CN202164386U - Single crystal furnace made of ultra-pure germanium - Google Patents
Single crystal furnace made of ultra-pure germanium Download PDFInfo
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- CN202164386U CN202164386U CN2011202266143U CN201120226614U CN202164386U CN 202164386 U CN202164386 U CN 202164386U CN 2011202266143 U CN2011202266143 U CN 2011202266143U CN 201120226614 U CN201120226614 U CN 201120226614U CN 202164386 U CN202164386 U CN 202164386U
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Abstract
The utility model relates to a detector-level single crystal furnace made of ultra-pure germanium single crystal. The single crystal furnace made of the ultra-pure germanium comprises a fixing device, a heating device, a cooling device, a venting device and a crystal pulling device, wherein the crystal pulling device comprises a pulling part and a hot melting part, the upper part of the pulling part is a seed crystal rod, a quartz rod is fixed at the lower part of the seed crystal rod, a seed crystal fixture is fixed at the front end of the quartz rod, and the front end socket of the seed crystal fixture is germanium seed crystal; the hot melting part is fixed in a quartz heat preservation ring, and is fixed on a lower flange and a base by a crucible rod, a quartz crucible is fixed at the top of the crucible rod, and the quartz crucible internally contains multiple crystal ingots. For the utility model, a reaction device has higher cleanness, the furnace body, the crucible and internal parts all use ultra-pure quartz parts to replace current graphite material, a high-frequency induction heating manner is adopted so that the impurity pollution generated due to direct heating by the electric resistance graphite can be avoided, the impurity mixing possibility in the product pulling process is reduced, and the purity of the product is guaranteed.
Description
Technical field
The utility model relates to the single crystal growing furnace of ultra-pure germanium single crystal preparation of detector grade.
Background technology
Existing military and national defense; Scientific research; The national economy every field all need be used the radiation detector of HpGe gamma-rays, x ray and the detection that energy spectrometer carries out radioprotective thereof, and is best a kind of of the gamma detector intermediate-resolution of all energy resolutions＜0.2% with the gamma detector that the HpGe monocrystalline is done.The germanium single crystal material of this detector grade, its clean impurity concentration must be less than 2 * 10
10Cm
-3Seek out highly purified germanium single crystal like this; Be purified to 5～6 9 purity with common chemical process after, also must carry out in two steps; The first step is to adopt special zone-refine method to obtain detector grade germanium polycrystalline material; Second step was to adopt special pulling monocrystal method, obtained the HpGe monocrystal material of big volume.
The industrial germanium single crystal ingot of semiconductor Germanium so far, the vertical pulling method that it continues to use always, the technology and the technology of also useful VGF method in the preparation of sun power germanium germanium single crystal; And all need mix and do not pursue the further purification of germanium itself; Cause the semiconductor Germanium monocrystalline purity produced,, the highlyest also possibly reach 8-9N generally at 5-6N; Technology in the semiconductor Germanium field of materials and technology also do not reach the purity requirement of 12～13N, and is at present domestic all by import.
The utility model content
The utility model purpose is to provide a kind of ultra-pure germanium single crystal stove that purity reaches 12～13 9 of preparing, for the autonomous innovation of high purity germanium detector in China nuclear radiation detection field provides technical foundation and material foundation.
For realizing this purpose, the technical scheme that the utility model is taked is:
A kind of ultra-pure germanium single crystal stove; Comprise stationary installation, heating unit, refrigerating unit, breather and crystal pulling apparatus; Said stationary installation is to be positioned at the round shape thermal isolating panel upper flange at two ends up and down; Lower flange and base, and upper sealing device and lower sealing device are provided with said heating unit, silica tube, quartzy insulating ring and said crystal pulling apparatus from outside to inside successively in the thermal isolating panel cavity;
Said heating unit comprises the ruhmkorff coil that is connected to the medium-high frequency power interface, and is fixed in the graphite heater between ruhmkorff coil and the silica tube;
Said refrigerating unit comprises upper flange water-in and the upper flange water outlet of being located at upper flange, is connected with water coolant in lower flange and the base simultaneously;
Said breather comprises inlet mouth and the air outlet of being located at thermal isolating panel top;
Said crystal pulling apparatus comprises and is threaded onto lifting part and being fixed in the heat-fused portion on lower flange and the base in the upper sealing device; The said part top that lifts is seed rod; Said seed rod top is threaded onto in the upper sealing device; Its underpart is quartz pushrod fixedly, and the quartz pushrod front end is seed holder fixedly, and said seed holder front end is the germanium seed crystal; Said heat-fused portion is fixed in the quartzy insulating ring, and it is fixed on lower flange and the base through crucible pole, and the crucible pole top is quartz crucible fixedly, splendid attire polycrystalline ingot in the said quartz crucible.
