CN1386899A - In-situ hot-wire chemical gas-phase deposition process for preparing MgB2 superconductor film - Google Patents
In-situ hot-wire chemical gas-phase deposition process for preparing MgB2 superconductor film Download PDFInfo
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- CN1386899A CN1386899A CN 02108906 CN02108906A CN1386899A CN 1386899 A CN1386899 A CN 1386899A CN 02108906 CN02108906 CN 02108906 CN 02108906 A CN02108906 A CN 02108906A CN 1386899 A CN1386899 A CN 1386899A
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Abstract
A superconductor MgB2 film is prepared by in-situ hot-wire chemical gas-phase deposition method, which is characterized by that the gas-state compound containing B and Mg takes part in splitting reaction under the action of hot wire to generate MgB2 compound, which is growing on substrate to become film. Said superconductor film has features of no MgO phase in it and 35K of zero resistance change temp.
Description
The present invention relates to a kind of new superconduction material-MgB
2The film in-situ preparation method.
Japan Akimitsu research group is at celestial platform on January 10 calendar year 2001 " transition group metallic oxide discussion " MgB that gone up reported first
2Have supraconductivity and superconduction critical transition temperature T
cUp to 39K, and on " Nature ", deliver.This is the highest T that has that finds at present
cThe binary simple compounds of value.Caused the scientist's of international coverage concern subsequently, the superconducting characteristic of this compound has been carried out extensive studies.Studies show that this compound has also that bigger coherence length, higher critical current density and critical magnetic field, big carrier density, crystal boundary non-ly weakly are connected, little anisotropy reaches bigger characteristics such as energy gap except that having high superconduction critical transition temperature.Therefore, can be applied at aspects such as height stream, High-Field and electronics.In the application aspect the electronics, require to prepare high-quality film for it, particularly, require the high-quality multilayer film of in-situ preparing preparation knot and multilayered structure device.But, the present MgB that reports
2The preparation of superconducting thin film mainly is an ex situ method of taking to deposit back anneal in the Mg steam.Seldom several study group have reported the in-situ preparing of this film, and they use the method for physical depositions such as pulsed laser deposition, molecular beam epitaxy and sputter, but resulting film T
cValue is all than the T of the film of ex situ method preparation
cBe worth low manyly, and these methods are difficult to solve the problem that contains the MgO dephasign in the film.
The object of the present invention is to provide a kind of MgB
2The hot-wire chemical gas-phase deposition process for preparing of superconducting thin film is owing to adopt the MgB of this method preparation
2Superconducting thin film has suppressed the formation of MgO dephasign in the film, and obtains superconduction performance preferably, therefore can be applicable to knot and multilayered structure electronics device MgB
2The preparation of superconducting thin film.
MgB provided by the present invention
2The superconducting thin film in-situ hot-wire chemical gas-phase deposition process for preparing is characterized in that: the reactant gases borine is generating MgB with the Mg vapor reaction after the cracking under heated filament 9 effects
2Compound is deposited on the substrate 6 of heated filament 9 belows, is grown to serve as superconducting thin film; Or generate MgB on substrate 6 surfaces with the Mg vapor reaction after the borine cracking
2, be grown to serve as superconducting thin film; Or dual mode haves both at the same time; At first, use bell-jar hot-wire chemical gas-phase deposition device, substrate 6 usefulness elargol are bonded on the chip bench 7, keep off with baffle plate 5; The technical pure Mg bar crucible 3 of packing into; Bell-jar vacuum chamber 10 is evacuated down to 10
-1The background pressure of Pa is opened the valve in the gas circuit, and feed 10: (1-2) argon gas of mixed and diluted in hydrogen gas bleed are 5 minutes; 6 to 350-500 ℃ of heated substrate, 9 to 900-1100 ℃ of heating heated filaments, the heating crucible makes the Mg evaporation for 3 to 600-650 ℃, feed the borine reactant gases of 10% volume content of argon-dilution immediately, and with the borine flow rate of reactive gas of 10% volume content of mass flowmeter 1,11 control blended argon gas and diluted in hydrogen gas and argon-dilution, its flow is respectively 300-400sccm and 3-10sccm, and opens baffle plate 5 beginning deposit films, and operating pressure is about 130-160Pa; Sedimentation rate is about 8nm/min, deposits the baffle plate 5 that finishes, and closes the valve of blended argon gas and diluted in hydrogen gas, disconnects heated filament 9 and crucible 3 heating power supplies, and substrate 6 is slowly cooled to room temperature, removes vacuum and takes out substrate 6.
Drawings and Examples
Fig. 1 is a bell-jar hot-wire chemical gas-phase deposition apparatus structure synoptic diagram
Fig. 1 is an embodiment (see figure 1) disclosed by the invention, and in seeing Fig. 1,1,11 is mass flowmeter, and 2 is hybrid bottle, 3 are evaporation Mg earthenware Crucible, and 4 is heating member, and 5 is plate washer, and 6 is substrate, 7 is the heating-type chip bench, and 8 is mechanical pump, and 9 is heated filament, and 10 is vacuum chamber.This invention uses the gaseous compound that contains B and Mg to make reaction gas, makes its cracking under heated filament 4 effects, and reaction generates MgB
2Compound also is grown to serve as film on substrate 6.
In the present invention, because the easily oxidizable of Mg bar, there is MgO in general Mg solid surface, but it has the fusing point far above Mg, is difficult to evaporate and deposit on the substrate, thereby has guaranteed the evaporation of purer Mg, has suppressed MgO and has formed in film.And for the physical method of present report, as pulse laser hydatogenesis and sputtering method, because MgB
2The target sintering process inevitably will form MgO impurity, so the MgO impurity in the target just inevitably with MgB
2Be evaporated simultaneously or sputter out, in film, form dephasign; The MgB that on white stone (001) monocrystal chip, prepares
2Superconducting thin film has the zero resistance transition temperature of 35K, has reached at present the highest level of report in the world.
MgB
2The hot-wire chemical gas-phase deposition process for preparing of superconducting thin film, this method is not appeared in the newspapers so far.Can make purified, as not contain MgO dephasign MgB with this method
2Superconducting thin film will play promoted effect in the application aspect the electronics device to this film.
Equipment used practicality of the present invention, simple, easy to operate, with low cost, the thin film preparation process controllability is strong, is suitable for high quality MgB
2The in-situ preparing of superconducting thin film.
Claims (2)
1. MgB
2The in-situ hot-wire chemical gas-phase deposition process for preparing of superconducting thin film is characterized in that: vacuum chamber (10) is evacuated down to 10
-1The background pressure of Pa feeds 10: (1-2) argon gas of mixed and diluted in hydrogen gas; Heated substrate (6) is to 350-500 ℃; Heating heated filament (9) is to 900-1200 ℃; Heating crucible (3) makes Mg evaporation to 600-650 ℃, feeds the borine reactant gases of 10% volume content of argon-dilution immediately; And with the borine flow rate of reactive gas of 10% volume content of mass flowmeter (1), (11) control blended argon gas and diluted in hydrogen gas and argon-dilution, operating pressure is about 130-160Pa; Borine cracking and Mg vapor reaction generate MgB
2Compound or generate MgB in substrate (6) surface reaction
2Compound also is grown to serve as film on substrate (6).
2. chemical gas-phase deposition process for preparing according to claim 1 is characterized in that: the borine flow rate of reactive gas of 10% volume content of argon gas and diluted in hydrogen gas and argon-dilution is respectively 300-400sccm and 3-10sccm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02108906XA CN1168847C (en) | 2002-03-30 | 2002-03-30 | In-situ hot-wire chemical gas-phase deposition process for preparing MgB2 superconductor film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02108906XA CN1168847C (en) | 2002-03-30 | 2002-03-30 | In-situ hot-wire chemical gas-phase deposition process for preparing MgB2 superconductor film |
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| Publication Number | Publication Date |
|---|---|
| CN1386899A true CN1386899A (en) | 2002-12-25 |
| CN1168847C CN1168847C (en) | 2004-09-29 |
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| CNB02108906XA Expired - Fee Related CN1168847C (en) | 2002-03-30 | 2002-03-30 | In-situ hot-wire chemical gas-phase deposition process for preparing MgB2 superconductor film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1619713B (en) * | 2003-10-22 | 2011-06-15 | 通用电气公司 | method of manufacture superconducting wire |
| CN103168115A (en) * | 2010-10-22 | 2013-06-19 | 应用材料公司 | Methods for enhancing tantalum filament life in hot wire chemical vapor deposition processes |
-
2002
- 2002-03-30 CN CNB02108906XA patent/CN1168847C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1619713B (en) * | 2003-10-22 | 2011-06-15 | 通用电气公司 | method of manufacture superconducting wire |
| CN103168115A (en) * | 2010-10-22 | 2013-06-19 | 应用材料公司 | Methods for enhancing tantalum filament life in hot wire chemical vapor deposition processes |
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| Publication number | Publication date |
|---|---|
| CN1168847C (en) | 2004-09-29 |
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