CN101235486A - Container for packaging solid high-purity metal organic compound and application thereof - Google Patents
Container for packaging solid high-purity metal organic compound and application thereof Download PDFInfo
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- CN101235486A CN101235486A CNA2007101350553A CN200710135055A CN101235486A CN 101235486 A CN101235486 A CN 101235486A CN A2007101350553 A CNA2007101350553 A CN A2007101350553A CN 200710135055 A CN200710135055 A CN 200710135055A CN 101235486 A CN101235486 A CN 101235486A
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Abstract
The invention relates to a container which packages organometallic compounds such as trimethyl indium and the like and comprises a bottle body, an air inlet pipe and an air outlet pipe, wherein a baffle plate is arranged in the bottle body and divides an inner cavity into a left cavity and a right cavity, the volume ratio between the left cavity and the right cavity is 6:4-8:2, the air inlet pipe is inserted in to the bottom of the left cavity, the air outlet pipe is inserted into the bottom of the right cavity, a reticular plate is arranged on the bottom of the right cavity, the bottom of the air inlet pipe is close to the reticular plate, a feed opening is arranged on the upper portion of the bottle body, and the central position of the feed opening is corresponded with the baffle plate. When the packaging container is used in MOCVD, a cavity body contains a solid source, the effective volume of the container can be sufficiently utilized, a path of carrier gas which is passed through the inside of the container is prolonged to more than two times of original length, the contact probability between the gas and the solid source is greatly increased, the gas phase partial pressure of the organometallic compounds in the gas outlet pipe is very stable, the technical requirements for vapor deposition procedures can be well satisfied, the availability ratio of the solid source is more than 90%, and the requirements for using a single bottle can be well satisfied.
Description
Technical field
The present invention relates to the Metalorganic chemical vapor deposition technology, relate in particular to, belong to the photoelectron new material technology field to realizing the stable and packaging container of vapour pressure of chemical vapor deposition processes to the organometallics solid source.
Background technology
Organometallicss such as high-purity trimethyl indium, be the important source material of grow light electronic material in metal organic chemical vapor deposition technology (MOCVD), chemical beam epitaxy (CBE) process, the indium phosphide that is widely used in growing, indium gallium arsenic nitrogen (InGaAsN), indium gallium arsenic (InGaAs), indium gallium phosphorus compound semiconductor film materials such as (InGaP).Purified trimethyl indium at room temperature is a solid, needs are encapsulated in this solid source in the steel cylinder when being used for MOCVD, control the steel cylinder temperature then, make its vapour pressure reach certain value, by continuing the mobile carrier gas, will under use temperature, bring MOCVD or CBE growing system into by the trimethyl indium in the gas-solid equilibrium state gas phase again.
When actual use discovery encapsulated trimethyl indium with common steel cylinder, the utilization ratio of trimethyl indium was lower; Again because trimethyl indium is a solid under environment for use, and the solid grain size can not be very even, cause the degree of tightness at each position of solid trimethyl indium in the conventional bottle of packing into inhomogeneous, be easy to cause so-called " channeling ", this will badly influence the stability of trimethyl indium vapour pressure, the vapour pressure instability that causes compound semiconductor film material process of growth, thereby the quality of the compound semiconductor film material that influence generates.In order to solve this technical barrier, researcher has carried out multiple trial, multinomial technical solution has been proposed, mainly contain: 1, in the packaging container of trimethyl indium, add multi-hole type inertia upholder (K.Sanoyoshi and T.Yago, JP1265511), the solid trimethyl indium is attached in the surface and duct of porous body, reduces the mutual congregation between the trimethyl indium solid as far as possible, increase the effect probability of carrier gas air-flow and trimethyl indium; 2, the encapsulation steel cylinder adopts dual cavity structure (M.L.Timmons, R.J.Colby, R.S.Stennick, EP1160355, JP2002083777), inside and outside two chambers separate with the multi-hole type metal sheet, inner cavity chamber's dress trimethyl indium solid also connects inlet pipe, and outer chamber connects escape pipe.Because the aperture of aperture is very little above the porous metal dividing plate, not only solid source does not arrive outer chamber, and the carrier gas that enters inner cavity chamber has only to have had more fully with solid source and contacts, runs up to after the certain pressure, could enter outer chamber by this metal partion (metp); 3, (G.R.Antell GB2223509), increases carrier gas air-flow and trimethyl indium solid effect chance with two steel cylinder differential concatenations that the trimethyl indium solid source is housed.
