CN102443853A - Preparation method of rare earth ion-doped large lead tungstate crystal - Google Patents
Preparation method of rare earth ion-doped large lead tungstate crystal Download PDFInfo
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- CN102443853A CN102443853A CN201110397518XA CN201110397518A CN102443853A CN 102443853 A CN102443853 A CN 102443853A CN 201110397518X A CN201110397518X A CN 201110397518XA CN 201110397518 A CN201110397518 A CN 201110397518A CN 102443853 A CN102443853 A CN 102443853A
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Abstract
The invention discloses a preparation method of a rare earth ion-doped large lead tungstate crystal. By the adoption of a crucible descent method, the preparation method is characterized in that the seed crystal is a round or square lead tungstate crystal with its radial dimension being 10-25mm; the crucible comprises a conical-form seed crystal end and the shoulder angle of the seed crystal end is 30-45 degrees; when the crystal grows, the maximum descent rate during the shoulder phase needs to be controlled within 0.4-0.8mm/h, and the maximum descent rate during the crystal growth phase is 0.8-1.2mm/h. By the adoption of the crucible descent method, the rare earth ion-dope PWO large crystal with its diameter being 50mm can be obtained from the growth of a minor-diameter seed crystal, and the prepared large crystal is not easy to crack during the machining process and can satisfy the application requirement of a luminescent material. In addition, the preparation technology provided by the invention is simple, and the grown crystal can satisfy the machining requirement without complex post-annealing, and the preparation method has industrial application values.
Description
Technical field
The present invention relates to a kind of preparation method of plumbous tungstate large single crystal of doping with rare-earth ions, belong to the crystal technique field.
Background technology
Plumbous tungstate (PbWO
4Be called for short PWO) characteristics such as crystal is not only luminous soon with it, high-density and cost are low and be widely used in fields such as high energy physics, nuclear medicine; And it also has that transparency range is wide, physical and chemical performance stable, thermal conductivity is high and characteristics such as damage threshold height; Make its condition that has possessed novel semi-conductor and light functional matrix material, thereby the luminescence studies of different doped P WO crystalline materials receives extensive concern just gradually.Because rare earth ion segregation coefficient in the PWO crystal is higher; Help being evenly distributed of high-concentration dopant and ionic concn; Mixing of rare earth ion also helps improving PWO crystalline laser damage threshold; Thereby the PWO crystal also is a kind of rare earth ion doped dielectric material that is suitable for, and has remarkable advantages in the laser crystals application facet.With the PWO crystal is matrix, mixes dissimilar rare earth ions (like Er
3+, Nd
3+), the research of can be used for Raman, going up luminescent materials such as changing, infrared.But often stress is bigger for the PWO crystal of high-temperature melting method preparation, and easy to crack in mechanical processing process, crystalline size does not reach request for utilization yet.
Summary of the invention
To the problems referred to above and the defective that prior art exists, the purpose of this invention is to provide a kind of preparation method of plumbous tungstate large single crystal of doping with rare-earth ions, make the large single crystal that makes can satisfy the application requiring of mechanical workout and luminescent material.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is following:
A kind of preparation method of plumbous tungstate large single crystal of doping with rare-earth ions; Be to adopt falling crucible method technology; Comprise that raw material is synthetic, seed crystal preparation and crucible preparation and crystal growth step, it is characterized in that: described raw material synthesizes synthetic the reaching that comprises plumbous tungstate polycrystal ingot rare earth oxide is mixed in the synthetic plumbous tungstate polycrystal ingot; Described seed crystal is that radial dimension is that 10～25mm, length are circular or square plumbous tungstate (PWO) crystal of 40～60mm; Described crucible comprises the seed crystal end, and said seed crystal end is cone-shaped structure, the shouldering angle of seed crystal end, and promptly the semiapex angle of circular cone is 30～45 degree; During crystal growth, needing control growing regional temperature gradient is 20～60 ℃/cm, and the shouldering stage, maximum fall off rate was 0.4～0.8mm/h, and the maximum fall off rate of crystal growth phase is 0.8～1.2mm/h.
