CN103173855B - HEM growing method under a kind of protection of inert gas - Google Patents
HEM growing method under a kind of protection of inert gas Download PDFInfo
- Publication number
- CN103173855B CN103173855B CN201310080414.5A CN201310080414A CN103173855B CN 103173855 B CN103173855 B CN 103173855B CN 201310080414 A CN201310080414 A CN 201310080414A CN 103173855 B CN103173855 B CN 103173855B
- Authority
- CN
- China
- Prior art keywords
- crystal
- hem
- crystal growing
- growing furnace
- mixed gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses the HEM growing method under a kind of protection of inert gas, it comprises following steps: (1), crystal is put into crystal growing furnace; (2), to seal in crystal growing furnace and to carry out vacuum-treat until vacuum tightness reaches 5-10 millitorr in stove; (3) volume ratio, being slowly filled with HE and AR in crystal growing furnace is the HE-AR inert mixed gas impurities removal of 1:1.5-3; (4), adopt well heater to start heating to crystal growing furnace, carry out HEM crystal growth, in-furnace temperature is not less than 2000 DEG C all the time, in crystal growing process, continues to be filled with HE-AR inert mixed gas until crystal growth completes.The invention has the beneficial effects as follows: utilize HE-AR inert mixed gas to achieve HEM crystal growth, the growth result of crystal is good, has evaded the problem of helium supply in the world, has saved production cost simultaneously, decreased procurement risk.
Description
Technical field
The present invention relates to the HEM growing method under a kind of protection of inert gas, belong to crystal production technical field.
Background technology
Sapphire crystal growth has following several mode: crystal pulling method, kyropoulos, HEM, pour mask method etc.Wherein HEM method becomes the main method of large-size sapphire growth in recent years gradually.Be filled with in the precious crystal growth stove of indigo plant He be used as shielding gas and take away crystal growth extremely thermal field get rid of foreign gas; it is a kind of running stores; and due to helium be the natural resource in universe; also be non-renewable scarcity strategic resource simultaneously, in the aerostatics such as the transmitting of satellite airship, missile armament industry, dirigible, low-temperature superconducting research, semiconductor production, Magnetic resonance imaging, specialty metal smelting and gas leak detection etc., there is important purposes.
But the reserve distribution of helium in the whole world is very uneven, and there is the helium resource compared with horn of plenty on the ground such as North America, north African and Russia, and China's helium resource is seriously deficient, only has Sichuan province to store a small amount of helium.For a long time, the industrial production of China and scientific experimentation helium (containing liquid helium) rely on external import substantially, so domestic helium price is relatively high, and delivery cycle in enormous quantities is very long.Simultaneously along with the development of China's national defense industrial technology, the demand of helium is increasing, once there is helium embargo in the eventuality, production cost is comparatively large with minimizing procurement risk, will affect national defense safety and the Economic development of China on a large scale.
Summary of the invention
The object of the present invention is to provide the HEM growing method under a kind of protection of inert gas, can save production cost while realizing HEM crystal growth and reduce procurement risk.
The object of the invention is to be achieved through the following technical solutions: the HEM growing method under a kind of protection of inert gas, it comprises following steps:
(1), crystal is put into crystal growing furnace;
(2), to seal in crystal growing furnace and to carry out vacuum-treat until vacuum tightness reaches 5-10 millitorr in stove;
(3) volume ratio, being slowly filled with HE and AR in crystal growing furnace is the HE-AR inert mixed gas impurities removal of 1:1.5-3;
(4), adopt well heater to start heating to crystal growing furnace, carry out HEM crystal growth, in-furnace temperature is not less than 2000 DEG C all the time, in crystal growing process, continues to be filled with HE-AR inert mixed gas until crystal growth completes.
The chemical fluid processing speed of described HE and AR inert mixed gas is 0.5-1CFH.
Described well heater is graphite heater.
Described crystal growing furnace is molybdenum crucible.
Simultaneously because well heater is graphite heater, crystal growing furnace is molybdenum crucible, except other gases outside rare gas element, all can at high temperature react.
Owing to needing to adopt new rare gas element to do shielding gas, need to study the impact that these two kinds different rare gas elementes are different on sapphire crystal: (1) due to the specific heat capacity of Ar and He different, need to consider that different inert gas flow amount is on the impact of thermal field, determines the flow of Ar according to calculation result; (2) due in the long brilliant stage, sapphire crystal furnace chamber inside needs to keep certain pressure, therefore, also needs to consider the impact due to gas difference on exhaust rate.
