CN101339906A - Preparation process of novel environmental semi-conductor photoelectronic material beta-FeSi2 film - Google Patents
Preparation process of novel environmental semi-conductor photoelectronic material beta-FeSi2 film Download PDFInfo
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- CN101339906A CN101339906A CNA2008100688618A CN200810068861A CN101339906A CN 101339906 A CN101339906 A CN 101339906A CN A2008100688618 A CNA2008100688618 A CN A2008100688618A CN 200810068861 A CN200810068861 A CN 200810068861A CN 101339906 A CN101339906 A CN 101339906A
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 title claims abstract description 11
- 230000007613 environmental effect Effects 0.000 title claims abstract description 9
- 229910006578 β-FeSi2 Inorganic materials 0.000 title 1
- 229910006585 β-FeSi Inorganic materials 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000000137 annealing Methods 0.000 claims abstract description 23
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 16
- 229910017082 Fe-Si Inorganic materials 0.000 claims abstract description 9
- 229910017133 Fe—Si Inorganic materials 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 230000005693 optoelectronics Effects 0.000 claims abstract description 7
- 239000010408 film Substances 0.000 claims abstract 10
- 239000010409 thin film Substances 0.000 claims abstract 7
- 229910005331 FeSi2 Inorganic materials 0.000 claims abstract 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 23
- 238000004544 sputter deposition Methods 0.000 claims description 19
- 238000005516 engineering process Methods 0.000 claims description 14
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910005347 FeSi Inorganic materials 0.000 claims 1
- 239000013077 target material Substances 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004062 sedimentation Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003708 ampul Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910021350 transition metal silicide Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
本发明公开了一种新型环境半导体光电子材料β－FeSi2薄膜的制备工艺，涉及一种Fe－Si化合物，首先采用磁控溅射方法在Si基片上沉积一层厚度50－150nm的金属Fe膜，随后在真空退火炉中880－920℃退火12－18小时获得Fe－Si化合物中的半导体相β－FeSi2薄膜，由于采用直流磁控溅射方法，使沉积在Si基片上的Fe膜厚度均匀、工艺简单、成本低，易于制备大面积β－FeSi2薄膜，易于工业化生产，又由于退火时间和温度能严格控制，产品质量稳定，重现性好。
The invention discloses a preparation process of a novel environmental semiconductor optoelectronic material β- FeSi2 thin film, which relates to a Fe-Si compound. First, a metal Fe film with a thickness of 50-150nm is deposited on a Si substrate by a magnetron sputtering method. , followed by annealing in a vacuum annealing furnace at 880-920°C for 12-18 hours to obtain the semiconductor phase β-FeSi 2 film in the Fe-Si compound. Due to the use of DC magnetron sputtering, the thickness of the Fe film deposited on the Si substrate is Uniform, simple process, low cost, easy to prepare large-area β- FeSi2 film, easy to industrial production, and because the annealing time and temperature can be strictly controlled, the product quality is stable and reproducible.
Description
Technical field:
The present invention relates to a kind of Fe-Si compound, specifically a kind of novel environmental semi-conductor photoelectronic material beta-FeSi
2The preparation technology of film and with the β-FeSi of this explained hereafter
2Film.
Background technology:
Low-temperature stabilization phase β-FeSi in the transition metal silicide Fe-Si compound
2Be the friendly semi-conducting material of a kind of novel environmental, have good photoelectric characteristic, simultaneously, the component of this material reserves on earth is abundant, nontoxic, and utilizes β-FeSi
2The technology of film preparation opto-electronic device is compatible mutually with existing silicon integrated circuit technology, therefore, and β-FeSi
2Film has important use at photoelectricity and thermoelectric field.Block β-FeSi
2Material generally adopts the sintering process preparation, and film β-FeSi
2Usually adopt methods such as molecular beam epitaxy, ion beam injection, magnetron sputtering preparation nanometer Fe film on silicon chip earlier, then the nanometer Fe film is heat-treated preparation β-FeSi
2Film, but adopt molecular beam epitaxy, ion beam injects heating treatment method and prepares β-FeSi
2Film is owing to complex process cost height, and film speed waits shortcoming slowly, the industrial production cost height, and adopt magnetron sputtering really to have above-mentioned advantage, the industrialization promotion production cost is low.
Summary of the invention:
Because β-FeSi
2Film environmental friendliness characteristic, collimation tape splicing crack character, with existing si-substrate integrated circuit technology compatibility mutually, make semi-conducting material β-FeSi
2The exploitation of film, application have crucial value.The objective of the invention is to find a kind of new production low-temperature stabilization phase β-FeSi
2The method of film, it is simple to make it to have technology, with low cost, is easy to prepare large area uniform film, is easy to realize suitability for industrialized production.
The present invention at first adopts magnetically controlled sputter method to deposit the metal Fe film of a layer thickness 50-150nm on the Si substrate, subsequently 880-920 ℃ of semiconductor phase β-FeSi that annealing obtained in the Fe-Si compound in 12-18 hour in vacuum annealing furnace
2Film.
The magnetically controlled sputter method of indication of the present invention, be to adopt dc magnetron sputtering method, in sputter, with purity is that 99.95% metallic iron is made target, make substrate with Si (100), the metal Fe film of the about 50-150nm of deposition one layer thickness on Si (100) substrate, the sputtering sedimentation condition: sputtering sedimentation under the room temperature, sputtering parameter is: back of the body end vacuum 2 * 10
-5Pa, sputtering pressure 1.0-2.5Pa, Ar throughput 15-30SCCM, sputtering power 80-110W, substrate bias-50V.
The vacuum annealing of indication of the present invention forms β-FeSi
2The method of film, be with magnetron sputtering deposition at the on-chip Fe film of Si, 880-920 ℃ of annealing obtained the semiconductor phase β-FeSi in the Fe-Si compound in 12-18 hour in vacuum annealing furnace
2Film, vacuum degree is better than 2 * 10 in the annealing process
-3Pa.
Operation divides following several steps to carry out
1. substrate and substrate clean
Substrate is selected Si (100) single-chip, single-sided polishing, resistivity 7-13 Ω cm for use.Each ultrasonic cleaning 10 minutes of packing into before the sputtering chamber in acetone, absolute ethyl alcohol and deionized water dries up with nitrogen.
2. the preparation of metal Fe film
Cleaned substrate is placed the sputter Sample Room, after cleaning, backwash sends into sputtering chamber, with purity is that 99.95% metallic iron is made target, make substrate with Si (100) single-chip, adopt dc magnetron sputtering method, at room temperature deposit thickness is the Fe film of 50-150nm on substrate, and splash-proofing sputtering process parameter is as follows: back of the body end vacuum 2 * 10
-5Pa, sputtering pressure 1.0-2.5Pa, Ar throughput 15-30SCCM, sputtering power 80-110W, substrate bias-50V, sedimentation time 10 minutes.
3. vacuum annealing forms β-FeSi
2Film
The Fe film of magnetron sputtering deposition places and adds a cover the molybdenum box, and the molybdenum box is put the uniform temperature zone of vacuum annealing furnace quartz ampoule into, is evacuated to 4.0 * 10
-4Be warming up to 880-920 ℃ behind the Pa, be incubated 12-18 hour, naturally cool to room temperature then, vacuum degree is better than 2.0 * 10 in whole annealing process
-3Pa.The annealing back obtains single phase β-FeSi
2Film.
Adopt the present invention to produce β-FeSi
2The technology of film owing to adopt the method for magnetron sputtering, makes that to be deposited on the on-chip iron film thickness of Si even, and technology is simple, and cost is low, is easy to prepare large area film, is easy to realize suitability for industrialized production; The counterdiffusion of atom phase also forms low-temperature stabilization semiconductor phase β-FeSi in the Fe-Si compound
2Because Fe film deposition in the technology, annealing temperature and annealing time can strictly be controlled, guarantee the steady quality of product of the present invention, good process repeatability uses goods of the present invention nontoxic, harmless to organism and environment for a long time, can be used for the semiconductor photoelectronic device field, as solar cell, Infrared Detectors and light-emitting diode etc.
To film sample, adopt X-ray diffraction (XRD) (Japanese D/MAX-2200 of science) and ESEM (SEM) (S3400N of Hitachi) that crystal structure and surface topography are characterized by method for preparing.See accompanying drawing 1 and accompanying drawing 2.
Description of drawings:
Fig. 1, magnetron sputtering β-FeSi
2The XRD spectrum of film.
Abscissa is represented the angle of diffraction, and ordinate is represented diffracted intensity, and XRD confirms to have formed single phase semiconductor β-FeSi
2Film, and have polycrystalline structure.
Fig. 2, magnetron sputtering β-FeSi
2The SEM image of film.
SEM image show sample crystal grain is the regular polyhedron shape and is distributed in the matrix, and intercrystalline is separated from one another.
Embodiment:
The concrete processing method of embodiment is as follows
1. with each ultrasonic cleaning 10 minutes in acetone, absolute ethyl alcohol and deionized water of Si (100) single-chip (resistivity 7-13 Ω cm) of single-sided polishing, dry up with nitrogen.
2. cleaned substrate is placed the sputter Sample Room, be evacuated to 2 * 10
-5Pa, charge into 99.999% pure Ar gas, regulate air pressure and to 7.0Pa, begin the backwash cleaning, subsequently substrate is sent into sputtering chamber, adopt dc magnetron sputtering method on the Si substrate, to deposit the Fe film, keeping Ar air pressure in the sputter procedure is by force 2.0Pa, Ar throughput 20SCCM, sputtering power 80W, substrate bias-50V, spatter beginning deposition Fe film on substrate after 10 minutes in advance, sedimentation time 10 minutes.
3. take out sputtering sedimentation at the on-chip Fe film of Si, place and add a cover the molybdenum box, the molybdenum box is put the uniform temperature zone of vacuum annealing furnace quartz ampoule into, is evacuated to 4.0 * 10
-4Be warming up to 900 ℃ behind the Pa, 900 ℃ of insulations 15 hours, naturally cool to room temperature then, vacuum degree is better than 2.0 * 10 in whole annealing process
-3Pa.The annealing back obtains single phase β-FeSi
2Film.
Confirm to have obtained single phase β-FeSi after the annealing 4.XRD measure
2The film (see figure 1).
Because the β-FeSi of this processes
2Film thickness is even, and area is big, and bigger application and development prospect is arranged, claimed technology of the present invention and with the β-FeSi of this explained hereafter
2Film product.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100688618A CN101339906A (en) | 2008-08-12 | 2008-08-12 | Preparation process of novel environmental semi-conductor photoelectronic material beta-FeSi2 film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100688618A CN101339906A (en) | 2008-08-12 | 2008-08-12 | Preparation process of novel environmental semi-conductor photoelectronic material beta-FeSi2 film |
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| Publication Number | Publication Date |
|---|---|
| CN101339906A true CN101339906A (en) | 2009-01-07 |
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|---|---|---|---|
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781753A (en) * | 2010-04-16 | 2010-07-21 | 贵州大学 | Technological method for preparing Cr-doped beta-FeSi2 films |
| CN101798680A (en) * | 2010-04-15 | 2010-08-11 | 贵州大学 | Magnetron sputtering preparation process for Mg2Si thin film made of environment-friendly semiconductor material |
| CN101820005A (en) * | 2010-04-16 | 2010-09-01 | 贵州大学 | Method for preparing Mn-doped beta-FeSi2 film |
| WO2012083519A1 (en) * | 2010-12-20 | 2012-06-28 | 海洋王照明科技股份有限公司 | Light emission apparatus and manufacturing method thereof |
| RU2485631C1 (en) * | 2012-01-19 | 2013-06-20 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2485632C1 (en) * | 2012-01-19 | 2013-06-20 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
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| RU2488920C1 (en) * | 2012-02-08 | 2013-07-27 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2488917C1 (en) * | 2012-02-08 | 2013-07-27 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2488918C1 (en) * | 2012-02-08 | 2013-07-27 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
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2008
- 2008-08-12 CN CNA2008100688618A patent/CN101339906A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798680A (en) * | 2010-04-15 | 2010-08-11 | 贵州大学 | Magnetron sputtering preparation process for Mg2Si thin film made of environment-friendly semiconductor material |
| CN101781753A (en) * | 2010-04-16 | 2010-07-21 | 贵州大学 | Technological method for preparing Cr-doped beta-FeSi2 films |
| CN101820005A (en) * | 2010-04-16 | 2010-09-01 | 贵州大学 | Method for preparing Mn-doped beta-FeSi2 film |
| WO2012083519A1 (en) * | 2010-12-20 | 2012-06-28 | 海洋王照明科技股份有限公司 | Light emission apparatus and manufacturing method thereof |
| CN103140944A (en) * | 2010-12-20 | 2013-06-05 | 海洋王照明科技股份有限公司 | Light emission apparatus and manufacturing method thereof |
| EP2657989A4 (en) * | 2010-12-20 | 2014-05-14 | Oceans King Lighting Science | Light emission apparatus and manufacturing method thereof |
| RU2485631C1 (en) * | 2012-01-19 | 2013-06-20 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2485632C1 (en) * | 2012-01-19 | 2013-06-20 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2488919C1 (en) * | 2012-02-08 | 2013-07-27 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2488920C1 (en) * | 2012-02-08 | 2013-07-27 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2488917C1 (en) * | 2012-02-08 | 2013-07-27 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
| RU2488918C1 (en) * | 2012-02-08 | 2013-07-27 | Учреждение Российской академии наук Институт автоматики и процессов управления Дальневосточного отделения РАН (ИАПУ ДВО РАН) | Method of making light-emitting element |
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Open date: 20090107 |