CN202164386U

CN202164386U - Single crystal furnace made of ultra-pure germanium

Info

Publication number: CN202164386U
Application number: CN2011202266143U
Authority: CN
Inventors: 白尔隽
Original assignee: Individual
Current assignee: YUNNAN LINCANG XINYUAN GERMANIUM CO Ltd; Shenzhen University
Priority date: 2011-06-30
Filing date: 2011-06-30
Publication date: 2012-03-14
Anticipated expiration: 2021-06-30

Abstract

The utility model relates to a single crystal furnace for detector-level ultra-high-purity germanium single crystal preparation. The ultra-high-purity germanium single crystal furnace includes a fixing device, a heating device, a cooling device, a ventilation device and a crystal pulling device. The crystal pulling device includes a pulling part and a hot melting part, and the upper part of the pulling part is a seed rod , the lower part of the seed rod is fixed with a quartz rod, and the front end of the quartz rod is fixed with a seed crystal fixture, and the front end of the seed crystal fixture is a germanium seed crystal; the hot-melt part is fixed in the quartz insulation ring, which is fixed to the lower flange through the crucible rod And on the base, a quartz crucible is fixed on the top of the crucible rod, and polycrystalline ingots are contained in the quartz crucible. The reaction equipment of the utility model has a higher cleanliness. The furnace body, crucible and internal parts are all replaced by high-purity quartz materials, and the high-frequency induction heating method is adopted to avoid impurity pollution caused by direct heating of resistance graphite. The possibility of mixing impurities in the process of drawing the product is reduced, and the purity of the product is guaranteed.

Description

Ultra-pure germanium single crystal stove

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

1. an ultra-high-purity germanium single crystal furnace, comprising a fixture, a heating device, a cooling device, a ventilation device and a crystal pulling device, is characterized in that,

The fixing device is an upper flange (16) positioned at the upper and lower ends of the cylindrical heat insulation cover (22), a lower flange and a base (17), and an upper sealing device (14) and a lower sealing device (15), The cavity of the thermal insulation cover (22) is sequentially provided with the heating device, the quartz tube (1), the quartz thermal insulation ring (4) and the crystal pulling device from the outside to the inside;

The heating device comprises an induction coil (7) connected to a medium-high frequency power supply interface (13), and a graphite heater (9) fixed between the induction coil (7) and the quartz tube (1);

The cooling device includes an upper flange water inlet (20) and an upper flange water outlet (21) arranged on the upper flange (16), and cooling water is passed through the lower flange and the base (17) at the same time;

The ventilation device comprises an air inlet (18) and an air outlet located at the top of the heat insulation cover (22)

(19):

The crystal pulling device includes a pulling part installed in the upper sealing device (14) and a hot-melt part fixed on the lower flange and the base (17), and the upper part of the pulling part is a seed rod (11) , the upper part of the seed rod (11) is worn in the upper sealing device (14), the lower part of which is a fixed quartz rod (5), the front end of the quartz rod (5) is fixed with a seed crystal clamp (6), and the seed crystal clamp ( 6) the front end is a germanium seed crystal (24); the hot-melt part is fixed in the quartz insulation ring (4), which is fixed on the lower flange and the base (17) by the crucible rod (12), and the crucible rod (12 ) is fixed on the top of the quartz crucible (2), and the polycrystalline ingot (23) is contained in the described quartz crucible (2).

2. The special equipment for preparing ultra-high-purity germanium single crystal according to claim 1, characterized in that cooling water is passed through the seed rod (11) and the crucible rod (12).

3. The special equipment for preparing ultra-high-purity germanium single crystal according to claim 1, characterized in that, the induction coil bracket (8) is fixed at the lower part of the induction coil (7).

4. The special equipment for preparing ultra-high-purity germanium single crystal according to claim 1, characterized in that, the graphite heater bracket (10) is fixed at the bottom of the graphite heater (9).

5. the special equipment for preparing ultra-high-purity germanium single crystal according to claim 1 is characterized in that, the top of the crucible rod (12) is fixed with a quartz crucible holder (3), and the top of the quartz crucible holder (3) is fixed with a quartz crucible ( 2).