CN1544711A - Method for growing gadolinium silicate single crystal - Google Patents
Method for growing gadolinium silicate single crystal Download PDFInfo
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- CN1544711A CN1544711A CNA2003101087714A CN200310108771A CN1544711A CN 1544711 A CN1544711 A CN 1544711A CN A2003101087714 A CNA2003101087714 A CN A2003101087714A CN 200310108771 A CN200310108771 A CN 200310108771A CN 1544711 A CN1544711 A CN 1544711A
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- 239000013078 crystal Substances 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910052688 Gadolinium Inorganic materials 0.000 title claims abstract description 13
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 title claims abstract description 13
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000003776 cleavage reaction Methods 0.000 abstract description 10
- 230000007017 scission Effects 0.000 abstract description 10
- 238000005336 cracking Methods 0.000 abstract description 7
- 230000017525 heat dissipation Effects 0.000 abstract 1
- UKOAOXYMPSILTM-UHFFFAOYSA-N gadolinium(3+);trisilicate Chemical compound [Gd+3].[Gd+3].[Gd+3].[Gd+3].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] UKOAOXYMPSILTM-UHFFFAOYSA-N 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009206 nuclear medicine Methods 0.000 description 2
- 230000005658 nuclear physics Effects 0.000 description 2
- 239000003129 oil well Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- -1 rare earth ion Chemical class 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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Abstract
A method for growing gadolinium silicate single crystals is characterized in that the key of the method is that the following procedures are adopted in the ending stage of growing the gadolinium silicate single crystals by a pulling method: and in the later stage of GSO crystal growth, namely after the length of the equal-diameter part of the crystal reaches a preset size, carrying out temperature rise growth of the crystal according to a temperature rise program of 5-50 ℃/h, gradually reducing the diameter of the crystal, growing the crystal at a constant temperature for about 5-30 mm after the tail diameter of the crystal reaches the same size as the seed crystal, then starting to adopt a slow temperature reduction program to reduce the temperature of the GSO crystal to room temperature, and finally taking out the GSO crystal. On one hand, the invention avoids the cracking of the crystal caused by quick pulling or manual pulling when the growth of the single crystal is finished; on the other hand, the shape of the tail part of the crystal is symmetrical and consistent with the shoulder part due to the ending procedure, so that the uniformity of heat dissipation of the crystal is greatly improved, and the probability of cracking and cleavage of the GSO crystal is reduced. Thereby greatly improving the yield of GSO and Ce-GSO crystals.
Description
Technical field
The present invention relates to gadolinium orthosilicate, particularly a kind of Czochralski grown gadolinium siliate (Gd
2SiO
5, hereinafter to be referred as GSO) or rear-earth-doped GSO crystalline method.Specifically, be in the crystal growth later stage, take special tailing-in technique to make the crystalline afterbody consistent, to reduce the probability of crystal cleavage with shoulder shape symmetry.GSO that is grown or Ce:GSO crystal can be widely used in fields such as high energy physics, nuclear physics, nuclear medicine, oil well detection and safety detection.
Background technology
Gadolinium siliate (Gd
2SiO
5, or GSO) be a kind of good luminous host crystalline material, rare earth ion doped GSO single crystal has luminescent properties preferably.For example the adulterated GSO crystal of rare-earth cerium ion (Ce) (Ce:GSO) is exactly a kind of high temperature scintillation crystal of excellent property, and this crystal has high light output (8000Ph/MeV), fast time decay (60ns), big effective atomic number (Z=59) and high-density (ρ=6.71g/cm
3) etc. characteristic, simultaneously the anti-irradiation ability of Ce:GSO crystalline is strong, also is difficult for deliquescence.Therefore, Ce:GSO has a wide range of applications in fields such as high energy physics nuclear physics, image nuclear medicine (PET), oil well explorations.
Gadolinium orthosilicate belongs to congruent melting compound, and fusing point is about 1950 ℃, therefore adopts induction heating iridium crucible Czochralski grown GSO or doping GSO single crystal usually.Because gadolinium orthosilicate belongs to P2
1/ c structure, along (100) face cleavage, and gadolinium siliate has very serious anisotropy (thermal expansion factor b axle is the twice of a and c axle) (referring to 109 (1991) the 386th pages of Journal of Crystal Growth).So, in Czochralski grown GSO crystal process, be easy to occur crystal cleavage, cleavage etc. (referring to the United States Patent (USP) of people such as Kurata application, the patent No. 5,667,583).