Though above-mentioned the 1st, the 2 two kind of method improved the stability of trimethyl indium vapour pressure to a certain extent, improved the rate of utilization of trimethyl indium, but all there is same deficiency, the effective volume that mainly is the encapsulation steel cylinder is seriously reduced, steel cylinder inner member more complicated, manufacturing and installation requirement are very high, and along with processing requirement constantly increases the solid source charge amount, this large vol steel cylinder difficulty aspect apparatus processing of two types is with increasing.Though there is not above problem in the 3rd kind of method, source bottle dismounting trouble, joint is more, increases the probability of gas leakage, and the expense and the trucking costs that encapsulate steel cylinder simultaneously will be multiplied; Two bottles of serial connection technologies were both uneconomical, also can not show a candle to single bottle easy to use.
Summary of the invention
The objective of the invention is: provide a kind of packaging solid metal-organic container, and the concrete application of this packaging container in the metal organic chemical vapor deposition (MOCVD) technology.Be intended to effectively solve for a long time the like product stable inadequately technical barrier of solid source vapour pressure in use, but also make full use of the effective volume of internal tank, improve the rate of utilization of packed solid metal-organic compound, satisfy single bottle of service requirements preferably.
Technical solution of the present invention is: the metal-organic container of a kind of packaging solid, comprise bottle, inlet pipe and escape pipe, and bottle is provided with charging opening, it is characterized in that: be provided with dividing plate in the described bottle, inner chamber is divided into left chamber and right chamber; Described inlet pipe is inserted the bottom in left chamber; Described escape pipe inserts the bottom in right chamber; Charging opening is arranged on the top of bottle, and between inlet pipe and escape pipe.
Further, the above-mentioned metal-organic container of a kind of packaging solid, the central position of described charging opening is relative with dividing plate; The bottom in described left chamber is provided with net slice, and the inlet pipe bottom is near net slice.The volumetric ratio preferable range in chamber, a left side and right chamber is 6: 4～8: 2; The inside of described charging opening is provided with supporting stopper.
Again further, the metal-organic container application of above-mentioned packaging solid is in metal organic chemical vapor deposition process, may further comprise the steps: 1. add solid metal-organic compound in chamber and the right chamber left in proportion, add back emitting and seal charging opening with supporting spiral shell from charging opening; 2. by carrier gas inlet and carrier gas outlet packaging container is inserted in the middle of the employed carrier gas gas circuit of metal organic chemical vapor deposition process; 3. with the temperature regulation of packaging container to design temperature and keep the stability of this temperature, make the vapour pressure of bottle interior solid metal-organic compound stable; 4. open intake valve and air outlet valve, make the steam of solid metal-organic compound flow into gas-phase deposition system, grow the compound semiconductor film material with carrier gas.
Further, the application of the metal-organic container of above-mentioned packaging solid in metal organic chemical vapor deposition process, 3. step adopts to have accurate temperature control and can be modulated to the cold-trap that requires use temperature carries out temperature control; The purity of described solid metal-organic compound is more than or equal to 99.999%, preferred trimethyl indium of this solid metal-organic compound or dicyclopentadienyl magnesium; Described carrier gas is hydrogen, nitrogen, argon gas or helium.
The outstanding substantive distinguishing features and the obvious improvement of technical solution of the present invention is mainly reflected in:
(1) container inner structure of the present invention is fairly simple, makes, installs all more convenient; Use the technology of two common bottom insert canal steel cylinders to compare with serial connection, the present invention has avoided the shortcoming that two steel cylinders need be connected with each other from the outside, has reduced the link of gas leakage, gives to manipulate to bring great convenience;
(2) the present invention has the advantage of the multiple way of prior art concurrently, cavity splendid attire solid source, and the additional proportion of solid source can be regulated as required, and the effective volume of packaging container can be fully used;
(3) when packaging container provided by the invention is used for MOCVD, compare with the common steel cylinder that use is onesize, carrier gas extends to more than the original twice in the distance of internal tank through solid source, gas and solid contact probability have been increased greatly, make that the interior metal-organic gaseous phase partial pressure of gas outlet tube is more stable, not only satisfy the processing requirement of back road vapour deposition operation, also made the overall utilization rate of the interior solid source of bottle bring up to more than 90%;
(4) the present invention uses the technology of two common bottom insert canal steel cylinders to compare with serial connection, has reduced by a steel cylinder, and the use funds reduce greatly.
Description of drawings
Below in conjunction with accompanying drawing technical solution of the present invention is described further:
Fig. 1: the structural representation of a kind of solid MO of the present invention source encapsulation steel cylinder.
