CN104928630A - Method for preparing FeSeTe film by pulse laser deposition coating technology - Google Patents
Method for preparing FeSeTe film by pulse laser deposition coating technology Download PDFInfo
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- CN104928630A CN104928630A CN201510262382.XA CN201510262382A CN104928630A CN 104928630 A CN104928630 A CN 104928630A CN 201510262382 A CN201510262382 A CN 201510262382A CN 104928630 A CN104928630 A CN 104928630A
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Abstract
The invention belongs to the field of novel Fe-based superconductors and particularly relates to a method for preparing a FeSeTe film by a pulse laser deposition coating technology. The method comprises the following steps: firstly, uniformly mixing and grinding Fe powder, Se powder and Te powder at a certain molar ratio; secondly, sintering the ground powder in a vacuum quartz tube at 700DEG C for 24 hours, performing quenching treatment when the sintered powder is at 400DEG C, grinding the sintered powder into powder again, pressing the powder in the size of a required target material, sintering the powder in the vacuum quartz tube at 700DEG C for 24 hours, and performing quenching treatment when the powder is at 400DEG C; adjusting laser parameters, performing pretreatment of the obtained target material, and performing film growth on a substrate within a certain time; and performing natural cooling in vacuum to obtain the required film. According to the method, the FeSeTe superconductive film is grown by utilizing the pulse laser deposition coating technology. The method has the advantages that the use is convenient, the coating speed is high, films of different components can be prepared, and the target material and the substrate are kept consistent in component more easily.
Description
Technical field
The invention belongs to new iron-based superconductor field, be specifically related to utilize pulsed laser deposition coating technique to prepare the technology of new iron-based superconductor iron selen-tellurjum high-temperature superconducting thin film.
Background technology
Earlier 1900s, superconducting phenomenon is surprisingly found in laboratory by Dutch physicist H Ka Molinangneisi, and people begin one's study various different types of superconductor subsequently, are devoted to improve constantly superconducting temperature, can be applied in human lives.The characteristic such as zero resistance nature, perfect diamganetism of superconductor is that very large contribution has been made in the development of the cause such as electric power, traffic.Before this, people concentrate on copper oxide aspect more to the research of high-temperature superconductor, along with going deep into of inquiring into, the research of this type I superconductors I runs into bottleneck, be difficult to breakthrough of reentrying, people just start the new iron-based superconductor finding other, and iron selen-tellurjum is exactly wherein a kind of.This high-temperature superconductor obtained by doping iron selenium causes the extensive concern of various countries' researcher.
The method preparing iron selen-tellurjum film at present has the methods such as magnetron sputtering, but uses magnetron sputtering method growth iron selen-tellurjum film, because the air pressure of growth chamber is higher, easily introduces impurity, unfavorable to the growth of film.Pulsed laser deposition coating technique is focused at target material surface by high energy laser beam, produces plasma body, is finally deposited on a kind of coating technique sinking to the bottom surface.Pulsed laser deposition plated film has lot of advantages, such as, more easily make target consistent with sixbstrate components, and coating speed is fast, and the film wide variety etc. that can prepare is one of major way of film growth.
Summary of the invention
The object of the present invention is to provide a kind of method preparing iron selen-tellurjum high-temperature superconducting thin film, the method uses pulsed laser deposition technique, can optimize the crystalline structure of iron selen-tellurjum, to obtain the superconductivity being better than iron selen-tellurjum bulk.
The technical solution used in the present invention is:
Utilize pulsed laser deposition coating technique to prepare a method for iron selen-tellurjum film, concrete preparation process is as follows:
A) by Fe, Se and Te powder by the grinding of certain mixed in molar ratio evenly;
B) the 700 DEG C of sintering in vitreosil pipe of the powder after grinding, after 24 hours, are carried out quench treatment when being cooled to 400 DEG C;
C) by step b) iron selen-tellurjum after sintering pulverizes again, then is pressed into the size of required target;
D) the 700 DEG C of sintering in vitreosil pipe suppressed, after 24 hours, are carried out quench treatment when being cooled to 400 DEG C, obtain target;
E) substrate and the target prepared are put into growth chamber, be evacuated to 10
-8mbar, extremely temperature required to silicon by the heater strip in substrate holder, wait until temperature-stable, air pressure to 10
-7about mbar;
F) adjust laser parameter, suitable laser energy, laser frequency are set;
G) pre-treatment is carried out to target, add baffle plate between target and substrate after, use laser hits target two minutes;
H) start laser deposition plated film, make target constantly rotate to keep hitting evenly, according to required plastics thickness control depositing time;
I), after having grown, close well heater, take out after making film naturally cool to room temperature in the vacuum chamber, obtain iron selen-tellurjum film.The inventive method is prepared iron selen-tellurjum superconducting thin film and is had following beneficial effect:
(1) utilize pulsed laser deposition coating technique to carry out the growth of iron selen-tellurjum superconducting thin film, there is the advantages such as easy to use, coating speed fast, can prepare heterogeneity film, more easily keep target consistent with sixbstrate components;
(2) the method can ensure to keep lower air pressure in growth chamber, overcomes the impurity that when using magnetron sputtering plating, high atmospheric pressure causes and introduces;
(3) film performance prepared of the inventive method is excellent, and have better crystalline structure, superconducting characteristic is improved.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention prepares the pld (pulsed laser deposition) growing system of iron selen-tellurjum film; Wherein, 1-growth chamber; 2-laser apparatus; 3-condenser lens; 4-incident laser; 5-substrate; 6-substrate holder; 7-target frame; 8-target.
Embodiment
Embodiment 1
1, FeSe
0.5te
0.5the preparation of target:
A) by more even than 1:0.5:0.5 mixed grinding for Fe, Se, Te massage that;
B) grinding after powder in vitreosil pipe 700 DEG C sintering 24 hours, carry out quench treatment when 400 DEG C;
C) the iron selen-tellurjum after sintering is pulverized again, then to be pressed into diameter be 1 inch, and thickness is the target of 2 millimeters;
D) the FeSe suppressed
0.5te
0.5in vitreosil pipe, 700 DEG C sinter 24 hours, carry out quench treatment when 400 DEG C.
2, pulsed laser deposition is at SrTiO
3grown FeSe
0.5te
0.5film process is as follows:
A) by SrTiO
3substrate and FeSe
0.5te
0.5target puts into growth chamber, is evacuated to 10
-8mbar, by the heater strip in substrate holder to silicon to 310 DEG C, waits until temperature-stable, air pressure to 10
-7about mbar;
B) adjust laser parameter, laser energy 585mJ, laser frequency 3Hz are set;
C) pre-treatment is carried out to target, add baffle plate between target and substrate after, use laser hits target two minutes;
D) start laser deposition plated film, make target constantly rotate to keep hitting evenly, depositing time is 10 minutes;
E), after having grown, close well heater, make FeSe
0.5te
0.5film takes out after naturally cooling to room temperature in the vacuum chamber.
Embodiment 2
1, FeSe
0.7te
0.3the preparation of target:
A) by more even than 1:0.7:0.3 mixed grinding for Fe, Se, Te massage that;
B) grinding after powder in vitreosil pipe 700 DEG C sintering 24 hours, carry out quench treatment when 400 DEG C;
C) the iron selen-tellurjum after sintering is pulverized again, then to be pressed into diameter be 1 inch, and thickness is the target of 2 millimeters;
D) the material suppressed in vitreosil pipe 700 DEG C sintering 24 hours, carry out quench treatment when 400 DEG C.
2, pulsed laser deposition is at LaAlO
3grown FeSe
0.7te
0.3film process is as follows:
A) by LaAlO
3substrate and FeSe
0.7te
0.3target puts into growth chamber, is evacuated to 10
-8mbar, by the heater strip in substrate holder to silicon to 310 DEG C, waits until temperature-stable, air pressure to 10
-7about mbar;
B) adjust laser parameter, laser energy 585mJ, laser frequency 3Hz are set;
C) pre-treatment is carried out to target, add baffle plate between target and substrate after, use laser hits target two minutes;
D) start laser deposition plated film, make target constantly rotate to keep hitting evenly, depositing time is 10 minutes;
E), after having grown, close well heater, make FeSe
0.7te
0.3film takes out after naturally cooling to room temperature in the vacuum chamber.
Claims (2)
1. utilize pulsed laser deposition coating technique to prepare a method for iron selen-tellurjum film, it is characterized in that, concrete preparation process is as follows:
A) by Fe, Se and Te powder by the grinding of certain mixed in molar ratio evenly;
B) the 700 DEG C of sintering in vitreosil pipe of the powder after grinding, after 24 hours, are carried out quench treatment when being cooled to 400 DEG C;
C) by step b) iron selen-tellurjum after sintering pulverizes again, then is pressed into the size of required target;
D) the 700 DEG C of sintering in vitreosil pipe suppressed, after 24 hours, are carried out quench treatment when being cooled to 400 DEG C, obtain target;
E) substrate and the target prepared are put into growth chamber, be evacuated to 10
-8mbar, extremely temperature required to silicon by the heater strip in substrate holder, wait until temperature-stable, air pressure to 10
-7about mbar;
F) adjust laser parameter, suitable laser energy, laser frequency are set;
G) pre-treatment is carried out to target, add baffle plate between target and substrate after, use laser hits target two minutes;
H) start laser deposition plated film, make target constantly rotate to keep hitting evenly, according to required plastics thickness control depositing time;
I), after having grown, close well heater, take out after making film naturally cool to room temperature in the vacuum chamber, obtain iron selen-tellurjum film.
2. a kind of method utilizing pulsed laser deposition plating method to prepare iron selen-tellurjum film according to claim 1, it is characterized in that, the mol ratio of described Fe, Se and Te powder is: 1:0.5:0.5 or 1:0.7:0.3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510262382.XA CN104928630A (en) | 2015-05-21 | 2015-05-21 | Method for preparing FeSeTe film by pulse laser deposition coating technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510262382.XA CN104928630A (en) | 2015-05-21 | 2015-05-21 | Method for preparing FeSeTe film by pulse laser deposition coating technology |
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| CN104928630A true CN104928630A (en) | 2015-09-23 |
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ID=54116050
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| CN201510262382.XA Pending CN104928630A (en) | 2015-05-21 | 2015-05-21 | Method for preparing FeSeTe film by pulse laser deposition coating technology |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105839056A (en) * | 2016-03-29 | 2016-08-10 | 中国科学院电工研究所 | Preparation method of iron base compound superconducting thin film |
| CN107017333A (en) * | 2015-10-01 | 2017-08-04 | 三星电子株式会社 | Thermoelectric structure body, thermo-electric device and its manufacture method |
| CN111719121A (en) * | 2019-07-29 | 2020-09-29 | 中国科学院上海微***与信息技术研究所 | Preparation method of CuFeSb film |
| CN112863761A (en) * | 2021-02-10 | 2021-05-28 | 上海交通大学 | Iron-selenium-tellurium superconducting material and preparation method thereof |
| CN112981326A (en) * | 2021-02-10 | 2021-06-18 | 上海交通大学 | Metal-based superconducting tape and preparation method thereof |
| CN113969395A (en) * | 2021-09-14 | 2022-01-25 | 上海交大平湖智能光电研究院 | Preparation method of phase change film based on pulse laser deposition |
| CN114150375A (en) * | 2021-12-10 | 2022-03-08 | 福建师范大学 | Method for preparing Fe-Sn-Se-Te quaternary film by magnetron co-sputtering |
| CN114892276A (en) * | 2022-04-01 | 2022-08-12 | 电子科技大学长三角研究院(湖州) | Spinel sulfide thin film material and preparation method thereof |
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| CN101550530A (en) * | 2009-04-03 | 2009-10-07 | 清华大学 | Prepare iron doped carbon membrane material with white light photoconductive effect by pulse laser deposition method |
| CN101867012A (en) * | 2009-04-20 | 2010-10-20 | 中国科学院物理研究所 | Preparation method of epitaxial iron-based superconducting thin film and prepared epitaxial iron-based superconducting thin film |
| CN103103480A (en) * | 2011-11-15 | 2013-05-15 | 中国科学院物理研究所 | Film deposition equipment and film deposition method |
| CN103510057A (en) * | 2013-10-21 | 2014-01-15 | 研创应用材料（赣州）有限公司 | Method for preparing novel conducting zinc indium tin oxide materials and films |
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2015
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101550530A (en) * | 2009-04-03 | 2009-10-07 | 清华大学 | Prepare iron doped carbon membrane material with white light photoconductive effect by pulse laser deposition method |
| CN101867012A (en) * | 2009-04-20 | 2010-10-20 | 中国科学院物理研究所 | Preparation method of epitaxial iron-based superconducting thin film and prepared epitaxial iron-based superconducting thin film |
| CN103103480A (en) * | 2011-11-15 | 2013-05-15 | 中国科学院物理研究所 | Film deposition equipment and film deposition method |
| CN103510057A (en) * | 2013-10-21 | 2014-01-15 | 研创应用材料（赣州）有限公司 | Method for preparing novel conducting zinc indium tin oxide materials and films |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107017333A (en) * | 2015-10-01 | 2017-08-04 | 三星电子株式会社 | Thermoelectric structure body, thermo-electric device and its manufacture method |
| CN105839056A (en) * | 2016-03-29 | 2016-08-10 | 中国科学院电工研究所 | Preparation method of iron base compound superconducting thin film |
| CN111719121A (en) * | 2019-07-29 | 2020-09-29 | 中国科学院上海微***与信息技术研究所 | Preparation method of CuFeSb film |
| CN111719121B (en) * | 2019-07-29 | 2021-10-08 | 中国科学院上海微***与信息技术研究所 | Preparation method of out-of-plane highly-oriented CuFeSb film |
| CN112863761A (en) * | 2021-02-10 | 2021-05-28 | 上海交通大学 | Iron-selenium-tellurium superconducting material and preparation method thereof |
| CN112981326A (en) * | 2021-02-10 | 2021-06-18 | 上海交通大学 | Metal-based superconducting tape and preparation method thereof |
| CN112863761B (en) * | 2021-02-10 | 2022-04-01 | 上海交通大学 | Iron-selenium-tellurium superconducting material and preparation method thereof |
| CN113969395A (en) * | 2021-09-14 | 2022-01-25 | 上海交大平湖智能光电研究院 | Preparation method of phase change film based on pulse laser deposition |
| CN113969395B (en) * | 2021-09-14 | 2023-09-08 | 上海交大平湖智能光电研究院 | Preparation method of phase-change film based on pulse laser deposition |
| CN114150375A (en) * | 2021-12-10 | 2022-03-08 | 福建师范大学 | Method for preparing Fe-Sn-Se-Te quaternary film by magnetron co-sputtering |
| CN114150375B (en) * | 2021-12-10 | 2023-11-17 | 福建师范大学 | Method for preparing Fe-Sn-Se-Te quaternary film by magnetron co-sputtering |
| CN114892276A (en) * | 2022-04-01 | 2022-08-12 | 电子科技大学长三角研究院(湖州) | Spinel sulfide thin film material and preparation method thereof |
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Application publication date: 20150923 |