CN101037795A - Sb doped P-type ZnO crystal film and preparation method thereof - Google Patents
Sb doped P-type ZnO crystal film and preparation method thereof Download PDFInfo
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- CN101037795A CN101037795A CN 200710066967 CN200710066967A CN101037795A CN 101037795 A CN101037795 A CN 101037795A CN 200710066967 CN200710066967 CN 200710066967 CN 200710066967 A CN200710066967 A CN 200710066967A CN 101037795 A CN101037795 A CN 101037795A
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- 239000013078 crystal Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims description 8
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000919 ceramic Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 4
- 238000004549 pulsed laser deposition Methods 0.000 claims description 7
- 238000000748 compression moulding Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 238000002679 ablation Methods 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
- 239000010980 sapphire Substances 0.000 claims description 2
- 238000000151 deposition Methods 0.000 abstract description 8
- 238000000465 moulding Methods 0.000 abstract description 4
- 239000013077 target material Substances 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 238000010186 staining Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
The invention discloses a method for preparing Sb-intermingled growing p-type ZnO crystal film, including the step of: weighing ZnO and SbO3 powder, wherein mol percent of Sb is 1.5-4%, mixing the powders uniformly by ball milling and compressed molding, and sintering them to produce Sb-intermingled ZnO ceramic target; placing the ceramic target and the substrate into the the growing chamber of pulse laser depositing apparatus, growing the film on the substrate by the pulse laser depositing method, annealing at the oxygen atmosphere after growing, cooling them to room temperature. The inventive method is simple, different-intermingling-concentration p-type ZnO crystal film can be produced by adjusting mol percent of Sb in the target matarials, and high-concentration intermingling can be carried out because intermingled elments come from the target materials; SbZn-2VZn complex is produced by making Sb to occupy the position of Zn, while to be induced to produce both empty positions of Zn, compared with N element in V group the producing energy of the complex is lower, accordingly the produced p-ZnO film has good the repeatability and the stability.
Description
Technical field
The present invention relates to the preparation method of p type ZnO crystal film, especially the preparation method of Sb doped p type ZnO crystal film.
Background technology
The n type of processability excellence and p type ZnO electrically conducting transparent crystal film are to realize the key of ZnO in the photoelectric field widespread use.The n type of ZnO mixes and realizes than being easier to, and the preparation of p type ZnO film is then relatively difficult.This is to have many native defects owing among the ZnO on the one hand, as zinc gap (Zn
i) and oxygen room (V
o) can produce height self compensation effect; Then be that reasons such as dark and acceptor impurity solid solubility is very low owing to acceptor level cause on the other hand.The real-time doping that how to realize having the p type ZnO film of excellent properties has become a bottleneck of present restriction zno-based photoelectric device development.
The doped element of the p-ZnO that reports all concentrates on V group element in the world at present, and for example N, P, As etc. wherein mix the most general with N again.But also there are some problems in the N element doping: low such as the solid solubility of being led, acceptor level is darker, and the repeatability and the stability of the conduction of p type are not high.
Summary of the invention
The objective of the invention is provides a kind of preparation method of Sb doped p type ZnO crystal film for overcoming the existing problem of above-mentioned N element doping.
The preparation method of Sb doped p type ZnO crystal film is to adopt pulsed laser deposition, may further comprise the steps:
The ZnO of 1) weighing purity＞99.99% and Sb
2O
3Powder, wherein the Sb molar content is 1.5～4%, with above-mentioned powder ball milling mix, compression moulding, then at 1000～1200 ℃ of sintering temperatures, make the ZnO ceramic target of mixing Sb;
2) put into pulsed laser deposition device growth room with ceramic target with through the substrate that cleans, the distance between target and the substrate remains 4～5.5cm, and growth room's vacuum tightness is evacuated to and is higher than 4 * 10
-4Pa, substrate heats to 400～600 ℃, the growth room feeds purity oxygen, control pressure is 0.1～1Pa, opens laser apparatus, allows laser beam focus on target surface ablation target, form twilight sunset, be deposited on the substrate, the growth ending rear film in 500～700 ℃ of annealing 10～30min, is cooled to room temperature under oxygen atmosphere.
The purity of above-mentioned pure oxygen is more than 99.99%.Said substrate can be silicon or sapphire or quartz or glass.
In order further to improve the conductivity of Sb doped p type ZnO crystal film, the Sb doped p type ZnO crystal film after the annealing can be slowly cooled to room temperature under the oxygen protection of 40～100Pa.
The present invention can prepare the p type ZnO crystal film of different levels of doping by the molar content of regulating Sb in the target, and growth time is by the thickness decision of required crystal film.
Beneficial effect of the present invention is: method is simple, and p type doping content can be controlled by the molar content of regulating Sb in the target; In the ZnO crystal film growth, realize being subjected to the real-time doping of main Sb; Because doped element from target, therefore can realize high-concentration dopant; The present invention compares with the N element doping, and Sb occupies the position of Zn, induces the room of 2 Zn simultaneously, forms Sb
Zn-2V
ZnComplex body, the formation of this complex body can be lower, thereby the p-ZnO film that makes has good repeatability and stable.
Description of drawings
Fig. 1 is the pulsed laser deposition device synoptic diagram that adopts according to the inventive method, and among the figure: 1 is laser apparatus; 2 is the growth room; 3 is target; 4 is substrate;
Fig. 2 is x ray diffraction (XRD) collection of illustrative plates of the p type ZnO crystal film that makes of the inventive method.
Embodiment
Below in conjunction with Fig. 1, the present invention is further illustrated by example.
1) weighing purity is 99.99% ZnO and Sb
2O
3Powder, wherein the molar content of Sb is 2%.With load weighted ZnO and Sb
2O
3Powder is poured in the ball grinder that agate ball is housed, and ball milling is 12 hours on ball mill, and purpose is to allow evenly also refinement to a certain extent of powder mixes.Then raw material is separated oven dry, add binding agent and grind compression moulding.The idiosome of moulding is put into sintering oven, and row is plain through low temperature (400 ℃), makes the binding agent volatilization, is warming up to 1200 ℃ of sintering again 2 hours, obtains mixing the ZnO ceramic target of Sb.
2) quartz substrate is fixed on the sample table after cleaning, puts into growth room 2.The ZnO ceramic target that to mix Sb is contained on the target frame, embeds then in the target holder of pulsed laser deposition device.The distance of regulating substrate 4 and target 3 is 4cm, and baffle plate is placed between substrate and the target.Growth room's vacuum tightness is evacuated to 4 * 10
-4Pa, substrate are heated to 550 ℃.Feed pure O
2, pressure is controlled at 1Pa.Open laser apparatus 1 (pulsed laser energy is 300mJ, frequency 3Hz), pre-deposition 10min removes staining of target material surface, the baffle plate of outwarding winding then, and deposit film, depositing time are 45min, the thick 300nm that is about of film.Substrate and target low speed rotation in the deposition process are to improve the homogeneity of film.The growth ending rear film is in-situ annealing 20min under oxygen atmosphere, and annealing temperature is 650 ℃.Above-mentioned ZnO crystal film is slowly cooled to room temperature under the oxygen protection of 70Pa.
The room temperature electric property of the Sb doped p type ZnO crystal film that makes is good: resistivity is 2.21 Ω cm, and hole concentration reaches 2.30 * 10
18Cm
-3, hall mobility is 1.23cm
2/ V.s.And the electric property of placing the several months rear film does not have considerable change.
X ray diffraction (XRD) collection of illustrative plates of above-mentioned film as shown in Figure 2, has only (0002) diffraction peak of ZnO to occur, and shows that the Sb doped p type ZnO crystal film that the inventive method makes has good crystal property.
1) weighing purity is 99.99% ZnO and Sb
2O
3Powder, wherein the molar content of Sb is 1.5%.With load weighted ZnO and Sb
2O
3Powder is poured in the ball grinder that agate ball is housed, and ball milling mixes, compression moulding.The idiosome of moulding is put into sintering oven, plain through 400 ℃ of rows, make the binding agent volatilization, be warming up to 1000 ℃ of sintering again 2 hours, obtain mixing the ZnO ceramic target of Sb.
2) silicon substrate is fixed on the sample table after cleaning, puts into the growth room.The ZnO ceramic target that to mix Sb places the target holder of pulsed laser deposition device.The distance of regulating substrate and target is 5.5cm, and baffle plate is placed between substrate and the target.Growth room's vacuum tightness is evacuated to 4 * 10
-4Pa, substrate are heated to 600 ℃.Feed pure O
2, pressure is controlled at 0.1Pa.Open laser apparatus (pulsed laser energy is 300mJ, frequency 3Hz), pre-deposition 10min removes staining of target material surface, the baffle plate of outwarding winding then, and deposit film, depositing time are 30min, the thick 200nm that is about of film.The growth ending rear film in 700 ℃ of in-situ annealing 10min, is cooled to room temperature under oxygen atmosphere.
The room temperature electric property of the Sb doped p type ZnO crystal film that makes: resistivity is 57.7 Ω cm, and hole concentration is 6.88 * 10
16Cm
-3, hall mobility is 1.57cm
2/ V.s.And the electric property of placing the several months rear film does not have considerable change.
1) weighing purity is 99.99% ZnO and Sb
2O
3Powder, wherein the molar content of Sb is 4%.With load weighted ZnO and Sb
2O
3Powder is poured in the ball grinder, and ball milling mixes, compression moulding.The idiosome of moulding is put into sintering oven, plain through 400 ℃ of rows, make the binding agent volatilization, be warming up to 1100 ℃ of sintering again 2 hours, obtain mixing the ZnO ceramic target of Sb.
2) glass substrate is fixed on the sample table after cleaning, puts into the growth room.The ZnO ceramic target that to mix Sb places the target holder of pulsed laser deposition device.The distance of regulating substrate and target is 4.5cm, and baffle plate is placed between substrate and the target.Growth room's vacuum tightness is evacuated to 4 * 10
-4Pa, substrate are heated to 400 ℃.Feed pure O
2, pressure is controlled at 0.7Pa.Open laser apparatus (pulsed laser energy is 300mJ, frequency 3Hz), pre-deposition 10min removes staining of target material surface, the baffle plate of outwarding winding then, and deposit film, depositing time are 45min, the thick 300nm that is about of film.The growth ending rear film in 500 ℃ of in-situ annealing 30min, is cooled to room temperature under oxygen atmosphere.
The room temperature electric property of the Sb doped p type ZnO crystal film that makes: resistivity is 1930 Ω cm, and hole concentration is 2.53 * 10
15Cm
-3, hall mobility is 1.28cm
2/ V.s.And the electric property of placing the several months rear film does not have considerable change.
Claims (4)
1.Sb the preparation method of doping growing P type ZnO crystal film is characterized in that step is as follows:
The ZnO of 1) weighing purity＞99.99% and Sb
2O
3Powder, wherein the Sb molar content is 1.5～4%, with above-mentioned powder ball milling mix, compression moulding, then at 1000～1200 ℃ of sintering temperatures, make the ZnO ceramic target of mixing Sb;
2) put into pulsed laser deposition device growth room with ceramic target with through the substrate that cleans, the distance between target and the substrate remains 4～5.5cm, and growth room's vacuum tightness is evacuated to and is higher than 4 * 10
-4Pa, substrate heats to 400～600 ℃, the growth room feeds purity oxygen, control pressure is 0.1～1Pa, opens laser apparatus, allows laser beam focus on target surface ablation target, form twilight sunset, be deposited on the substrate, the growth ending rear film in 500～700 ℃ of annealing 10～30min, is cooled to room temperature under oxygen atmosphere.
2. the method for Sb doping growing P type ZnO crystal film according to claim 1 is characterized in that said substrate is silicon or sapphire or quartz or glass.
3. the method for Sb doping growing P type ZnO crystal film according to claim 1, the purity that it is characterized in that pure oxygen is more than 99.99%.
4. the method for Sb doping growing P type ZnO crystal film according to claim 1, postcooling to the room temperature that it is characterized in that annealing is to carry out under the oxygen protection of 40～100Pa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710066967XA CN100432302C (en) | 2007-01-29 | 2007-01-29 | Sb doped P-type ZnO crystal film and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710066967XA CN100432302C (en) | 2007-01-29 | 2007-01-29 | Sb doped P-type ZnO crystal film and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101037795A true CN101037795A (en) | 2007-09-19 |
| CN100432302C CN100432302C (en) | 2008-11-12 |
Family
ID=38888960
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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| CN (1) | CN100432302C (en) |
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