The implication of each Reference numeral sees the following form among the figure:
| Reference numeral | Implication | Reference numeral | Implication | Reference numeral | Implication |
| 1 | |
2 | |
3 | |
| 4 | |
5 | |
6 | |
| 7 | |
8 | |
9 | |
| 10 | |
11 | The |
12 | Solid metal-organic compound |
Embodiment
As Fig. 1, the metal-organic container of a kind of packaging solid comprises bottle 1, inlet pipe 5 and escape pipe 9, is provided with dividing plate 2 in the bottle 1, and inner chamber is divided into left chamber and right chamber, and the volumetric ratio in left chamber and right chamber is 6: 4～8: 2, preferred 7: 3; Inlet pipe 5 is inserted the bottom in left chamber; Escape pipe 9 inserts the bottom in right chamber; The bottom in chamber, a left side is provided with net slice 6, and inlet pipe 5 bottoms are near net slice 6; Charging opening 7 is arranged on the top of bottle 1, and between inlet pipe 5 and escape pipe 9, the central position of charging opening 7 is relative with dividing plate 2; The inside of charging opening 7 is provided with supporting stopper 8.
The metal-organic container of above-mentioned packaging solid can play good effect in metal organic chemical vapor deposition process.May further comprise the steps during application:
1. add solid metal-organic compound 12 in chamber and the right chamber left in proportion from charging opening 7, add back emitting and seal charging opening 7 with supporting spiral shell;
2. by carrier gas inlet 3 and carrier gas outlet 11 packaging container is inserted in the middle of the employed carrier gas gas circuit of metal organic chemical vapor deposition process;
3. with the temperature regulation of packaging container to design temperature and keep the stability of this temperature, make the vapour pressure of bottle interior solid metal-organic compound stable;
4. open intake valve 4 and air outlet valve 10, make the steam of solid metal-organic compound flow into gas-phase deposition system, grow the compound semiconductor film material with carrier gas.
During concrete the application, packed solid source can be to be the solid organometallics under the room temperatures such as trimethyl indium, dicyclopentadienyl magnesium, its purity 〉=99.999%, even 〉=99.9999%; Employed carrier gas can be hydrogen, nitrogen, argon gas or helium; Step 3. in, adopt to have accurate temperature control and can be modulated to the cold-trap that requires use temperature and carry out temperature control.
Through the actual detected test, when ambient temperature changed, metal-organic gaseous phase partial pressure was highly stable in the gas outlet tube of packaging container of the present invention, is affected hardly, for whole M OCVD process provides reliable assurance.
In sum, container inner structure of the present invention is fairly simple, makes, installs all more convenient; Use the technology of two common bottom insert canal steel cylinders to compare with serial connection, the present invention has avoided the shortcoming that two steel cylinders need be connected with each other from the outside, has reduced the link of gas leakage, gives to manipulate to bring great convenience; The present invention has the advantage of the multiple way of prior art concurrently, cavity splendid attire solid source, and the additional proportion of solid source can be regulated as required, and the effective volume of packaging container can be fully used; When packaging container provided by the invention is used for MOCVD, compare with the common steel cylinder that use is onesize, carrier gas extends to more than the original twice in the distance of internal tank through solid source, gas and solid contact probability have been increased greatly, make that the interior metal-organic gaseous phase partial pressure of gas outlet tube is more stable, not only satisfy the processing requirement of back road vapour deposition operation, also made the overall utilization rate of the interior solid source of bottle bring up to more than 90%.The present invention uses the technology of two common bottom insert canal steel cylinders to compare with serial connection, has reduced by a steel cylinder, and the use funds reduce greatly, and economic benefit and social effect are remarkable, have the good actual application meaning.
Below only be concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.All employing equivalents or equivalence are replaced and the technical scheme of formation, all drop within the rights protection scope of the present invention.
Claims (10)
1. the container of a packaging solid high-purity metal organic compound comprises bottle [1], inlet pipe [5] and escape pipe [9], and bottle [1] is provided with charging opening [7], it is characterized in that: be provided with dividing plate [2] in the described bottle [1], inner chamber is divided into left chamber and right chamber; Described inlet pipe [5] is inserted the bottom in left chamber; Described escape pipe [9] inserts the bottom in right chamber; Charging opening [7] is arranged on the top of bottle [1], and is positioned between inlet pipe [5] and the escape pipe [9].
2. the container of a kind of packaging solid high-purity metal organic compound according to claim 1, it is characterized in that: the central position of described charging opening [7] is relative with dividing plate [2].
3. the container of a kind of packaging solid high-purity metal organic compound according to claim 1, it is characterized in that: the bottom in described left chamber is provided with net slice [6], and the bottom of inlet pipe [5] is near net slice [6].
4. the container of a kind of packaging solid high-purity metal organic compound according to claim 1, it is characterized in that: the volumetric ratio in described left chamber and right chamber is 6: 4～8: 2.
5. the container of a kind of packaging solid high-purity metal organic compound according to claim 1, it is characterized in that: the inside of described charging opening [7] is provided with supporting stopper [8].
6. the container application of the described a kind of packaging solid high-purity metal organic compound of claim 1 may further comprise the steps in metal organic chemical vapor deposition process:
1. add solid metal-organic compound [12] in chamber and the right chamber left in proportion from charging opening [7], add back emitting and seal charging opening [7] with supporting spiral shell;
2. by carrier gas inlet [3] and carrier gas outlet [11] packaging container is inserted in the middle of the employed carrier gas gas circuit of metal organic chemical vapor deposition process;
3. with the temperature regulation of packaging container to design temperature and keep the stability of this temperature, make the vapour pressure of bottle interior solid metal-organic compound stable;
4. open intake valve [4] and air outlet valve [10], make the steam of solid metal-organic compound flow into gas-phase deposition system, grow the compound semiconductor film material with carrier gas.
7. by the application of container in metal organic chemical vapor deposition process of the described a kind of packaging solid high-purity metal organic compound of claim 6, it is characterized in that: 3. step adopts to have accurate temperature control and can be modulated to the cold-trap that requires use temperature carries out temperature control.
8. by the application of container in metal organic chemical vapor deposition process of claim 6 or 7 described a kind of packaging solid high-purity metal organic compounds, it is characterized in that: the purity of described solid metal-organic compound [12] is more than or equal to 99.999%.
9. by the application of container in metal organic chemical vapor deposition process of the described a kind of packaging solid high-purity metal organic compound of claim 8, it is characterized in that: described solid metal-organic compound is trimethyl indium or dicyclopentadienyl magnesium.
10. by the application of container in metal organic chemical vapor deposition process of claim 6 or 7 described a kind of packaging solid high-purity metal organic compounds, it is characterized in that: described carrier gas is hydrogen, nitrogen, argon gas or helium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101350553A CN101235486A (en) | 2007-11-07 | 2007-11-07 | Container for packaging solid high-purity metal organic compound and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101350553A CN101235486A (en) | 2007-11-07 | 2007-11-07 | Container for packaging solid high-purity metal organic compound and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101235486A true CN101235486A (en) | 2008-08-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101350553A Pending CN101235486A (en) | 2007-11-07 | 2007-11-07 | Container for packaging solid high-purity metal organic compound and application thereof |
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| CN (1) | CN101235486A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101533876B (en) * | 2009-04-14 | 2013-03-20 | 长春理工大学 | Method for passivating amorphous InGaAs thin-film material |
| CN105401133A (en) * | 2014-09-15 | 2016-03-16 | 刘祥林 | Metal organic source feeding apparatus |
| CN108531885A (en) * | 2018-05-31 | 2018-09-14 | 江苏南大光电材料股份有限公司 | The solid metal-organic compound tandem temperature difference uses system and its application |
| CN111172513A (en) * | 2020-03-09 | 2020-05-19 | 江苏南大光电材料股份有限公司 | Container for packaging solid high-purity metal organic compound and application thereof |
| CN111304742A (en) * | 2020-02-28 | 2020-06-19 | 木昇半导体科技(苏州)有限公司 | MO source bottle serial source supply device for MOCVD |
| CN114059038A (en) * | 2020-08-07 | 2022-02-18 | 吕宝源 | Method and system for transferring solid metal organic compound |
| CN115819791A (en) * | 2022-12-16 | 2023-03-21 | 烟台大学 | Method for regulating MOF morphology by controlling protective gas pressure |
-
2007
- 2007-11-07 CN CNA2007101350553A patent/CN101235486A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101533876B (en) * | 2009-04-14 | 2013-03-20 | 长春理工大学 | Method for passivating amorphous InGaAs thin-film material |
| CN105401133A (en) * | 2014-09-15 | 2016-03-16 | 刘祥林 | Metal organic source feeding apparatus |
| CN105401133B (en) * | 2014-09-15 | 2018-03-13 | 刘祥林 | A kind of metal organic source feeding device |
| CN108531885A (en) * | 2018-05-31 | 2018-09-14 | 江苏南大光电材料股份有限公司 | The solid metal-organic compound tandem temperature difference uses system and its application |
| CN111304742A (en) * | 2020-02-28 | 2020-06-19 | 木昇半导体科技(苏州)有限公司 | MO source bottle serial source supply device for MOCVD |
| CN111172513A (en) * | 2020-03-09 | 2020-05-19 | 江苏南大光电材料股份有限公司 | Container for packaging solid high-purity metal organic compound and application thereof |
| CN114059038A (en) * | 2020-08-07 | 2022-02-18 | 吕宝源 | Method and system for transferring solid metal organic compound |
| CN114059038B (en) * | 2020-08-07 | 2024-02-09 | 吕宝源 | Solid metal organic compound transformation method and transformation system thereof |
| CN115819791A (en) * | 2022-12-16 | 2023-03-21 | 烟台大学 | Method for regulating MOF morphology by controlling protective gas pressure |
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Open date: 20080806 |