaBi (WO
4)
2Crystal still is a kind of good Cherenkov radiation detection scintillation crystal.In addition, double-tungstate crystal also has bigger third-order non-linear effect χ
3, the some of them host crystal also has higher gain Raman shifting Laser emission, thus double-tungstate crystal in the Solid State Laser field, Raman shifting Laser emission and flash detection field be with a wide range of applications.(referring to; Journal of Crystal Growth, 1999 the 206th phase 60-64 pages or leaves; Referring to: Journal of Physics and Chemistry of Solids, 2002 the 63rd phase 95-105 pages or leaves).
Belong to monoclinic K (Re in the double-tungstate crystal
xMe
1-x) (WO
4)
2Crystal (Re=Nd, Yb, Ho, Pr, Eu, Er etc., Me=Y, Bi, Gd, La, Dy, Lu, 0≤x≤0.2) is generally non-congruent melting compound, and (fusing assistant is K to adopt the flux method growth usually
2O and WO
3); And belong to the Na (Re of tetragonal system in the double-tungstate crystal
xMe
1-x) (WO
4)
2Crystal (Re=Nd, Yb, Ho, Pr, Eu, Er etc., Me=Y, Bi, Gd, La, Dy, Lu, 0≤x≤0.2) is generally congruent melting compound, adopts usually and grows from the melt of stoichiometric ratio, generally adopts crystal pulling method or falling crucible method to grow.(referring to: Journal of CrystalGrowth in 2002, the 240th volume (3-4 phase), 495-462 page or leaf; Referring to: calendar year 2001, Optical Materials, the 16th volume 43-46 page or leaf).
Owing to contain basic metal in the double-tungstate crystal: as Na, K etc. because alkaline carbonate has lower fusing point, are generally less than 900 ℃ of (for example, NaCO
3Fusing point is 850 ℃), in the process of growing crystal, often be easy to volatilization and cause serious scarce alkali metal in the double-tungstate crystal, thereby in double-tungstate crystal, formed the point defect of a large amount of non-stoichiometrics.
Formerly the double-tungstate crystal of technology growth has following significant disadvantages: (1) is because the low saturated vapo(u)r of alkaline carbonate fusing point forces down easy volatilization, easy nonstoichiometry ratio in crystal growing process, cause the skew of fusing point to bring difficulty to crystal growth on the one hand, Sheng Chang double-tungstate crystal is the non-stoichiometric crystal on the other hand; (2) have more point defect in the double-tungstate crystal of non-stoichiometric, be called as the trap center of photon-electron etc., cause the reduction of laser or scintillation photons quantum yield, this will limit the application of crystal in fields such as laser and flash detections greatly.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiency that prior art can not obtain the stoichiometric ratio double-tungstate crystal, and a kind of method for preparing the double-tungstate crystal of homogeneous and controllable stoichiometric ratio is provided.
Technical solution of the present invention is to make full use of Na
2CO
3, K
2CO
3Feature etc. the volatile diffusion of low melting point, adopt vapor transport equilibration (Vapor Transport Equilibration, be called for short VTE) technology, in the atmosphere of high temperature, rich alkali metal vapour, by regulating parameters such as mixing component proportioning, temperature and time, the control alkalimetal ion spreads in the non-stoichiometric double-tungstate crystal, treats to prepare after the diffusive equilibrium double-tungstate crystal of stoichiometric ratio, to satisfy the needs in fields such as laser and flash detection.
Stoichiometric ratio double-tungstate crystal A (Re of the present invention
xMe
1-x) (WO
4)
2The preparation method, its concrete processing step is as follows:
＜1〉in platinum crucible, is placed with the A (Re of band pore
xMe
1-x) (WO
4)
2Polycrystal piece and corresponding alkali metal carbonate A
2CO
3(A represents alkali metal, Na and K) mixture block;
＜2〉the double-tungstate wafer with non-stoichiometric places or is suspended from the platinum wire, adds to be coated with A (Re
xMe
1-x) (WO
4)
2Polycrystal piece and corresponding alkali metal carbonate A
2CO
3It is airtight that the mixture block of (A represents alkali metal, Na and K) and the crucible cover of thermopair, crucible top add the platinum lid, places resistance furnace;
＜3〉about this resistance furnace heat temperature raising to 600～800 ℃, constant temperature 20～100 hours, basic metal A (Na
+Perhaps K
+) ion diffusion is to the double-tungstate A (Re of non-metering ratio
xMe
1-x) (WO
4)
2In the wafer, the rate of temperature fall with 40-60 ℃/h is cooled to the A (Re that room temperature can obtain stoichiometric ratio then
xMe
1-x) (WO
4)
2Double-tungstate crystal.