As further preferred version, synthesizing of described plumbous tungstate polycrystal ingot is with PbO, WO
3Powder was inserted in the platinum crucible after mixing in 1: 1 in molar ratio, and reheat to 1200～1400 ℃ are incubated 10～20 minutes and make the complete frit reaction of raw material; Then melt is cooled off fast, process PWO polycrystal ingot.
As further preferred version, described rare earth oxide is Nd
2O
3, Er
2O
3, Yb
2O
3In any one or the mixture more than two kinds.
As further preferred version, the doping content scope of described rare earth ion is 0.01～5.0at%.
As further preferred version, described seed crystal is plumbous tungstate (PWO) crystal that is oriented to < 001>direction, but is not limited to this direction.
As further preferred version, described crystal growth comprises following process:
The PWO polycrystal ingot that 1. will be doped with rare earth oxide is inserted in the platinum crucible, puts into seed crystal then and seals crucible;
2. the seed crystal end of the platinum crucible pottery of packing into is drawn down pipe down, fill with aluminum oxide powder in the space therebetween, will draw then down that pipe is placed on the decline platform, through 10～15 hours furnace temperature is risen to 1250～1280 ℃, is incubated 4～6 hours then;
3. promote and draw pipe down, make the raw material fusing in the crucible, after all melting into melt, be incubated 0.5～1.5 hour again;
4. when inoculation temp reaches 1050～1130 ℃, begin to carry out crystal growth;
5. growth ending naturally cools to room temperature, takes out crystal, promptly gets the plumbous tungstate large single crystal of described doping with rare-earth ions.
Compared with prior art; The present invention is through the platinum crucible of specified shape and specific crystal growth condition; Use falling crucible method technology; Realized adopting that (10～25mm) seeded growth obtains the PWO large single crystal that diameter reaches the doping with rare-earth ions of 50mm, and the large single crystal that makes is not easy to crack in mechanical workouts such as cutting, grinding and polishing, the application requiring of luminescent materials such as can satisfying Raman, go up conversion, be infrared than small dia; And preparation technology of the present invention is simple, and the crystal after the growth need not complicated annealing aftertreatment, can satisfy the mechanical workout requirement, has industrial applications and is worth.
Description of drawings
Fig. 1 is the structural representation of the platinum crucible that uses among the present invention, among the figure: 1 expression seed crystal end; α representes the shouldering angle of seed crystal end;
The Nd that Fig. 2 makes for embodiment 1
3+(0.5at%): PWO crystalline fluorogram;
The Er that Fig. 3 makes for embodiment 3
3+(0.5at%): PWO crystalline fluorogram.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further elaboration.
Used crystal growth equipment adopts the structure of the growth apparatus described in the Chinese patent ZL94114075.X among the embodiment.
The building-up process of used PWO polycrystal ingot is following among the embodiment: be 99.99% PbO, WO with purity
31: 1 in molar ratio precise proportioning of powder and mix after, insert in the platinum crucible, in resistance furnace, be heated to 1200～1400 ℃, be incubated 10～20 minutes and make the complete frit reaction of raw material; Melt is cooled off fast, process PWO polycrystal ingot.
The structural representation of used platinum crucible is as shown in Figure 1 among the embodiment, comprises the seed crystal end 1 that is cone-shaped structure.
A) use thickness to process structure shown in Figure 1, be of a size of the crucible of Φ 40 * 200mm, wherein: the shouldering angle α of seed crystal end=30 degree as the platinum of 0.14mm;
B) employing is oriented to < 001 >, and the PWO monocrystalline that is of a size of Φ 20 * 50mm is as seed crystal;
C) with purity be 99.99% Nd
2O
3Mix in the PWO polycrystal ingot Nd
3+Doping is 0.5at%;
D) will be doped with Nd
2O
3PWO polycrystal ingot insert in the platinum crucible; Put into seed crystal then and seal crucible; Adopt descent method to carry out crystal growth: the seed crystal end of the platinum crucible pottery of packing into is down drawn pipe down, and fill with aluminum oxide powder in the space therebetween, and will drawing down then, pipe is placed on the decline platform; Through 12 hours furnace temperature is risen to 1250 ℃, be incubated 6 hours then; Promote gradually again and draw pipe down, the raw material in the crucible is melted gradually, after all melting into melt, be incubated 1 hour again; When inoculation temp reaches 1100 ℃, begin to carry out crystal growth, control growing regional temperature gradient is 40 ℃/cm, and shouldering stage fall off rate is 0.4mm/h, and the crystal growth phase fall off rate is 1.0mm/h; Growth ending is cut off the electricity supply, and naturally cools to room temperature, takes out crystal, promptly gets the 0.5at% rare earth ion Nd that mixes
3+The plumbous tungstate large single crystal.
The Nd that Fig. 2 makes for present embodiment
3+(0.5at%): the PWO crystal is 808nm in excitation wavelength, and the fluorogram when detecting wavelength region 870～1500nm is visible by Fig. 2: prepared Nd
3+(0.5at%): the PWO crystal is at 889nm, 1063nm, and there is glow peak at the 1332nm place.
Embodiment 2
A) use thickness to process structure shown in Figure 1, be of a size of the crucible of Φ 50 * 300mm, wherein: the shouldering angle α of seed crystal end=45 degree as the platinum of 0.14mm;
B) employing is oriented to < 001 >, and the PWO monocrystalline that is of a size of Φ 25 * 60mm is as seed crystal;
C) with purity be 99.99% Nd
2O
3Mix in the PWO polycrystal ingot Nd
3+Doping is 1.0at%;
D) will be doped with Nd
2O
3PWO polycrystal ingot insert in the platinum crucible; Put into seed crystal then and seal crucible; Adopt descent method to carry out crystal growth: the seed crystal end of the platinum crucible pottery of packing into is down drawn pipe down, and fill with aluminum oxide powder in the space therebetween, and will drawing down then, pipe is placed on the decline platform; Through 15 hours furnace temperature is risen to 1280 ℃, be incubated 4 hours then; Promote gradually again and draw pipe down, the raw material in the crucible is melted gradually, after all melting into melt, be incubated 1 hour again; When inoculation temp reaches 1070 ℃, begin to carry out crystal growth, control growing regional temperature gradient is 30 ℃/cm, and shouldering stage fall off rate is 0.6mm/h, and the crystal growth phase fall off rate is 1.2mm/h; Growth ending is cut off the electricity supply, and naturally cools to room temperature, takes out crystal, promptly gets the 1.0at% rare earth ion Nd that mixes
3+The plumbous tungstate large single crystal.
Embodiment 3
A) use thickness to process structure shown in Figure 1, be of a size of the crucible of 40 * 40 * 200mm, wherein: the shouldering angle α of seed crystal end=30 degree as the platinum of 0.14mm;
B) employing is oriented to < 001 >, and the PWO monocrystalline that is of a size of 15 * 15 * 50mm is as seed crystal;
C) with purity be 99.99% Er
2O
3Mix in the PWO polycrystal ingot Er
3+Doping is 0.5at%;
D) will be doped with Er
2O
3PWO polycrystal ingot insert in the platinum crucible; Put into seed crystal then and seal crucible; Adopt descent method to carry out crystal growth: the seed crystal end of the platinum crucible pottery of packing into is down drawn pipe down, and fill with aluminum oxide powder in the space therebetween, and will drawing down then, pipe is placed on the decline platform; Through 12 hours furnace temperature is risen to 1250 ℃, be incubated 6 hours then; Promote gradually again and draw pipe down, the raw material in the crucible is melted gradually, after all melting into melt, be incubated 1 hour again; When inoculation temp reaches 1100 ℃, begin to carry out crystal growth, control growing regional temperature gradient is 45 ℃/cm, and shouldering stage fall off rate is 0.4mm/h, and the crystal growth phase fall off rate is 0.8mm/h; Growth ending is cut off the electricity supply, and naturally cools to room temperature, takes out crystal, promptly gets the 0.5at% rare earth ion Er that mixes
3+The plumbous tungstate large single crystal.