Formerly in the technology, when Czochralski grown GSO crystal or adulterated GSO crystal, when the isometrical size of crystal reaches predetermined length dimension, usually adopt fast pull rate or adopt manually to lift crystal and melt are broken away from, so far crystal growth finishes (referring to the United States Patent (USP) of people such as Kurata application, the patent No. 5,690,731; Referring to Proceedings of the Internatial Conference on Inorganic Scintillators andtheir Applications in 1997,295-298 page or leaf).Lifting soon that formerly the technology growth later stage takes makes crystal and melt disengaging have following shortcoming: first, because the temperature higher (about 1950 ℃) at solid-liquid interface place, thermograde big (50-200 ℃/mm), the GSO crystal that breaks away from melt will stand bigger thermal shocking (crystal and melt distance generally are about 2-5mm) in a short period of time, be easy to make GSO crystal cleavage, cracking; Second, the GSO crystalline lower end that breaks away from melt usually is dimpling or smooth interface, this moment, crystal mainly leaned on radiation and thermal convection and melt to carry out heat exchange, crystal is led away heat by crystalline shoulder and seed crystal simultaneously, because ununiformity (the nearly planar interface in bottom of heat conduction, top is taper, as shown in Figure 1), is easy to cause GSO crystalline cracking cleavage.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiency of above-mentioned technology formerly, and a kind of growth method of gadolinium silicate single crystal is provided, to reduce the probability of crystal cleavage cleavage.
Technical solution of the present invention is:
A kind of growth method of gadolinium silicate single crystal, be characterized in crystal pulling method, taking following epilogue: in the GSO crystal growth later stage, be after the length of crystal equal-diameter part reaches predetermined size, carry out the crystalline growth that heats up by heating schedule 5-50 ℃/h slowly, because the crystalline heat absorption is dispelled the heat greater than crystalline, crystal will form and the symmetrical consistent cone shape of shoulder, diameter is tapered, when treating that the crystal tail diameter reaches identical with seed size, after the constant temperature growth 5-30mm length, adopt slowly cooling process that the GSO crystal is reduced to room temperature again, take out the pure or adulterated GSO crystal of being grown at last.
Owing to adopt above-mentioned epilogue in the GSO crystal growth later stage, the shape of crystal afterbody and size are consistent with crystalline shoulder symmetry substantially, have greatly improved crystalline heat radiation homogeneity, have reduced the crystalline cracking.
Adopt the Frequency Induction Heating crystal pulling method, in conjunction with tailing-in technique of the present invention, growth GSO and Ce:GSO crystalline concrete steps are as follows:
(1) the solid-state polycrystal raw material of GSO that will prepare in advance or Ce:GSO is packed in the Ir crucible, and the GSO seed crystal of certain orientation is packed in the seed chuck, in the crystal pulling method monocrystalline burner hearth of simultaneously they being packed in the lump;
(2) in neutral atmosphere or reducing atmosphere, adopt Frequency Induction Heating Ir crucible, the polycrystal raw material in the fusion crucible, and, constant temperature 1-3 hour, make the complete homogenizing of melt in the crucible in the temperature 2000-2150 ℃ of scope that is higher than crystalline melting point 50-100 ℃;
(3) cool the temperature to the crystalline fusing point and sow for 1950 ℃, promptly allow seed crystal contact, after constant temperature 0.5-1 hour, adopt the lifting crystal growth that heats up slowly, the promptly so-called necking down stage with melt;
When (4) diameter dimension for the treatment of growing crystal is less than the seed crystal diameter, adopting slowly, cooling process carries out the crystalline shouldering, when treating that the crystalline diameter dimension reaches predetermined size, beginning constant temperature isodiametric growth, in the above-mentioned crystal growing process, the crystalline speed of growth is about 1-5mm/h, and the crystalline velocity of rotation is about 10-30RPM;
When (5) isometrical crystal length reaches predetermined size, begin to adopt the epilogue of the present invention growth that heats up: carry out the crystalline growth that heats up by heating schedule 5-50 ℃/h slowly, make the consistent cone shape of the basic symmetry of crystal formation and shoulder, diameter is tapered, when treating that the crystal tail diameter reaches identical with seed size, after constant temperature growth 5-30mm is long, begin to adopt slowly cooling process that the GSO crystal is reduced to room temperature.
The present invention compares with technology formerly, its advantage is: the epilogue that adopts above-mentioned precision, lift fast or manually lift when avoiding crystal growth to finish on the one hand and cause crystal to stand excessive thermograde impact, thereby solved the cracking that therefore the GSO crystal causes; On the other hand,, greatly improved the homogeneity of crystal heat radiation, reduced the probability of GSO crystalline cracking and cleavage because epilogue makes the shape of crystal afterbody consistent with the shoulder symmetry.Thereby crystalline yield rates such as GSO and Ce:GSO have greatly been improved.
Description of drawings
Fig. 1: the GSO crystal synoptic diagram that does not adopt the epilogue growth;
Fig. 2: the GSO crystal synoptic diagram that adopts the epilogue growth.
Embodiment
The invention will be further described below by embodiment, but should not limit protection scope of the present invention with this.
