CN108408261A - The collection device and its method of trimethyl gallium - Google Patents
The collection device and its method of trimethyl gallium Download PDFInfo
- Publication number
- CN108408261A CN108408261A CN201810442455.7A CN201810442455A CN108408261A CN 108408261 A CN108408261 A CN 108408261A CN 201810442455 A CN201810442455 A CN 201810442455A CN 108408261 A CN108408261 A CN 108408261A
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- Prior art keywords
- cold
- trap
- trimethyl gallium
- branch
- storage tank
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
- B65D81/18—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient
- B65D81/20—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas
- B65D81/2007—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas under vacuum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
- B65D81/18—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient
- B65D81/20—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas
- B65D81/2069—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas in a special atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D85/00—Containers, packaging elements or packages, specially adapted for particular articles or materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Abstract
The present invention relates to the collection device of trimethyl gallium and methods, trimethyl gallium container filling, collection storage tank, the first cold-trap and the second cold-trap are sequentially ingressed into main line, trimethyl gallium container filling is connected to the front end of main line by connecting branch, collect storage tank, the first cold-trap and the second cold-trap respectively by forward to branch with go out to branch to connect main line, trimethyl gallium container filling, collection storage tank, the first cold-trap and the second cold-trap respectively connect tail gas pipe-line system, vacuum line system is connected to the rear end of main line, and nitrogen pipeline system connects main line.Remaining trimethyl gallium in trimethyl gallium container filling is passed through in vacuum collecting to collection storage tank and cold-trap, collect a large amount of remaining trimethyl galliums in storage tank collection trimethyl gallium container filling, cold-trap collects a small amount of residual trimethyl gallium in the environment of immersing in liquid nitrogen, and tail gas is discharged by tail gas pipe-line system.By vacuum collecting, trimethyl gallium spontaneous combustion risk is reduced, effect on environment, waste is avoided to recycle.
Description
Technical field
The present invention relates to a kind of collection device of trimethyl gallium and its methods, and in particular to Metalorganic chemical vapor deposition
(MOCVD) in after the use of trimethyl gallium storage container internal surplus recovery processing.
Background technology
Currently, trimethyl gallium is stored in steel cylinder in Metalorganic chemical vapor deposition (MOCVD), steel cylinder after use
Residue is inside had, trimethyl gallium belongs to pyrophoric chemicals, directly discarded to will produce safety problem, and causes damages to environment, leads to
Garbage collection can be recycled by crossing vacuum recycling, while eliminate the influence to environment.
The sources MO have very active chemical property, it is extremely sensitive to air and steam, in air can moment spontaneous combustion, meet
High-explosive then occurs for water.Therefore, the recycling in the sources MO is needed closed and without O2, without H2It is carried out in the environment of O.
Invention content
The purpose of the present invention is overcoming the shortcomings of the prior art, collection device and its side of a kind of trimethyl gallium are provided
Method.
The purpose of the present invention is achieved through the following technical solutions：
The collection device of trimethyl gallium, feature are：Including trimethyl gallium container filling, collection storage tank, the first cold-trap, second
Cold-trap, vacuum line system and nitrogen pipeline system, the trimethyl gallium container filling collect storage tank, the first cold-trap and the
Two cold-traps are sequentially ingressed into main line, and the trimethyl gallium container filling is connected to the front end of main line by connecting branch, described
Collect storage tank, the first cold-trap and the second cold-trap respectively by forward to branch with go out to branch to connect main line, the front three
Base gallium container filling, collection storage tank, the first cold-trap and the second cold-trap respectively connect tail gas pipe-line system, the vacuum line
System is connected to the rear end of main line, and the nitrogen pipeline system connects main line.
Further, the collection device of above-mentioned trimethyl gallium, wherein first cold-trap and the second cold-trap are placed in liquid nitrogen
In Dewar tank.
Further, the collection device of above-mentioned trimethyl gallium, wherein the trimethyl gallium container filling and collection storage tank
Between main line be equipped with valve.
Further, the collection device of above-mentioned trimethyl gallium, wherein it is described collect storage tank forward to branch and going out to branch
Main line between road is equipped with valve.
Further, the collection device of above-mentioned trimethyl gallium, wherein first cold-trap forward to branch and going out to branch
Main line between road is equipped with valve.
Further, the collection device of above-mentioned trimethyl gallium, wherein second cold-trap forward to branch and going out to branch
Main line between road is equipped with valve.
Further, the collection device of above-mentioned trimethyl gallium, wherein the access point of the nitrogen pipeline system, which is located at, to be received
Collection storage tank forward to branch and go out on the main line between branch.
Further, the collection device of above-mentioned trimethyl gallium, wherein the connection branch of trimethyl gallium container filling and
The connecting line of its tail gas pipe-line system is equipped with valve.
