CN101168836A - Method for preparing bismuth telluride alloy thin film by employing cosputtering sedimentation method - Google Patents
Method for preparing bismuth telluride alloy thin film by employing cosputtering sedimentation method Download PDFInfo
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- CN101168836A CN101168836A CNA2006100162694A CN200610016269A CN101168836A CN 101168836 A CN101168836 A CN 101168836A CN A2006100162694 A CNA2006100162694 A CN A2006100162694A CN 200610016269 A CN200610016269 A CN 200610016269A CN 101168836 A CN101168836 A CN 101168836A
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Abstract
The invention relates to a method for preparing bismuth telluride alloy membrane through a co-sputtering and sedimentation method. The invention is implemented on a magnetism control sputtering instrument, a high purity bismuth sheet is stuck on a high purity bismuth target through conducting glue, and the compound target is taken as the sputtering target material to perform co-sputtering; the single crystal silicon chip is taken as the membrane lining bottom. The invention has the technology parameters that: the bottom vacuum degree is higher than 1.0*10-3Pa, the working argon gas pressure is 0.2 to 3Pa, the target base distance is 4 to 10cm, the base sheet table is rotated for 5 to 15 circles per minute, the membrane lining bottom temperature is 100 to 300 DEG C, the sputtering power source power is 20 to 100W, and the annealing temperature is 200 to 300 DEG C. The invention has the advantages that the sedimentation membrane components can be easily adjusted by changing the size and quantity of the sticking target on the standard target material; in particular, to the sputtering compound target with larger deposited membrane component difference, and the exploration of the optimum component doping quantity, the method is simple, the feasibility is strong, the product quality is reliable, and the reproducibility is good.
Description
(1) technical field
The present invention relates to a kind of method for preparing the Tellurobismuthite alloy firm, particularly a kind of method that adopts the cosputtering sedimentation to prepare the Tellurobismuthite alloy firm.
(2) background technology
With the thermo-electric device of semi-conductor thermoelectric material preparation, advantages such as having miniaturization, in light weight, noiseless, do not use heat-transfer medium, be pollution-free has great application prospect in thermoelectric power generation and refrigerating field.Tellurobismuthite (Bi
2Te
3) compound and solid solution alloy thereof be that to study also be one of the most sophisticated thermoelectric material the earliest, the best thermoelectric figure of merit of its block materials is about 1 under the room temperature, and present most of thermoelectric cooling elements all adopt this class material.Because Tellurobismuthite block materials thermoelectric figure of merit is lower, so the thermoelectric conversion efficiency of thermoelectric material is lower; Its low dimensional structures then has higher thermoelectric figure of merit, and conversion efficiency of thermoelectric is higher, so the research of bismuth telluride thin film material becomes the focus of current thermoelectric research field.
The method for preparing bismuth telluride thin film is a lot, as vacuum vapor deposition, pulsed laser deposition, metal organic vapor phase epitaxy method, electrodip process, sol-gel method, molecular beam epitaxy and sputtering method etc., wherein since sputtering method technology simple, do not have waste liquid exhaust gas emission, film quality height, be easy to advantage such as scale operation, become a kind of preferred bismuth telluride thin film preparation method.Yet when adopting Tellurobismuthite as sputtering target material, because bismuth (Bi) is different with the sputtering raste of tellurium (Te), and the saturation vapour pressure of Bi and Te differs 4-5 the order of magnitude, to such an extent as to the thin film composition of sputtering sedimentation and the bigger deviation of target composition appearance; And the thermoelectricity capability of Tellurobismuthite and composition are closely related, thus when using Tellurobismuthite target sputter-deposited thin films, often can not get meeting the film of stoichiometric ratio, thereby can not meet the needs of production.
(3) summary of the invention
The objective of the invention is at the shortcoming in the above-mentioned technology of preparing, provide a kind of simple to operate and reliable quality to adopt the cosputtering sedimentation to prepare the method for Tellurobismuthite alloy firm.