In order to solve above two problems, first we need according to thermodynamic principles, calculates He thermal losses, then according to the anti-aeration quantity pushing away Ar of different thermal capacitances.For different gas, need to select different under meters to mate with proportional valve.
The specific heat at constant pressure of helium is 5.1932J/ (g*K), the specific heat at constant pressure of argon gas is 0.5208J/ (g*K), so be converted into mol ratio thermal capacitance to be respectively 20.7884J/ (mol*K) and 20.8J/ (mol*K), from specific heat, the helium filling 1 liter needs to fill the argon gas of 1.0006 liters, is about 1:1.
From above-mentioned calculating, we can determine, can carry out argon gas replace the part of helium as long as under meter and valve to be increased the special model of a set of argon gas.Buying argon gas stream gauge, accesses inflation system by argon gas, can bring into use.
Visible; by HE-AR inert mixed gas; from principle; helium can play good promoter action to crystal structure as micro-molecular gas; and argon gas as macromole gas owing to being heavier than air; as shielding gas, it can drive away other foreign gases in furnace chamber, well can protect the vacuum environment required for crystal growth.
The present invention substitutes the helium of strategic importance by the relatively cheap argon gas of research, partly can evade the problem of helium supply in the world strategically; From cost, the helium price of the pure 5N-50L bottle of a bottle height is at about 1500-2000, as long as and the argon gas about 300 of one bottle of same purity and volume, price be 1/5 less than; From crystal growth, every platform stove can save about 60,000 expenses every year.
Beneficial effect of the present invention is: utilize HE-AR inert mixed gas to achieve HEM crystal growth, and the growth result of crystal is good, and part has evaded the problem of helium supply in the world, has saved production cost simultaneously, has decreased procurement risk.
Embodiment
Technical scheme of the present invention is further described below in conjunction with embodiment, but described in claimed scope is not limited to.
Embodiment 1
A HEM growing method under protection of inert gas, it comprises following steps:
(1), crystal is put into crystal growing furnace;
(2), to seal in crystal growing furnace and to carry out vacuum-treat until vacuum tightness reaches 5 millitorrs in stove;
(3) volume ratio, being slowly filled with HE and AR in crystal growing furnace is the HE-AR inert mixed gas impurities removal of 1:2.5;
(4), adopt well heater to start heating to crystal growing furnace, carry out HEM crystal growth, in-furnace temperature is not less than 2000 DEG C all the time, in crystal growing process, continues to be filled with HE-AR inert mixed gas until crystal growth completes.
The chemical fluid processing speed of described HE and AR inert mixed gas is 0.7CFH.
Described well heater is graphite heater.
Described crystal growing furnace is molybdenum crucible.
Embodiment 2
A HEM growing method under protection of inert gas, it comprises following steps:
(1), crystal is put into crystal growing furnace;
(2), to seal in crystal growing furnace and to carry out vacuum-treat until vacuum tightness reaches 10 millitorrs in stove;
(3) volume ratio, being slowly filled with HE and AR in crystal growing furnace is the HE-AR inert mixed gas impurities removal of 1:1.5;
(4), adopt well heater to start heating to crystal growing furnace, carry out HEM crystal growth, in-furnace temperature is not less than 2000 DEG C all the time, in crystal growing process, continues to be filled with HE-AR inert mixed gas until crystal growth completes.
The chemical fluid processing speed of described HE and AR inert mixed gas is 1CFH.
Embodiment 3
A HEM growing method under protection of inert gas, it comprises following steps:
(1), crystal is put into crystal growing furnace;
(2), to seal in crystal growing furnace and to carry out vacuum-treat until vacuum tightness reaches 5 millitorrs in stove;
(3) volume ratio, being slowly filled with HE and AR in crystal growing furnace is the HE-AR inert mixed gas impurities removal of 1:3;
(4), adopt well heater to start heating to crystal growing furnace, carry out HEM crystal growth, in-furnace temperature is not less than 2000 DEG C all the time, in crystal growing process, continues to be filled with HE-AR inert mixed gas until crystal growth completes.
The chemical fluid processing speed of described HE and AR inert mixed gas is 0.5CFH.
Embodiment 4
A HEM growing method under protection of inert gas, it comprises following steps:
(1), crystal is put into crystal growing furnace;
(2), to seal in crystal growing furnace and to carry out vacuum-treat until vacuum tightness reaches 8 millitorrs in stove;
(3) volume ratio, being slowly filled with HE and AR in crystal growing furnace is the HE-AR inert mixed gas impurities removal of 1:2;
(4), adopt well heater to start heating to crystal growing furnace, carry out HEM crystal growth, in-furnace temperature is not less than 2000 DEG C all the time, in crystal growing process, continues to be filled with HE-AR inert mixed gas until crystal growth completes.
