CN204356256U - The solid rectifying purification devices in solid-state MO source - Google Patents
The solid rectifying purification devices in solid-state MO source Download PDFInfo
- Publication number
- CN204356256U CN204356256U CN201520013678.3U CN201520013678U CN204356256U CN 204356256 U CN204356256 U CN 204356256U CN 201520013678 U CN201520013678 U CN 201520013678U CN 204356256 U CN204356256 U CN 204356256U
- Authority
- CN
- China
- Prior art keywords
- solid
- rectifying
- product
- receiving tank
- source
- 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
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model relates to the solid rectifying purification devices in solid-state MO source, rectifying still is placed in rectifying still heating system, rectifying still connects rectifying tower, rectifying tower is connected and installed system cooling and Reflux Control System, front-end volatiles receiving tank receives valve by front-end volatiles and is connected to discharge nozzle, product sublimates receiving tank by product reception valve connection discharge nozzle, and the discharge nozzle the other end is connected to system cooling and Reflux Control System; When rectifying purifying starts; open front-end volatiles and receive valve; close product and receive valve; lower-boiling impurity is collected in front-end volatiles receiving tank; after front-end volatiles receive and terminate; open product and receive valve; close front-end volatiles and receive valve; product vaporization crystallization of sublimating is sublimated in receiving tank at product; front-end volatiles receiving tank and product receiving tank of sublimating passes into nitrogen buffer protection, guarantees to keep anaerobic in system anhydrous, receives to terminate rear closedown product and receive valve; take off product to sublimate receiving tank, realize solid-state MO source rectification and purification.
Description
Technical field
The utility model relates to a kind of solid rectifying purification devices of solid-state MO source, belongs to chemical technology field.
Background technology
The method of modern growth compound semiconductor material has the multiple technologies such as metal organic chemical vapor deposition (MOCVD), molecular beam epitaxy (MBE), chemical beam epitaxy (CBE) and rheotaxy (LPE); special MOCVD technology is the method can carrying out large-scale production compound semiconductor film material the best at present.In MOCVD epitaxy process use the base mateiral of most critical to be the high-purity metal organic compound (be called for short MO source) that purity is greater than 99.9999% (>6N), MO source is also the propping material of CBE epitaxy technology.
High-purity MO source is the key raw material of MOCVD technology, but solid-state MO source is the product of the most difficult purification, adopts traditional solid purifying process as methods such as recrystallization, distillation, zone meltings, is difficult to solid-state MO source purity to be purified to more than 6N.Such as adopt recrystallization to need to add new solvent, need except purification except adding solvent, also need the filtration after carrying out recrystallization, steam the process of solvent, operate very loaded down with trivial details, quality is also unstable; Because the most fusing point of this kind of solid is higher, distillation adopts Decompression Sublimation mostly, and condition is harsher, and very easily introduces new impurity in the process of system recovery normal pressure; Because solid-state MO source is all very sensitive to empty G&W, purify and must carry out under the prerequisite of isolated air, the equipment of zone melting obviously cannot meet the demands.So general solid purifying process is not all suitable for purification and the suitability for industrialized production in solid-state MO source.
Utility model content
The purpose of this utility model is to provide the solid rectifying purification devices in the solid-state MO source of a kind of high-purity metal organic compound gas deposition (MOCVD) technology epitaxy.
The purpose of this utility model is achieved through the following technical solutions:
The solid rectifying purification devices in solid-state MO source, feature is: comprise rectifying still, rectifying tower, system cooling and Reflux Control System, front-end volatiles receiving tank and product are sublimated receiving tank, described rectifying still is placed in rectifying still heating system, rectifying still connects and arranges rectifying tower, rectifying tower is connected and installed system cooling and Reflux Control System, described front-end volatiles receiving tank receives valve by front-end volatiles and is connected to discharge nozzle, described product sublimate receiving tank by product receive valve be connected to discharge nozzle, the other end of discharge nozzle is connected to system cooling for reflux and cut Controlling System.
Further, the solid rectifying purification devices in above-mentioned solid-state MO source, described system cooling and Reflux Control System comprise steam state MO source recirculation cooler and coupled reflux ratio adjustment control.
Further, the solid rectifying purification devices in above-mentioned solid-state MO source, described front-end volatiles receiving tank connects nitrogen buffer protection pipeline.