The Er that Fig. 3 makes for present embodiment
3+(0.5at%): the PWO crystal is 980nm in excitation wavelength, and the fluorogram when detecting wavelength region 1400～1700nm is visible by Fig. 3: prepared Er
3+(0.5at%): the PWO crystal has glow peak at the 1533nm place.
Embodiment 4
A) use thickness to process structure shown in Figure 1, be of a size of the crucible of Φ 50 * 400mm, wherein: the shouldering angle α of seed crystal end=45 degree as the platinum of 0.14mm;
B) employing is oriented to < 001 >, and the PWO monocrystalline that is of a size of Φ 20 * 60mm is as seed crystal;
C) with purity be 99.99% Er
2O
3Mix in the PWO polycrystal ingot Er
3+Doping is 1.0at%;
D) will be doped with Er
2O
3PWO polycrystal ingot insert in the platinum crucible; Put into seed crystal then and seal crucible; Adopt descent method to carry out crystal growth: the seed crystal end of the platinum crucible pottery of packing into is down drawn pipe down, and fill with aluminum oxide powder in the space therebetween, and will drawing down then, pipe is placed on the decline platform; Through 13 hours furnace temperature is risen to 1260 ℃, be incubated 5 hours then; Promote gradually again and draw pipe down, the raw material in the crucible is melted gradually, after all melting into melt, be incubated 1 hour again; When inoculation temp reaches 1080 ℃, begin to carry out crystal growth, control growing regional temperature gradient is 25 ℃/cm, and shouldering stage fall off rate is 0.8mm/h, and the crystal growth phase fall off rate is 1.0mm/h; Growth ending is cut off the electricity supply, and naturally cools to room temperature, takes out crystal, promptly gets the 1.0at% rare earth ion Er that mixes
3+The plumbous tungstate large single crystal.
Embodiment 5
A) use thickness to process structure shown in Figure 1, be of a size of the crucible of Φ 50 * 400mm, wherein: the shouldering angle α of seed crystal end=30 degree as the platinum of 0.14mm;
B) employing is oriented to < 001 >, and the PWO monocrystalline that is of a size of Φ 25 * 55mm is as seed crystal;
C) with purity be 99.99% Yb
2O
3And Nd
2O
3Mix in the PWO polycrystal ingot, wherein: Yb
3+Doping is 3.0at%, Nd
3+Doping is 1.0at%;
D) will be doped with Yb
2O
3And Nd
2O
3PWO polycrystal ingot insert in the platinum crucible; Put into seed crystal then and seal crucible; Adopt descent method to carry out crystal growth: the seed crystal end of the platinum crucible pottery of packing into is down drawn pipe down, and fill with aluminum oxide powder in the space therebetween, and will drawing down then, pipe is placed on the decline platform; Through 14 hours furnace temperature is risen to 1270 ℃, be incubated 5 hours then; Promote gradually again and draw pipe down, the raw material in the crucible is melted gradually, after all melting into melt, be incubated 1 hour again; When inoculation temp reaches 1060 ℃, begin to carry out crystal growth, control growing regional temperature gradient is 50 ℃/cm, and shouldering stage fall off rate is 0.6mm/h, and the crystal growth phase fall off rate is 1.0mm/h; Growth ending is cut off the electricity supply, and naturally cools to room temperature, takes out crystal, promptly gets the 4.0at% that mixes by rare earth ion Yb
3+And Nd
3+The plumbous tungstate large single crystal of mixing altogether.