Further, the collection device of above-mentioned trimethyl gallium, wherein collect storage tank forward to branch and go out to branch with
And its connecting line of tail gas pipe-line system is equipped with valve.
Further, the collection device of above-mentioned trimethyl gallium, wherein the first cold-trap forward to branch and go out to branch with
And its connecting line of tail gas pipe-line system is equipped with valve.
Further, the collection device of above-mentioned trimethyl gallium, wherein the second cold-trap forward to branch and go out to branch with
And its connecting line of tail gas pipe-line system is equipped with valve.
First cold-trap and the second cold-trap are placed in immersing in liquid nitrogen environment by the collection method of trimethyl gallium of the present invention, it is ensured that
First cold-trap and the second condenser temperature are less than -30 DEG C；To the air in device into line replacement, it is ensured that without air；
It is vacuum-treated by vacuum line system to collecting storage tank, so that collection pressure of storage tank is reached 10~50kPa, make
The trimethyl gallium in trimethyl gallium container filling is collected with the vacuum collected in storage tank, collect pressure of storage tank reach 60~
It is vacuum-treated again after 90kPa, repeatedly after operation repeatedly, it is ensured that a large amount of trimethyl galliums in trimethyl gallium container filling are received
After collection is transferred in collection storage tank, the branch of storage tank is collected in cut-out；It is cold by the first cold-trap of vacuum line system pair and second again
Trap is vacuum-treated, and remaining a small amount of trimethyl gallium is transferred to low temperature by vacuum collecting by the first cold-trap and the second cold-trap
The first cold-trap and the second cold-trap in, the first cold-trap and the second condenser temperature are below -30 DEG C in operating process；
It is by nitrogen pipeline system that trimethyl gallium is filling after pressure reaches 0~15kPa in trimethyl gallium container filling
Container is inflated to 100~130kPa, carries out being evacuated to 0~15kPa again, is so repeated as many times, by the filling appearance of trimethyl gallium
Trimethyl gallium displacement in device is clean；
After trimethyl gallium container filling is inflated to 100~130kPa after displacement is clean, valve is closed, trimethyl gallium is filling
Container is detachable；
It realizes and remaining trimethyl gallium in trimethyl gallium container filling is passed through into vacuum collecting to collection storage tank and first
In cold-trap and the second cold-trap, collect storage tank and collect a large amount of remaining trimethyl galliums in trimethyl gallium container filling, the first cold-trap and
Second cold-trap collects a small amount of residual trimethyl gallium in the environment of immersing in liquid nitrogen, and tail gas is discharged by tail gas pipe-line system.
The present invention has significant advantages and beneficial effects compared with prior art, embodies in the following areas：
Remaining trimethyl gallium in trimethyl gallium container filling is collected by vacuum collecting to collecting in storage tank and cold-trap
Storage tank collects a large amount of remaining trimethyl galliums in trimethyl gallium container filling, and cold-trap is collected a small amount of residual in the environment of immersing in liquid nitrogen
Trimethyl gallium, tail gas is stayed to be discharged by tail gas pipe-line system.By vacuum collecting, trimethyl gallium spontaneous combustion risk can be reduced,
Influence of the waste to environment can be reduced, while waste can be recycled, production cost is saved.Simple operation, safety are collected,
It can be suitably used for the container of various different sizes simultaneously, the container of especially larger specification is effectively shortened working hours, significantly carried
High trimethyl gallium collection efficiency.
Description of the drawings
Fig. 1：The structural schematic diagram of the present invention.
Specific implementation mode
For a clearer understanding of the technical characteristics, objects and effects of the present invention, specific implementation is now described in detail
Scheme.
As shown in Figure 1, the collection device of trimethyl gallium, including trimethyl gallium container filling 101, collection storage tank 102, first
Cold-trap 103, the second cold-trap 104, vacuum line system 106 and nitrogen pipeline system 105, trimethyl gallium container filling 101 are received
Collection storage tank 102, the first cold-trap 103 and the second cold-trap 104 are sequentially ingressed into main line, and trimethyl gallium container filling 101 passes through connection
Branch is connected to the front end of main line, collects storage tank 102, the first cold-trap 103 and the second cold-trap 104 respectively by forward to branch
Road with go out to branch to connect main line, trimethyl gallium container filling 101 collects storage tank 102, the first cold-trap 103 and the second cold-trap
104 respectively connect tail gas pipe-line system, and vacuum line system 106 is connected to the rear end of main line, nitrogen pipeline system 105
Connect main line.
Wherein, trimethyl gallium container filling 101 and the main line collected between storage tank 102 are equipped with valve.
That collects storage tank 102 is equipped with valve forward to branch and the main line gone out between branch.
First cold-trap 103 is equipped with valve forward to branch and the main line gone out between branch.
Second cold-trap 104 is equipped with valve forward to branch and the main line gone out between branch.
The access point of nitrogen pipeline system 105 forward to branch and goes out the main line between branch positioned at collection storage tank
On, the connecting line of nitrogen pipeline system 105 is equipped with valve.
The connection branch of trimethyl gallium container filling 101 and the connecting line of its offgas duct road system are equipped with valve.
Collect storage tank 102 forward to branch and go out and be equipped with valve to branch and the connecting line of its offgas duct road system
Door.
First cold-trap 103 forward to branch and go out and be equipped with valve to branch and the connecting line of its offgas duct road system
Door.
Second cold-trap 104 forward to branch and go out and be equipped with valve to branch and the connecting line of its offgas duct road system
Door.
The air in device is discharged for vacuum line system, tail gas pipe-line system, nitrogen pipeline system, can will make in container
It is collected with remaining trimethyl gallium.
It is vacuum-treated by vacuum line system to collecting storage tank 102, by collecting the vacuum of storage tank 102 by front three
Trimethyl gallium in base gallium container filling 101, which is transferred to, collects storage tank 102, reuses vacuum line system by remaining trimethyl
Gallium is collected into the cold-trap of sub-cooled.
Trimethyl gallium boiling point is 55.8 DEG C under one atmospheric pressure, and in the environment of 101.3~0kPa, boiling point continuously decreases,
Trimethyl gallium is caused constantly to vaporize, its fusing point is -15.8 DEG C under an atmospheric pressure, will under low temperature (- 30~-200 DEG C) environment
Trimethyl gallium is collected into cold-trap, is in the process replaced trimethyl gallium by the displacement of nitrogen system and the transfer of vacuum system dry
Only, clean to replace atmosphere, multiple displacement can be carried out by nitrogen system and vacuum system.
When concrete application, the system after pipeline connection is hunted leak using helium mass spectrometer leak detector, can be carried out after qualified in next step
Operation.
The Dewar tank for assembling cold-trap is added into liquid nitrogen, it is ensured that the first cold-trap 103 and 104 temperature of the second cold-trap are less than -30 DEG C,
To the air in system into line replacement, it is ensured that without air in system.
By being vacuum-treated to collecting storage tank 102, so that 102 pressure of collection storage tank is reached 10~50kPa, reuse receipts
The vacuum collected in storage tank 102 collects the trimethyl gallium in trimethyl gallium container filling 101, collects 102 pressure of storage tank and reaches 60
It is vacuum-treated again after~90kPa, after operating several times repeatedly, it is ensured that a large amount of front threes in trimethyl gallium container filling 101
After base gallium has been transferred in collection storage tank 102, the branch of storage tank is collected in cut-out, will using the first cold-trap 103 and the second cold-trap 104
Remaining a small amount of trimethyl gallium is transferred to by vacuum in the cold-trap of low temperature, and two-stage condenser temperature needs all low in operating process
In -30 DEG C.
After pressure reaches 0~15kPa in trimethyl gallium container filling 101, container is filled by nitrogen pipeline system 105
Gas is carried out being evacuated to 0~15kPa again, be so repeated a further three times, you can by the trimethyl in container to 100~130kPa
Gallium displacement is clean.
After trimethyl gallium container filling 101 is inflated to 100~130kPa after displacement is clean, valve is closed, by trimethyl
Gallium container filling 101 is dismantled from system.
Working continuously for trimethyl gallium collection can be carried out by repeating the above steps.
In conclusion the present invention by remaining trimethyl gallium in trimethyl gallium container filling by vacuum collecting to collect storage
In tank and cold-trap, a large amount of remaining trimethyl galliums in storage tank collection trimethyl gallium container filling are collected, cold-trap is in immersing in liquid nitrogen
A small amount of residual trimethyl gallium is collected in environment, tail gas is discharged by tail gas pipe-line system.By vacuum collecting, three can be reduced
Methyl gallium spontaneous combustion risk, can reduce influence of the waste to environment, while can recycle waste, save production cost.It receives
Collect simple operation, safety, while can be suitably used for the container of various different sizes, the container of especially larger specification effectively contracts
The short working time significantly improves trimethyl gallium collection efficiency.
It should be noted that：The foregoing is merely the preferred embodiment of the present invention, are not limited to the power of the present invention
Sharp range；The description above simultaneously, should can be illustrated and implement for the special personage of correlative technology field, thus it is other without departing from
The equivalent change or modification completed under disclosed spirit, should be included in claim.
Claims (10)
1. the collection device of trimethyl gallium, it is characterised in that：Including trimethyl gallium container filling, collecting storage tank, the first cold-trap, the
Two cold-traps, vacuum line system and nitrogen pipeline system, the trimethyl gallium container filling, collect storage tank, the first cold-trap and
Second cold-trap is sequentially ingressed into main line, and the trimethyl gallium container filling is connected to the front end of main line, institute by connecting branch
State collect storage tank, the first cold-trap and the second cold-trap respectively by forward to branch with go out to branch to connect main line, described three
Methyl gallium container filling, collection storage tank, the first cold-trap and the second cold-trap respectively connect tail gas pipe-line system, the vacuum tube
Road system is connected to the rear end of main line, and the nitrogen pipeline system connects main line.
2. the collection device of trimethyl gallium according to claim 1, it is characterised in that：First cold-trap and the second cold-trap
It is placed in Dewar container for liquefied nitrogen tank.
3. the collection device of trimethyl gallium according to claim 1, it is characterised in that：The trimethyl gallium container filling with
The main line collected between storage tank is equipped with valve.
4. the collection device of trimethyl gallium according to claim 1, it is characterised in that：It is described collect storage tank forward to branch
It is equipped with valve with the main line gone out between branch.
5. the collection device of trimethyl gallium according to claim 1, it is characterised in that：First cold-trap forward to branch
It is equipped with valve with the main line gone out between branch.
6. the collection device of trimethyl gallium according to claim 1, it is characterised in that：Second cold-trap forward to branch
It is equipped with valve with the main line gone out between branch.
7. the collection device of trimethyl gallium according to claim 1, it is characterised in that：The access of the nitrogen pipeline system
Point forward to branch and goes out on the main line between branch positioned at collection storage tank.
8. the collection device of trimethyl gallium according to claim 1, it is characterised in that：The connection of trimethyl gallium container filling
Branch and the connecting line of its offgas duct road system are equipped with valve.
9. the collection device of trimethyl gallium according to claim 1, it is characterised in that：Collect storage tank forward to branch and going out
It is equipped with valve to branch and the connecting line of its offgas duct road system；First cold-trap forward to branch and go out to branch and
The connecting line of its tail gas pipe-line system is equipped with valve；Second cold-trap forward to branch and going out to branch and its offgas duct road
The connecting line of system is equipped with valve.
10. realizing the collection method of trimethyl gallium using claim 1 described device, it is characterised in that：
First cold-trap and the second cold-trap are placed in immersing in liquid nitrogen environment, it is ensured that the first cold-trap and the second condenser temperature are less than -30
℃；To the air in device into line replacement, it is ensured that without air；
It is vacuum-treated by vacuum line system to collecting storage tank, so that collection pressure of storage tank is reached 10~50kPa, use receipts
The vacuum collected in storage tank collects the trimethyl gallium in trimethyl gallium container filling, after collection pressure of storage tank reaches 60~90kPa
It is vacuum-treated again, repeatedly after operation repeatedly, it is ensured that a large amount of trimethyl galliums in trimethyl gallium container filling collect transfer
To after collecting in storage tank, the branch of storage tank is collected in cut-out；It is carried out again by the first cold-trap of vacuum line system pair and the second cold-trap
It is vacuum-treated, remaining a small amount of trimethyl gallium is transferred to the first of low temperature by vacuum collecting by the first cold-trap and the second cold-trap
In cold-trap and the second cold-trap, the first cold-trap and the second condenser temperature are below -30 DEG C in operating process；
After pressure reaches 0~15kPa in trimethyl gallium container filling, by nitrogen pipeline system by trimethyl gallium container filling
It is inflated to 100~130kPa, carries out being evacuated to 0~15kPa again, is so repeated as many times, it will be in trimethyl gallium container filling
Trimethyl gallium displacement it is clean；
After trimethyl gallium container filling is inflated to 100~130kPa after displacement is clean, valve, trimethyl gallium container filling are closed
Detachably；
It realizes and remaining trimethyl gallium in trimethyl gallium container filling is passed through into vacuum collecting to collection storage tank and the first cold-trap
In the second cold-trap, a large amount of remaining trimethyl galliums in storage tank collection trimethyl gallium container filling, the first cold-trap and second are collected
Cold-trap collects a small amount of residual trimethyl gallium in the environment of immersing in liquid nitrogen, and tail gas is discharged by tail gas pipe-line system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810442455.7A CN108408261B (en) | 2018-05-10 | 2018-05-10 | Method for collecting trimethylgallium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810442455.7A CN108408261B (en) | 2018-05-10 | 2018-05-10 | Method for collecting trimethylgallium |
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| Publication Number | Publication Date |
|---|---|
| CN108408261A true CN108408261A (en) | 2018-08-17 |
| CN108408261B CN108408261B (en) | 2023-09-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810442455.7A Active CN108408261B (en) | 2018-05-10 | 2018-05-10 | Method for collecting trimethylgallium |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN108408261B (en) | 2023-09-01 |
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