CN103695002B - Inorganic scintillation material - Google Patents
Inorganic scintillation material Download PDFInfo
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- CN103695002B CN103695002B CN201310733515.8A CN201310733515A CN103695002B CN 103695002 B CN103695002 B CN 103695002B CN 201310733515 A CN201310733515 A CN 201310733515A CN 103695002 B CN103695002 B CN 103695002B
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- alkaline
- scintillation material
- earth metal
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Abstract
The invention discloses a kind of inorganic scintillation material.The chemical constitution of this inorganic scintillation material has following general formula: La
1-ace
am
bx
cbr
d, wherein M is one or both in alkaline-earth metal Mg, Ca, Sr, Ba, and X is one in Cl, I or two kinds, 0.01≤a≤1,0.0001≤b≤0.002,0.0001 & lt; C≤0.6,2.4 & lt; D≤3, and 3+2b=c+d.Chemical constitution meets the inorganic scintillation material of above-mentioned general formula, has the feature such as high light yield, fast decay, high energy resolution.
Description
Technical field
The present invention relates to scintillation material field, in particular to a kind of inorganic scintillation material.
Background technology
Scintillation material can be used for the detection of the high energy particles such as energetic ray and neutron such as alpha-ray, gamma-rays, X-ray, extensive application in nuclear medicine, high energy physics, safety inspection, industrial non-destructive flaw detection, space physics and core mine locating etc.
Scintillation material is applied with the form of single crystal usually, also can be pottery or other forms in some circumstances.
The performance requriements of different Application Areass to scintillation material is not quite similar.But for most of Application Areas, all wish that scintillation material has as far as possible high photoyield, as far as possible short fall time and as far as possible high energy resolution.Particularly for the nuclear medical imaging apparatus of PET (positron emission tomography) scanner (PositronEmissionTomographb, PET) and so on, these parameters are most important to imaging precision.People also wish that scintillation material has stable physicochemical property simultaneously, not deliquescence, are easy to processing.
The scintillation material that current commercial PET adopts mainly silicic acid lutetium (Lu
2si
2o
5) and yttrium luetcium silicate (the silicic acid lutetium of doped yttrium) crystal, but these crystal still can not meet the requirement of the Novel PET adopting flight time (Time-of-Flight, TOF) technology completely.Particularly their longer fall times (about 47ns), lower energy resolution (about 10%), have impact on image quality and the spatial resolution of instrument.Therefore, people attempt to search out the more superior new scintillator crystal materials of performance, to improve the performance of TOF-PET further always.
The people such as E.V.D.vanLoef LaBr disclosed in the calendar year 2001
3: Ce crystal, compare the crystal such as silicic acid lutetium, yttrium luetcium silicate and there is higher light output (about 60000ph/MeV), faster fall time (about 30ns) and higher energy resolution (about 3%), thus become the strong candidate of PET scintillator crystal materials of new generation.People have carried out much work to improve LaBr further
3: the performance of Ce crystal.Wherein, doping is a kind of effective means.
Summary of the invention
The present invention aims to provide a kind of inorganic scintillation material, compares LaBr
3: Ce over-all properties more superior, the inorganic scintillation material that is more suitable for TOF-PET application demand.
To achieve these goals, according to an aspect of the present invention, a kind of inorganic scintillation material is provided.The chemical constitution of this inorganic scintillation material has following general formula: La
1-ace
am
bx
cbr
d, wherein M is one or both in alkaline-earth metal Mg, Ca, Sr, Ba, and X is one in Cl, I or two kinds, 0.01≤a≤1,0.0001≤b≤0.002,0.0001<c≤0.6,2.4<d≤3, and 3+2b=c+d.
Further, M is one or both in Mg, Ca, and X is I, or I and Cl.
Further, M is one or both in Sr, Ba, and X is Cl, or Cl and I.
Further, M is Mg, X is I.
Further, M is Ca, X is I.
Further, M is Sr, X is Cl.
Further, M is Ba, X is Cl.
Further, 0.01≤a≤0.1.