Further, all be connected with water coolant in said seed rod and the crucible pole.
Further, said ruhmkorff coil bottom fixed inductor carriage.
Further, the fixing graphite heater carriage in said graphite heater bottom.
Further, quartzy crucible tray is fixed at said crucible pole top, and quartz crucible jacking portion is quartz crucible fixedly.
The utility model advantage is:
1, the utility model conversion unit degree of cleaning are higher, and body of heater, crucible and internals all use high purity quartz spare to substitute used graphite material, reduced to draw the possibility that mixes impurity in the product process, ensured product gas purity;
2, the utility model places ruhmkorff coil and graphite heater outside the drawing container silica tube, adopts the high-frequency induction heating mode, avoids directly adding with resistance graphite the contaminating impurity of thermogenesis;
3, it is resistant to elevated temperatures like the molybdenum seed rod that the utility model lifts the part employing; Feeding water coolant simultaneously mixes impurity in the monocrystalline that draws out to prevent seed rod under heating condition, reacting; Fixing ultra clean quartz pushrod of seed crystal club head and quartzy anchor clamps are from the purity of a plurality of links guarantee monocrystalline.
4, the utility model adopts resistant to elevated temperatures like the molybdenum crucible bar; Feeding water coolant simultaneously mixes impurity in the monocrystalline that draws out to prevent crucible pole under heating condition, reacting; The crucible club head is fixed ultra clean quartz crucible holder and quartz crucible, ensures the purity of finished product monocrystalline from a plurality of links.
Description of drawings
Fig. 1 is the ultra-pure germanium single crystal stove of the utility model one-piece construction figure.
Fig. 2 is the furnace chamber position partial enlarged drawing of Fig. 1.
Embodiment
The utility model purpose is to provide a kind of and prepares every square centimeter of dislocation less than 5000; Purity reaches ultra-pure germanium single crystal stove of 12-13N; The prepared germanium monocrystal that goes out can be used for making detector and is widely used in military and national defense; Customs's frontier inspection, food hygiene detection, various military and civil areas such as environmental monitoring.
As Fig. 1 and shown in Figure 2 be the ultra-pure germanium single crystal furnace accretion of the utility model composition.This single crystal growing furnace comprises stationary installation, heating unit, refrigerating unit, breather and crystal pulling apparatus five parts.
Said stationary installation is the upper flange 16 that is positioned at round shape thermal isolating panel two ends about in the of 22, and lower flange and base 17, thermal isolating panel are respectively equipped with upper sealing device 14 and lower sealing device 15 in two ends about in the of 22.Be provided with said heating unit, silica tube 1, quartzy insulating ring 4 and said crystal pulling apparatus in thermal isolating panel 22 cavitys from outside to inside successively.
Said heating unit comprises the ruhmkorff coil 7 that is connected to medium-high frequency power interface 13, and is fixed in the graphite heater 9 between ruhmkorff coil 7 and the silica tube 1.Said ruhmkorff coil 7 bottom fixed inductor carriages 8, said graphite heater 9 bottoms fixedly graphite heater carriage 10 are positioned at same height to guarantee well heater and polycrystalline ingot 23, and polycrystalline ingot 23 is effectively heated.
Said refrigerating unit comprises upper flange water-in 20 and the upper flange water outlet 21 of being located at upper flange 16, is connected with water coolant simultaneously in lower flange and the base 17.
