CN102925866B - Preparation technology for single-phase Mg2Si semiconductor film - Google Patents
Preparation technology for single-phase Mg2Si semiconductor film Download PDFInfo
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- CN102925866B CN102925866B CN201210455881.7A CN201210455881A CN102925866B CN 102925866 B CN102925866 B CN 102925866B CN 201210455881 A CN201210455881 A CN 201210455881A CN 102925866 B CN102925866 B CN 102925866B
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Abstract
The invention discloses a preparation technology for a single-phase Mg2Si semiconductor film. The preparation technology comprises processes as follows: 1, evaporating to deposit an Mg film on an Si substrate, wherein an Si sheet is cleaned and dried and then fixed on a sample frame above a resistance thermal evaporation chamber, and Mg particles are positioned in an evaporation crucible for vapor deposition; and 2, annealing: transferring an Si sheet carried out vapor deposition into a high vacuum annealing furnace for annealing under low-vacuum atmosphere, so as to obtain the single-phase Mg2Si semiconductor film. By adopting the preparation technology, the shortcomings that experimental conditions are severe, the cost is higher, the industrial popularization is hard to carry out and the like are overcome; and the problems that the quality of Mg2Si is finally influenced as impurities such as MgO oxide are generated when an electron beam evaporation and depositing technology is adopted and annealing is carried out under an argon atmosphere in the annealing process of an annealing furnace are solved.
Description
Technical field
The present invention relates to a kind of single-phase Mg
2the preparation technology of Si semiconductor film.
Background technology
Mg
2si, as a kind of metal silicide environment-friendly semiconductor material having good development prospect, has following characteristics: the raw material resources of element M g, Si are abundant, earth's crust standing stock are large, cheap; Element nontoxic pollution-free, Mg
2si is corrosion-resistant, anti-oxidant.Environment-friendly semiconductor Mg
2why Si material has broad application prospects, and also because it has a series of excellent characteristic, as its preparation method is mutually compatible with existing Si base microelectronic technique, decreases production unit and to upgrade the cost pressure brought; 1.2-1.8 μm of infrared rays wave band is applicable to modern communication device; Have good ohmic contact with N-shaped Si, contact resistivity is 2.2 × 10
-7wcm, than a metal A l also little order of magnitude.Meanwhile, Mg
2si is considered to the thermoelectric material of a kind of thermoelectrical efficiency high (ZT>1).In photoelectricity and pyroelectricity Quality Research, as a kind of narrow bandgap semiconductor material, Mg
2si has certain application prospect in field of infrared sensors, and by adulterating, different element is analyzed, and demonstrates Mg
2si has good thermoelectric material application prospect.In a word, Mg
2si thin-film material has important application prospect in photoelectric device, electron device, energy device field, poisonous or easily cause the semiconductor material of environmental pollution before being expected to progressively to replace, and has larger social benefit and environmental benefit.Multiple technologies have been had to be applied to Mg at present
2the preparation of Si thin-film material, comprising: pulsed laser deposition, molecular beam epitaxy, ion beam synthesis etc., all there is experiment condition harshness in these methods, cost is higher, be difficult to the shortcomings such as industrialization promotion, adopt electron-beam evaporation technique, in annealing process, adopt argon atmosphere to anneal in the lehr, find the generation having the impurity such as MgO oxide compound, finally affect Mg
2the quality of Si.
Summary of the invention
The technical problem to be solved in the present invention: a kind of single-phase Mg is provided
2the preparation technology of Si semiconductor film, to overcome the experiment condition harshness that prior art exists, cost is higher, is difficult to the shortcomings such as industrialization promotion, and adopts electron-beam evaporation technique, has the impurity such as MgO oxide compound, finally affects Mg
2the problems such as the quality of Si.Technical solution of the present invention:
A kind of single-phase Mg
2the preparation technology of Si semiconductor film, it comprises following process: the first, hydatogenesis Mg film on Si substrate, and first by Si sheet cleaning-drying, be fixed on by Si sheet on the specimen holder above resistance heat evaporator room, Mg particle is placed in evaporator crucible, carries out evaporation; The second, annealing process, the Si sheet after evaporation completes is placed in high vacuum annealing furnace and carries out the annealing of rough vacuum atmosphere, finally prepares single-phase Mg
2si semiconductor film.
In Si sheet cleaning-drying process, first Si sheet is cut to desired shape size, used dehydrated alcohol, acetone ultrasonic cleaning, re-use deionized water ultrasonic cleaning; Dry under the sample cleaned up being placed in loft drier 70 DEG C of conditions.Compressing tablet is used to be fixed on the specimen holder above resistance heat evaporator room by Si sheet.
Before carrying out evaporation, first resistance heat evaporator room is vacuumized, when vacuum tightness is less than or equal to 2.0 × 10
-4during Pa, start evaporation; Evaporation current is progressively added to 80 A, formally starts evaporation; The power of resistance-type thermal evaporation during evaporation is 16 ~ 19 KW, and vaporator rate remains on 18-24 nm/min, and evaporation time is 15-18 min.
In annealing process, the annealing furnace back end vacuum in high vacuum annealing furnace is less than or equal to 10
-3pa, regulates angle valve before annealing, makes vacuum remain on 10
-1pa-10
-2between Pa.
In annealing process, annealing time 3-7 h, annealing temperature 350 DEG C-450 DEG C.
Prepare single-phase Mg on a si substrate
2si semiconductor film, the Mg namely prepared on a si substrate
2not containing other phase materials such as MgO or Mg crystal grain in Si semiconductor film.
Beneficial effect of the present invention:
Annealing way under employing the present invention-rough vacuum condition, has prepared single-phase Mg
2si semiconductor film, the Mg of synthesis
2containing the impurity such as MgO or Mg crystal grain in Si film, be Mg
2the device of Si semiconductor film develops and lays a good foundation.
The present invention adopts resistance-type thermal evaporation deposition and rough vacuum annealing technology, prepares single-phase Mg
2si semiconductor film.The ultimate principle of resistance-type thermal evaporation deposition technology is that evaporating materials is put into suitable resistance heating body, and energising makes evaporating materials direct heating evaporate, thus evaporating materials is deposited on substrate in a gaseous form form film; First the present invention adopts resistance-type evaporation technique to deposit 280-480 nm pure metal Mg film on Si monocrystal chip, forming Si/Mg membrane structure, annealing with being placed in vacuum annealing furnace.Annealing furnace back end vacuum is less than or equal to 10
-3pa, regulates angle valve before annealing, makes back end vacuum remain on 10
-1pa-10
-2between Pa; Annealing time 3-7 hour, annealing temperature 350 DEG C-450 DEG C, obtains single-phase Mg
2si semiconductor film; Preparation technology of the present invention, carries out anneal under rough vacuum condition, avoids other gases such as oxygen and enter in treating processes, the single-phase Mg of preparation
2si semiconductor film, not containing other phase impurity substances such as MgO or Mg crystal grain, equally, if anneal in high vacuum conditions, because metal M g is high-vapor-pressure element, causes all or part of volatilization of metal M g, is unfavorable for that Si, Mg atomic diffusion is to form Mg
2si film.Therefore the present invention carries out anneal under adopting rough vacuum condition, to obtain single-phase Mg
2si semiconductor film, compared with prior art, it is lower that the present invention has production cost, can carry out the advantage of suitability for industrialized production, solves the experiment condition harshness that prior art exists, cost is higher, be difficult to the shortcomings such as industrialization promotion, and adopt electron-beam evaporation technique, in annealing process, adopt argon atmosphere to anneal in the lehr, there is the generation of the impurity such as MgO oxide compound, finally affect Mg
2the problems such as the quality of Si, the present invention has prepared the single-phase Mg not containing the impurity such as MgO or Mg crystal grain
2si semiconductor film is Mg
2the device of Si semiconductor film develops and lays a good foundation.
Accompanying drawing explanation
Fig. 1 is sample X-ray diffractogram of the present invention, is respectively the X-ray diffractogram of 3-7 h at 400 DEG C of annealing times;
Fig. 2 is Sample Scan Electronic Speculum figure of the present invention, is respectively the scanning electron microscope (SEM) photograph of 3 h at 400 DEG C of annealing times;
Fig. 3 is Sample Scan Electronic Speculum figure of the present invention, is respectively the scanning electron microscope (SEM) photograph of 4 h at 400 DEG C of annealing times;
Fig. 4 is Sample Scan Electronic Speculum figure of the present invention, is respectively the scanning electron microscope (SEM) photograph of 5 h at 400 DEG C of annealing times;
Fig. 5 is Sample Scan Electronic Speculum figure of the present invention, is respectively the scanning electron microscope (SEM) photograph of 6 h at 400 DEG C of annealing times;
Fig. 6 is Sample Scan Electronic Speculum figure of the present invention, is respectively the scanning electron microscope (SEM) photograph of 7 h at 400 DEG C of annealing times;
Fig. 7 is sample X-ray diffractogram of the present invention, at the X-ray diffractogram of 300-450 DEG C of annealing temperature 5 h.
Embodiment
Embodiment 1:
(1) test Si sheet is cut to required size; First, use dehydrated alcohol, acetone ultrasonic oscillation 20 minutes respectively, object removes silicon chip surface organism, re-uses deionized water ultrasonic cleaning 5 times, each 10 minutes; Till drying under finally the sample cleaned up being placed in loft drier 70 DEG C of conditions;
(2) test Si sheet is less due to area, uses shell fragment to be fixed on the specimen holder above deposited chamber.High-purity Mg particle is directly placed in evaporator crucible;
(3) deposited chamber is vacuumized, when vacuum tightness is less than or equal to 2.0 × 10
-4during Pa, and keep for some time;
(4) when vacuum tightness is less than or equal to 2.0 × 10 again
-4during Pa, heating current is progressively added to 80 A, starts evaporation; The power of resistance-type thermal evaporation during evaporation is 18 KW, and vaporator rate remains on 18-24 nm/min, and evaporation time is 16 min;
(5) evaporation naturally cools to room temperature after completing, then takes out and be placed in high vacuum annealing furnace, and annealing furnace back end vacuum is less than or equal to 10
-3pa, regulates angle valve before annealing, makes back end vacuum remain on 10
-1pa-10
-2between Pa.Annealing time 3-7 h, annealing temperature 400 DEG C, forms single-phase Mg
2si semiconductor film.
Fig. 1 is the X-ray diffractogram of sample prepared by 400 DEG C of different annealing times, visible in figure, and except substrate Si diffraction peak, each diffraction peak is Mg
2si diffraction peak, and with PDF standard spectrum (card number: 65-9365) diffraction peak one_to_one corresponding, under preparation condition of the present invention is described, prepared single-phase Mg
2si semiconductor film film.
Fig. 2 to Fig. 6 is the scanning electron microscope (SEM) photograph of sample surface morphology prepared by 400 DEG C of different annealing times, result display Mg
2si crystal grain is good to sample surfaces coverage, and grain-size is comparatively large, and surface is comparatively smooth.Testing under the annealing conditions adopted, all there is the Mg that crystalline state is good
2si film occurs.
Embodiment 2:
(1) test Si sheet is cut to required size; First, clean 20 min with dehydrated alcohol, acetone ultrasonic oscillation respectively, object removes silicon chip surface organism, re-uses deionized water ultrasonic oscillation and clean 5 times, each 10 min.Toast, to surperficial complete drying under finally the sample cleaned up being placed in loft drier 80 DEG C of conditions;
(2) test Si sheet is less due to area, uses shell fragment to be fixed on the specimen holder above deposited chamber.Mg particle is directly placed in evaporator crucible;
(3) deposited chamber is vacuumized, when vacuum tightness is less than or equal to 2.0 × 10
-4during Pa, and keep for some time;
(4) when vacuum tightness is less than or equal to 2.0 × 10 again
-4during Pa, start evaporation; Evaporation current is progressively added to 80 A, formally starts evaporation; The power of resistance-type thermal evaporation during evaporation is 16 ~ 19KW, and vaporator rate remains on 18 ~ 24 nm/min, and evaporation time is 16 min;
(5) evaporation naturally cools to room temperature after completing, then takes out and be placed in high vacuum annealing furnace.Annealing furnace back end vacuum is less than or equal to 10
-3pa, regulates angle valve before annealing, makes back end vacuum remain on 10
-1pa-10
-2between Pa.Annealing time 5h, annealing temperature 350-450 DEG C, prepare single-phase Mg
2si semiconductor film.
Fig. 7 is annealing time is 5 hours, and the X-ray diffractogram of the sample prepared when different annealing temperature is visible in figure, and except substrate Si diffraction peak, each diffraction peak is Mg
2si diffraction peak, and with PDF standard spectrum (card number: 65-9365) diffraction peak one_to_one corresponding, under preparation condition of the present invention is described, prepared single-phase Mg
2si semiconductor film film.
Claims (2)
1. a single-phase Mg
2the preparation technology of Si semiconductor film, it is characterized in that: it comprises following process: the first, hydatogenesis Mg film on Si substrate, first by Si sheet cleaning-drying, is fixed on Si sheet on the specimen holder above resistance heat evaporator room, Mg particle is placed in evaporator crucible, carries out evaporation; The second, annealing process, the Si sheet after evaporation completes is placed in high vacuum annealing furnace and carries out the annealing of rough vacuum atmosphere, and in annealing process, the annealing furnace back end vacuum in high vacuum annealing furnace is less than or equal to 10
-3pa, regulates angle valve before annealing, makes vacuum remain on 10
-1pa-10
-2between Pa, in annealing process, annealing time 3-7 h, annealing temperature 350 DEG C-450 DEG C, finally prepares single-phase Mg
2si semiconductor film; In Si sheet cleaning-drying process, first Si sheet is cut to desired shape size, used dehydrated alcohol, acetone ultrasonic cleaning, re-use deionized water ultrasonic cleaning; Dry under the sample cleaned up being placed in loft drier 70 DEG C of conditions, use compressing tablet to be fixed on the specimen holder above resistance heat evaporator room by Si sheet; Before carrying out evaporation, first resistance heat evaporator room is vacuumized, when vacuum tightness is less than or equal to 2.0 × 10
-4during Pa, start evaporation; Evaporation current is progressively added to 80 A, formally starts evaporation; The power of resistance-type thermal evaporation during evaporation is 16 ~ 19 kW, and vaporator rate remains on 18-24 nm/min, and evaporation time is 15-18 min.
2. single-phase Mg according to claim 1
2the preparation technology of Si semiconductor film, is characterized in that: prepared single-phase Mg on a si substrate
2si semiconductor film, the Mg namely prepared on a si substrate
2not containing MgO or Mg crystal grain phase material in Si semiconductor film.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210455881.7A CN102925866B (en) | 2012-11-14 | 2012-11-14 | Preparation technology for single-phase Mg2Si semiconductor film |
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|---|---|---|---|
| CN201210455881.7A CN102925866B (en) | 2012-11-14 | 2012-11-14 | Preparation technology for single-phase Mg2Si semiconductor film |
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| Publication Number | Publication Date |
|---|---|
| CN102925866A CN102925866A (en) | 2013-02-13 |
| CN102925866B true CN102925866B (en) | 2015-03-11 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105441877B (en) * | 2015-12-10 | 2018-02-23 | 贵州大学 | The technique that resistance-type thermal evaporation prepares ferrimagnet Fe3Si films |
| CN105483617A (en) * | 2015-12-29 | 2016-04-13 | 贵州大学 | Method for preparing Mg2Si film on non-silicon substrate |
| CN109825803A (en) * | 2019-03-05 | 2019-05-31 | 贵州大学 | Environment-friendly semiconductor material Mg2The preparation method of Ge film |
| CN110373636B (en) * | 2019-09-02 | 2022-04-12 | 西安邮电大学 | Preparation method of molybdenum silicide transition metal compound film material |
| CN112802957B (en) * | 2021-02-01 | 2023-04-07 | 河南理工大学 | Preparation device and preparation method of porous silicon and magnesium silicide composite material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798674A (en) * | 2010-04-15 | 2010-08-11 | 贵州大学 | Process for preparing environment-friendly semiconductor material Mg2Si film by electron beam evaporation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798674A (en) * | 2010-04-15 | 2010-08-11 | 贵州大学 | Process for preparing environment-friendly semiconductor material Mg2Si film by electron beam evaporation method |
Non-Patent Citations (1)
| Title |
|---|
| 环境友好半导体Mg2Si薄膜的研究进展;赵珂杰等;《中国光学与应用光学》;20101031;第3卷(第5期);446-451页 * |
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Granted publication date: 20150311 Termination date: 20171114 |