CN101054724A - Method of preparing barium yttrium borate and barium yttrium borate crystal and use thereof - Google Patents
Method of preparing barium yttrium borate and barium yttrium borate crystal and use thereof Download PDFInfo
- Publication number
- CN101054724A CN101054724A CN 200710063683 CN200710063683A CN101054724A CN 101054724 A CN101054724 A CN 101054724A CN 200710063683 CN200710063683 CN 200710063683 CN 200710063683 A CN200710063683 A CN 200710063683A CN 101054724 A CN101054724 A CN 101054724A
- Authority
- CN
- China
- Prior art keywords
- crystal
- barium
- yttrium borate
- barium yttrium
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention discloses a preparation method and uses of a barium borate Yt crystal. Compared to the technology in existence, the monocrystal barium borate Yt in accordance with the present invention is characterized by its high luminescence intensity and light-emitting efficiency, sensitive responses and the like. Furthermore, in accordance with the present invention, said process can be used for getting barium borate Yt single crystal at conditions of air atmosphere and about 1019 DEG C, with mild experiment conditions and short reaction time; and the crystal obtained through the method possesses is characterized by its excellent quality, low material cost, simple equipment, being easy to extend. Said barium borate Yt crystal exhibits some characteristics such as high efficiency and quick-speed, when used for X-ray exploration.
Description
Technical field
The present invention relates to scintillation crystal and growth method thereof and purposes, particularly relate to a kind of employing Czochralski method growth barium yttrium borate crystal and the purposes aspect flicker (as the X-X-ray detection X) thereof.
Background technology
Have some crystal energetic ray (as, X-ray, gamma-radiation) or the irradiation of high energy particle under can launch UV-light or visible light, this phenomenon is called scintillation effect, the crystal with scintillation effect is called scintillation crystal.Good scintillation crystal should have three important performance index, i.e. the fall time and the high-density of high light yield, weak point.Business-like representative scintillation crystal has Bi
4Ge
3O
12(BGO), Gd
2SiO
5(GSO), PbWO
4(PWO) etc.BGO has higher photoyield, but grow fall time (～300ns); The fall time of PWO, but very short photoyield was not again very high.Barium yttrium borate is the borate compound that Inst. of Physics, CAS's crystal growth group is found first, (consults document 1:Li, X.Z.; Wang, C.; Chen, X.L.; Li, H.; Jia, L.S.; Wu, L.; Du Y.X.; Xu, Y.P.Inorg.Chem.2004,43,8555).Its spacer is P6
3/ m, basic structural unit are the B that is arranged in parallel along the c axle
3O
6The plane group, Y-O
6Octahedron is arranged in the middle of the parallel group.This Y-O
6Octahedron be with PWO in WO
4Group is similar, has served as the luminescence center of crystal under energetic ray excites (consulting document 2:A.A.Annenkov, M.V.Korzhik, P.Lecoq, Nucl.Instr.andMeth.A 2002,490,30.).People such as C.J.Duan have studied the luminosity of barium yttrium borate under x-ray excited of powdered form, and the luminescence center of finding it is about 385nm, and be that 27ns (consults document 3:Duan, C. fall time; Yuan, J.; Zhao, J.; J.Solid.State.Chem.2005,178,3698.).Relatively lack this fall time at last, but above-mentioned research only relates to the characteristic of Powdered barium yttrium borate, and for the characteristic research of single crystal barium yttrium borate, still nobody relates at present.
Summary of the invention
One of purpose of the present invention provides a kind of barium yttrium borate crystal with good blinking characteristic, and higher luminous intensity and speed of response are faster arranged under x-ray excited;
Another object of the present invention provides a kind of preparation method of barium yttrium borate crystal;
A further object of the present invention provides a kind of purposes of barium yttrium borate crystal.
For achieving the above object, the present invention adopts following technical scheme:
A kind of barium yttrium borate, described barium yttrium borate are single crystal.