Said breather comprises inlet mouth 18 and the air outlet 19 of being located at thermal isolating panel 22 tops; Before the pulling process; In the silica tube 1 of sealing, feed highly purified hydrogen with 19 discharges of the air in the silica tube 1 from inlet mouth 18 from the air outlet; The purity of said hydrogen is greater than 6N, and flow is 0.5-2L/min.Highly purified hydrogen makes and keeps hydrogen environment completely in the silica tube 1; Not only can avoid the reaction of airborne oxygen and polycrystalline ingot and influence the monocrystalline product gas purity; Simultaneously, hydrogen also can be reduced into water with the oxygen element in the polycrystalline ingot and further improve the monocrystalline product gas purity.
Said crystal pulling apparatus comprises and is threaded onto lifting part and being fixed in the heat-fused portion on lower flange and the base 17 in the upper sealing device 14.
The said part top that lifts is seed rod 11, and said seed rod 11 is processed by high temperature material, is preferably to have the highly purified molybdenum seed rod 11 of HMP.Said seed rod 11 tops are threaded onto in the upper sealing device 14, and its underpart is quartz pushrod 5 fixedly, and quartz pushrod 5 front ends are seed holder 6 fixedly, and said seed holder 6 front ends are germanium seed crystals 24.Feed water coolant in the seed rod 11 simultaneously, be used to prevent that seed rod 11 from reacting and impurity is mixed in the monocrystalline that draws out under heating condition.
Said heat-fused portion is fixed in the quartzy insulating ring 4, and it is fixed on lower flange and the base 17 through crucible pole 12, and quartzy crucible tray 3 is fixed at crucible pole 12 tops, and quartz crucible holder 3 tops are quartz crucible 2 fixedly, splendid attire polycrystalline ingot 23 in the said quartz crucible 2.Said crucible pole 12 is processed by high temperature material, is preferably to have the highly purified molybdenum crucible bar of HMP.Be connected with water coolant in the said crucible pole 12, be used to prevent that crucible pole 12 from reacting and impurity is mixed in the monocrystalline that draws out under heating condition.
Above content is the further explain that combines concrete preferred implementation that the utility model is done, and can not assert that the practical implementation of the utility model is confined to these explanations.For the those of ordinary skill of technical field under the utility model, under the prerequisite that does not break away from the utility model design, can also make some simple deduction or replace, all should be regarded as belonging to the protection domain of the utility model.
Claims (5)
1. a ultra-pure germanium single crystal stove comprises stationary installation, heating unit, refrigerating unit, breather and crystal pulling apparatus, it is characterized in that,
Said stationary installation is for being positioned at round shape thermal isolating panel (22) upper flange at two ends (16) up and down; Lower flange and base (17); And upper sealing device (14) and lower sealing device (15), be provided with said heating unit, silica tube (1), quartzy insulating ring (4) and said crystal pulling apparatus in thermal isolating panel (22) cavity from outside to inside successively;
Said heating unit comprises the ruhmkorff coil (7) that is connected to medium-high frequency power interface (13), and is fixed in the graphite heater (9) between ruhmkorff coil (7) and the silica tube (1);
Said refrigerating unit comprises upper flange water-in (20) and the upper flange water outlet (21) of being located at upper flange (16), and lower flange and base are connected with water coolant in (17) simultaneously;
Said breather comprises inlet mouth (18) and the air outlet of being located at thermal isolating panel (22) top
(19)：
Said crystal pulling apparatus comprises and is threaded onto lifting part and being fixed in the heat-fused portion on lower flange and the base (17) in the upper sealing device (14); The said part top that lifts is seed rod (11); Said seed rod (11) top is threaded onto in the upper sealing device (14); Its underpart is quartz pushrod (5) fixedly, and quartz pushrod (5) front end is seed holder (6) fixedly, and said seed holder (6) front end is germanium seed crystal (24); Said heat-fused portion is fixed in the quartzy insulating ring (4), and it is fixed on lower flange and the base (17) through crucible pole (12), and crucible pole (12) top is quartz crucible (2) fixedly, the interior splendid attire polycrystalline ingot of said quartz crucible (2) (23).
2. ultra-pure germanium single crystal according to claim 1 prepares specific equipment, it is characterized in that, all is connected with water coolant in said seed rod (11) and the crucible pole (12).
3. ultra-pure germanium single crystal according to claim 1 prepares specific equipment, it is characterized in that said ruhmkorff coil (7) bottom fixed inductor carriage (8).
