CN1622302A - Three buffer layer method for preparing high quality zinc oxide monocrystalline film - Google Patents
Three buffer layer method for preparing high quality zinc oxide monocrystalline film Download PDFInfo
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- CN1622302A CN1622302A CNA2004100863252A CN200410086325A CN1622302A CN 1622302 A CN1622302 A CN 1622302A CN A2004100863252 A CNA2004100863252 A CN A2004100863252A CN 200410086325 A CN200410086325 A CN 200410086325A CN 1622302 A CN1622302 A CN 1622302A
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Abstract
The present invention discloses method of preparing high quality monocrystal ZnO film. The preparation method has the steps of pre-treating the surface of sapphire to correct and control the atom structure of sapphire substrate for the single polarity and single domain growth of ZnO film; and subsequent three buffering layer process comprising first sapphire nitriding to form super-thin monopolar AlN layer on the surface of sapphire, then depositing 3-6 nm thick island MgO layer and 10-20 nm thick low temperature ZnO layer successively and final depositing high temperature epitaxial ZnO layer to release the mismatching strain fully and to obtain high quality ZnO film with atom level smoothness. The three buffering layer process is superior to available two-step growth process, and the prepared film has RMS roughness within 1 nm and can meet the requirement of making high performance photoelectronic device.
Description
Technical field
The present invention relates to a kind of method for preparing wide bandgap semiconductor zinc oxide (ZnO) monocrystal thin films, thus especially on Sapphire Substrate preparation eliminate the method that strain that Macrolattice mismatch caused obtains high-quality atomically smooth monocrystal thin films during zinc-oxide film.
Background technology
ZnO has multiple superior function, has a wide range of applications at aspects such as nesa coating, surface acoustic wave device and piezoelectric ceramic.ZnO also is an a kind of direct transition type II-VI family semiconductor, and the room temperature energy gap is 3.37eV.Because its very high free exciton binding energy (60meV), ZnO has become another important semiconductor material with wide forbidden band behind gallium nitride (GaN), aspect the low threshold value of preparation, the high efficiency short-wavelength light electronic device very wide application prospect is being arranged.The preparation of high-quality ZnO epitaxial film is the basic point that realizes its device application.And at the ZnO/Al with enormous industrial using value
2O
3Preparation high-quality ZnO epitaxial film has very big challenge in the extension system.About the same with the epitaxial growth of GaN, above-mentioned system need solve problems such as the thin film strain that big mismatch heterostructure system brought is big, defect concentration height equally.
The epitaxy technology employing of existing ZnO film has developed quite ripe GaN thin film epitaxy technology (being the two step method technology) and has obtained progress to a certain degree.But before the growing ZnO epitaxial layer, introduce the strain that ZnO low temperature buffer layer part relaxation causes owing to the big mismatch of lattice.But because oxide and nitride exist very big difference in many aspects, compare with GaN, the preparation ZnO film exists, and the saturated vapour pressure of Zn is big, thereby little its migration length that causes of the coefficient of viscosity is short, and very easily shortcoming such as island growth is difficult to fully discharge misfit strain.At characteristics and the Sapphire Substrate surface atom architectural characteristic of ZnO self, develop technology convenient and practical and that can address the above problem simultaneously, seem very urgent.Our result of study shows, the sapphire nitriding process can solve ZnO directly the grow easy generation rotation farmland that is caused and the farmland problem of turning one's coat on sapphire, but because aluminium nitride (AlN) thin layer that nitrogenize generated does not have relaxation, do not play the effect that reduces lattice mismatch, thereby limited the further raising of ZnO epitaxial film quality.
Summary of the invention
The purpose of this invention is to provide a kind of new method that on Sapphire Substrate, prepares high quality zinc oxide monocrystalline film, this method is by adopting AlN, MgO and ZnO three buffer layer technology, can eliminate lattice mismatch strain, rotation farmland and the farmland of turning one's coat in the ZnO monocrystal thin films effectively, have atomically smooth high quality zinc oxide monocrystalline film thereby grow.
The objective of the invention is to realize by the following technical solutions:
1. preliminary treatment is carried out on the Sapphire Substrate surface, revised and control the atomic structure of Sapphire Substrate, to realize the unipolarity growth of ZnO film;
2. adopt the three buffer layer legal system to be equipped with zinc-oxide film, promptly at first utilize the sapphire nitriding to form aluminium nitride superthin layer (AlN) on the surface, deposition of magnesium island layer and zinc oxide cryosphere then, on the zinc oxide cryosphere, deposit high-temperature oxydation zinc epitaxial loayer again, realize the abundant release of misfit strain, obtain the atomically smooth high-quality zinc oxide film of single polarity.
Further, described Sapphire Substrate surface preparation is the technology that obtains single oxygen terminal surface, it is characterized in that: under 100 ~ 300 ℃, carry out oxygen plasma treatment, underlayer temperature is 100 ~ 300 ℃, radio-frequency power is 300 ~ 450W, oxygen flow is 1 ~ 3sccm, to obtain the Sapphire Substrate of oxygen terminal surface.
Further, described sapphire nitriding is the underlayer nitriding treatment process that obtains aluminium nitride (AlN) superthin layer, it is characterized in that carrying out nitrogen plasma treatment to obtain aluminium nitride (AlN) superthin layer under 100 ~ 300 ℃ of underlayer temperatures, under 300 ~ 450W radio-frequency power and nitrogen flow.
Further, described three buffer layer legal system is equipped with the method for zinc oxide monocrystalline film, it is characterized in that on aluminium nitride (AlN) superthin layer that the sapphire nitriding forms, deposition of magnesium island layer and zinc oxide cryosphere successively are at last at 580 ~ 700 ℃ of high-temperature oxydation zinc epitaxial loayers of growth 500 ~ 1500nm down.
Further, described magnesium oxide island layer is 3 ~ 6nm, and the zinc oxide cryosphere is 10 ~ 20nm.
A kind of three buffer layer legal system is equipped with the method for oxygen polarity zinc oxide monocrystalline film, comprises the steps:
1) molybdenum is plated at the Sapphire Substrate back side, and carry out chemical polishing and handle, the Sapphire Substrate after will cleaning then imports conventional radio frequency plasma accessory molecule beam epitaxy growing system;
2) carry out 20 ~ 40 minutes radio frequency oxygen plasma treatment under 100 ~ 300 ℃ of low temperature, radio-frequency power is 300 ~ 450W, and oxygen flow is 1 ~ 3sccm, to obtain the Sapphire Substrate of oxygen terminal surface;
3) under 100 ~ 300 ℃ of low temperature Sapphire Substrate is carried out nitrogenize, obtain aluminium nitride (AlN) superthin layer, radio frequency nitrogen plasma irradiation method is adopted in nitrogenize, and used radio-frequency power is 400 ~ 500W, nitrogen flow 2 ~ 3.5sccm, and the processing time is 30 ~ 90 minutes;
4) magnesium oxide buffering layer that is 3 ~ 6nm at 350 ~ 450 ℃ of following growth thickness, and under 700 ~ 900 ℃ of temperature, oxygen atmosphere, anneal; Annealing time is 10 ~ 30 minutes;
5) the zinc oxide cryosphere that is 10 ~ 20nm at 350 ~ 450 ℃ of following growth thickness; And under 700 ~ 900 ℃ of temperature, oxygen atmosphere, anneal; Annealing time is 10 ~ 30 minutes;
6) 580 ~ 700 ℃ of growths of carrying out epitaxial loayer; Oxygen, zinc line are adjusted near stoichiometric(al) the scope of rich slightly zinc in the time of will growing by the temperature of rising or reduction zinc diffusion furnace; Promptly adjust zinc oxygen than between 1 ~ 1.5; Behind the zinc-oxide film growth ending, under 700 ~ 900 ℃ of temperature, oxygen atmosphere, anneal; Annealing time is 10 ~ 30 minutes.
Further, it is characterized in that the described radio frequency oxygen plasma treatment time is 25 ~ 35 minutes.
The three buffer layer method of the preparation ZnO film that we propose, be after carrying out Sapphire Substrate nitrogenize acquisition AlN superthin layer, low temperature depositing MgO, ZnO resilient coating successively again, deposit high-temperature oxydation zinc epitaxial loayer then, its objective is that introducing AlN, MgO on known two one-step growth methods progressively eliminates between sapphire and the zinc oxide lattice mismatch up to 18.3% as template, allow the strain that causes by the big mismatch of lattice fully discharge, thereby when having overcome two one-step growth legal systems and being equipped with ZnO film, the deficiency that thin film strain can't be eliminated fully.RHEED home position observation and high-resolution-ration transmission electric-lens test result show that the AlN superthin layer that forms after the nitrogenize has very big strain, do not form the lattice of oneself, though this layer can play important effect aspect the rotation farmland eliminating, and be less to reducing the lattice mismatch role.We find the complete soon relaxation of the MgO that grows and form island layer, thereby have reduced the lattice mismatch between ZnO and the Sapphire Substrate very effectively on nitration case.
In addition; we find that also ZnO directly grows on the sapphire after the nitrogenize; its nitration case is easy to oxidizedly fall; that the thickness of AlN thin layer becomes is very little (~ 1nm); and after increasing the MgO resilient coating; be used for the stronger ionic bond effect between Mg and the O, make that the AlN thin layer is well protected, its thickness reaches about 3nm.
Test result by atomic force microscope (AFM) shows: the RMS roughness of utilizing the ZnO film that the present invention prepares all below 1nm, satisfies the requirement of making the high-performance optical electronic device fully.
Description of drawings
Fig. 1 is the concise and to the point program and the sample structure of preparation ZnO sample on the Sapphire Substrate.
Fig. 2 is a preparation ZnO film process chart on the Sapphire Substrate;
The home position observation of the reflection high energy electron diffraction pattern when Fig. 3 is the embodiment of the invention 1 preparation oxygen polarity ZnO monocrystal thin films is figure as a result;
Fig. 4 is the atomic force microscope figure on the prepared oxygen polarity ZnO monocrystal thin films surface of the embodiment of the invention 1;
Fig. 5 for the high-resolution-ration transmission electric-lens cross section picture of the prepared oxygen polarity ZnO monocrystal thin films sample of the embodiment of the invention 1 and with the result's who only adopts nitriding process to obtain contrast.
The present invention is described in detail below in conjunction with preparation method of the present invention and accompanying drawing.
Embodiment
Embodiment 1 three buffer layer method prepares high-quality oxygen polarity ZnO monocrystal thin films on sapphire
The present invention as shown in Figure 1 prepares the concise and to the point program and the sample structure of ZnO sample, and detailed process flow figure of the present invention as shown in Figure 2, and the three buffer layer method prepares high-quality oxygen polarity ZnO monocrystal thin films on Sapphire Substrate concrete steps are as follows:
1. commercially available Sapphire Substrate adopts magnetically controlled sputter method to carry out back side plating molybdenum and chemical polishing is handled, and the Sapphire Substrate after will cleaning then imports conventional radio frequency plasma accessory molecule beam epitaxy growing system.2 * 10
-10In the base vacuum about mBar, be heated to 200 ℃ and carry out 30 minutes oxygen RF plasma processing, with the clean surface, and the Sapphire Substrate of formation oxygen terminal surface.During oxygen plasma treatment, radio-frequency power is 400W, and oxygen flow is 3sccm.Selecting the purpose of low temperature is the desorption that prevents surperficial oxygen atom.
2. when underlayer temperature is 300 ℃, Sapphire Substrate is carried out sufficient nitrogenize, obtain the AlN superthin layer.Radio frequency nitrogen plasma irradiation method is adopted in nitrogenize, and used radio-frequency power is 480W, nitrogen flow 3sccm, and the processing time is 60 minutes.
3. be MgO resilient coating about 3nm at 450 ℃ of following growth thickness.And under being 750 ℃, oxygen atmosphere, temperature anneals; Annealing time is 20 minutes;
4. be ZnO layer about 15nm at 400 ℃ of following growth thickness; And under being 750 ℃, oxygen atmosphere, temperature anneals; Annealing time is 10 minutes.
5. 650 ℃ of growths of carrying out the ZnO epitaxial loayer; Zinc, oxygen line are adjusted near stoichiometric(al) the scope of rich slightly zinc in the time of will growing by the temperature of rising or reduction zinc diffusion furnace, promptly adjust zinc oxygen than between 1 ~ 1.5; Behind the ZnO film growth ending, under being 750 °, oxygen atmosphere, temperature anneals; Annealing time is 30 minutes.
In above-mentioned preparation thin-film process, we utilize the reflection high energy electron diffraction instrument that sample is carried out home position observation, its result as shown in Figure 3, wherein (a) is the Sapphire Substrate surface, (b) be Sapphire Substrate surface after the nitrogenize, (c) be the MgO buffer-layer surface, (d) for having 3 * 3 ZnO epi-layer surface of structure again.The result shows that sapphire surface has formed single domain AlN superthin layer by behind the above-mentioned the 2nd nitriding process that goes on foot, and its strain discharges as yet.And the MgO film of deposition has formed three-dimensional island layer subsequently, and misfit strain has obtained abundant release, and the lattice size that is reflected from the RHEED pattern is decreased to about 9% with the mismatch of ZnO.In addition, shown clear sharp keen 3 * 3 structures again, shown that this film is high-quality single oxygen polarity ZnO film in the ZnO epi-layer surface.Fig. 3 also shows by the three buffer layer growth technique simultaneously can obtain single farmland monocrystal thin films, has eliminated the rotation farmland fully and has turned one's coat the farmland.Figure 4 shows that the atomic force microscope figure of this sample surfaces, the clear demonstration highly is the growth step of 0.52nm among the figure, show by the three buffer layer method, the strain of ZnO epitaxial loayer obtains relaxation, thereby realized the two-dimensional growth pattern, obtain the surface of atomically flating, satisfied the requirement of making the high-performance optical electronic device fully.Figure 5 shows that this sample high-resolution-ration transmission electric-lens the cross section picture and with the contrast of the sample that only adopts nitriding process and obtained; show among the figure that MgO is a cube phase; this layer not only greatly reduces the lattice mismatch of ZnO extension; simultaneously also protected nitration case to avoid oxidation effectively, made the thickness of AlN bring up to 3nm from 1nm.
Claims (8)
1. method for preparing zinc oxide monocrystalline film, its step is as follows:
1. preliminary treatment is carried out on the Sapphire Substrate surface, revised and control the atomic structure of Sapphire Substrate, to realize the unipolarity growth of zinc-oxide film;
2. adopt the three buffer layer legal system to be equipped with zinc-oxide film, promptly at first utilize the sapphire nitriding to form unipolarity aluminium nitride superthin layer on the surface, deposition of magnesium island layer and zinc oxide cryosphere successively then, deposit high-temperature oxydation zinc epitaxial loayer at last, realize the abundant release of misfit strain, obtain the atomically smooth high-quality zinc oxide film of single polarity.
2. the method for preparing zinc oxide monocrystalline film as claimed in claim 1, described Sapphire Substrate surface preparation is the technology that obtains single oxygen terminal surface, it is characterized in that: under 100 ~ 300 ℃, carry out oxygen plasma treatment, underlayer temperature is 100 ~ 300 ℃, radio-frequency power is 300 ~ 450W, oxygen flow is 1 ~ 3sccm, to obtain the Sapphire Substrate of oxygen terminal surface.
3. the method for preparing zinc oxide monocrystalline film as claimed in claim 1, described sapphire nitriding is the underlayer nitriding treatment process that obtains the aluminium nitride superthin layer, it is characterized in that carrying out nitrogen plasma treatment to obtain the aluminium nitride superthin layer under 100 ~ 300 ℃ of underlayer temperatures, under 300 ~ 450W radio-frequency power and nitrogen flow.
4. the method for preparing zinc oxide monocrystalline film as claimed in claim 1, described magnesium oxide island layer is 3 ~ 6nm, the zinc oxide cryosphere is 10 ~ 20nm.
5. the method for preparing zinc oxide monocrystalline film as claimed in claim 1, the method that is equipped with zinc oxide monocrystalline film by the three buffer layer legal system, it is characterized in that adopting successively aluminium nitride superthin layer, magnesium oxide island layer and zinc oxide cryosphere as resilient coating, last depositing zinc oxide epitaxial loayer.
6. the method for preparing zinc oxide monocrystalline film as claimed in claim 5, it is characterized in that on the aluminium nitride superthin layer that the sapphire nitriding forms, deposition of magnesium island layer and zinc oxide cryosphere successively are at last at 580 ~ 700 ℃ of high-temperature oxydation zinc epitaxial loayers of growth 500 ~ 1500nm down.
7. a three buffer layer legal system is equipped with the method for oxygen polarity zinc oxide monocrystalline film, comprises the steps:
1) molybdenum is plated at the Sapphire Substrate back side, and carry out chemical polishing and handle, the Sapphire Substrate after will cleaning then imports conventional radio frequency plasma accessory molecule beam epitaxy growing system;
2) carry out 20 ~ 40 minutes radio frequency oxygen plasma treatment under 100 ~ 300 ℃ of low temperature, radio-frequency power is 300 ~ 450W, and oxygen flow is 1 ~ 3sccm, to obtain the Sapphire Substrate of oxygen terminal surface;
3) under 100 ~ 300 ℃ of low temperature Sapphire Substrate is carried out nitrogenize, obtain the aluminium nitride superthin layer, radio frequency nitrogen plasma irradiation method is adopted in nitrogenize, and used radio-frequency power is 400 ~ 500W, nitrogen flow 2 ~ 3.5sccm, and the processing time is 60 ~ 120 minutes;
4) magnesium oxide buffering layer that is 3 ~ 6nm at 350 ~ 450 ℃ of following growth thickness, and under 700 ~ 900 ℃ of temperature, oxygen atmosphere, anneal; Annealing time is 10 ~ 30 minutes;
5) the zinc oxide cryosphere that is 10 ~ 20nm at 350 ~ 450 ℃ of following growth thickness; And under 700 ~ 900 ℃ of temperature, oxygen atmosphere, anneal; Annealing time is 10 ~ 30 minutes;
6) 580 ~ 700 ℃ of growths of carrying out high-temperature oxydation zinc epitaxial loayer; Behind the zinc-oxide film growth ending, under 700 ~ 900 ℃ of temperature, oxygen atmosphere, anneal; Annealing time is 10 ~ 30 minutes.
8. three buffer layer legal system as claimed in claim 7 is equipped with the method for oxygen polarity zinc oxide monocrystalline film, it is characterized in that the described radio frequency oxygen plasma treatment time is 25 ~ 35 minutes.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422394C (en) * | 2006-03-20 | 2008-10-01 | 中国科学院物理研究所 | Method for preparing high-quality ZnO single-crystal film on si (111) substrate |
| CN100545314C (en) * | 2005-12-14 | 2009-09-30 | 中国科学院物理研究所 | Be used to prepare the in-situ treatment method of sapphire substrate of high-quality zinc oxide film |
| CN103132144A (en) * | 2011-11-23 | 2013-06-05 | 中国科学院物理研究所 | Method for preparing Cu2O film |
| CN103811354A (en) * | 2014-01-26 | 2014-05-21 | 中山大学 | Method of improving crystalline quality of heteroepitaxy layer |
| CN104790033A (en) * | 2015-04-03 | 2015-07-22 | 南京大学 | Method for growing high-quality ZnO thin-film material on ZnO single-crystal substrate at low temperature |
| CN105742158A (en) * | 2016-02-15 | 2016-07-06 | 厦门大学 | Method for growing zinc oxide film on magnesium oxide substrate |
| CN110634972A (en) * | 2019-09-30 | 2019-12-31 | 东北财经大学 | Cuprous oxide/zinc-copper oxide/zinc oxide device with magnesium nitride shell |
| CN117637442A (en) * | 2023-12-08 | 2024-03-01 | 松山湖材料实验室 | Ultrathin aluminum nitride single crystal composite substrate, preparation method thereof and ultraviolet light-emitting device |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3423631B2 (en) * | 1998-02-05 | 2003-07-07 | キヤノン株式会社 | Method for forming zinc oxide thin film, method for manufacturing semiconductor element substrate using the same, and method for manufacturing photovoltaic element |
| JP4647131B2 (en) * | 2001-05-08 | 2011-03-09 | 独立行政法人科学技術振興機構 | Method for forming thin film crystals |
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Cited By (9)
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| CN100545314C (en) * | 2005-12-14 | 2009-09-30 | 中国科学院物理研究所 | Be used to prepare the in-situ treatment method of sapphire substrate of high-quality zinc oxide film |
| CN100422394C (en) * | 2006-03-20 | 2008-10-01 | 中国科学院物理研究所 | Method for preparing high-quality ZnO single-crystal film on si (111) substrate |
| CN103132144A (en) * | 2011-11-23 | 2013-06-05 | 中国科学院物理研究所 | Method for preparing Cu2O film |
| CN103811354A (en) * | 2014-01-26 | 2014-05-21 | 中山大学 | Method of improving crystalline quality of heteroepitaxy layer |
| CN104790033A (en) * | 2015-04-03 | 2015-07-22 | 南京大学 | Method for growing high-quality ZnO thin-film material on ZnO single-crystal substrate at low temperature |
| CN105742158A (en) * | 2016-02-15 | 2016-07-06 | 厦门大学 | Method for growing zinc oxide film on magnesium oxide substrate |
| CN105742158B (en) * | 2016-02-15 | 2018-10-09 | 厦门大学 | A kind of method of magnesia substrate growth zinc-oxide film |
| CN110634972A (en) * | 2019-09-30 | 2019-12-31 | 东北财经大学 | Cuprous oxide/zinc-copper oxide/zinc oxide device with magnesium nitride shell |
| CN117637442A (en) * | 2023-12-08 | 2024-03-01 | 松山湖材料实验室 | Ultrathin aluminum nitride single crystal composite substrate, preparation method thereof and ultraviolet light-emitting device |
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