Above-mentioned processing step＜1〉described in A (Re
xMe
1-x) (WO
4)
2And A
2CO
3The scope of choosing of the weight ratio of mixture block is [A (Re
xMe
1-x) (WO
4)
2]/[A
2CO
3]=(10～98): (90～2).Double-tungstate A (Re wherein
xMe
1-x) (WO
4)
2A represents alkali metal in the polycrystal piece: K, Na; Re represents doped with rare-earth elements: Nd, Yb, Ho, Pr, Eu, elements such as Er; Me represents Y, Bi, Gd, La, Dy, elements such as Lu; 0≤x≤0.2.
Above-mentioned processing step＜2〉described in the non-stoichiometric double-tungstate crystal can pass through the A (Re of growth such as crystal pulling method, falling crucible method or flux method
xMe
1-x) (WO
4)
2Crystal, (wherein A represents alkali metal: K, Na; Re represents doped with rare-earth elements: Nd, Yb, Ho, Pr, Eu, Er; Me represents Y, Bi, Gd, La, Dy, elements such as Lu; 0≤x≤0.2).
Above-mentioned processing step＜2〉described in resistance furnace also available silicon kryptol stone, Si-Mo rod stove or other stove by Electric heating replace.
Above-mentioned processing step＜3〉described in constant temperature time look size, thermostat temperature and the double-tungstate polycrystal of double-tungstate wafer and the ratio of alkaline carbonate mixture block changes in above-mentioned constant temperature time scope.Generally speaking, wafer big more (thickness is thick, area is big), thermostat temperature are low more, and then constant temperature time is longer.
The present invention prepares the stoichiometric ratio double-tungstate crystal and compares than double-tungstate crystal with formerly technology growth is non-metering, its advantage is: made full use of the volatile characteristics of alkali-metal low melting point, by gas phase transmission diffusion alkalimetal ion is diffused in the double-tungstate crystal of non-metering ratio, thereby obtained the double-tungstate crystal of stoichiometric ratio, significantly reduced the non-stoichiometric point defect that exists in the crystal, can satisfy the needs of double-tungstate crystal in luminous fields such as laser, flickers.
Description of drawings
Fig. 1 is a vapor transport equilibration experimental installation synoptic diagram.
Embodiment
Used vapor transport equilibration (VTE) technology of the present invention prepares the experimental installation synoptic diagram of stoichiometric ratio double-tungstate crystal and sees Fig. 1, in the platinum crucible 1, be placed with the double-tungstate polycrystal and the alkaline carbonate mixture block 3 of certain proportioning of band pore 2, material piece 3 tops are platinum wires 4, use crystal pulling method, the double-tungstate wafer 5 of the non-metering ratio of descent method or flux method growth places on the platinum wire 4, material piece 3 tops have platinum sheet 6 and double-tungstate polycrystal and alkaline carbonate mixed powder 7 to cover, thermopair 8 inserts in the powders 7, and crucible 1 top adds platinum and covers 9 airtight.
Adopt the VTE technology how to prepare the concrete process flow steps of the double-tungstate crystal of stoichiometric ratio below in conjunction with the specific embodiment explanation.
Embodiment 1: the doping 20%Nd ionic NaBi (WO of preparation stoichiometric ratio
4)
2Crystal
Step of preparation process is as follows:
＜1〉in platinum crucible 1, is placed with 20% adulterated NaBi (WO of band pore 2
4)
2And Na
2CO
3Mixture block 3 is chosen [NaNd
0.2Bi
0.8(WO
4)
2]/[Na
2CO
3]=98: 2 weight ratio;
＜2〉with 20% adulterated Nd of the non-metering ratio of crystal pulling method or descent method for growing: NaBi (WO
4)
2Crystal places or is suspended from the platinum wire, adds to be coated with NaBi (WO
4)
2And Na
2CO
3The crucible cover of mixed powder 7 and thermopair 8, crucible top add platinum and cover 9 airtightly, place resistance furnace;
＜3〉about heat temperature raising to 800 ℃, constant temperature 100 hours, the Na ion diffusion is to NaBi (WO
4)
2In the crystal, reduce to room temperature with the cooling rate of 40 ℃/h then, obtain the NaBi (WO that mixes Nd of stoichiometric ratio at last
4)
2Crystal.
Embodiment 2: the pure NaBi (WO of preparation stoichiometric ratio
4)
2Crystal
The processing step of preparation is as follows:
＜1〉in platinum crucible 1, is placed with the NaBi (WO of band pore 2
4)
2And Na
2CO
3Mixture block 3 is chosen [NaBi (WO
4)
2]/[Na
2CO
3]=50: 50 weight ratio;
＜2〉with the NaBi (WO of the non-metering ratio of crystal pulling method or descent method for growing
4)
2Crystal places or is suspended from the platinum wire, adds to be coated with NaBi (WO
4)
2And Na
2CO
3The crucible cover of mixed powder 7 and thermopair 8, crucible top add platinum and cover 9 airtightly, place resistance furnace;
＜3〉about heat temperature raising to 700 ℃, constant temperature 40 hours, the Na ion diffusion is to NaBi (WO
4)
2In the crystal, reduce to room temperature with the cooling rate of 50 ℃/h then, obtain stoichiometric ratio NaBi (WO at last
4)
2Crystal.
Embodiment 3: the KGd (WO of the doping 5%Yb of preparation stoichiometric ratio
4)
2Crystal
The processing step of preparation is as follows:
＜1〉in platinum crucible 1, is placed with the KGd (WO that mixes 15%Yb of band pore 2
4)
2And K
2CO
3Mixture block 3 is chosen [KYb
0.05Gd
0.95(WO
4)
2]/[K
2CO
3]=80: 20 weight ratio;
＜2〉KGd (WO of the 5%Yb of the non-metering ratio that flux method is grown
4)
2Crystal places or is suspended from the platinum wire, adds to be coated with KYb
0.05Gd
0.95(WO
4)
2And K
2CO
3The crucible cover of mixed powder 7 and thermopair 8, crucible top add platinum and cover 9 airtightly, place resistance furnace;
＜3〉about heat temperature raising to 650 ℃, constant temperature 60 hours, the K ion diffusion is to the adulterated KGd (WO of 5%Yb
4)
2In the crystal, reduce to room temperature with the cooling rate of 60 ℃/h then, obtain the adulterated KGd (WO of stoichiometric ratio 5%Yb at last
4)
2Crystal.
Embodiment 4: the KGd (WO of the doping 2%Er of preparation stoichiometric ratio
4)
2Crystal
The processing step of preparation is as follows:
＜1〉in platinum crucible 1, is placed with the KGd (WO that mixes 2%Er of band pore 2
4)
2And K
2CO
3Mixture block 3 is chosen [Ker
0.02Gd
0.98(WO
4)
2]/[K
2CO
3]=10: 90 weight ratio;
＜2〉KGd (WO of the 2%Er of the non-metering ratio that flux method is grown
4)
2Crystal places or is suspended from the platinum wire, adds to be coated with Ker
0.02Gd
0.98(WO
4)
2And K
2CO
3The crucible cover of mixed powder 7 and thermopair 8, crucible top add platinum and cover 9 airtightly, place resistance furnace;
＜3〉about heat temperature raising to 750 ℃, constant temperature 50 hours, the K ion diffusion is to the adulterated KGd (WO of 2%Er
4)
2In the crystal,, obtain the adulterated KGd (WO of stoichiometric ratio 2%Er at last then with the near room temperature of the cooling rate of 50 ℃/h
4)
2Crystal.