Further, 0.0002≤b≤0.0015.
Further, 0.0004≤c≤0.4.The chemical constitution of inorganic scintillation material of the present invention has following general formula: La
1-ace
am
bx
cbr
d, wherein M is one or both in alkaline-earth metal Mg, Ca, Sr, Ba, and X is one in Cl, I or two kinds, 0.01≤a≤1,0.0001≤b≤0.002,0.0001<c≤0.6,2.4<d≤3, and 3+2b=c+d.Chemical constitution meets the inorganic scintillation material of above-mentioned general formula, has the feature such as high light yield, fast decay, high energy resolution.
Embodiment
It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.The present invention is described in detail below in conjunction with embodiment.
According to a kind of typical embodiment of the present invention, provide a kind of inorganic scintillation material.The chemical constitution of this inorganic scintillation material has following general formula: La
1-ace
am
bx
cbr
d, wherein M is one or both in alkaline-earth metal Mg, Ca, Sr, Ba, and X is one in Cl, I or two kinds, 0.01≤a≤1,0.0001≤b≤0.002,0.0001<c≤0.6,2.4<d≤3, and 3+2b=c+d.Chemical constitution meets the inorganic scintillation material of above-mentioned general formula, has the feature such as high light yield, fast decay, high energy resolution.
Preferably, alkaline-earth metal and halide-ions combination M/X have following rule: when M is one or both in Mg, Ca, X must contain I, and namely when M is one or both in Mg, Ca, X is I, or I and Cl; When M is one or both in Sr, Ba, X must contain Cl, and when namely M is one or both in Sr, Ba, X is Cl, or Cl and I.
Concrete, the preferred alkaline-earth metal of the present invention and halide-ions combination M/X can be following several: Mg/I, Ca/I, Sr/Cl, Ba/Cl.
Inorganic scintillation material of the present invention, normally single crystal, but also can be powder, pottery or polycrystal.
Scintillation material of the present invention can adopt the muriate of the muriate of La, Ce, bromide, iodide and alkaline-earth metal, bromide, iodide to be raw material; according to the stoichiometric ratio of chemical constitution general formula; under anhydrous and oxygen-free environment, (in the glove box as Ar gas shielded) weighs mixing, obtains after 700 ~ 900 DEG C of thermal treatment.Especially, for monocrystal material, mixing raw material can be packaged in vitreosil crucible, adopt Bridgman method growth to obtain.
Scintillation material chemical structure of the present invention and LaBr
3: Ce is substantially identical, can regard the LaBr through alkaline-earth metal ions and halide-ions co-doped as
3: Ce.The present invention is mixing altogether by divalent alkaline-earth metal ion and halide-ions to the topmost contribution of prior art, realizes LaBr
3: the Effective Regulation of Ce crystal property and lifting.
The doping of independent divalent alkaline-earth metal ion can significantly improve LaBr
3: the energy resolution of Ce crystal, but also can be with simultaneously and serve counter productive.Divalent alkaline-earth metal ion is at LaBr
3the position of trivalent La ion is occupied in lattice.Mg
2+, Ca
2+, Sr
2+, Ba
2+ionic radius be followed successively by 72pm, 100pm, 118pm, 135pm, La
3+ionic radius be 103.2pm.Except Ca
2+ionic radius and La
3+comparatively close in addition, Mg
2+, Sr
2+and Ba
2+ionic radius all with La
3+differ larger.Therefore, when adopting separately alkaline-earth metal ions doping, there is lattice mismatch and valence state mismatch, cause alkaline-earth metal ions to be difficult to enter lattice, doping content is very limited simultaneously.This doping difficulty very easily causes crystal growth defect, causes crystal growth difficulty.Meanwhile, alkaline-earth metal ions doping easily introduces the lattice imperfections such as atom vacancy, and they will play the part of the role of carrier traps in flashing process, cause the prolongation of fall time, and this is that pole does not wish to see.In addition, independent alkaline-earth metal ions doping does not almost have obvious castering action to the photoyield of crystal.
During independent employing halide-ions doping, halide-ions mainly occupies Br
-position.Although there is larger difference (Cl equally in halide-ions radius
-, Br
-, I
-radius 181pm, 196pm and 220pm successively of ion), but because valence state is identical and character is very similar, in fact the doping of Cl, I ion is substantially unrestricted.Because the doping of a large amount of halide-ions can cause LaBr
3: the considerable change of Ce Crystal Band Structure, therefore the doping of Cl, I ion is to LaBr
3: the photoyield of Ce crystal has remarkably influenced.Under suitable conditions, halide-ions is (as Cl
-, I
-) adulterate and can significantly improve LaBr
3: the photoyield of Ce crystal.But independent halide-ions did not improve significantly to fall time and energy resolution, its deterioration under some condition, also can be caused on the contrary.
From above result, although independent alkaline-earth metal ions or halide-ions doping can bring certain benefit separately, be all difficult to realize LaBr
3: the General Promotion of the Key Performance Indicator such as Ce crystal photoyield, energy resolution, fall time.
Original intention of the present invention is to solve the problem that alkaline earth metal doping concentration is low, be easy to cause lattice defect.Basic ideas are, when alkaline-earth metal ions doping causes lattice dilatation, select the collaborative doping of halide-ions that can cause Lattice Contraction; When alkaline-earth metal ions doping causes Lattice Contraction, select the collaborative doping of halide-ions that can cause lattice dilatation.Such as, when alkaline-earth metal ions used is Mg
2+, Ca
2+time, select the I ion larger than Br ionic radius to mix altogether; When alkaline-earth metal ions used is Sr
2+, Ba
2+time, select the Cl ion less than Br ionic radius to mix altogether; When alkaline-earth metal ions used is Mg
2+, Ca
2+, Sr
2+, Ba
2+in the combination of any two kinds time, according to alkaline-earth metal ions doping, the impact effect of lattice size is selected to kind or its combination of halide-ions Cl, I.This poising action in ionic radius by alkaline-earth metal ions and halide-ions, reduce the lattice mismatch that alkaline-earth metal ions doping causes, reduce doping energy barrier, thus improve the doping content of alkaline-earth metal ions, and reduce the lattice defect caused because of doping.
Experimental result shows, the method serves desired result really, and the doping content of alkaline-earth metal ions has had and significantly improves, and is also easier to grow complete transparent crystal.Scintillation properties test show, after alkaline-earth metal ions and halide-ions are mixed altogether, not only make crystal energy resolution be improved significantly, also significantly increase the photoyield of crystal, be unexpectedly the fall time also effectively shortening crystal simultaneously.To the improvement of attenuation characteristic, its reason may be halide-ions mix in the concentration or the degree of depth that reduce to reduce while lattice mismatch carrier traps altogether, improve the rate of migration of current carrier and the recombination rate of electron-hole pair, thus decrease the slow decay composition of crystal.This illustrates, alkaline-earth metal ions and halide-ions not only have good synergy in doping process, like this too in flashing process.This also can explain further, why from the doping combination that lattice match angle is not so suitable, as Mg
2+with Cl
-combination, or Sr
2+with I
-combination, also effectively can improve the attenuation characteristic of crystal, although the improvement effect of this combination is not as Mg
2+with I
-, Sr
2+with Cl
-combination so obvious.
It should be noted that, halide-ions selected in the present invention is only for Cl
-and I
-, and do not comprise F
-.Although from the angle of lattice match, F
-combine with suitable alkaline-earth metal ions, also can play the effect reducing lattice mismatch, but F
-introducing there is obvious negative effect, namely cause the photoyield of crystal to decline to a great extent, this be be unwilling to see.The appearance of this situation may with F
-cross strong electronegativity relevant.
In the present invention, Ce ion is luminescence center, and its performance of concentration to scintillation material of the present invention has material impact.The preferred Ce ion content of the present invention is 0.01≤a≤0.1, preferably a=0.05.This mainly considers from photoyield, fall time, energy resolution three and obtains.
Although being mixed with altogether of halide-ions helps improve the concentration of alkaline-earth metal ions in crystal, but because the structure of alkaline earth metal halide and rare earth halide exists very big-difference, the doping content of alkaline-earth metal ions remains very limited generally, and its doping b value can not more than 0.002.The alkaline earth metal doping of excessive concentrations easily causes thing phase segregation, can cause serious lattice defect equally.Therefore the preferred alkaline earth ion doping of the present invention is 0.0002≤b≤0.0015.
The doping of halide-ions is compared alkaline-earth metal ions and is varied widely space.Cl, I ion can solid solution continuous in Br ion, and its doping is unrestricted in theory.Although the raising of halogen ion concentration contributes to the doping content improving alkaline-earth metal ions, but too much halide-ions doping can cause the decline of crystal photoyield or the prolongation of fall time equally, the negative effect that this synergistic effect that should mix together is adulterated by independent halide-ions cover relevant.Therefore the preferred halide-ions doping of the present invention is 0.0004≤c≤0.4.
Because the doping of alkaline-earth metal ions and halide-ions all has a greater change space, simultaneously independent alkaline-earth metal ions doping and halide-ions doping are to LaBr
3: the impact of Ce Scintillation Properties is not quite similar, and in fact the present invention also provides a kind of Effective Regulation LaBr
3: the method for Ce Scintillation Properties, namely by regulating the doping content of alkaline-earth metal ions and halide-ions, there is a certain single index improved with stressing in photoyield, fall time and energy resolution, to meet the differentiated demand of different application environment to crystal property.This is for LaBr
3: the application of Ce crystal other field outside TOF-PET is also of great advantage.
Further illustrate beneficial effect of the present invention below in conjunction with specific embodiments.
Comparative example 1
The anhydrous LaBr of 119.89g is accurately taken in the glove box of Ar atmosphere protection
3and the anhydrous CeBr of 6.33g (99.99%)
3(99.99%), mix in the quartz crucible of rear loading diameter 25mm.After being taken out from glove box by quartz crucible, access vacuum system vacuumizes, when vacuum tightness reaches 1 × 10 rapidly
-3scorification sealing during Pa.Crucible is placed in bridgman crystal stove and carries out single crystal growing.High-temperature zone temperature is 850 DEG C, and cold zone temperature is 700 DEG C, gradient zones thermograde about 10 DEG C/cm, and crucible fall off rate is 0.5-2mm/h, total growth time about 15 days.Gained crystal clear, colorless, length is about 5cm.Crystal is cut in glove box the cylindric sample of Φ 25mm × 25mm, carries out the test of photoyield, fall time and energy resolution.
Comparative example 2
The anhydrous LaBr of 119.89g is accurately taken in glove box
3(99.99%), the anhydrous CeBr of 6.33g
3and the anhydrous MgBr of 0.0069g (99.99%)
2(99.99%), mix in rear loading quartz crucible.All the other operations are all identical with comparative example 1.
Comparative example 3
The anhydrous LaBr of 113.58g is accurately taken in glove box
3(99.99%), the anhydrous CeCl of 4.11g
3and the anhydrous LaCl of 5.01g (99.99%)
3(99.99%), mix in rear loading quartz crucible.All the other operations are all identical with comparative example 1.
Embodiment 1
The anhydrous LaBr of 119.89g is accurately taken in glove box
3(99.99%), the anhydrous CeBr of 6.33g
3and the anhydrous MgI of 0.0185g (99.99%)
2(99.99%), mix in rear loading quartz crucible.All the other operations are all identical with comparative example.
Embodiment 2-16 is except proportioning raw materials difference, and all the other operations are all identical with embodiment 1.
Detailed comparisons's situation of all embodiments is in table 1.
Table 1
From embodiment, scintillator performance of the present invention compares LaBr
3: Ce is significantly increased, and particularly have the energy resolution of higher light output, shorter fall time and Geng Gao, this is very useful to the application of this crystal in TOF-PET.The lifting of this over-all properties, is not that alkaline-earth metal ions or halide-ions adulterate separately achieved, and could must be realized by mixing altogether of the two.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. an inorganic scintillation material, is characterized in that, the chemical constitution of described inorganic scintillation material has following general formula: La
1-ace
am
bx
cbr
d, wherein M is one or both in alkaline-earth metal Mg, Ca, Sr, Ba, and X is one in Cl, I or two kinds, 0.01≤a < 1,0.0001≤b≤0.002,0.0001<c≤0.6,2.4<d≤3, and 3+2b=c+d.
2. inorganic scintillation material according to claim 1, is characterized in that, M is one or both in Mg, Ca, and X is I, or I and Cl.
3. inorganic scintillation material according to claim 1, is characterized in that, M is one or both in Sr, Ba, and X is Cl, or Cl and I.
4. inorganic scintillation material according to claim 2, is characterized in that, M is Mg, X is I.
5. inorganic scintillation material according to claim 2, is characterized in that, M is Ca, X is I.
6. inorganic scintillation material according to claim 3, is characterized in that, M is Sr, X is Cl.
7. inorganic scintillation material according to claim 3, is characterized in that, M is Ba, X is Cl.
8. inorganic scintillation material according to any one of claim 1 to 7, is characterized in that, 0.01≤a≤0.1.
9. inorganic scintillation material according to any one of claim 1 to 7, is characterized in that, 0.0002≤b≤0.0015.
10. inorganic scintillation material according to any one of claim 1 to 7, is characterized in that, 0.0004≤c≤0.4.
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| CN106745163B (en) * | 2015-11-24 | 2018-10-19 | 有研稀土新材料股份有限公司 | High-pure anhydrous compound rare-earth halide and preparation method thereof |
| CN110938868B (en) * | 2019-11-01 | 2022-02-22 | 有研稀土新材料股份有限公司 | Rare earth halide scintillating material |
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| US20050178978A1 (en) * | 2004-02-13 | 2005-08-18 | Konica Minolta Medical & Graphic, Inc. | Radiation image conversion panel |
| CN1892251A (en) * | 2005-06-29 | 2007-01-10 | 通用电气公司 | High energy resolution scintillators having high light output |
| CN101701154A (en) * | 2009-11-03 | 2010-05-05 | 上海新漫传感技术研究发展有限公司 | Brominated rare earth scintillating materials and preparation method of Brominated rare earth scintillating crystals |
| US20120305778A1 (en) * | 2011-06-06 | 2012-12-06 | Saint-Gobain Ceramics & Plastics, Inc. | Scintillation crystal including a rare earth halide, and a radiation detection system including the scintillation crystal |
-
2013
- 2013-12-26 CN CN201310733515.8A patent/CN103695002B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101928A (en) * | 1993-08-06 | 1995-04-26 | 三菱金属株式会社 | Infrared light-excited light-emitting substance |
| US20050087698A1 (en) * | 2003-10-23 | 2005-04-28 | Konica Minolta Medical & Graphic, Inc. | Radiation image conversion panel |
| US20050178978A1 (en) * | 2004-02-13 | 2005-08-18 | Konica Minolta Medical & Graphic, Inc. | Radiation image conversion panel |
| CN1892251A (en) * | 2005-06-29 | 2007-01-10 | 通用电气公司 | High energy resolution scintillators having high light output |
| CN101701154A (en) * | 2009-11-03 | 2010-05-05 | 上海新漫传感技术研究发展有限公司 | Brominated rare earth scintillating materials and preparation method of Brominated rare earth scintillating crystals |
| US20120305778A1 (en) * | 2011-06-06 | 2012-12-06 | Saint-Gobain Ceramics & Plastics, Inc. | Scintillation crystal including a rare earth halide, and a radiation detection system including the scintillation crystal |
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Address after: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee after: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee after: Youyan Technology Group Co.,Ltd. Address before: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee before: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee before: GENERAL Research Institute FOR NONFERROUS METALS Address after: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee after: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee after: China Youyan Technology Group Co.,Ltd. Address before: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee before: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee before: Youyan Technology Group Co.,Ltd. |
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