A kind of preparation method of barium yttrium borate crystal, this method may further comprise the steps: at first with YBa
3B
9O
18The polycrystal raw material platinum crucible of packing into, platinum alloy crucible is put into monocrystal growing furnace, make temperature rising in the monocrystalline process furnace so that the polycrystal raw material fusing, use the polycrystal behind the platinum filament contact melting then, cooling rate with 0.5-2 ℃/h makes the polycrystal of fusing be cooled to 1018-1022 ℃ again, promptly on platinum filament, obtain the barium yttrium borate seed crystal, the seed crystal that obtains is fixed on the seed rod of platinum folder, and seed rod put into polycrystal after the fusing, rotary seed crystal rod, and make melt temperature remain on above-mentioned cooled temperature, with the speed cooling of 0.01-0.05 ℃/h, temperature is reduced to 1016-1018 ℃, obtains crystal on seed rod then, crystal is pulled out melt, reduce to room temperature with the speed of 30-50 ℃/h and obtain barium yttrium borate crystal.
Further, in barium yttrium borate polycrystalline melting process, temperature is elevated to 1019-1040 ℃ in the monocrystalline process furnace.
Further, described YBa
3B
9O
18Polycrystal raw material prepares through following step: at first with analytically pure yttrium oxide, barium carbonate, boric acid by 1: 3: the mol ratio of 9.0-9.1 is put into platinum crucible after grinding and mixing in agate mortar, platinum crucible is put into retort furnace, make in the retort furnace temperature be elevated to 920-940 ℃ and kept this temperature 12-72 hour, stop heating after making the abundant solid state reaction of reactant, cool to room temperature promptly obtains YBa
3B
9O
18Polycrystal.
Further, described analytically pure yttrium oxide, barium carbonate, boric acid purity is not less than 99.9%.
Further, described monocrystal growing furnace is MoSi
2U type resistor rod heating single crystal pulling stove.
A kind of purposes of barium yttrium borate crystal, described barium yttrium borate crystal is used for the X-X-ray detection X.
Compared with the prior art, the invention provides a kind of single crystal barium yttrium borate, characteristic such as with respect to the polycrystalline barium yttrium borate, the single crystal barium yttrium borate has luminous intensity and luminous efficiency height, be quick on the draw;
In addition, the present invention adopts the Czochralski method to carry out the barium yttrium borate crystal growth, can obtain the barium yttrium borate single crystal under the temperature condition in air atmosphere about 1019 ℃, the experiment condition gentleness, reaction times is short, and this growth method obtains, and crystal mass is good, raw materials cost is cheap, equipment is simple, be easy to popularization;
The present invention also provides a kind of purposes of barium yttrium borate crystal, and barium yttrium borate crystal is used for the X-X-ray detection X, the X-ray of injecting wherein efficiently can be converted to the UV-light or the visible light that can conveniently write down apace.
Description of drawings
Fig. 1 is the barium yttrium borate polycrystalline x-ray diffraction pattern that adopts the inventive method preparation;
Fig. 2 is the barium yttrium borate monocrystalline typical case photo that adopts the inventive method growth;
Fig. 3 is barium yttrium borate monocrystalline and the luminescent properties curve of PWO under x-ray excited that adopts the inventive method preparation.
Embodiment
Embodiment 1
At first prepare the barium yttrium borate polycrystal raw material:
With analytically pure yttrium oxide (Y
2O
3), barium carbonate (BaCO
3), boric acid (H
3BO
3) being 1: 3 in molar ratio: the ratio of 9.0-9.1 is put into platinum crucible after grinding and mixing in agate mortar, platinum crucible is put into retort furnace, be heated to 920 ℃ and kept 72 hours in this temperature, in heat-processed, grind 3 times, make the abundant solid state reaction of reactant, powered-down makes the sample furnace cooling promptly obtain YBa to room temperature then
3B
9O
18Polycrystalline.The x-ray diffraction pattern of the sample that obtains shows that resulting powder is a barium yttrium borate as shown in Figure 1.Above-mentioned analytically pure yttrium oxide, barium carbonate, boric acid purity is not less than 99.9%;
Utilize the above-mentioned raw materials growth to obtain the barium yttrium borate monocrystalline:
The YBa that above-mentioned reaction is obtained
3B
9O
18The polycrystal raw material platinum crucible of packing into is put into monocrystal growing furnace and is carried out crystal growth, and the monocrystalline process furnace is MoSi
2U type resistor rod heating single crystal pulling stove, and with the temperature of DWT-702 and EUROTHERM 818 joint program temperature regulators control monocrystalline process furnace, at first temperature in the monocrystalline process furnace is risen to 1040 ℃, so that the polycrystalline powder fully melts, utilize the polycrystal of platinum filament contact melting, cooling rate with 0.5 ℃/h makes the polycrystal of fusing slowly cool to 1018 ℃ again, promptly obtains the barium yttrium borate seed crystal on platinum filament.The seed crystal that obtains is fixed on the seed rod of platinum folder, and seed rod put into melt, speed of rotation rotary seed crystal rod with 15 rev/mins, and make melt temperature remain on 1018 ℃, with the speed cooling of 0.01 ℃/h, temperature is reduced to 1016 ℃ then, on seed rod, obtain the crystal of wanting, crystal is pulled out melt, reduce to room temperature with the speed of 30 ℃/h and obtain barium yttrium borate crystal, as shown in Figure 2.