Embodiment 1: adopt the present invention's gadolinium siliate GSO single crystal of growing
Press the induction heating Czochralski grown:
Step (1): the GSO polycrystal raw material that will prepare is in advance packed in the Ir gold crucible of φ 80 * 60mm, and the b axle GSO seed crystal that will be of a size of φ 4 * 60mm packs in the seed chuck, and they are packed in the crystal pulling method monocrystalline burner hearth in the lump;
Step (2): at N
2In the atmosphere, adopt the polycrystal raw material in the Frequency Induction Heating Ir crucible melting crucible, and, make the complete homogenizing of melt in the crucible 2000 ℃ of constant temperature 1 hour;
Step (3): cool the temperature to the crystalline fusing point and sow for 1950 ℃, constant temperature is after 0.5 hour, adopts slowly and heat up (50 ℃/h) carry out lifting crystal growth, promptly so-called necking down stage;
Step (4): when the diameter for the treatment of growing crystal is 2mm, begin to adopt slowly that cooling process carries out the crystalline shouldering, when treating that the crystalline diameter dimension reaches φ 35mm, beginning constant temperature isodiametric growth;
Step (5): when isometrical crystal length reaches 60mm, by slowly heating up (50 ℃/h) carry out crystalline to grow, make crystal formation and the symmetrical consistent cone shape of shoulder, diameter is tapered, treat that the crystal tail diameter reaches when being about φ 4mm, after the constant temperature growth 15mm length, begin to adopt slowly cooling process that the GSO crystal is reduced to room temperature.
In the above-mentioned GSO crystal growth, the crystalline speed of growth is about 5mm/h, and the crystalline velocity of rotation is about 30RPM.At last the GSO crystal of Qu Chuing transparent, complete, do not ftracture.
Embodiment 2: with induction heating Czochralski grown Ce:GSO crystal
Step (1): pack into the Ir gold crucible of φ 80 * 60mm of the Ce:GSO polycrystal raw material that will prepare in advance, the b axle GSO seed crystal of φ 4 * 60mm is packed in the seed chuck, and in the crystal pulling method monocrystalline burner hearth of packing into simultaneously;
Step (2): at N
2And 1vol% (volume ratio) H
2Mixed atmosphere in, adopt Frequency Induction Heating Ir crucible, the polycrystal raw material in the fusion crucible, and, make the complete homogenizing of melt in the crucible 2150 ℃ of constant temperature 2 hours;
Step (3) (4): growth Ce:GSO crystal, diameter dimension is about φ 35mm;
Step (5): when electrical path length such as crystal reach 60mm, slowly heat up (5 ℃/h) carry out crystalline to grow, make crystal formation and the symmetrical consistent cone shape of shoulder, diameter is tapered, treat that the crystal tail diameter reaches when being about φ 4mm, after the about 30mm length of constant temperature growth, begin to adopt slowly cooling process that the Ce:GSO crystal is reduced to room temperature.In process of growth, the crystalline speed of growth is about 1mm/h, and the crystalline velocity of rotation is about 10RPM.At last the Ce:GSO crystal of Qu Chuing transparent, complete, do not ftracture.
Embodiment 3: with induction heating Czochralski grown Ce:GSO crystal
Step (1): pack into the Ir gold crucible of φ 80 * 60mm of the Ce:GSO polycrystal raw material that will prepare in advance, the b axle GSO seed crystal of φ 4 * 60mm is packed in the seed chuck, and in the crystal pulling method monocrystalline burner hearth of packing into simultaneously;
Step (2): at N
2In the atmosphere, adopt Frequency Induction Heating Ir crucible, the polycrystal raw material in the fusion crucible, and, make the complete homogenizing of melt in the crucible 2050 ℃ of constant temperature 3 hours;
Step (3) (4): growth Ce:GSO crystal, diameter dimension is about φ 35mm;
Step (5): when electrical path length such as crystal reach 60mm, slowly heat up (20 ℃/h) carry out crystalline to grow, make crystal formation and the symmetrical consistent cone shape of shoulder, diameter is tapered, treat that the crystal tail diameter reaches when being about φ 4mm, after the about 30mm length of constant temperature growth, begin to adopt slowly cooling process that the Ce:GSO crystal is reduced to room temperature.The crystalline speed of growth is about 2mm/h, and the crystalline velocity of rotation is about 20RPM.At last the Ce:GSO crystal of Qu Chuing transparent, complete, do not ftracture.
Claims (2)
1, a kind of growth method of gadolinium silicate single crystal, the key that it is characterized in that this method is to adopt following program in the ending stage of Czochralski grown gadolinium silicate single crystal: in the GSO crystal growth later stage, be after the length of crystal equal-diameter part reaches predetermined size, heating schedule by 5-50 ℃/h carries out crystalline intensification growth, the crystalline diameter is tapered, when treating that the crystal tail diameter reaches identical with seed size, after the about 5-30mm length of constant temperature growth, begin to adopt slowly cooling process that the GSO crystal is reduced to room temperature again, take out the GSO crystal at last.
2, the growth method of gadolinium silicate single crystal according to claim 1 is characterized in that the concrete steps of this method are as follows:
(1) solid-state polycrystal raw material such as GSO that will prepare in advance or Ce: GSO etc. is packed in the iridium crucible, and the GSO seed crystal of certain orientation is packed in the seed chuck, in the monocrystalline burner hearth of the crystal pulling method of simultaneously they being packed in the lump;
(2) in neutral atmosphere or reducing atmosphere, adopt the polycrystal raw material in the Frequency Induction Heating iridium crucible fusion crucible, and the temperature 2000-2150 that is higher than crystalline melting point ℃ constant temperature 1-3 hour, make the complete homogenizing of melt in the crucible;
(3) cool the temperature to the crystalline fusing point and sow for 1950 ℃, after constant temperature 0.5-1 hour, adopting heats up slowly carries out lifting crystal growth, promptly so-called necking down stage;
When (4) diameter dimension for the treatment of growing crystal is less than the seed crystal diameter, beginning to adopt slowly, cooling process carries out the crystalline shouldering, when treating that the crystalline diameter dimension reaches predetermined size, beginning constant temperature isodiametric growth, in the crystal growing process, the crystalline speed of growth is 1-5mm/h, and the crystalline velocity of rotation is 10-30RPM;
When (5) isometrical crystal length reaches predetermined size, begin to adopt the epilogue growth that heats up: by 5-50 ℃/h slowly heating schedule carry out the crystalline growth that heats up, make crystal formation and the symmetrical consistent cone shape of shoulder, when treating that the crystal tail diameter reaches identical with seed size, behind the constant temperature growth 5-30mm, begin to adopt slowly cooling process that the GSO crystal is reduced to room temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365172C (en) * | 2006-04-12 | 2008-01-30 | 中国科学院上海光学精密机械研究所 | Yb-Er-codoped gadolinium silicate laser crystal and preparation method thereof |
| CN101899711A (en) * | 2010-06-25 | 2010-12-01 | 中国科学院上海光学精密机械研究所 | Thulium-doped gadolinium silicate laser crystal and preparation method thereof |
| CN103757702A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院福建物质结构研究所 | Method for preparing high-temperature inorganic scintillation crystal |
| CN104372399A (en) * | 2014-11-28 | 2015-02-25 | 英利能源（中国）有限公司 | Single crystal silicon finishing method and single crystal silicon preparing method |
| CN106676621A (en) * | 2017-02-21 | 2017-05-17 | 宁夏协鑫晶体科技发展有限公司 | Tailing method and preparation method of direct-pulling silicon monocrystals |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0692781A (en) * | 1992-09-16 | 1994-04-05 | Hitachi Chem Co Ltd | Production of single crystal and apparatus therefor |
| JP3892489B2 (en) * | 1994-03-30 | 2007-03-14 | 日立化成工業株式会社 | Processing method of rare earth silicate single crystal |
| US5667583A (en) * | 1994-03-30 | 1997-09-16 | Hitachi Chemical Co. Ltd. | Method of producing a single crystal of a rare-earth silicate |
| US5690731A (en) * | 1994-03-30 | 1997-11-25 | Hitachi Chemical Company Ltd. | Method of growing single crystal |
| JP3904093B2 (en) * | 1994-09-30 | 2007-04-11 | 日立化成工業株式会社 | Single crystal growth method |
| CN1122730C (en) * | 2001-12-26 | 2003-10-01 | 中国科学院上海光学精密机械研究所 | Growth method of quadrivalent chromium-doped magnesium silicate crystal |
-
2003
- 2003-11-21 CN CNB2003101087714A patent/CN1295386C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365172C (en) * | 2006-04-12 | 2008-01-30 | 中国科学院上海光学精密机械研究所 | Yb-Er-codoped gadolinium silicate laser crystal and preparation method thereof |
| CN101899711A (en) * | 2010-06-25 | 2010-12-01 | 中国科学院上海光学精密机械研究所 | Thulium-doped gadolinium silicate laser crystal and preparation method thereof |
| CN103757702A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院福建物质结构研究所 | Method for preparing high-temperature inorganic scintillation crystal |
| CN104372399A (en) * | 2014-11-28 | 2015-02-25 | 英利能源（中国）有限公司 | Single crystal silicon finishing method and single crystal silicon preparing method |
| CN106676621A (en) * | 2017-02-21 | 2017-05-17 | 宁夏协鑫晶体科技发展有限公司 | Tailing method and preparation method of direct-pulling silicon monocrystals |
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