CN102400213A - Method for epitaxially growing alumina single crystal film - Google Patents
Method for epitaxially growing alumina single crystal film Download PDFInfo
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- CN102400213A CN102400213A CN2011103669061A CN201110366906A CN102400213A CN 102400213 A CN102400213 A CN 102400213A CN 2011103669061 A CN2011103669061 A CN 2011103669061A CN 201110366906 A CN201110366906 A CN 201110366906A CN 102400213 A CN102400213 A CN 102400213A
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Abstract
The invention discloses a method for epitaxially growing an alumina single crystal film by adopting a pulsed laser deposition method. The target is a ceramic target obtained by hydraulic forming of alumina powder; and the alumina single crystal film is grown on a sapphire substrate under the laser frequency of 3 to 10 Hz at the temperature of between 450 and 650 DEG C in a growth chamber of a pulsed laser deposition device by using pure O2 as a growth atmosphere and controlling the pressure intensity of the O2 at 0.5 to 5Pa. By the method, epitaxial growth of the alumina single crystal film on the sapphire substrate can be realized. The alumina single crystal film prepared by adopting the method has good repeatability and stability.
Description
Technical field:
The present invention relates to method, the especially method of epitaxy aluminium oxide single crystal film of monocrystal thin films preparation.
Background technology:
Aluminum oxide film has numerous advantages,, the transparency high like good in optical property, physical strength and hardness and good insulating, wear-resisting, against corrosion and unreactiveness etc., extremely people's attention.Have a wide range of applications in many fields such as machinery, microelectronics, optics, chemical industry, medical science.Therefore, the scientific worker just never stopped the research-and-development activity of aluminum oxide film.Originally the preparation of aluminum oxide film is through industrial CVD method, but the CVD sedimentation is very high to temperature requirement, generally surpasses 1000 ℃, has limited the application of deposition of aluminium oxide on the surface of some non-refractories such as carbide substrate.So the continuous research experiment of people attempts in the PVD field, to find a kind of low temperature, high speed sedimentation.Pulsed laser deposition has deposition parameter and is prone to control, is prone to keep advantages such as film film quality consistent with the target composition, growth is good; Have broad application prospects; So far, also do not use pulsed laser deposition epitaxy aluminium oxide single crystal film on sapphire.
Summary of the invention:
The objective of the invention is to realize the epitaxy of aluminium oxide single crystal film, provide a kind of on sapphire the growth method of extension aluminium oxide single crystal film.
The technical scheme that the present invention adopts is:
The method of epitaxy aluminium oxide single crystal film: adopt pulsed laser deposition, comprise the steps:
1) weighing alumina powder, shaped by fluid pressure makes target then;
2) substrate after will cleaning is put into the growth room of pulsed laser deposition device, and the distance between target and the substrate is 4.5～5.5 cm, and growth room's back of the body end vacuum tightness is evacuated to 1 * 10
-4～1 * 10
-3Pa, heated substrate then, making underlayer temperature is 450 ~ 750 ℃, with pure O
2Be growth atmosphere, control O
2Pressure 0.5 ~ 5 Pa, laser frequency is 3 ~ 10 Hz, and laser energy is 250～350 mJ, grows, and the film after the growth is cooled to room temperature with 3～10 ℃/min.
Described substrate is a sapphire.
The purity of said alumina powder is 99.99%.
The present invention is through epitaxy aluminium oxide single crystal film on Sapphire Substrate, and the time of its growth is by required thickness decision.
Compared with prior art, the invention has the advantages that:
The present invention is through epitaxy aluminium oxide single crystal film on Sapphire Substrate, and the time of its growth is by required thickness decision; Can realize the epitaxy of aluminium oxide single crystal film; The aluminium oxide single crystal film of preparation has good repeatability and stable.
Description of drawings:
Fig. 1 is the pulsed laser deposition device synoptic diagram that the inventive method adopts, and among the figure: 1 is laser apparatus; 2 is the growth room; 3 is target; 4 is substrate;
Fig. 2 is x XRD X (XRD) collection of illustrative plates of the aluminium oxide single crystal film of embodiment 2.
Embodiment:
Below in conjunction with accompanying drawing, the present invention is done further explain through embodiment:
Embodiment 1
1) getting purity is 99.99% alumina powder, with powder at high temperature hydraulic pressure to become thickness be 3 mm, diameter is the disk of 50 mm, obtains target.
2) with the sapphire be substrate, put into the growth room of pulsed laser deposition device after substrate surface is cleaned, growth room's back of the body end vacuum tightness is evacuated to 1 * 10
-4Pa, heated substrate then, making underlayer temperature is 450 ℃, is target with the alumina-ceramic target, the distance of adjustment substrate and target is 4.5 cm, with pure O
2Be growth atmosphere, control O
2Pressure 0.5 Pa, laser frequency is 3 Hz, and laser energy is 250 mJ, and the time of growth is 30 min.The growth back obtains aluminium oxide single crystal film with the speed cool to room temperature of 3 ℃/min.
Embodiment 2
1) getting purity is 99.99% alumina powder, with powder at high temperature hydraulic pressure to become thickness be 3 mm, diameter is the disk of 50 mm, obtains target.
2) with the sapphire be substrate, put into the growth room of pulsed laser deposition device after substrate surface is cleaned, growth room's back of the body end vacuum tightness is evacuated to 5 * 10
-4Pa, heated substrate then, making underlayer temperature is 600 ℃, is target with the alumina-ceramic target, the distance of adjustment substrate and target is 5 cm, with pure O
2Be growth atmosphere, control O
2Pressure 2 Pa, laser frequency is 5 Hz, and laser energy is 300 mJ, and the time of growth is 30 min.The growth back obtains aluminium oxide single crystal film with the speed cool to room temperature of 5 ℃/min.
Its x XRD X (XRD) collection of illustrative plates of the aluminium oxide single crystal film that makes is seen Fig. 2.
Embodiment 3
1) getting purity is 99.99% alumina powder, with powder at high temperature hydraulic pressure to become thickness be 3 mm, diameter is the disk of 50 mm, obtains target.
2) with the sapphire be substrate, put into the growth room of pulsed laser deposition device after substrate surface is cleaned, growth room's back of the body end vacuum tightness is evacuated to 1 * 10
-3Pa, heated substrate then, making underlayer temperature is 750 ℃, is target with the alumina-ceramic target, the distance of adjustment substrate and target is 5.5 cm, with pure O
2Be growth atmosphere, control O
2Pressure 5 Pa, laser frequency is 10 Hz, and laser energy is 350 mJ, and the time of growth is 30 min.The growth back obtains aluminium oxide single crystal film with the speed cool to room temperature of 10 ℃/min.
The foregoing description is merely preferred implementation of the present invention, and in addition, the present invention can also have other implementations.Need to prove that under the prerequisite that does not break away from the utility model design, any conspicuous improvement and modification all should fall within protection scope of the present invention.
Claims (3)
1. the method for epitaxy aluminium oxide single crystal film is characterized in that: adopt pulsed laser deposition, comprise the steps:
1) weighing alumina powder, shaped by fluid pressure makes target then;
2) substrate after will cleaning is put into the growth room of pulsed laser deposition device, and the distance between target and the substrate is 4.5～5.5 cm, and growth room's back of the body end vacuum tightness is evacuated to 1 * 10
-4～1 * 10
-3Pa, heated substrate then, making underlayer temperature is 450 ~ 750 ℃, with pure O
2Be growth atmosphere, control O
2Pressure 0.5 ~ 5 Pa, laser frequency is 3 ~ 10 Hz, and laser energy is 250～350 mJ, grows, and the film after the growth is cooled to room temperature with 3～10 ℃/min.
2. the method for epitaxy aluminium oxide single crystal film according to claim 1 is characterized in that: described substrate is a sapphire.
3. the method for epitaxy aluminium oxide single crystal film according to claim 1 is characterized in that: the purity of said alumina powder is 99.99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103669061A CN102400213A (en) | 2011-11-18 | 2011-11-18 | Method for epitaxially growing alumina single crystal film |
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| CN2011103669061A CN102400213A (en) | 2011-11-18 | 2011-11-18 | Method for epitaxially growing alumina single crystal film |
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| CN102400213A true CN102400213A (en) | 2012-04-04 |
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| CN2011103669061A Pending CN102400213A (en) | 2011-11-18 | 2011-11-18 | Method for epitaxially growing alumina single crystal film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014146947A1 (en) * | 2013-03-18 | 2014-09-25 | Apple Inc. | Break resistant and shock resistant sapphire plate |
| WO2014146948A1 (en) * | 2013-03-18 | 2014-09-25 | Apple Inc. | Surface-tensioned sapphire plate |
| US9718249B2 (en) | 2012-11-16 | 2017-08-01 | Apple Inc. | Laminated aluminum oxide cover component |
| US9745662B2 (en) | 2013-03-15 | 2017-08-29 | Apple Inc. | Layered coatings for sapphire substrate |
| US11269374B2 (en) | 2019-09-11 | 2022-03-08 | Apple Inc. | Electronic device with a cover assembly having an adhesion layer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051593A (en) * | 2010-11-29 | 2011-05-11 | 中山大学佛山研究院 | Method and device for epitaxially growing metal oxide transparent conductive film |
-
2011
- 2011-11-18 CN CN2011103669061A patent/CN102400213A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051593A (en) * | 2010-11-29 | 2011-05-11 | 中山大学佛山研究院 | Method and device for epitaxially growing metal oxide transparent conductive film |
Non-Patent Citations (1)
| Title |
|---|
| 赵丹等: "生长温度对激光分子束外延AlN薄膜的影响", 《硅酸盐学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9718249B2 (en) | 2012-11-16 | 2017-08-01 | Apple Inc. | Laminated aluminum oxide cover component |
| US9745662B2 (en) | 2013-03-15 | 2017-08-29 | Apple Inc. | Layered coatings for sapphire substrate |
| WO2014146947A1 (en) * | 2013-03-18 | 2014-09-25 | Apple Inc. | Break resistant and shock resistant sapphire plate |
| WO2014146948A1 (en) * | 2013-03-18 | 2014-09-25 | Apple Inc. | Surface-tensioned sapphire plate |
| US9617639B2 (en) | 2013-03-18 | 2017-04-11 | Apple Inc. | Surface-tensioned sapphire plate |
| US9750150B2 (en) | 2013-03-18 | 2017-08-29 | Apple Inc. | Break resistant and shock resistant sapphire plate |
| TWI615278B (en) * | 2013-03-18 | 2018-02-21 | 蘋果公司 | Surface-tensioned sapphire plate |
| DE102013004558B4 (en) | 2013-03-18 | 2018-04-05 | Apple Inc. | Method for producing a surface-strained sapphire disk, surface-strained sapphire disk and electrical device with a transparent cover |
| US11269374B2 (en) | 2019-09-11 | 2022-03-08 | Apple Inc. | Electronic device with a cover assembly having an adhesion layer |
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Effective date of abandoning: 20161214 |
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