Embodiment 6
A) use thickness to process structure shown in Figure 1, be of a size of the crucible of 45 * 45 * 250mm, wherein: the shouldering angle α of seed crystal end=30 degree as the platinum of 0.14mm;
B) employing is oriented to < 001 >, and the PWO monocrystalline that is of a size of 25 * 25 * 60mm is as seed crystal;
C) with purity be 99.99% Yb
2O
3And Er
2O
3Mix in the PWO polycrystal ingot, wherein: Yb
3+Doping is 3.0at%, Er
3+Doping is 1.0at%;
D) will be doped with Yb
2O
3And Er
2O
3PWO polycrystal ingot insert in the platinum crucible; Put into seed crystal then and seal crucible; Adopt descent method to carry out crystal growth: the seed crystal end of the platinum crucible pottery of packing into is down drawn pipe down, and fill with aluminum oxide powder in the space therebetween, and will drawing down then, pipe is placed on the decline platform; Through 14 hours furnace temperature is risen to 1270 ℃, be incubated 5 hours then; Promote gradually again and draw pipe down, the raw material in the crucible is melted gradually, after all melting into melt, be incubated 1 hour again; When inoculation temp reaches 1060 ℃, begin to carry out crystal growth, control growing regional temperature gradient is 55 ℃/cm, and shouldering stage fall off rate is 0.8mm/h, and the crystal growth phase fall off rate is 1.2mm/h; Growth ending is cut off the electricity supply, and naturally cools to room temperature, takes out crystal, promptly gets the 4.0at% that mixes by rare earth ion Yb
3+And Er
3+The plumbous tungstate large single crystal of mixing altogether.
Visible in sum: the present invention is through the platinum crucible of specified shape and specific crystal growth condition; Use falling crucible method technology; Realized that (10～25mm) seeded growth obtains the PWO large single crystal that diameter reaches the doping with rare-earth ions of 50mm than small dia in employing; And the crystal after the growth need not complicated annealing aftertreatment, can satisfy mechanical workout require and satisfy Raman, go up conversion, the application requiring of luminescent material such as infrared, have industrial applications and be worth.
Be necessary at last to be pointed out that at this: above embodiment only is used for technical scheme of the present invention is done further detailed explanation; Can not be interpreted as the restriction to protection domain of the present invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (6)
1. the preparation method of the plumbous tungstate large single crystal of a doping with rare-earth ions; Be to adopt falling crucible method technology; Comprise that raw material is synthetic, seed crystal preparation and crucible preparation and crystal growth step, it is characterized in that: described raw material synthesizes synthetic the reaching that comprises plumbous tungstate polycrystal ingot rare earth oxide is mixed in the synthetic plumbous tungstate polycrystal ingot; Described seed crystal is that radial dimension is that 10～25mm, length are circular or square plumbous tungstate (PWO) crystal of 40～60mm; Described crucible comprises the seed crystal end, and said seed crystal end is cone-shaped structure, the shouldering angle of seed crystal end, and promptly the semiapex angle of circular cone is 30～45 degree; During crystal growth, needing control growing regional temperature gradient is 20～60 ℃/cm, and the shouldering stage, maximum fall off rate was 0.4～0.8mm/h, and the maximum fall off rate of crystal growth phase is 0.8～1.2mm/h.
2. the preparation method of the plumbous tungstate large single crystal of doping with rare-earth ions according to claim 1 is characterized in that: described plumbous tungstate polycrystal ingot synthetic is with PbO, WO
3Powder was inserted in the platinum crucible after mixing in 1: 1 in molar ratio, and reheat to 1200～1400 ℃ are incubated 10～20 minutes and make the complete frit reaction of raw material; Then melt is cooled off fast, process PWO polycrystal ingot.