4. ultra-pure germanium single crystal according to claim 1 prepares specific equipment, it is characterized in that, said graphite heater (9) bottom is graphite heater carriage (10) fixedly.
5. ultra-pure germanium single crystal according to claim 1 prepares specific equipment, it is characterized in that, quartzy crucible tray (3) is fixed at said crucible pole (12) top, and quartz crucible holder (3) top is quartz crucible (2) fixedly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202266143U CN202164386U (en) | 2011-06-30 | 2011-06-30 | Single crystal furnace made of ultra-pure germanium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202266143U CN202164386U (en) | 2011-06-30 | 2011-06-30 | Single crystal furnace made of ultra-pure germanium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202164386U true CN202164386U (en) | 2012-03-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011202266143U Expired - Lifetime CN202164386U (en) | 2011-06-30 | 2011-06-30 | Single crystal furnace made of ultra-pure germanium |
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| CN (1) | CN202164386U (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206859A (en) * | 2011-06-30 | 2011-10-05 | 白尔隽 | Ultrahigh-purity germanium single crystal preparation process and special equipment |
| CN103422163A (en) * | 2013-09-06 | 2013-12-04 | 上海森松压力容器有限公司 | Device and method for growing sapphire single crystals |
| CN105803530A (en) * | 2015-01-19 | 2016-07-27 | 丰田自动车株式会社 | Single crystal production apparatus |
| CN108342770A (en) * | 2017-01-25 | 2018-07-31 | 上海新昇半导体科技有限公司 | Seedholder and single crystal pulling stove |
| CN112725890A (en) * | 2020-12-25 | 2021-04-30 | 清远先导材料有限公司 | Crystal growth apparatus and crystal growth method |
-
2011
- 2011-06-30 CN CN2011202266143U patent/CN202164386U/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206859A (en) * | 2011-06-30 | 2011-10-05 | 白尔隽 | Ultrahigh-purity germanium single crystal preparation process and special equipment |
| CN102206859B (en) * | 2011-06-30 | 2013-02-13 | 白尔隽 | Ultrahigh-purity germanium single crystal preparation process and special equipment |
| CN103422163A (en) * | 2013-09-06 | 2013-12-04 | 上海森松压力容器有限公司 | Device and method for growing sapphire single crystals |
| CN105803530A (en) * | 2015-01-19 | 2016-07-27 | 丰田自动车株式会社 | Single crystal production apparatus |
| US9982366B2 (en) | 2015-01-19 | 2018-05-29 | Toyota Jidosha Kabushiki Kaisha | Single crystal production apparatus |
| CN108342770A (en) * | 2017-01-25 | 2018-07-31 | 上海新昇半导体科技有限公司 | Seedholder and single crystal pulling stove |
| CN112725890A (en) * | 2020-12-25 | 2021-04-30 | 清远先导材料有限公司 | Crystal growth apparatus and crystal growth method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: SHENZHEN UNIV Effective date: 20131030 Owner name: YUNNAN LINCANG XINYUAN GERMANIUM CO., LTD. Free format text: FORMER OWNER: BAI ERJUN Effective date: 20131030 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Bai Erjuan Inventor after: Zheng Zhipeng Inventor after: Gao Dexi Inventor after: Mi Jiarong Inventor after: Sun Huibin Inventor after: Xie Tianmin Inventor after: Zhao Haige Inventor after: Li Xueyang Inventor before: Bai Erjuan |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: BAI ERJUN TO: BAI ERJUN ZHENG ZHIPENG GAO DEXI MI JIARONG SUN HUIBIN XIE TIANMIN ZHAO HAIGE LI XUEYANG Free format text: CORRECT: ADDRESS; FROM: 518060 SHENZHEN, GUANGDONG PROVINCE TO: 677000 LINCANG, YUNNAN PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20131030 Address after: 677000 Yunnan province Lincang Linxiang District busy River Street office busy River Community magpie nest Group No. 168 Patentee after: Yunnan Lincang Xinyuan Germanium Co., Ltd. Patentee after: Shenzhen University Address before: 518060 Institute of nuclear technology, Shenzhen University, 3688 Nanhai Road, Shenzhen, Guangdong, Nanshan District, China Patentee before: Bai Erjuan |
|
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20120314 |