At first prepare the barium yttrium borate polycrystal raw material:
With analytically pure yttrium oxide (Y
2O
3), barium carbonate (BaCO
3), boric acid (H
3BO
3) being 1: 3 in molar ratio: the ratio of 9.0-9.1 is put into platinum crucible after grinding and mixing in agate mortar, platinum crucible is put into retort furnace, be heated to 930 ℃ and kept 24 hours in this temperature, in heat-processed, grind 3 times, make the abundant solid state reaction of reactant, powered-down makes the sample furnace cooling promptly obtain YBa to room temperature then
3B
9O
18Polycrystalline.The x-ray diffraction pattern of the sample that obtains shows that resulting powder is a barium yttrium borate as shown in Figure 1.Above-mentioned analytically pure yttrium oxide, barium carbonate, boric acid purity is not less than 99.9%;
Utilize the above-mentioned raw materials growth to obtain the barium yttrium borate monocrystalline:
The YBa that above-mentioned reaction is obtained
3B
9O
18The polycrystal raw material platinum crucible of packing into is put into monocrystal growing furnace and is carried out crystal growth, and the monocrystalline process furnace is MoSi
2U type resistor rod heating single crystal pulling stove, and with the temperature of DWT-702 and EUROTHERM 818 joint program temperature regulators control monocrystalline process furnace, at first temperature in the monocrystalline process furnace is risen to 1040 ℃, so that the polycrystalline powder fully melts, utilize the polycrystal of platinum filament contact melting, cooling rate with 1 ℃/h makes the polycrystal of fusing slowly cool to 1019 ℃ again, promptly obtains the barium yttrium borate seed crystal on platinum filament; The seed crystal that obtains is fixed on the seed rod of platinum folder, and seed rod put into melt, speed of rotation rotary seed crystal rod with 10 rev/mins, and make melt temperature remain on 1019 ℃, with the speed cooling of 0.03 ℃/h, temperature is reduced to 1017 ℃ then, on seed rod, obtain the crystal of wanting, crystal is pulled out melt, reduce to room temperature with the speed of 40 ℃/h and obtain barium yttrium borate crystal, as shown in Figure 2.
At first prepare the barium yttrium borate polycrystal raw material:
With analytically pure yttrium oxide (Y
2O
3), barium carbonate (BaCO
3), boric acid (H
3BO
3) being 1: 3 in molar ratio: the ratio of 9.0-9.1 is put into platinum crucible after grinding and mixing in agate mortar, platinum crucible is put into retort furnace, be heated to 940 ℃ and kept this temperature 12 hours, in heat-processed, grind 5 times, make the abundant solid state reaction of reactant, powered-down makes the sample furnace cooling promptly obtain YBa to room temperature then
3B
9O
18Polycrystalline.The x-ray diffraction pattern of the sample that obtains shows that resulting powder is a barium yttrium borate as shown in Figure 1.Above-mentioned analytically pure yttrium oxide, barium carbonate, boric acid purity is not less than 99.9%;
Utilize the above-mentioned raw materials growth to obtain the barium yttrium borate monocrystalline:
The YBa that above-mentioned reaction is obtained
3B
9O
18The polycrystal raw material platinum crucible of packing into is put into monocrystal growing furnace and is carried out crystal growth, and the monocrystalline process furnace is MoSi
2U type resistor rod heating single crystal pulling stove, and with the temperature of DWT-702 and EUROTHERM 818 joint program temperature regulators control monocrystalline process furnace, at first temperature in the monocrystalline process furnace is risen to 1040 ℃, so that the polycrystalline powder fully melts, utilize the polycrystal of platinum filament contact melting, cooling rate with 2 ℃/h makes the polycrystal of fusing slowly cool to 1022 ℃ again, promptly obtains the barium yttrium borate seed crystal on platinum filament.The seed crystal that obtains is fixed on the seed rod of platinum folder, and seed rod put into melt, speed of rotation rotary seed crystal rod with 20 rev/mins, and make melt temperature remain on 1022 ℃, with the speed cooling of 0.05 ℃/h, temperature is reduced to 1018 ℃ then, on seed rod, obtain the crystal of wanting, crystal is pulled out melt, reduce to room temperature with the speed of 50 ℃/h and obtain barium yttrium borate crystal, as shown in Figure 2.
With identical X-ray parameter, measure barium yttrium borate crystal and PWO crystalline luminous intensity that the foregoing description obtains, the result as shown in Figure 3, the luminous intensity of barium yttrium borate crystal is PWO crystalline 7-8 times as we can see from the figure, luminescence center is about 400nm, the X-ray is used the tungsten target target from the F-30X-gamma ray source, and crystalline thickness to be measured is 1mm.
The scintillation crystal barium yttrium borate of method for preparing can be used for flicker especially for the X-X-ray detection X, described barium yttrium borate can efficiently convert the X-ray of injecting wherein to visible light or UV-light apace, luminous scope is 350-500nm, therefore can be used for the making of X-gamma ray detector.
Above embodiment shows that with yttrium oxide, barium carbonate, boric acid are raw material, can grow barium yttrium borate crystal with the Czochralski method.Be noted that the above embodiments just illustrate the present invention with concrete example, and should not be limitation of the present invention.Simultaneously, those of ordinary skill in the art knows, on design of the present invention basis, to various modifications and variations that the present invention carried out all at the protection domain of this patent.
Those of ordinary skill in the art may obtain the barium yttrium borate crystal sample, and is applied in other flicker measurement application, and these all do not exceed design of the present invention and scope.
Claims (7)
1, a kind of barium yttrium borate is characterized in that, described barium yttrium borate is a single crystal.
2, a kind of preparation method of barium yttrium borate crystal is characterized in that, this method may further comprise the steps:
At first with YBa
3B
9O
18The polycrystal raw material platinum crucible of packing into, platinum alloy crucible is put into monocrystal growing furnace, make temperature rising in the monocrystalline process furnace so that the polycrystal raw material fusing, use the polycrystal behind the platinum filament contact melting then, cooling rate with 0.5-2 ℃/h makes the polycrystal of fusing be cooled to 1018-1022 ℃ again, promptly on platinum filament, obtain the barium yttrium borate seed crystal, the seed crystal that obtains is fixed on the seed rod of platinum folder with the platinum filament binding, and seed rod put into polycrystal after the fusing, rotary seed crystal rod, and make melt temperature remain on above-mentioned cooled temperature, with the speed cooling of 0.01-0.05 ℃/h, be cooled to 1016-1018 ℃ then, on seed rod, obtain crystal, crystal is pulled out melt, reduce to room temperature with the speed of 30-50 ℃/h and obtain barium yttrium borate crystal.
3, the preparation method of barium yttrium borate crystal as claimed in claim 2 is characterized in that, in barium yttrium borate polycrystalline melting process, temperature is elevated to 1019-1040 ℃ in the monocrystalline process furnace.
4, the preparation method of barium yttrium borate crystal as claimed in claim 2 is characterized in that, described YBa
3B
9O
18Polycrystal raw material prepares through following step: at first with analytically pure yttrium oxide, barium carbonate, boric acid by 1: 3: the mol ratio of 9.0-9.1 is put into platinum crucible after grinding and mixing in agate mortar, platinum crucible is put into retort furnace, make in the retort furnace temperature be elevated to 920-940 ℃ and kept this temperature 12-72 hour, stop heating after making the abundant solid state reaction of reactant, cool to room temperature promptly obtains YBa
3B
9O
18Polycrystal.
5, the preparation method of barium yttrium borate crystal as claimed in claim 3 is characterized in that, described analytically pure yttrium oxide, and barium carbonate, boric acid purity is not less than 99.9%.
6, the preparation method of barium yttrium borate crystal as claimed in claim 2 is characterized in that, described monocrystal growing furnace is MoSi
2U type resistor rod heating single crystal pulling stove.