Technical scheme of the present invention:
A kind of method that adopts the cosputtering sedimentation to prepare the Tellurobismuthite alloy firm, on magnetic control sputtering device, implement, it is characterized in that: the high purity tellurium sheet is made the paster target, be pasted on the high purity bismuth standard target, carry out co-sputtered as sputtering target material with this composition target with conductive resin; The high purity tellurium sheet is a garden shape, and diameter is the 30-50% of standard target radius, and quantity 3-6 sheet is distributed on the standard target; As film-substrate, place sputtering target platform opposite with monocrystalline silicon piece; Its processing parameter is: the base vacuum degree is higher than 1.0 * 10
-3Pa, work argon pressure 0.2-3 Pa, target-substrate distance 4-10 cm, chip bench rotation per minute 5-15 circle, 100-300 ℃ of film-substrate temperature, shielding power supply power 20-100 W, annealing temperature 200-300 ℃, annealing time 0.5-2 hour.
A kind of above-mentioned employing cosputtering sedimentation prepares the method for Tellurobismuthite alloy firm, it is characterized in that: the high purity tellurium sheet is square, and the length of side is the 30-50% of standard target radius, and quantity 3-6 sheet is distributed on the standard target.
A kind of above-mentioned employing cosputtering sedimentation prepares the method for Tellurobismuthite alloy firm, it is characterized in that: make standard target with the high purity tellurium sheet, make the paster target with the high purity bismuth sheet.
A kind of above-mentioned employing cosputtering sedimentation prepares the method for Tellurobismuthite alloy firm, it is characterized in that: with quartz plate or sheet glass as film-substrate.
Advantage of the present invention is: how much are area size by changing paster target on the standard target and quantity, can adjust the composition of deposit film at an easy rate; Increase or reduce the paster target gradually and cover area on the standard target, can realize the continuous variation of deposit film composition, and needn't every change primary components all make the standard target of a corresponding composition again; Especially have than big difference for the sedimentary thin film composition of sputter compound target, and explore the optimal components doping, this method is simple, workable, reliable product quality, favorable reproducibility.
(4) embodiment
Embodiment: a kind of method that adopts the cosputtering sedimentation to prepare the Tellurobismuthite alloy firm, on magnetic control sputtering device, to implement, its processing step is as follows:
1) with the high purity tellurium sheet of 4 diameter 12mm, thick 1mm, on the uniform high purity bismuth target that is pasted on diameter 60mm, and making the tellurium sheet be centered close to the bismuth target center of circle is the center of circle, on the annulus of diameter 30mm, the composition target that above-mentioned stickup forms is as the cosputtering target, and is fixed on the sputtering target platform towards chip bench with the tellurium sheet;
2) with monocrystalline silicon piece (100) as film-substrate;
3) vacuum chamber is evacuated to vacuum tightness and is higher than 3 * 10
-5Pa adjusts slide valve, charges into high-purity argon gas then in vacuum chamber, and keeps argon gas at 1.0Pa, the Si substrate is placed carry out backwash cleaning 10 minutes on the backwash platform;
4) backwash is closed argon gas after cleaning and finishing, and places substrate on the sample table again and opens heating power supply, and substrate is heated to 200 ℃;
5) charge into argon gas to vacuum chamber again, the adjustments of gas under meter makes argon pressure be stabilized in 0.5Pa; Adjust the sputter pattern to just spattering, the adjustment target-substrate distance is 7cm; Open the radio-frequency sputtering power supply, the sputter output rating is 30W, pre-sputter 15min; Open the chip bench rotary power source, the adjusting speed of rotation is 10rpm; The baffle plate of opening then between chip bench and the sputtering target platform begins the formal sputtering deposit film; Close shielding power supply and argon gas after 30 minutes, continue insulation one hour; Reduce to room temperature with the speed of 3-5 ℃/min then;
6) close slide valve, molecular pump, mechanical pump in order, open purging valve and in vacuum chamber, slowly pour air, treat that air pressure and barometric point balance are opened vacuum chamber later in the vacuum chamber, take out sample, finish plated film.
