CN101748480B - Method for growing ZnO epitaxial film on Si substrate - Google Patents
Method for growing ZnO epitaxial film on Si substrate Download PDFInfo
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- CN101748480B CN101748480B CN2009101537198A CN200910153719A CN101748480B CN 101748480 B CN101748480 B CN 101748480B CN 2009101537198 A CN2009101537198 A CN 2009101537198A CN 200910153719 A CN200910153719 A CN 200910153719A CN 101748480 B CN101748480 B CN 101748480B
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- zno
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- growth
- resilient coating
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Abstract
The invention discloses a method for growing a ZnO epitaxial film on a Si substrate, which comprises the steps of: firstly, growing a Lu2O3 or Sc3O3 or Gd2O3 monocrystal film buffer layer on the Si substrate by adopting a reaction molecular beam epitaxy method; secondly, growing a ZnO film periodically on the Sin substrate with the monocrystal film buffer layer, depositing a ZnO buffer layer with thickness of 5-20nm at a temperature of 200-280 DEG C, raising the temperature to 500-700 DEG C, depositing a ZnO film with thickness of less than 500nm, reducing the temperature to 200-280 DEG C at a speed of not more than 5 DEG C/min, depositing a ZnO buffer layer with thickness of 5-20nm again, raising the temperature to 500-700 DEG C, and depositing the ZnO film with the thickness of less than 500nm again; and repeating the growth steps, and growing multiple periods to obtain the ZnO epitaxial film with thickness of micrometers and without microcracks. The method is simple and is easy to implement.
Description
Technical field
The present invention relates to the growing method of ZnO epitaxial film, especially the method for growing ZnO epitaxial film on the Si substrate.
Background technology
ZnO is the direct gap semiconductor material, and its room temperature energy gap is 3.37eV, and the room-temperature exciton binding energy is 60meV, is the ideal material of photoelectric devices such as preparation blue light-ultraviolet light-emitting diodes and laser.At present, high-quality zno-based material all is to be grown in sapphire or ScAlMgO
4On the substrate.But the insulating properties of Sapphire Substrate and high rigidity make element manufacturing complicated more, and ScAlMgO
4Price is very high, and this all makes the production cost of device rise.With respect to sapphire and ScAlMgO
4, how the Si material because its unique character, has started on the Si substrate upsurge of growing high-quality zno-based material in recent years.
Si is a first generation semi-conducting material, also is the most ripe semi-conducting material, and it can make large-sized monocrystalline, processing technology maturation, low price.Growing ZnO thin-film on the Si single crystalline substrate helps making electric injection device, because Si has good conductivity.Can make full use of simultaneously the Si planar technique and the photoetching technique of semiconductor industry maturation, the photoelectricity that helps the ZnO device is integrated, and therefore growing ZnO epitaxial film has broad application prospects on the Si substrate.
Yet owing to have bigger lattice mismatch (15%) and thermal mismatching (56%) between Si and the ZnO, the Si surface is easy to oxidation simultaneously, and the silicon dioxide of formation generally is amorphous state, therefore is difficult to realize directly epitaxial growth of ZnO film on the Si substrate.In order to overcome above-mentioned difficulties, the scientific research personnel has carried out a large amount of research to this.Discovery one deck resilient coating of growing on the Si substrate can be implemented in epitaxial growth of ZnO film on the Si substrate.But when the thickness of epitaxial loayer reaches 500nm when above, during from the epitaxial temperature cool to room temperature, cracking just appears in the ZnO epitaxial film; Thickness is thick more, and fine fisssure is serious more.Therefore how obtaining several micron thickness and non-microcracked ZnO epitaxial film on the Si substrate, is the main bottleneck of silica-based ZnO material of restriction and device development.
Summary of the invention
The objective of the invention is for overcoming on the above-mentioned Si substrate ZnO epitaxial film cracking problem, provide a kind of on the Si substrate method of the several micron thickness of growth and non-microcracked ZnO epitaxial film.
The method of growing ZnO epitaxial film on the Si substrate of the present invention may further comprise the steps:
1) adopts the reaction molecular beam epitaxy method X that on the Si substrate, grows
2O
3The monocrystal thin films resilient coating, X
2O
3Be Lu
2O
3Or Sc
2O
3Or Gd
2O
3, X
2O
3The monocrystal thin films buffer layer thickness is 30～100nm, growth conditions: with the X source is reaction source, 650～750 ℃ of underlayer temperatures, and regulating growth room's oxygen pressure is 1 * 10
-6Torr～3 * 10
-6Torr;
2) will have X
2O
3The Si substrate of monocrystal thin films resilient coating is put into the growth room, at first substrate is heated to 200～280 ℃, the thick ZnO resilient coating of deposition one deck 5～20nm, be warming up to 500～700 ℃ then, deposit the ZnO film of a layer thickness, it is cooled to 200～280 ℃ with the speed smaller or equal to 5 ℃/min, deposit the thick ZnO resilient coating of one deck 5～20nm once more less than 500nm, be warming up to 500～700 ℃, deposit the ZnO film of a layer thickness once more less than 500nm; Repeat above-mentioned growth step, grow a plurality of cycles, behind the growth ending film is cooled to room temperature with the speed cooling smaller or equal to 5 ℃/min, get final product.
Among the present invention, said Si substrate is (111) Si single crystalline substrate.ZnO film growth employing cycle growth, its periodicity is by the thickness decision of required ZnO epitaxial film.
Beneficial effect of the present invention is:
The present invention is by first epitaxial growth one deck monocrystal thin films resilient coating on the Si substrate, having cycle growth ZnO resilient coating and ZnO film on the Si substrate of monocrystal thin films resilient coating then, obtain several micron thickness and non-microcracked ZnO epitaxial film, solved ZnO epitaxial film cracking problem on the Si substrate.The inventive method is simple, is easy to realize.The ZnO epitaxial film that makes has good optical property and electric property.
Description of drawings
Fig. 1 is grow on (111) the Si single crystalline substrate structural representation of 3 cycle ZnO epitaxial films of the present invention, and 1 is the monocrystal thin films resilient coating; 2 is the ZnO resilient coating; 3 is ZnO film.
Embodiment
1) adopt reaction molecular beam epitaxy method, (111) Si single crystalline substrate is heated to 700 ℃, regulating growth room's oxygen pressure is 2 * 10
-6Torr, the reaction source of employing are the Lu source, and Lu grows on (111) Si single crystalline substrate
2O
3The monocrystal thin films resilient coating, control monocrystal thin films buffer layer thickness is 30nm;
2) step 1) growth had thick (111) Lu of 30nm
2O
3(111) Si single crystalline substrate of resilient coating is fixed on the sample stage after cleaning, put into the growth room, at first substrate is heated to 240 ℃, and the thick ZnO resilient coating of deposition one deck 15nm is warming up to 600 ℃ subsequently, the deposition ZnO film, control ZnO film thickness is 300nm, and its speed with 4 ℃/min slowly is cooled to 240 ℃, deposits the thick ZnO resilient coating of one deck 15nm once more, be warming up to 600 ℃ subsequently, deposit the ZnO film that a layer thickness is 300nm once more; Repeat above-mentioned growth step, grow 5 cycles.The growth ending rear film is slowly lowered the temperature with the speed of 4 ℃/min and is cooled to room temperature, makes the thick and non-microcracked ZnO epitaxial film of 1.5 μ m.
1) adopt reaction molecular beam epitaxy method, (111) Si single crystalline substrate is heated to 750 ℃, regulating growth room's oxygen pressure is 3 * 10
-6Torr, the reaction source of employing are the Sc source, and Sc grows on (111) Si single crystalline substrate
2O
3The monocrystal thin films resilient coating, control monocrystal thin films buffer layer thickness is 60nm;
2) step 1) growth had thick (111) Sc of 60nm
2O
3(111) Si single crystalline substrate of resilient coating is fixed on the sample stage after cleaning, put into the growth room, at first substrate is heated to 200 ℃, and the thick ZnO resilient coating of deposition one deck 10nm is warming up to 550 ℃ subsequently, the deposition ZnO film, control ZnO film thickness is 400nm, and its speed with 5 ℃/min slowly is cooled to 200 ℃, deposits the thick ZnO resilient coating of one deck 10nm once more, be warming up to 550 ℃ subsequently, deposit the ZnO film that a layer thickness is 400nm once more; Repeat above-mentioned growth step, grow 3 cycles.The growth ending rear film is slowly lowered the temperature with the speed of 5 ℃/min and is cooled to room temperature, makes the thick and non-microcracked ZnO epitaxial film of 1.2 μ m.
1) adopt reaction molecular beam epitaxy method, (111) Si single crystalline substrate is heated to 700 ℃, regulating growth room's oxygen pressure is 1 * 10
-6Torr, the reaction source of employing are the Gd source, and Gd grows on (111) Si single crystalline substrate
2O
3The monocrystal thin films resilient coating, control monocrystal thin films buffer layer thickness is 100nm;
2) step 1) growth had thick (111) Gd of 100nm
2O
3(111) Si single crystalline substrate of resilient coating is fixed on the sample stage after cleaning, put into the growth room, at first substrate is heated to 280 ℃, and the thick ZnO resilient coating of deposition one deck 20nm is warming up to 650 ℃ subsequently, the deposition ZnO film, control ZnO film thickness is 300nm, and its speed with 3 ℃/min slowly is cooled to 280 ℃, deposits the thick ZnO resilient coating of one deck 20nm once more, be warming up to 650 ℃ subsequently, deposit the ZnO film that a layer thickness is 300nm once more; Repeat above-mentioned growth step, grow 8 cycles.The growth ending rear film is slowly lowered the temperature with the speed of 3 ℃/min and is cooled to room temperature, makes the thick and non-microcracked ZnO epitaxial film of 2.4 μ m.
Claims (2)
1.Si the method for growing ZnO epitaxial film on the substrate is characterized in that may further comprise the steps:
1) adopts the reaction molecular beam epitaxy method X that on the Si substrate, grows
2O
3The monocrystal thin films resilient coating, X
2O
3Be Lu
2O
3Or Sc
2O
3Or Gd
2O
3, X
2O
3The monocrystal thin films buffer layer thickness is 30～100nm, growth conditions: with the X source is reaction source, 650～750 ℃ of underlayer temperatures, and regulating growth room's oxygen pressure is 1 * 10
-6Torr～3 * 10
-6Torr;
2) will have X
2O
3The Si substrate of monocrystal thin films resilient coating is put into the growth room, at first substrate is heated to 200～280 ℃, the thick ZnO resilient coating of deposition one deck 5～20nm, be warming up to 500～700 ℃ then, deposit the ZnO film of a layer thickness, it is cooled to 200～280 ℃ with the speed smaller or equal to 5 ℃/min, deposit the thick ZnO resilient coating of one deck 5～20nm once more less than 500nm, be warming up to 500～700 ℃, deposit the ZnO film of a layer thickness once more less than 500nm; Repeat above-mentioned growth step, grow a plurality of cycles, behind the growth ending film is cooled to room temperature with the speed cooling smaller or equal to 5 ℃/min, get final product.
2. the method for growing ZnO epitaxial film on the Si substrate according to claim 1 is characterized in that said Si substrate is (111) Si single crystalline substrate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101537198A CN101748480B (en) | 2009-11-02 | 2009-11-02 | Method for growing ZnO epitaxial film on Si substrate |
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|---|---|---|---|
| CN2009101537198A CN101748480B (en) | 2009-11-02 | 2009-11-02 | Method for growing ZnO epitaxial film on Si substrate |
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| CN101748480A CN101748480A (en) | 2010-06-23 |
| CN101748480B true CN101748480B (en) | 2011-11-30 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031597A (en) * | 2012-12-25 | 2013-04-10 | 浙江大学 | Na-Be codoped p-ZnO film growth method |
| CN110767532A (en) * | 2019-10-15 | 2020-02-07 | 中国电子科技集团公司第十一研究所 | Processing method of silicon-based composite substrate |
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2009
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