7, the purposes of the described barium yttrium borate crystal of a kind of claim 2 is characterized in that, described barium yttrium borate crystal is used for the X-X-ray detection X.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710063683 CN101054724A (en) | 2007-02-07 | 2007-02-07 | Method of preparing barium yttrium borate and barium yttrium borate crystal and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710063683 CN101054724A (en) | 2007-02-07 | 2007-02-07 | Method of preparing barium yttrium borate and barium yttrium borate crystal and use thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101054724A true CN101054724A (en) | 2007-10-17 |
Family
ID=38794769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710063683 Pending CN101054724A (en) | 2007-02-07 | 2007-02-07 | Method of preparing barium yttrium borate and barium yttrium borate crystal and use thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101054724A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021651B (en) * | 2009-09-11 | 2013-01-02 | 中国科学院上海硅酸盐研究所 | Cerium-doped rare earth borate scintillating crystal and Bridgman preparation method thereof |
-
2007
- 2007-02-07 CN CN 200710063683 patent/CN101054724A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021651B (en) * | 2009-09-11 | 2013-01-02 | 中国科学院上海硅酸盐研究所 | Cerium-doped rare earth borate scintillating crystal and Bridgman preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108221055B (en) | Intrinsically luminous scintillation crystal magnesium tantalate and preparation method and application thereof | |
| Feng et al. | Growth and luminescence characteristics of cerium-doped yttrium pyrosilicate single crystal | |
| CN105543963A (en) | Rare earth scintillation crystal prepared from low-cost rare earth raw materials and low-cost growth process of rare earth scintillation crystal | |
| CN105986320A (en) | Sc/Ce-codoped lutetium silicate and lutetium yttrium silicate crystals and melt-process growth method thereof | |
| Yiting et al. | Study on phase diagram of Bi2O3 SiO2 system for Bridgman growth of Bi4Si3O12 single crystal | |
| CN109161968B (en) | Red long-afterglow single crystal material and preparation method thereof | |
| Yokota et al. | Cathodoluminescence of Ce-doped Gd2SiO5 and Gd9. 33 (SiO4) 6O2 phosphor under continuous electron irradiation | |
| He et al. | YBa3B9O18: a promising scintillation crystal | |
| CN105969354A (en) | Cerium-doped gadolinium disilicate luminescent material and preparation method thereof | |
| CN1587447A (en) | Process for preparing high temperature cerium blended lutetium pyrosilicate scintillation monocrystal | |
| CN105332056A (en) | Divalent metal cation and cerium co-doped lutetium aluminum garnet crystal for laser illumination and preparation method thereof | |
| CN108441959A (en) | Mix Cerium aluminate gadolinium lutetium garnet crystal preparation method | |
| CN106149054A (en) | Mix Cerium aluminate gadolinium yttrogarnet high temperature scintillation crystal and preparation method thereof | |
| CN101054724A (en) | Method of preparing barium yttrium borate and barium yttrium borate crystal and use thereof | |
| CN101377018A (en) | Novel scintillation crystal material NaLa(WO4)2 doped with Ce<3+> | |
| CN1308415C (en) | Photoluminescence crystal material strontium borate lithium | |
| CN1259465C (en) | Preparation of divalent cerium ion dosed rare earth silicate scintillating crystal | |
| Yakubovskaya et al. | Nanocrystalline zinc and cadmium tungstates: morphology, luminescent and scintillation properties | |
| Pidol et al. | Czochralski growth and physical properties of cerium-doped lutetium pyrosilicate scintillators Ce3+: Lu2Si2O7 | |
| CN115367767A (en) | Lithium sodium yttrium borate, cerium doped compound and crystal thereof, and preparation method and application thereof | |
| He et al. | Growth and optical properties of YBa3B9O18: Ce crystals | |
| CN1283852C (en) | Method for growing gadolinium orthosilicate scintillation crystal | |
| CN101701154B (en) | Brominated rare earth scintillating materials and preparation method of Brominated rare earth scintillating crystals | |
| Yokota et al. | Growth and Scintillation Properties of Ce: Li (Ca, Ba) AlF $ _ {{6}} $ Scintillator Crystals | |
| CN101377019A (en) | Novel scintillation crystal material NaY(WO4)2 doped with Ce<3+> |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |