CN100575565C - The method for preparing aluminium nitride film at the lithium aluminate crystal wafer surface low-temperature - Google Patents
The method for preparing aluminium nitride film at the lithium aluminate crystal wafer surface low-temperature Download PDFInfo
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- CN100575565C CN100575565C CN200710048012A CN200710048012A CN100575565C CN 100575565 C CN100575565 C CN 100575565C CN 200710048012 A CN200710048012 A CN 200710048012A CN 200710048012 A CN200710048012 A CN 200710048012A CN 100575565 C CN100575565 C CN 100575565C
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- aluminium nitride
- nitride film
- lialo
- lithium aluminate
- wafer surface
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Abstract
A kind of on lithium aluminate crystal wafer low temperature prepare the method for aluminium nitride film, with (100) γ-LiAlO of polishing
2Wafer places and flows or sealing ammonia atmosphere environment, in the temperature range of room temperature to 800 ℃, is incubated 0.1 to 120 hour, to (100) γ-LiAlO
2Wafer surface is carried out nitriding treatment, at (100) γ-LiAlO
2Wafer surface obtains (0001) aluminium nitride film of one deck high C-axis orientation.This surface coverage has (100) γ-LiAlO of (0001) aluminium nitride film
2The surfaceness of wafer obviously reduces, and stability is improved significantly.Nitrogenize (100) γ-LiAlO with the inventive method preparation
2Wafer can be used as substrate and is used for extension and prepares wide bandgap semiconductor film, thick film and functional devices such as GaN, aluminium nitride, InGaN, ZnO.
Description
Technical field
The present invention relates to aluminium nitride film, particularly a kind of method for preparing aluminium nitride film at the lithium aluminate crystal wafer surface low-temperature.
Technical background
Aluminium nitride belongs to direct band-gap semicondictor, and its energy gap is 6.2eV, is important short-wave long light-emitting material, because it has a lot of excellent physical chemistry, paid attention to by people.Aluminium nitride has high breaking down field strength, high heat conductance, high resistivity and high chemical stability, and its thermal expansivity is close with silicon simultaneously, can be used for encapsulation, media isolated and the insulating material of electron device and unicircuit, is particularly suited for the high temperature high-power component.Aluminium nitride also has good piezoelectricity, high acoustic surface wave propagation speed and higher electromechanical coupling factor, is the preferred piezoelectric of GHz level surface acoustic wave (SAW) and bulk wave device (BAW).Wherein, BAW is a kind of technology based on acoustic bulk wave resonance, and the inverse piezoelectric effect by piezoelectric membrane becomes sound wave to form resonance electric energy conversion, and (0001) aluminium nitride can be used to make high performance bulk accoustic wave filter.In addition, the broad-band gap of aluminium nitride also makes it be fit to making and is not subjected to sunlight interferential solar-blind UV detector, such detector can be applicable to comprise that guided missile approaches fields such as system, UV meter measuring device, satellite communications, flame and thermal sensor, its advantage is not to be subjected to sunlight to disturb, and false alarm rate is low, volume is little, manufacturing is simple, easy to use.
Though aluminium nitride has important use to be worth, but aluminum-nitride single crystal also is difficult to growth at present, and the stage that the preparation of aluminium nitride film still is in the equipment complexity, involves great expense, is difficult to industrialization, and the employed method for preparing aluminium nitride film requires substrate is heated to higher temperature usually, and the development need of integrated optical device is carried out film preparation under lower temperature, to avoid the thermal damage to substrate material.Prepared aluminium nitride film under the lower temperature and (seen Journal ofApplied Physics 91 though have to be reported in, 2499 (2002)), but because of its nitrogenize is the extraordinary sapphire wafer of chemical stability, need to add radio-frequency unit and produce plasma body, so preparation cost is still than higher.Therefore, improve the preparation method of aluminium nitride film, under simple processing condition, obtain finer and close, more even, more high purity, aluminium nitride film more cheaply, have great practical value.
On the other hand, lithium aluminate, γ-LiAlO
2Lattice matched substrates material as a kind of epitaxy GaN, InGaN, aluminium nitride, ZnO film has caused people's great attention, but its chemical stability at high temperature can not show a candle to sapphire, cause lithium to pollute to growing environment and epitaxial film easily, this becomes the matter of utmost importance of its development of restriction.
Summary of the invention
The objective of the invention is to overcome above-mentioned prior art problem, a kind of method at lithium aluminate crystal wafer surface preparation aluminium nitride film is provided, at (100) γ-LiAlO
2The method of the aluminium nitride film of wafer surface preparation high C-axis orientation solves the expensive problem of preparation (0001) aluminium nitride film at present.
Technical conceive of the present invention is by low temperature ammonia nitrogenize (100) γ-LiAlO
2Wafer is at (100) γ-LiAlO
2The aluminium nitride film of wafer surface preparation high C-axis orientation obtains (0001) aluminium nitride/(100) γ-LiAlO
2Compound substrate.
Concrete technical solution of the present invention is as follows:
A kind ofly prepare the method for aluminium nitride film, lithium aluminate crystal wafer is placed the container of ammonia atmosphere, the low temperature nitriding treatment is carried out on the lithium aluminate crystal wafer surface, obtain aluminium nitride film on the lithium aluminate surface at the lithium aluminate crystal wafer surface low-temperature.
The concrete steps of the described method for preparing aluminium nitride film at the lithium aluminate crystal wafer surface low-temperature are as follows:
1. with polished lithium aluminate crystal wafer, promptly (100) γ-LiAlO2 wafer places the container of flowing of higher degree or sealing ammonia atmosphere;
2. in the temperature range of room temperature to 800 ℃, be incubated 0.1 to 120 hour, drop to room temperature then, obtain at (100) γ-LiAlO
2Cover (0001) aluminium nitride film wafer on the wafer surface, take out wafer.
Described container is Glass Containers or quartz container or metal vessel.
The air pressure of the ammonia in the described container is 1 normal atmosphere, but is not limited to 1 normal atmosphere, and ammonia purity is greater than 99% in the container.
Technique effect of the present invention:
The present invention is directed to the problem of γ-LiAlO2 wafer poor heat stability in HVPE and MOCVD high-temperature atmosphere and γ-LiAlO2 wafer than the problem that is easier to hydrolysis, by the simple gas nitriding technology of technology, make γ-LiAlO on the lithium aluminate crystal wafer surface at a lower temperature
2Wafer surface evenly covers the stable aluminium nitride film of physical and chemical performance, not only can reduce the preparation cost of aluminium nitride film, and has solved γ-LiAlO
2Wafer under hot conditions, the problem of lithium diffusion (volatilization) and under cold condition than the problem that is easier to hydrolysis, raising γ-LiAlO
2The stability of wafer, thus significant.
The present invention has that but equipment is very simple, energy consumption is low or even the zero even film forming of energy consumption low temperature big area, and is with low cost, be easy to realize advantage such as industrialization.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 gained sample
Fig. 2 is the XRD figure spectrum of embodiment 2 gained samples
Fig. 3 is the XRD figure spectrum of embodiment 3 gained samples
Fig. 4 is the XRD figure spectrum of embodiment 4 gained samples
Fig. 5 is the XRD figure spectrum of embodiment 5 gained samples
Fig. 6 is the XRD figure spectrum of embodiment 6 gained samples
Fig. 7 is the XRD figure spectrum of embodiment 7 gained samples
Fig. 8 is embodiment 7 gained sample aluminium nitride (0002) X-ray diffraction rocking curves
Fig. 9 is the XRD figure spectrum of embodiment 8 gained samples
Figure 10 is the rocking curve of embodiment 8 gained sample aluminium nitride (0002) crystal face X-ray diffractions
Figure 11 is the XRD figure spectrum of embodiment 9 gained samples
Figure 12 is the XRD figure spectrum of embodiment 10 gained samples
Figure 13 is the rocking curve of embodiment 10 gained sample aluminium nitride (0002) crystal face X-ray diffractions
Figure 14 is the XRD figure spectrum of embodiment 11 gained samples
Figure 15 is the rocking curve of embodiment 11 gained sample aluminium nitride (0002) X-ray diffractions
Figure 16 is the XRD figure spectrum of embodiment 12 gained samples
Figure 17 is the rocking curve of embodiment 12 gained sample aluminium nitride (0002) crystal face X-ray diffractions
Figure 18 is the XRD figure spectrum of embodiment 13 gained samples
Figure 19 is the XRD figure spectrum of embodiment 14 gained samples.
Figure 20 is the XRD figure spectrum of embodiment 15 gained samples.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but should not limit protection scope of the present invention with this.
Embodiment 1
With polished (100) γ-LiAlO
2Sample wafer places Glass Containers, can certainly be in silica tube or the metal vessel etc., pours into purity and be 99.9% ammonia in this container, air pressure is 1 normal atmosphere, seals this container, and this container is placed under the room temperature, open the container of this sealing after 72 hours, take out sample.Fig. 1 is the XRD figure spectrum of present embodiment gained sample, and the diffraction peak that is positioned at 34.86 °, 36.46 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002) and γ-LiAlO
2(400), can judge (0001) aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated the high C-axis preferred orientation thus.
In addition, other condition is the same, and ammonia air pressure is at-10 normal atmosphere of 100Pa (need vacuumize container before filling ammonia this moment) in the sealed vessel, perhaps ammonia purity changes between 99%-99.9999%, seals 1 day under the room temperature respectively, 2 days, 5 days, after 30 days, at (100) γ-LiAlO
2The aluminium nitride film that has all occurred (0001) orientation on the wafer surface respectively.
With polished (100) γ-LiAlO
2Sample wafer places on the quartz boat of quartz tube furnace, and an end of silica tube has two inlet mouths to link to each other with nitrogengas cylinder with the ammonia bottle by rubber hose respectively, and another termination rubber hose also inserts this rubber hose in vent gas treatment water.The program that configures heats up to quartz tube furnace, when temperature is raised to 100 ℃ of holding temperatures, begin to feed purity and be 99.9% mobile ammonia, and under this temperature, be incubated 2 hours, the ammonia that flows in this insulating process slowly flows into from tube furnace silica tube one end always, flows into the vent gas treatment water by rubber hose from the silica tube the other end.Insulation stops to feed ammonia after finishing, and furnace temperature is slowly reduced to room temperature.Fig. 2 is the XRD figure spectrum of embodiment 2 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), γ-LiAlO
2(400), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.
In addition, ammonia purity changes the not significantly influence to the result between 99%-99.9999%.
Embodiment 3
150 ℃ of following soaking times are 5 hours, and other condition is with embodiment 2.Fig. 3 is the XRD figure spectrum of embodiment 3 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), γ-LiAlO
2(400), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.
Embodiment 4
200 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Fig. 4 is the XRD figure spectrum of embodiment 4 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.
Embodiment 5
200 ℃ of following soaking times are 3 hours, and other condition is with embodiment 2.Fig. 5 is the XRD figure spectrum of embodiment 5 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 °, 73.19 °, 77.42 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), γ-LiAlO
2(400), aluminium nitride (0004), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.
Embodiment 6
200 ℃ of following soaking times are 5 hours, and other condition is with embodiment 2.Fig. 6 is the XRD figure spectrum of embodiment 6 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), γ-LiAlO
2(400), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.
Embodiment 7
300 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Fig. 7 is the XRD figure spectrum of embodiment 7 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), γ-LiAlO
2(400), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.Fig. 8 is embodiment 7 gained sample aluminium nitride (0002) X-ray diffraction rocking curves, and its full width at half maximum (FWHM) is 1.8 °.
400 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Fig. 9 is the XRD figure spectrum of embodiment 8 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.Figure 10 is the rocking curve of embodiment 8 gained sample aluminium nitride (0002) crystal face X-ray diffractions, and its full width at half maximum (FWHM) is 2.6 °.
Embodiment 9
500 ℃ of following soaking times are 0.1 hour, and other condition is with embodiment 2.Figure 11 is the XRD figure spectrum of embodiment 9 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), γ-LiAlO
2(400), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.
Embodiment 10
500 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Figure 12 is the XRD figure spectrum of embodiment 10 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.Figure 13 is the rocking curve of embodiment 10 gained sample aluminium nitride (0002) crystal face X-ray diffractions, and its full width at half maximum (FWHM) is 1.0 °.
Embodiment 11
600 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Figure 14 is the XRD figure spectrum of embodiment 11 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0001) orientation thus.Figure 15 is the rocking curve of embodiment 11 gained sample aluminium nitride (0002) X-ray diffractions, and its full width at half maximum (FWHM) is 0.2 °.
Embodiment 12
700 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Figure 16 is the XRD figure spectrum of embodiment 12 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0002) orientation thus.Figure 17 is the rocking curve of embodiment 12 gained sample aluminium nitride (0002) crystal face X-ray diffractions, and its full width at half maximum (FWHM) is 0.19 °.
Embodiment 13
800 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Figure 18 is the XRD figure spectrum of embodiment 13 gained samples, and the diffraction peak that is positioned at 34.86 °, 36.46 ° among the figure corresponds respectively to γ-LiAlO
2(200), aluminium nitride (0002), can judge the aluminium nitride film that on the lithium aluminate crystal wafer surface, has generated height (0002) orientation thus.
Embodiment 14
850 ℃ of following soaking times are 1 hour, and other condition is with embodiment 2.Figure 19 is the XRD figure spectrum of embodiment 14 gained samples, and the diffraction peak that is positioned at 34.86 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), (400), can judge thus on the lithium aluminate crystal wafer surface, not generate aluminium nitride film.
850 ℃ of following soaking times are 1 hour, and insulation stops to feed ammonia after finishing, and change into feeding the flowing nitrogen protection, and furnace temperature is reduced to room temperature by setup program, and other condition is with embodiment 2.Figure 20 is the XRD figure spectrum of embodiment 15 gained samples, and the diffraction peak that is positioned at 34.86 °, 73.19 ° among the figure corresponds respectively to γ-LiAlO
2(200), (400), can judge thus on the lithium aluminate crystal wafer surface, not generate aluminium nitride film.
By contrasting via nitride not and finding through atomic force microscope (AFM) photo of the lithium aluminate crystal wafer of nitriding treatment: the surfaceness through lithium aluminate crystal wafer after the ammonia nitrogenize obviously reduces, and the scraggly physical abuse zone that former cause polishing is introduced on the lithium aluminate crystal wafer surface also has been flattened some, and the part wafer surface also presents orderly striated structure.
In addition, γ-LiAlO
2Wafer has weak hydrolysis phenomenon, usually γ-the LiAlO after the chemically machinery polished
2Wafer is exposed in the bigger air of psychromatic ratio, and after the time grown, because hydrolysis, glazed surface can be subjected to certain influence, and this gives γ-LiAlO
2Wafer is preserved has increased difficulty and cost.Nitrogenize rear surface in the various embodiments described above is detected (100) γ-LiAlO that is coated with aluminium nitride film
2Wafer was put into water 5 minutes, took out to dry up the back with the AFM observation, found that the glazed surface roughness does not change, and illustrates that aluminium nitride film has played provide protection.
With (100) γ-LiAlO
2The surface coverage that obtains in wafer and the various embodiments described above has (100) γ-LiAlO of the aluminium nitride film of c axle orientation
2Wafer is put into HVPE or MOCVD atmosphere in the lump, carries out GaN film growth test by the common processing condition of HVPE or MOCVD, and the experimental result of two kinds of wafers of contrast finds that the surface is coated with (100) γ-LiAlO of the aluminium nitride film of c axle orientation
2The thermostability of wafer is largely increased, and shows tangible macroscopic defects and wafer cracking phenomena not to occur.
Claims (3)
1, a kind of method for preparing aluminium nitride film at the lithium aluminate crystal wafer surface low-temperature, it is characterized in that lithium aluminate crystal wafer is placed the container of ammonia atmosphere, the low temperature nitriding treatment is carried out on the lithium aluminate crystal wafer surface, obtain aluminium nitride film on the lithium aluminate surface, its concrete steps are as follows:
1. with polished lithium aluminate crystal wafer, i.e. (100) γ-LiAlO
2Wafer places the container of flowing of higher degree or sealing ammonia atmosphere;
2. in the temperature range of room temperature to 800 ℃, be incubated 0.1 to 120 hour, drop to room temperature then, obtain at (100) γ-LiAlO
2Cover (0001) aluminium nitride film wafer on the wafer surface, take out wafer.
2, according to claim 1ly prepare the method for aluminium nitride film, it is characterized in that described container is Glass Containers or metal vessel at the lithium aluminate crystal wafer surface low-temperature.
3, according to claim 1ly prepare the method for aluminium nitride film at the lithium aluminate crystal wafer surface low-temperature, it is characterized in that the air pressure of the ammonia in the container is 1 normal atmosphere, ammonia purity is greater than 99% in the container.
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| CN101958236B (en) * | 2009-07-20 | 2012-12-19 | 上海半导体照明工程技术研究中心 | Semiconductor substrate and preparation method thereof |
| CN103996756B (en) * | 2014-05-30 | 2017-01-18 | 广州市众拓光电科技有限公司 | Film coating method and application thereof |
| CN108761949B (en) * | 2018-05-29 | 2020-11-10 | 中国科学院上海硅酸盐研究所 | Solid ion conducting layer and solid electrochromic device comprising same |
| CN113308742A (en) * | 2020-12-28 | 2021-08-27 | 中国科学院福建物质结构研究所 | Application of aluminum nitride single crystal material in piezoelectric material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050103257A1 (en) * | 2003-11-13 | 2005-05-19 | Xueping Xu | Large area, uniformly low dislocation density GaN substrate and process for making the same |
| US20070138505A1 (en) * | 2005-12-12 | 2007-06-21 | Kyma Technologies, Inc. | Low defect group III nitride films useful for electronic and optoelectronic devices and methods for making the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050103257A1 (en) * | 2003-11-13 | 2005-05-19 | Xueping Xu | Large area, uniformly low dislocation density GaN substrate and process for making the same |
| US20070138505A1 (en) * | 2005-12-12 | 2007-06-21 | Kyma Technologies, Inc. | Low defect group III nitride films useful for electronic and optoelectronic devices and methods for making the same |
Non-Patent Citations (2)
| Title |
|---|
| Study on the hydrolytic property and thermal stability of LiAlO2substrate. Jun Zou等.Journal of Crystal Growth,Vol.294. 2006 * |
| Y-LiAlO2衬底上生长GaN的研究进展. 黄涛华等.激光与光电子学进展，第43卷第12期. 2006 * |
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