The chemical fluid processing speed of described HE and AR inert mixed gas is 0.8CFH.
Claims (1)
1. the HEM growing method under protection of inert gas, is characterized in that: it comprises following steps:
(1), crystal is put into crystal growing furnace;
(2), to seal in crystal growing furnace and to carry out vacuum-treat until vacuum tightness reaches 5 ~ 10 millitorrs in stove;
(3) volume ratio, being slowly filled with HE and AR in crystal growing furnace is the HE-AR inert mixed gas impurities removal of 1:1.5 ~ 3;
(4), adopt well heater to start heating to crystal growing furnace, carry out HEM crystal growth, in-furnace temperature is not less than 2000 DEG C all the time, in crystal growing process, continues to be filled with HE-AR inert mixed gas until crystal growth completes;
Described well heater is graphite heater;
Described crystal growing furnace is molybdenum crucible;
The chemical fluid processing speed of described HE and AR inert mixed gas is 0.5 ~ 1CFH.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310080414.5A CN103173855B (en) | 2013-03-12 | 2013-03-12 | HEM growing method under a kind of protection of inert gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310080414.5A CN103173855B (en) | 2013-03-12 | 2013-03-12 | HEM growing method under a kind of protection of inert gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103173855A CN103173855A (en) | 2013-06-26 |
| CN103173855B true CN103173855B (en) | 2016-01-06 |
Family
ID=48634025
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310080414.5A Active CN103173855B (en) | 2013-03-12 | 2013-03-12 | HEM growing method under a kind of protection of inert gas |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103173855B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116411338A (en) * | 2023-06-12 | 2023-07-11 | 内蒙古晶环电子材料有限公司 | Material boiling process for producing sapphire single crystal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102625864A (en) * | 2009-09-02 | 2012-08-01 | Gt晶体系统有限责任公司 | High-temperature process improvements using helium under regulated pressure |
-
2013
- 2013-03-12 CN CN201310080414.5A patent/CN103173855B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102625864A (en) * | 2009-09-02 | 2012-08-01 | Gt晶体系统有限责任公司 | High-temperature process improvements using helium under regulated pressure |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103173855A (en) | 2013-06-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20230055938A1 (en) | Process for synthesizing indium phosphide by liquid phosphorus injection method | |
| CN103173855B (en) | HEM growing method under a kind of protection of inert gas | |
| CN108557788A (en) | A kind of black phosphorus method for preparing single crystal of low energy consumption | |
| CN102899714A (en) | Growth process and growth container of phosphorus-silicon-cadmium single crystal | |
| CN206754801U (en) | A kind of special residue processing unit of MO sources steel cylinder | |
| CN102358618B (en) | Gas-liquid exchange type liquid lithium lead alloy bubbler | |
| CN104913798A (en) | Atom dispensing device used for preparing atomic gas chamber and preparation method of atomic gas chamber | |
| Ren et al. | Removal of Cu, Mn and Na in multicrystalline silicon by directional solidification under low vacuum condition | |
| Teng et al. | Numerical investigation of the effect of heat shield shape on the oxygen impurity distribution at the crystal–melt interface during the process of Czochralski silicon crystal growth | |
| CN108622912A (en) | The production method of high temperature covering agent grade boric oxide | |
| CN107419328A (en) | A kind of preparation method of P-type silicon foundry alloy | |
| CN211328764U (en) | Trimethyl indium low temperature purification device | |
| CN102660698A (en) | Vacuum induction melting method for titanium-containing hydrogen storage alloy | |
| CN108328919A (en) | A kind of drawing optical fibers cooling tube helium recovery unit | |
| CN100552416C (en) | The supervising device of fluid sample produced under low temperature and method thereof | |
| CN102928276B (en) | Manufacturing method of inclusion standard sample synthesized by fused silica capillary | |
| CN110172614B (en) | Method for preparing samarium cobalt alloy | |
| CN206709595U (en) | A kind of tantalum anode block malleation sintering equipment of batch (-type) | |
| CN202040536U (en) | High-precision filling system for trace filling of working media | |
| CN103526050B (en) | Production technology for welded pipe level sponge titanium | |
| CN106917026A (en) | A kind of negative thermal expansion material Zn0.5Sn0.5NMn3And preparation method thereof | |
| CN108395448B (en) | Diborane preparation device and preparation method thereof | |
| CN203549376U (en) | Helium charging device | |
| CN102978582A (en) | Production device of pure tungsten capillary tube | |
| Li et al. | Development and application of a structured/unstructured combined mesh scheme for global modeling of a directional solidification process of silicon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |