CN101381891A - Method for preparing MgZnO single crystal film - Google Patents
Method for preparing MgZnO single crystal film Download PDFInfo
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- CN101381891A CN101381891A CNA2008102245296A CN200810224529A CN101381891A CN 101381891 A CN101381891 A CN 101381891A CN A2008102245296 A CNA2008102245296 A CN A2008102245296A CN 200810224529 A CN200810224529 A CN 200810224529A CN 101381891 A CN101381891 A CN 101381891A
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Abstract
The invention discloses a method for preparing an MgZnO single crystal film. In the method, a MgZnO buffer layer with middle Mg component is utilized to effectively alleviate the influence generated due to the lattice distortion brought by the Mg-O bond with strong ionicity, thereby facilitating the following growth of a MgZnO film with high Mg component. By utilizing the method, the invention has the advantages of accurately controlling the Mg component in the MgZnO alloy film, solving the difficult problem of the phase separation easily occured during the growth of the MgZnO alloy film and further obtaining the high-quality alloy film with wide forbidden band and a matching structure; moreover, the preparation method also has excellent repeatability and controllability, and can be applied to the preparation of high-performance MgZnO-based photoelectron and microelectron devices.
Description
Technical field
The present invention relates to semiconductor microactuator electronics, photoelectron material technical field, especially a kind of method for preparing the MgZnO monocrystal thin films.
Background technology
As one of semi-conductive key foundation material of the third generation, ZnO has very superior photoelectric properties, its free exciton energy gap is that 3.37eV, free exciton bound energy are 60meV, become another important semiconductor material with wide forbidden band after GaN (the free exciton bound energy is 25meV), very wide application prospect has been arranged in low threshold value, high efficiency short-wavelength light field of electronic devices.Recently, along with going deep into day by day and the adulterated preliminary realization of its p type that photoelectron, the microelectronics aspect of performance of zno-based MgZnO alloy material are studied, it directly applies to microelectronics, opto-electronic device such as field effect transistor, ultraviolet light-emitting diode and laser diode has become one of potential application that is expected in the zno-based material.
In the various application of photoelectric semiconductor material, photodiode and laser diode are important component parts in the modern semiconductors industry, and boundless market outlook are arranged.Along with the application of the non-equilibrium growing technologies of hi-tech such as molecular beam epitaxy (MBE) and chemical vapor deposition (CVD), the red laser of GaAs based Multiple Quantum Well heterojunction structure obtained using widely in the eighties in last century.More short wavelength laser (for example green glow, royal purple optical band) succeed in developing and commercialization will play huge pushing effect to the development of information industry.For wide bandgap semiconductor Zinc oxide-base material, its huge free exciton bound energy makes that exciton can be in room temperature (26meV) to such an extent as to the existence of higher temperature.Nearest studies show that, by inelastical scattering mechanism between biexction, can make that the threshold value of the stimulated radiation of ZnO reduces greatly under the room temperature.For the MgZnO alloy firm of wurtzite phase, its excitonic luminescence efficient even more taller than ZnO, and show excellently more in the hot operation zone.Secondly, for the ZnO/MgZnO system, the intrinsic polarized electric field make its at the interface ZnO one side produced two-dimensional electron gas, mobility is greatly improved, and makes this material system aspect the high-frequency high-power field effect transistor wide prospect being arranged.High Mg component MgZnO alloy firm exists stronger polarized electric field, therefore the electronics in the quantum well is had stronger restriction, thereby can increase substantially device performance.
Wurtzite phase MgZnO alloy firm be by salt mine phase MgO and wurtzite mutually the ZnO alloy form.Owing to the greatest differences on two kinds of material structures, the maximum solid solution degree of MgO in ZnO is 0.05 under equilibrium conditions.A large amount of experiments show: even under nonequilibrium growing technology, the single wurtzite phase MgZnO film of high Mg component also is to be difficult to obtain, and main difficulty is that being separated appears in high Mg component growth for Thin Film extremely easily.
Therefore, high Mg component MgZnO film and corresponding epitaxial structure that exploitation can be applicable to ultraviolet light-emitting diode, ultraviolet laser diode and field effect transistor are the bases of realizing a series of device application, play a part very important to the development of Zinc oxide based semiconductor industry.
Summary of the invention
Problem at the prior art existence, the object of the present invention is to provide a kind of method of on the ZnO template, making high Mg component MgZnO thin-film material, can accurately control the ratio of component of Mg, Zn in the MgZnO ternary alloy film, overcome MgZnO ternary alloy film and be prone to a difficult problem that is separated, thereby obtain the alloy firm of high Mg component, and this method can guarantee that experiment has good repeatability.
For achieving the above object, a kind of method for preparing the MgZnO monocrystal thin films of the present invention is specially:
1) adopts molecular beam epitaxial method, the zinc oxide template is imported the growth room, under ultrahigh vacuum(HHV) (UHV) condition, the zinc oxide template is warming up under 500 ℃～900 ℃ high temperature heat-treats, at 300 ℃～700 ℃ substrate surface is carried out active-oxygen plasma then and handle;
2) under 350 ℃～650 ℃ temperature condition, the zinc oxide template is carried out the epitaxy of medium Mg component MgZnO buffer layer;
3) under 350 ℃～650 ℃ temperature condition, the zinc oxide template is carried out the epitaxy of high Mg component MgZnO layer.
Further, zinc-oxide film or block that described zinc oxide template is single terminal surface, i.e. zinc polarity zinc-oxide film or block, oxygen polarity zinc-oxide film or block and non-polar plane zinc-oxide film or block; The non-polar plane of zinc oxide comprises ZnO (10-10) face (being the m face) and ZnO (11-20) face (being a face).
Further, described active oxygen refers to the oxygen that comprises oxygen plasma or ozone.
Further, the component of Mg is 10%～30% in the described medium Mg component MgZnO buffer layer.
Further, described MgZnO buffer layer is a wurtzite structure.
Further, the component of Mg is 30%～50% in the described high Mg component MgZnO layer.
A kind of method for preparing the MgZnO monocrystal thin films of the present invention, by present method make medium Mg component MgZnO buffer layer effectively relaxation the influence that lattice distortion produced that brings of strong ionic Mg-O key, thereby help follow-up high Mg component MgZnO growth for Thin Film, suppressed the formation that is separated, thereby obtain the alloy firm of high Mg component, and this method can guarantee that experiment has good repeatability
Description of drawings
Fig. 1 prepares the process flow sheet of high Mg component MgZnO monocrystal thin films on the ZnO template for the present invention;
Fig. 2 be among the embodiment 1 the Mg component up to the RHEED in-situ observation figure in 49% the wurtzite phase MgZnO monocrystal thin films process of growth.
Fig. 3 be among the embodiment 1 the Mg component up to the XRD test result of 49% wurtzite phase MgZnO monocrystal thin films.
Fig. 4 be among the embodiment 1 the Mg component up to the reflectance spectrum of 49% wurtzite phase MgZnO monocrystal thin films.
Fig. 5 be among the embodiment 2 the Mg component up to the XRD test result of 47% wurtzite phase MgZnO monocrystal thin films.
Embodiment
On the process for sapphire-based zinc-oxide film, make the method for Mg component up to 49% wurtzite phase MgZnO monocrystal thin films:
Process flow sheet of the present invention as shown in Figure 1, utilization prepares the method for zinc polarity zinc-oxide film on Sapphire Substrate, obtain the zinc oxide template, further utilize and monitor the metal source beam flow changing method in the active gas environment in real time, Mg, Zn line have been carried out accurate control, thereby prepared the Mg component up to 49% wurtzite phase MgZnO monocrystal thin films, concrete steps are:
1) adopts molecular beam epitaxial method, the zinc oxide template for preparing on the Sapphire Substrate is imported the growth room, carry out pre-treatment then, promptly under ultrahigh vacuum(HHV) (UHV) condition, the zinc oxide template is warming up to carries out thermal treatment in 30 minutes under 750 ℃ of high temperature, at 500 ℃ substrate surface is carried out 30 minutes active-oxygen plasmas then and handle;
2) underlayer temperature carries out the growth of the medium Mg component of Zn polarity MgZnO buffer layer under 450 ℃ of conditions, and the line of Mg is 1.2 * 10
14Atoms/cm
2S, the line of Zn are 2.5 * 10
14Atoms/cm
2S, oxygen radio-frequency plasma power is 340W, oxygen flow is 2.6sccm;
3) underlayer temperature is under 450 ℃ of conditions, the high Mg component of epitaxy MgZnO film, and the line of Mg is 1.8 * 10
14Atoms/cm
2S, the line of Zn are 2.5 * 10
14Atoms/cm
2S, oxygen radio-frequency plasma power is 340W, oxygen flow is 2.6sccm.
Fig. 2 is that the Mg component of the embodiment of the invention 1 manufacturing is up to the RHEED in-situ observation figure in 49% the wurtzite phase MgZnO monocrystal thin films process of growth.Wherein, Fig. 2 (a) is a wurtzite phase ZnO buffer layer, and bright and sharp point-like striped shows: through pre-treatment, zinc oxide surface cleans more, and the arrangement of surface atom layer complete sum more is orderly, for epitaxy provides a good template; Fig. 2 (b) is the mutually medium Mg component of a wurtzite MgZnO buffer layer, and the electron diffraction striped shows that its structure is single wurtzite structure; Fig. 2 (c) is the MgZnO epitaxial film, and thin sharp diffraction spot shows that high Mg component MgZnO epitaxial film not only inherited the wurtzite structure of ZnO buffer layer, and because the introducing membrane stress of MgZnO buffer layer obtains good relaxation, has higher quality.
Fig. 3 is the XRD test result of the Mg component of the embodiment of the invention 1 manufacturing up to 49% wurtzite phase MgZnO monocrystal thin films; Wherein the peak position of ZnO is 34.41 degree, and the MgZnO peak position is 34.61 degree, and the sapphire peak position is 41.7 degree, does not have other structure peak positions, and the prepared MgZnO film of this method is single wurtzite structure; Illustration corresponds respectively to the peak position (high angle peak position, 34.68 degree) of medium Mg component MgZnO buffer layer (low angle peak position) and high Mg component epitaxial film for the MgZnO peak position is carried out bimodal match; From the halfwidth of MgZnO epitaxial film peak position, film has higher crystalline quality.
Fig. 4 is the prepared Mg component of the embodiment of the invention 1 up to the reflectance spectrum of 49% wurtzite phase MgZnO monocrystal thin films.Wherein, the peak position of medium Mg component MgZnO buffer layer is 3.72 electron-volts, and corresponding Mg component is 19.4%; The peak position of high Mg component MgZnO is 4.37 electron-volts, and wherein the low strength peak position in the illustration is the diffusion layer of Mg component.
Making the Mg component on silicon-based zinc oxide thin film is the method for 47% wurtzite phase MgZnO monocrystal thin films:
Process flow sheet of the present invention as shown in Figure 1, utilization prepares the zinc polarity zinc-oxide film on Si (111) substrate method obtains the zinc oxide template, further utilize and monitor the metal source beam flow changing method in the active gas environment in real time, Mg, Zn line have been carried out accurate control, thereby prepared the Mg component up to 47% wurtzite phase MgZnO monocrystal thin films, concrete steps are:
1) adopts molecular beam epitaxial method, the zinc oxide template for preparing on Si (111) substrate is imported the growth room, carry out pre-treatment then.Promptly under ultrahigh vacuum(HHV) (UHV) condition, the zinc oxide template is warming up to carries out thermal treatment in 30 minutes under 600 ℃ of high temperature, at 450 ℃ substrate surface is carried out 30 minutes active-oxygen plasmas then and handle;
2) underlayer temperature carries out the growth of the medium Mg component of Zn polarity MgZnO buffer layer under 450 ℃ of conditions, and the line of Mg is 1 * 10
14Atoms/cm
2S, the line of Zn are 2 * 10
14Atoms/cm
2S, oxygen radio-frequency plasma power is 340W, oxygen flow is 2.6sccm;
3) underlayer temperature is under 450 ℃ of conditions, the high Mg component of epitaxy MgZnO film, and the line of Mg is 1.4 * 10
14Atoms/cm
2S, the line of Zn are 2 * 10
14Atoms/cm
2S, oxygen radio-frequency plasma power is 340W, oxygen flow is 2.6sccm.