Claims (4)
1, a kind of stoichiometric ratio double-tungstate crystal A (Re
xMe
1-x) (WO
4)
2The preparation method, it is characterized in that the concrete processing step of this method is as follows:
＜1〉in platinum crucible, is placed with the A (Re of band pore
xMe
1-x) (WO
4)
2Polycrystal piece and corresponding alkali metal carbonate A
2CO
3Mixture block, wherein A represents alkali metal, Na and K, Re represents doped with rare-earth elements: Nd, Yb, Ho, Pr, Eu, Er element; Me represents Y, Bi, Gd, La, Dy, Lu element; 0≤x≤0.2;
＜2〉the double-tungstate wafer with non-stoichiometric places or is suspended from the platinum wire, adds to be coated with A (Re
xMe
1-x) (WO
4)
2Polycrystal piece and corresponding alkali metal carbonate A
2CO
3Mixture block and the crucible cover of thermopair, it is airtight that the crucible top adds platinum lid, places resistance furnace;
＜3〉about this resistance furnace heat temperature raising to 600～800 ℃, constant temperature 20～100 hours, basic metal A ion diffusion is to the double-tungstate A (Re of non-metering ratio
xMe
1-x) (WO
4)
2In the wafer, the rate of temperature fall with 40-60 ℃/h is cooled to the A (Re that room temperature can obtain stoichiometric ratio then
xMe
1-x) (WO
4)
2Double-tungstate crystal.
2, stoichiometric ratio double-tungstate crystal A (Re according to claim 1
xMe
1-x) (WO
4)
2The preparation method, it is characterized in that described A (Re
xMe
1-x) (WO
4)
2And A
2CO
3The scope of choosing of the weight ratio of mixture block is [A (Re
xMe
1-x) (WO
4)
2]/[A
2CO
3]=(10～98): (90～2).
3, stoichiometric ratio double-tungstate crystal A (Re according to claim 1
xMe
1-x) (WO
4)
2The preparation method, it is characterized in that described non-stoichiometric double-tungstate crystal can pass through the A (Re of crystal pulling method, falling crucible method or flux method growth
xMe
1-x) (WO
4)
2Crystal.
4, stoichiometric ratio double-tungstate crystal A (Re according to claim 1
xMe
1-x) (WO
4)
2The preparation method, it is characterized in that described constant temperature time looks the ratio of the size of double-tungstate wafer, thermostat temperature and double-tungstate polycrystal and alkali tungstates mixture block and change in above-mentioned constant temperature time scope, generally speaking, wafer is big more, thermostat temperature is low more, and then constant temperature time is longer.
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|---|---|---|---|
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|---|---|---|---|
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| CN1277000C true CN1277000C (en) | 2006-09-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101140138B (en) * | 2007-01-23 | 2012-02-29 | 北京核心动力科技有限公司 | Crucible with temperature sensor protecting equipment |
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|---|---|---|---|---|
| CN100395380C (en) * | 2006-04-21 | 2008-06-18 | 北京工业大学 | Process for preparing barium tungstate single crystal with improved doping concentration of rare earth ion |
| CN100412157C (en) * | 2006-06-09 | 2008-08-20 | 中国科学院上海硅酸盐研究所 | X-ray excited rare-earth ion blended tungstate flash luminous material and its preparing method |
| CN101775655B (en) * | 2010-01-13 | 2013-07-17 | 福州高意通讯有限公司 | Laser crystal and preparation method thereof |
| CN102888654A (en) * | 2012-10-22 | 2013-01-23 | 中国科学院福建物质结构研究所 | Praseodymium-doped lutetium potassium tungstate laser crystal and preparation method thereof |
| CN103320128A (en) * | 2013-06-24 | 2013-09-25 | 上海大学 | Red light-emitting tungstate fluorescent powder |
| CN103834400B (en) * | 2014-03-13 | 2015-06-17 | 重庆理工大学 | Calcium tungstate fluorescent powder and preparation method thereof |
| CN107216150B (en) * | 2017-06-30 | 2020-01-31 | 武汉工程大学 | low-temperature co-fired ceramic materials and preparation method thereof |
| CN110004493A (en) * | 2019-02-21 | 2019-07-12 | 中国科学院上海硅酸盐研究所 | A kind of growing method of wolframic acid lanthanum (gadolinium) sodium crystal |
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2003
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101140138B (en) * | 2007-01-23 | 2012-02-29 | 北京核心动力科技有限公司 | Crucible with temperature sensor protecting equipment |
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| CN1546749A (en) | 2004-11-17 |
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