Further, the solid rectifying purification devices in above-mentioned solid-state MO source, described product receiving tank of sublimating connects nitrogen buffer protection pipeline.
Further, the solid rectifying purification devices in above-mentioned solid-state MO source, described rectifying tower is provided with rectifying tower heated for controlling temperature module.
Substantive distinguishing features and the progress of technical solutions of the utility model are mainly reflected in:
Realize first carrying out rectification and purification to solid-state MO source, obtain highly purified MO source, and production operation facilitates controlled, the quality stability of product is good, the MO source purity finally obtained reaches more than 99.9999%, and adopt reception of sublimating, can control to receive the even shape of solid particulate, meet the requirement of MOCVD epitaxy growth for solid MO source.Can direct packaging, prevent the secondary that may exist in other operating process to stain, preferably resolve purity and the granularity problem in MO source.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, technical solutions of the utility model are described further:
Fig. 1: structural representation of the present utility model.
Embodiment
Research and develop a kind of solid rectification system of solid-state MO source, the MO source purity finally obtained can reach 99.9999%, and can direct packaging use to client, and the secondary avoided in general purification process process stains.
As shown in Figure 1, the solid rectifying purification devices in solid-state MO source, comprise rectifying still 2, rectifying tower 4, system cooling and Reflux Control System 5, front-end volatiles receiving tank 9 and product are sublimated receiving tank 10, rectifying still 2 is placed in rectifying still heating system 1, rectifying still 2 connects and arranges rectifying tower 4, rectifying tower 4 is provided with rectifying tower heated for controlling temperature module 3, rectifying tower 4 is connected and installed system cooling and Reflux Control System 5, system cooling and Reflux Control System 5 comprise steam state MO source recirculation cooler and coupled reflux ratio adjustment control, front-end volatiles receiving tank 9 receives valve 7 by liquefaction pipe 8 and front-end volatiles and is connected to discharge nozzle 6, product receiving tank 10 of sublimating receives valve 12 by vaporizing tube 11 and product and is connected to discharge nozzle 6, the other end of discharge nozzle 6 is connected to system cooling and Reflux Control System 5.Front-end volatiles receiving tank 9 connects nitrogen buffer protection pipeline A, and nitrogen buffer protection pipeline A is connected to nitrogen buffer protection tank, and product receiving tank 10 of sublimating connects nitrogen buffer protection pipeline B, and nitrogen buffer protection pipeline B is connected to nitrogen buffer protection tank.
The solid rectifying purification process in solid-state MO source, thick for solid MO source product is loaded in rectifying still 2, in rectifying still 2, by heating, solid-state MO source is converted into liquid state, control temperature is at 100 ~ 160 DEG C, then, liquid enters rectifying tower 4, the temperature controlling rectifying tower 4 is 50 ~ 160 DEG C, carry out rectifying separation, the MO source of steam state enters system cooling and Reflux Control System 5, in system cooling and Reflux Control System 5, control temperature is 80 ~ 120 DEG C, by steam state MO source recirculation cooler, the MO source of steam state is converted into liquid reflux to get off, again by the adjustment discharging in MO source of reflux ratio adjustment control and the ratio of backflow, thus the impurity in removing MO source, obtain high-purity MO product-derived, when rectifying purifying starts, first open front-end volatiles and receive valve 7, close product and receive valve 12, lower-boiling impurity is made to be collected in front-end volatiles receiving tank 9, the temperature that front-end volatiles receive controls at 0 ~ 20 DEG C, after front-end volatiles receive and terminate, open product and receive valve 12, close front-end volatiles and receive valve 7, vaporize crystallization of sublimating of product is made to sublimate in receiving tank 10 at product, product sublimate receive temperature control at-20 ~ 10 DEG C, front-end volatiles receiving tank 9 and product receiving tank 10 of sublimating passes into nitrogen buffer protection, guarantee in system, to keep anaerobic anhydrous, reception terminates rear closedown product and receives valve 12, take off product to sublimate receiving tank 10.Solid-state MO source is trimethyl indium or two luxuriant magnesium etc.