Fig. 5 is the XRD test result of the Mg component of the embodiment of the invention 2 manufacturings up to 47% wurtzite phase MgZnO monocrystal thin films; Wherein Si (111) peak position is positioned at 28.44 degree, and the peak position of high Mg component MgZnO epitaxial film is 34.67 degree, and corresponding Mg component is 47%, does not have other structure peak positions, and the prepared MgZnO film of this method is single wurtzite structure; Illustration is the bimodal match to the MgZnO peak position, and the low angle peak position is corresponding to medium Mg component MgZnO buffer layer, and corresponding Mg component is 17%; Because the thickness of used zinc oxide template has only several nanometers, its peak position is not presented in the test result of XRD; From the halfwidth of MgZnO epitaxial film peak position, film has higher crystalline quality.
A kind of method for preparing the MgZnO monocrystal thin films of the present invention is utilized medium Mg component MgZnO buffer layer, effectively relaxation the influence that lattice distortion produced that brings of strong ionic Mg-O key, thereby help follow-up high Mg component MgZnO growth for Thin Film.Utilize this method, can accurately control Mg component in the MgZnO alloy firm, overcome and very easily occurred the difficult problem that is separated in the growth of MgZnO alloy firm, thereby can obtain the broad stopband, the high quality alloy firm of structure matching, and this preparation method possesses good repeatability and controllability, can be applied in superior MgZnO base optical electronic of processability and microelectronic device.
Claims (6)
1, a kind of method for preparing the MgZnO monocrystal thin films is specially:
1) adopts molecular beam epitaxial method, the zinc oxide template is imported the growth room, under ultrahigh vacuum(HHV) (UHV) condition, the zinc oxide template is warming up under 500 ℃～900 ℃ high temperature heat-treats, at 300 ℃～700 ℃ substrate surface is carried out active-oxygen plasma then and handle;
2) under 350 ℃～650 ℃ temperature condition, the zinc oxide template is carried out the epitaxy of medium Mg component MgZnO buffer layer;
3) under 350 ℃～650 ℃ temperature condition, the zinc oxide template is carried out the epitaxy of high Mg component MgZnO layer.
2, the method for preparing the MgZnO monocrystal thin films as claimed in claim 1, it is characterized in that, zinc-oxide film or block that described zinc oxide template is single terminal surface, i.e. zinc polarity zinc-oxide film or block, oxygen polarity zinc-oxide film or block and non-polar plane zinc-oxide film or block; The non-polar plane of zinc oxide comprises ZnO (10-10) face (being the m face) and ZnO (11-20) face (being a face).
3, the method for preparing the MgZnO monocrystal thin films as claimed in claim 1 is characterized in that, described active oxygen refers to the oxygen that comprises oxygen plasma or ozone.
4, the method for preparing the MgZnO monocrystal thin films as claimed in claim 1 is characterized in that, the component of Mg is 10%～30% in the described medium Mg component MgZnO buffer layer.
5, the method for preparing the MgZnO monocrystal thin films as claimed in claim 1 is characterized in that, described MgZnO buffer layer is a wurtzite structure.
6, the method for preparing the MgZnO monocrystal thin films as claimed in claim 1 is characterized in that, the component of Mg is 30%～50% in the described high Mg component MgZnO layer.
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Cited By (8)
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|---|---|---|---|---|
| CN102569483A (en) * | 2011-12-19 | 2012-07-11 | 北京交通大学 | MgZnO solar-blind photoresistor and preparation method thereof |
| CN102623521A (en) * | 2011-01-31 | 2012-08-01 | 中国科学院物理研究所 | Method for preparing cuprous oxide film |
| CN102776567A (en) * | 2011-05-10 | 2012-11-14 | 中国科学院物理研究所 | Method for preparing wurtzite phase MxZn1-xO single crystal film on Si substrate |
| CN103204537A (en) * | 2013-02-06 | 2013-07-17 | 内蒙古大学 | Preparation method for nano-material with wurtzite structure |
| CN103972310A (en) * | 2014-04-30 | 2014-08-06 | 中国科学院长春光学精密机械与物理研究所 | Method for manufacturing zinc-oxide-based p-type materials |
| CN103972311A (en) * | 2014-04-30 | 2014-08-06 | 中国科学院长春光学精密机械与物理研究所 | Method for manufacturing zinc-oxide-based p-type materials |
| CN108538970A (en) * | 2018-03-09 | 2018-09-14 | 华灿光电（浙江）有限公司 | A kind of preparation method of light emitting diode |
| CN109637925A (en) * | 2018-12-19 | 2019-04-16 | 中国科学院福建物质结构研究所 | Magnesium zinc oxide film and preparation method thereof |
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| CN1327042C (en) * | 2005-03-28 | 2007-07-18 | 中国科学院半导体研究所 | Method for growing single-crystal zinc oxide film by using zinc oxide buffer layer |
| CN101168837A (en) * | 2006-12-29 | 2008-04-30 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing MgZnO thin film with high content of magnesium |
| CN100494486C (en) * | 2007-05-08 | 2009-06-03 | 中国科学院上海光学精密机械研究所 | Method for developing m-face or a-face ZnO film by metal organic chemical vapour deposition |
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2008
- 2008-10-20 CN CN2008102245296A patent/CN101381891B/en active Active
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| CN102623521A (en) * | 2011-01-31 | 2012-08-01 | 中国科学院物理研究所 | Method for preparing cuprous oxide film |
| CN102776567A (en) * | 2011-05-10 | 2012-11-14 | 中国科学院物理研究所 | Method for preparing wurtzite phase MxZn1-xO single crystal film on Si substrate |
| CN102776567B (en) * | 2011-05-10 | 2015-07-22 | 中国科学院物理研究所 | Method for preparing wurtzite phase MxZn1-xO single crystal film on Si substrate |
| CN102569483A (en) * | 2011-12-19 | 2012-07-11 | 北京交通大学 | MgZnO solar-blind photoresistor and preparation method thereof |
| CN103204537A (en) * | 2013-02-06 | 2013-07-17 | 内蒙古大学 | Preparation method for nano-material with wurtzite structure |
| CN103972310A (en) * | 2014-04-30 | 2014-08-06 | 中国科学院长春光学精密机械与物理研究所 | Method for manufacturing zinc-oxide-based p-type materials |
| CN103972311A (en) * | 2014-04-30 | 2014-08-06 | 中国科学院长春光学精密机械与物理研究所 | Method for manufacturing zinc-oxide-based p-type materials |
| CN103972310B (en) * | 2014-04-30 | 2016-04-27 | 中国科学院长春光学精密机械与物理研究所 | A kind of preparation method of zinc oxide based p type material |
| CN103972311B (en) * | 2014-04-30 | 2016-06-01 | 中国科学院长春光学精密机械与物理研究所 | The preparation method of a kind of Zinc oxide-base p-type material |
| CN108538970A (en) * | 2018-03-09 | 2018-09-14 | 华灿光电（浙江）有限公司 | A kind of preparation method of light emitting diode |
| CN109637925A (en) * | 2018-12-19 | 2019-04-16 | 中国科学院福建物质结构研究所 | Magnesium zinc oxide film and preparation method thereof |
| CN109637925B (en) * | 2018-12-19 | 2021-02-12 | 中国科学院福建物质结构研究所 | Magnesium zinc oxide film and preparation method thereof |
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