(equipment is Philips PW1700 CoK α, λ=1.78897 to carrying out the XRD test according to present method bismuth telluride thin film that the cosputtering deposition makes on monocrystalline silicon substrate
), the result shows: all diffraction peaks and Bi
2Te
3Standard diffraction peak unanimity, and the diffraction peak of simple substance Bi and Te does not occur, obvious film prepared in accordance with the present invention has been alloying fully, rather than exists with simple mechanically mixing form, and promptly cosputtering simple substance Bi and Te can form the Tellurobismuthite alloy firm; Utilize Sirion 200 emissions surface sweeping Electronic Speculum (acceleration voltage is 5kV) that the cross section of this film is tested, the result shows: sedimentary bismuth telluride thin film thickness is 300nm on silicon chip, and smooth surface is smooth, and pore-free such as is mingled with at defective, section is evenly fine and close, the film quality excellence.
Claims (4)
1. method that adopts the cosputtering sedimentation to prepare the Tellurobismuthite alloy firm, on magnetic control sputtering device, implement, it is characterized in that: the high purity tellurium sheet is made the paster target, be pasted on the high purity bismuth standard target, carry out co-sputtered as sputtering target material with this composition target with conductive resin; The high purity tellurium sheet is a garden shape, and diameter is the 30-50% of standard target radius, and quantity 3-6 sheet is distributed on the standard target; As film-substrate, place sputtering target platform opposite with monocrystalline silicon piece; Its processing parameter is: the base vacuum degree is higher than 1.0 * 10
-3Pa, work argon pressure 0.2-3Pa, target-substrate distance 4-10cm, chip bench rotation per minute 5-15 circle, 100-300 ℃ of film-substrate temperature, shielding power supply power 20-100W, annealing temperature 200-300 ℃, annealing time 0.5-2 hour.
2. employing cosputtering sedimentation according to claim 1 prepares the method for Tellurobismuthite alloy firm, it is characterized in that: the high purity tellurium sheet is square, and the length of side is the 30-50% of standard target radius, and quantity 3-6 sheet is distributed on the standard target.
3. employing cosputtering sedimentation according to claim 1 prepares the method for Tellurobismuthite alloy firm, it is characterized in that: make standard target with the high purity tellurium sheet, make the paster target with the high purity bismuth sheet.
4. prepare the method for Tellurobismuthite alloy firm according to claim 1 or 3 described employing cosputtering sedimentations, it is characterized in that: with quartz plate or sheet glass as film-substrate.
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| CN101434455B (en) * | 2008-12-01 | 2011-01-12 | 北京航空航天大学 | Method for preparing bismuth telluride nano-wire array by physical vapour deposition |
| CN102199752A (en) * | 2010-03-22 | 2011-09-28 | 昆明物理研究所 | Magneto-controlled sputter growing method for amorphous cadmium telluride thin films |
| CN102515561A (en) * | 2011-12-16 | 2012-06-27 | 大连交通大学 | Preparation technology of Cu (In, al) Se2thin film |
| CN104152856A (en) * | 2014-07-11 | 2014-11-19 | 西南交通大学 | Method for preparing Bi2Se3 thin film by virtue of magnetron sputtering process |
| CN104392823A (en) * | 2014-12-01 | 2015-03-04 | 南京理工大学 | Resonant damping enhanced FeCo-based high-frequency soft magnetic thin film and manufacturing method thereof |
| CN104495763A (en) * | 2014-12-12 | 2015-04-08 | 上海申和热磁电子有限公司 | Preparation method of bismuth-telluride-base thermoelectric material |
| CN106399937A (en) * | 2016-06-17 | 2017-02-15 | 中国科学院电工研究所 | Method for preparing preferred-orientation bismuth telluride thermoelectric thin film |
| CN106498354A (en) * | 2016-09-18 | 2017-03-15 | 中国科学院电工研究所 | A kind of method for preparing hexagonal Spiral morphology Tellurobismuthite. thermal electric film |
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| CN101434455B (en) * | 2008-12-01 | 2011-01-12 | 北京航空航天大学 | Method for preparing bismuth telluride nano-wire array by physical vapour deposition |
| CN102199752A (en) * | 2010-03-22 | 2011-09-28 | 昆明物理研究所 | Magneto-controlled sputter growing method for amorphous cadmium telluride thin films |
| CN102199752B (en) * | 2010-03-22 | 2013-02-20 | 昆明物理研究所 | Magneto-controlled sputter growing method for amorphous cadmium telluride thin films |
| CN102515561A (en) * | 2011-12-16 | 2012-06-27 | 大连交通大学 | Preparation technology of Cu (In, al) Se2thin film |
| CN104152856A (en) * | 2014-07-11 | 2014-11-19 | 西南交通大学 | Method for preparing Bi2Se3 thin film by virtue of magnetron sputtering process |
| CN104152856B (en) * | 2014-07-11 | 2017-05-31 | 西南交通大学 | A kind of magnetron sputtering method prepares Bi2Se3The method of film |
| CN104392823A (en) * | 2014-12-01 | 2015-03-04 | 南京理工大学 | Resonant damping enhanced FeCo-based high-frequency soft magnetic thin film and manufacturing method thereof |
| CN104495763A (en) * | 2014-12-12 | 2015-04-08 | 上海申和热磁电子有限公司 | Preparation method of bismuth-telluride-base thermoelectric material |
| CN106399937B (en) * | 2016-06-17 | 2018-07-27 | 中国科学院电工研究所 | A method of preparing preferred orientation bismuth telluride thermal electric film |
| CN106399937A (en) * | 2016-06-17 | 2017-02-15 | 中国科学院电工研究所 | Method for preparing preferred-orientation bismuth telluride thermoelectric thin film |
| CN106498354A (en) * | 2016-09-18 | 2017-03-15 | 中国科学院电工研究所 | A kind of method for preparing hexagonal Spiral morphology Tellurobismuthite. thermal electric film |
| CN106498354B (en) * | 2016-09-18 | 2018-09-25 | 中国科学院电工研究所 | A method of preparing hexagonal Spiral morphology bismuth telluride thermal electric film |
| CN107881475A (en) * | 2016-09-30 | 2018-04-06 | 江西理工大学 | A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method |
| CN107881475B (en) * | 2016-09-30 | 2019-11-01 | 江西理工大学 | A method of Ni-Co-Mn-Ti alloy firm is prepared by magnetron sputtering DC sputturing method |
| CN110678993A (en) * | 2017-03-07 | 2020-01-10 | 马勒国际有限公司 | Method for producing a thermoelectric module |
| CN108004518A (en) * | 2017-10-17 | 2018-05-08 | 云南大学 | Size uniform, high density MnGe quantum dots are prepared based on ion beam sputtering technology |
| CN109943820A (en) * | 2019-04-12 | 2019-06-28 | 大连理工大学 | One kind being applied to anti-corrosion Ti-Ta alloy film material of detecting head surface high-temperature electric conduction and preparation method thereof |
| CN112813399A (en) * | 2021-02-04 | 2021-05-18 | 郑州大学 | High-entropy metal glass protective coating and preparation method thereof |
| CN114032501A (en) * | 2021-11-01 | 2022-02-11 | 吉林大学 | Method for compatibility of far infrared transparency and electric conductivity in thin film material |
| CN114032501B (en) * | 2021-11-01 | 2023-09-22 | 吉林大学 | Method for compatible far infrared transparency and conductivity in film material |
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