Embodiment 1
The thick product of a certain amount of solid trimethyl indium is joined in rectifying still 2, thick product is disposable adding, heating trimethyl indium is to 100 ~ 160 DEG C, the temperature controlling rectifying tower 4 is 50 ~ 160 DEG C, the temperature of hierarchy of control cooling and Reflux Control System 5 is 80 ~ 120 DEG C, open front-end volatiles and receive valve 7, close product and receive valve 12, the temperature that front-end volatiles receive controls at 0 ~ 20 DEG C, lower-boiling impurity is made to be collected in front-end volatiles receiving tank, after front-end volatiles receive and terminate, open product and receive valve, close front-end volatiles and receive valve, product sublimate receive temperature control at-20 ~ 10 DEG C, vaporize crystallization of sublimating of product is made to sublimate in receiving tank at product, take off product to sublimate receiving tank, the trimethyl indium purity obtained after testing reaches 99.99998%.
Embodiment 2
The thick product of luxuriant for 10Kg solid two magnesium is joined in rectifying still 2, be heated to 100 ~ 160 DEG C, two luxuriant magnesium first little by little melt, progressively all become liquid, continue to be heated to two luxuriant magnesium boilings, two luxuriant magnesium enter system cooling and Reflux Control System 5, control the heating of rectifying tower 4, two luxuriant magnesium are separated step by step in system cooling and Reflux Control System 5, the two luxuriant magnesium containing impurity such as cyclopentadiene enter into front-end volatiles receiving tank 9, after continuing for some time, pass through Controlling System, make high purity product enter into product to sublimate receiving tank 10, after product receives and terminates, take off product to sublimate receiving tank 10, required ultra-pure MO source is in tank, the purity of two luxuriant magnesium is higher than 99.99998% after testing.Whole rectification system maintains the temperature at 80 ~ 170 DEG C by heating means, make solid MO source liquefy, MO source after rectifying purifying, then is sublimated in receiving tank in crystalline particulate in product through vaporizing and sublimating, and the product that rectifying obtains is sublimated by liquid direct boiling again and changed granular crystals into.
Whole rectification system, by heating means, makes solid MO source liquefy, then through high precision rectification, makes product obtain purifying, and in crystalline particulate.Whole rectification system requires that stopping property is fabulous, in whole rectifying purge process, as long as the temperature set according to each functional area just can make rectifying purifying implement smoothly, the most important thing is to guarantee that MO source is not separated out in pipeline, and the purity in MO source can reach 99.99998%, solve the high purity requirement in MO source very well, also by the temperature condition controlling vaporization and sublimate, the granular size in control MO source, makes the granularity in MO source can meet the requirement of End-Customer.
In sum, the utility model adopts solid rectifying, obtain highly purified MO source, and production operation facilitates controlled, the quality stability of product is good, the MO source purity finally obtained reaches more than 99.9999%, and receive product uniform particles shape, and can direct packaging, prevent the secondary that may exist in other operating process to stain, preferably resolve purity and the granularity problem in MO source, meet the demand of End-Customer.
It is to be understood that: the above is only preferred implementation of the present utility model; for those skilled in the art; under the prerequisite not departing from the utility model principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection domain of the present utility model.
Claims (5)
1. the solid rectifying purification devices in solid-state MO source, it is characterized in that: comprise rectifying still (2), rectifying tower (4), system cooling and Reflux Control System (5), front-end volatiles receiving tank (9) and product are sublimated receiving tank (10), described rectifying still (2) is placed in rectifying still heating system (1), rectifying still (2) upper connection arranges rectifying tower (4), rectifying tower (4) is connected and installed system cooling and Reflux Control System (5), described front-end volatiles receiving tank (9) receives valve (7) by front-end volatiles and is connected to discharge nozzle (6), described product receiving tank (10) of sublimating receives valve (12) by product and is connected to discharge nozzle (6), the other end of discharge nozzle (6) is connected to system cooling for reflux and cut Controlling System (5).
2. the solid rectifying purification devices in solid-state MO source according to claim 1, is characterized in that: described system cooling and Reflux Control System (5) comprise steam state MO source recirculation cooler and coupled reflux ratio adjustment control.
3. the solid rectifying purification devices in solid-state MO source according to claim 1, is characterized in that: described front-end volatiles receiving tank (9) connects nitrogen buffer protection pipeline.
4. the solid rectifying purification devices in solid-state MO source according to claim 1, is characterized in that: described product receiving tank (10) of sublimating connects nitrogen buffer protection pipeline.