3. the preparation method of the plumbous tungstate large single crystal of doping with rare-earth ions according to claim 1, it is characterized in that: described rare earth oxide is Nd
2O
3, Er
2O
3, Yb
2O
3In any one or the mixture more than two kinds.
4. the preparation method of the plumbous tungstate large single crystal of doping with rare-earth ions according to claim 1, it is characterized in that: the doping content of described rare earth ion is 0.01～5.0at%.
5. the preparation method of the plumbous tungstate large single crystal of doping with rare-earth ions according to claim 1, it is characterized in that: described seed crystal is plumbous tungstate (PWO) crystal that is oriented to < 001>direction.
6. the preparation method of the plumbous tungstate large single crystal of doping with rare-earth ions according to claim 1 is characterized in that, described crystal growth comprises following process:
The PWO polycrystal ingot that 1. will be doped with rare earth oxide is inserted in the platinum crucible, puts into seed crystal then and seals crucible;
2. the seed crystal end of the platinum crucible pottery of packing into is drawn down pipe down, fill with aluminum oxide powder in the space therebetween, will draw then down that pipe is placed on the decline platform, through 10～15 hours furnace temperature is risen to 1250～1280 ℃, is incubated 4～6 hours then;
3. promote and draw pipe down, make the raw material fusing in the crucible, after all melting into melt, be incubated 0.5～1.5 hour again;
4. when inoculation temp reaches 1050～1130 ℃, begin to carry out crystal growth;
5. growth ending naturally cools to room temperature, takes out crystal, promptly gets the plumbous tungstate large single crystal of described doping with rare-earth ions.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732946A (en) * | 2012-06-13 | 2012-10-17 | 上海大学 | Preparation method of F and Er ion double-doped green luminescent lead tungstate crystal |
| CN106757306A (en) * | 2016-12-26 | 2017-05-31 | 中国科学院上海硅酸盐研究所 | Crucible and growing method for preparing heavy in section crystal of lead tungstate |
| CN109913941A (en) * | 2019-02-12 | 2019-06-21 | 南京同溧晶体材料研究院有限公司 | A kind of mold and growing method of the heterogeneous rare earth ion doped crystal of high-melting-point arc seeded growth |
| 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 |
| CN114875473A (en) * | 2022-05-30 | 2022-08-09 | 福建福晶科技股份有限公司 | Crystal preparation method for improving KGW crystal quality and utilization rate |
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| CN1313517A (en) * | 2001-04-29 | 2001-09-19 | 中国科学院上海硅酸盐研究所 | Acousto-optic modulator made of lead tungstate crystal modified by rare-earth ions |
| CN101092746A (en) * | 2006-12-27 | 2007-12-26 | 中国科学院上海硅酸盐研究所 | Combined different valence ions doped crystal of lead tungstate with high light yield, and prepartion method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102732946A (en) * | 2012-06-13 | 2012-10-17 | 上海大学 | Preparation method of F and Er ion double-doped green luminescent lead tungstate crystal |
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| CN109913941A (en) * | 2019-02-12 | 2019-06-21 | 南京同溧晶体材料研究院有限公司 | A kind of mold and growing method of the heterogeneous rare earth ion doped crystal of high-melting-point arc seeded growth |
| CN109913941B (en) * | 2019-02-12 | 2024-03-26 | 南京同溧晶体材料研究院有限公司 | Die and growth method for growing rare earth ion doped crystal by heterogeneous high-melting-point arc seed crystal |
| 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 |
| CN114875473A (en) * | 2022-05-30 | 2022-08-09 | 福建福晶科技股份有限公司 | Crystal preparation method for improving KGW crystal quality and utilization rate |
| CN114875473B (en) * | 2022-05-30 | 2023-11-14 | 福建福晶科技股份有限公司 | Crystal preparation method for improving KGW crystal quality and utilization rate |
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|---|---|
| CN102443853B (en) | 2014-11-05 |
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