5. the solid rectifying purification devices in solid-state MO source according to claim 1, is characterized in that: described rectifying tower (4) is provided with rectifying tower heated for controlling temperature module (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520013678.3U CN204356256U (en) | 2015-01-08 | 2015-01-08 | The solid rectifying purification devices in solid-state MO source |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520013678.3U CN204356256U (en) | 2015-01-08 | 2015-01-08 | The solid rectifying purification devices in solid-state MO source |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204356256U true CN204356256U (en) | 2015-05-27 |
Family
ID=53257737
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520013678.3U Active CN204356256U (en) | 2015-01-08 | 2015-01-08 | The solid rectifying purification devices in solid-state MO source |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204356256U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610326A (en) * | 2015-01-08 | 2015-05-13 | 江苏南大光电材料股份有限公司 | Solid rectification and purification device and method of solid MO source |
| CN109651196A (en) * | 2018-12-27 | 2019-04-19 | 江阴苏利化学股份有限公司 | A kind of technique of the tower rewinding of continuously sublimating of Bravo |
| CN115043884A (en) * | 2022-06-15 | 2022-09-13 | 江苏南大光电材料股份有限公司 | System and method for preparing magnesium chloride |
-
2015
- 2015-01-08 CN CN201520013678.3U patent/CN204356256U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610326A (en) * | 2015-01-08 | 2015-05-13 | 江苏南大光电材料股份有限公司 | Solid rectification and purification device and method of solid MO source |
| CN109651196A (en) * | 2018-12-27 | 2019-04-19 | 江阴苏利化学股份有限公司 | A kind of technique of the tower rewinding of continuously sublimating of Bravo |
| CN109651196B (en) * | 2018-12-27 | 2021-06-29 | 江阴苏利化学股份有限公司 | Process for tower-type continuous desublimation and material collection of chlorothalonil |
| CN115043884A (en) * | 2022-06-15 | 2022-09-13 | 江苏南大光电材料股份有限公司 | System and method for preparing magnesium chloride |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104610326A (en) | Solid rectification and purification device and method of solid MO source | |
| KR102469913B1 (en) | Method for distilling dimethyl sulfoxide, and multi-stage distillation column | |
| CN107501230B (en) | Device and method for preparing electronic grade ethylene carbonate by coupling crystallization and rectification | |
| CN204356256U (en) | The solid rectifying purification devices in solid-state MO source | |
| JP4791680B2 (en) | Method and apparatus for isolating pure or substantially pure organometallic compounds | |
| CN104119256B (en) | A kind of dimethyl sulfoxide (DMSO) method of purification and equipment | |
| WO2016008312A1 (en) | New purification method of organic solid material | |
| CN103466549B (en) | High-purity chlorine gas rectifying technology and equipment thereof | |
| CN114380784A (en) | Method and device for preparing electronic grade propylene carbonate by rectification and melt crystallization coupling | |
| CN103130624B (en) | Method of gradually evaporating/condensing to concentrate formaldehyde | |
| CN106748883B (en) | A method of being thermally integrated three tower variable-pressure rectification separating acetonitriles-Methanol-benzene ternary azeotrope | |
| CN216777931U (en) | Vacuum purification device of methyl pyrrolidone waste liquid | |
| CN101531400B (en) | Method for preparing antimony pentafluoride | |
| CN211999866U (en) | Preparation facilities of high-purity gallium | |
| CN111304468B (en) | Preparation device and production method of high-purity gallium | |
| CN111202999B (en) | Rectification device and method for extracting high-purity mesitylene product from oil generated by isomerization reaction of trimethylbenzene | |
| CN210663575U (en) | Food-grade carbon dioxide preparation system | |
| CN114797145A (en) | Differential pressure thermal coupling rectification process for coal-to-ethylene glycol byproduct | |
| JP5644637B2 (en) | Group III nitride semiconductor crystal manufacturing method | |
| CN107586970A (en) | A kind of method for purifying magnesium | |
| CN216798744U (en) | Intermittent rectification and purification device for dimethyl sulfoxide | |
| WO2010116500A1 (en) | Trichlorosilane cooling tower and trichlorosilane manufacturing method using the same | |
| CN114773228B (en) | Method for refining acetonitrile by rectification-melt crystallization coupling process | |
| JP2008266290A (en) | Method for recovering cyclohexanone oxime | |
| CN114681942B (en) | Complete pressure swing coupling rectification device and rectification method for tertiary butanol recovery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |