CN100459179C - Production of ZnO/mgB heterojunction material - Google Patents

Production of ZnO/mgB heterojunction material Download PDF

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Publication number
CN100459179C
CN100459179C CNB2005101078269A CN200510107826A CN100459179C CN 100459179 C CN100459179 C CN 100459179C CN B2005101078269 A CNB2005101078269 A CN B2005101078269A CN 200510107826 A CN200510107826 A CN 200510107826A CN 100459179 C CN100459179 C CN 100459179C
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mgb
film
zno
boron
zinc oxide
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CN1941424A (en
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赵嵩卿
周岳亮
赵昆
刘震
王淑芳
韩鹏
陈正豪
吕惠宾
程波林
何萌
杨国桢
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Institute of Physics of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention is concerned with hetero-structures material and production method of ZnO/MgB2. There are MgB2 and ZnO films with both thickness of 10 nanometer-10 micron. Produce forerunner MgB2 film with routine method, vacuum the forerunner MgB2 film and 0.1-3.0 g magnesium in close quartz tube and agglomerate into MgB2 film in a muffle furnace. Input MgB2 film and zinc oxide target into the vacuum room of impulse laser deposit equipment with1*10-3-5*10-8Pa vacuum and at150DEG C-600DEG C. Focus molecule impulse laser with 120 millijoule and 450 millijoule to zinc oxide target or the target of impure zinc oxide to get ZnO/MgB2 hetero-structures. The hetero-structures can be used at the detector with far infrared and visible light and ultraviolet radiation.

Description

A kind of ZnO/MgB 2Heterojunction material and preparation method
Technical field
The present invention relates to a kind of heterojunction material and preparation method, particularly relate to a kind of ZnO/MgB infrared, visible, that use to ultraviolet light detector for preparing 2Heterojunction material and preparation method.
Background technology
Nearly decades, because the peculiar physical property of zinc oxide has caused people's very big interest, people have made various heterojunction with zinc oxide and other materials, comprising: La 0.7Sr 0.3MnO 3/ ZnO and ZnO/ diamond thin or the like are as document Ashutosh Tiwari, C.Jin, D.Kumar, and J.Narayan, Appl.Phys.Lett., Vol.83,1773 (2003) and C.X.Wang, G.W.Yang, T.C.Zhang, H.W.Liu, Y.H.Han, J.F.Luo, C.X.Gao, G.T.Zou, Diamond and Related Materials 12 (2003) 1548-1552 are described.Above-mentioned heterojunction generally is used for doing luminescent device or rectifying device.And in numerous documents, also do not find zinc oxide and MgB 2The heterojunction of making and to zinc oxide heterogeneous knot is reported as photo-detector.The invention provides a kind of zinc oxide and MgB 2The preparation method of heterojunction, the heterojunction for preparing with the method can be used as the photo-detector manufacturing.
Summary of the invention
The objective of the invention is to: a kind of ZnO/MgB that can be used for infrared light to the long light-detecting device of ultraviolet light all-wave is provided 2Heterojunction material, and preparation ZnO/MgB 2The method of heterojunction material.
The object of the present invention is achieved like this:
ZnO/MgB provided by the invention 2Heterojunction material is included in growth one deck magnesium diboride film (MgB on the substrate 2), growth layer of ZnO film on the magnesium diboride film, wherein the magnesium diboride film thickness is in 10 nanometers～10 micron; ZnO film thickness is in 10 nanometers～10 micron.
Preparation ZnO/MgB provided by the invention 2The method of heterojunction material is utilized the equipment and the technology that prepare film, carries out according to the following steps:
1. at first prepare pioneer MgB 2Film: adopt conventional pulse laser made membrane method, chemical vapour deposition technique, sputtering method, physical vaporous deposition or supersonic spraying, preparation thickness is 10 nanometers～10 micron MgB on magnesium oxide or white stone substrate 2Pioneer's boron film, this MgB 2It rises and falls the surface of pioneer's boron film less than 50nm;
2. the MgB that then step 1 is being prepared 2The magnesium of pioneer's boron film and 0.1～3.0 gram is enclosed in the quartz ampoule, and this quartz ampoule volume is 1～10 cubic centimetre, and quartz ampoule is evacuated down to 10 -3～10 -5The handkerchief rear enclosed is placed on sintering in the Muffle furnace, and temperature is 700～1200 degrees centigrade, and making magnesium steam and boron reaction time is 40-60 minute, obtains high-quality MgB 2Film;
3. the zinc oxide target of oxygenerating zinc target or doping: (wherein the doping zinc-oxide powder comprises: mix 0.5～5% (press the atomic ratio of zinc oxide and doped chemical boron, aluminium, gallium, indium) boron, aluminium, gallium or indium (or oxide of boron, aluminium, gallium, indium composition) Zinc oxide powder or doping zinc-oxide powder, through well-mixed doping zinc-oxide powder) be pressed into diameter be 1～10 centimetre, thickness is the cake of 0.5～20 millimeters thick, wherein institute's applied pressure is 10～100MP; Put into the electric furnace sintering then, its temperature is under 900～1500 degrees centigrade, and sintering obtained the zinc oxide target of high-purity zinc oxide target or doping in 4～48 hours, and it is installed on the target position in the pulsed laser deposition equipment vacuum chamber; The MgB of step 2 preparation 2Film is installed on the interior chip bench of pulsed laser deposition equipment vacuum chamber, with molecular pump vacuum chamber is extracted into 1 * 10 -3～5 * 10 -5The vacuum of Pa is simultaneously with the MgB on the chip bench 2It is 150 ℃-600 ℃ that film is heated to temperature;
4. opening excimer pulse laser, is that the burnt excimer pulsed laser to 450 milli Jiao of 120 millis focuses on zinc oxide target or the doping zinc-oxide target bombardment zinc oxide target with energy, deposit, range 30-50 millimeter sedimentation time 10-200 minute, obtains ZnO/MgB 2Heterojunction.
In above-mentioned technical scheme, described preparation MgB 2The technology of pioneer's boron film also comprises with the high-quality MgB of the direct preparation of pulse laser, chemical vapour deposition technique, sputtering method, physical vaporous deposition, supersonic spraying or other the method for preparing film 2Pioneer's boron film.
In above-mentioned technical scheme, described preparation MgB 2The raw material of pioneer's boron film and the purity of magnesium are high-purity, described Zinc oxide powder is high-purity Zinc oxide powder (purity is 99.9-99.9999%), and the purity of the oxide that described boron, aluminium, gallium and indium are formed is high-purity (purity is 99.9-99.9999%).
Advantage of the present invention:
The present invention has prepared ZnO/MgB first 2Heterojunction material, it is a kind of novel superconductor and heterojunction semiconductor, and prepared heterojunction material has been found the photogenic voltage signal of infrared light first, as shown in Figure 1, and can go out infrared detector with this material preparation, simultaneously also can be as the preparation ultraviolet light detector.It both can also can expand zinc oxide and MgB as the detection of ultraviolet light as the detection of infrared light 2The range of application of film.
Method of the present invention is simple, can use pulsed laser deposition, chemical vapour deposition technique, sputtering method, physical vaporous deposition, supersonic spraying or the preparation of other method for manufacturing thin film.
Description of drawings
Fig. 1 represents ZnO/MgB 2The photogenic voltage signal of heterojunction material infrared light
Embodiment
Embodiment 1, below in an embodiment in conjunction with ZnO/MgB of the present invention 2The heterojunction material preparation method is to ZnO/MgB of the present invention 2Heterojunction material is elaborated:
Preparation ZnO/MgB 2Heterojunction material, its preparation method may further comprise the steps:
1. at first, adopt conventional pulse laser filming technology, preparation thickness is the MgB of 100 nanometers on magnesium oxide or white stone substrate 2Pioneer's boron film; Then the MgB that makes 2High-purity magnesium metal of pioneer's boron film and 0.3 gram is enclosed in the quartz ampoule, and the quartz ampoule volume is 3 cubic centimetres, and the quartz ampoule vacuum is extracted into 10 -5Handkerchief is put into the Muffle furnace sintering with quartz ampoule, and wherein sintering temperature is 900 ℃, makes the reaction of magnesium steam and boron, the reaction time be obtained in 40 minutes 600nm thick, rise and fall less than the MgB of 10nm 2Film;
Purity be 99.99% Zinc oxide powder be pressed into diameter be 1～10 centimetre, thickness is the cake of 0.5～20 millimeters thick, wherein institute's applied pressure is all can between 10～100MP; Put into the electric furnace sintering then, its sintering temperature is under 1500 degrees centigrade, and sintering obtained the high-purity zinc oxide target in 24 hours, and the high-purity zinc oxide target is installed on the target position in the pulsed laser deposition equipment vacuum chamber; The MgB of step 1 preparation 2Pioneer's film is installed on the interior chip bench of pulsed laser deposition equipment vacuum chamber, with molecular pump vacuum chamber is extracted into 5 * 10 -4The vacuum that Pa is above, and remain on 5 * 10 -4Under the vacuum more than the Pa, simultaneously with the MgB on the chip bench 2It is 350 ℃ that pioneer's film is heated to temperature;
3. open excimer pulse laser, with energy is that 250 millis excimer pulsed laser burnt, that wavelength is 248nm focuses on the high-purity zinc oxide target of step 2 preparation, the bombardment zinc oxide target, deposit, 50 millimeters of ranges, sedimentation time 20 minutes, thickness be the ZnO film thickness of growing on the magnesium diboride film of 100nm in 100 nanometers, obtain ZnO/MgB 2Heterojunction.
Embodiment 2
Preparation ZnO/MgB 2Heterojunction material, its preparation method may further comprise the steps:
1. at first, the high-quality preparation MgB of preparation 2Film adopts chemical vapour deposition technique to prepare high-quality boron film, is extracted into 10 in that boron film and 0.6 magnesium that restrains are enclosed in vacuum then -5Handkerchief, volume are that sintering kept 950 degrees centigrade of temperature 60 minutes in 5 cubic centimetres of quartz ampoules, make the reaction of magnesium steam and boron, obtain the thick fluctuating of 600nm less than 50nm MgB 2Film.
2. be equipped with the doping zinc-oxide target with the pressure sintering legal system, is the Zinc oxide powder of high-purity (purity is 99.9%-99.999%) and purity that 99.999% high purity boron powder fully mixes in zinc and 1: 0.05 ratio of boron atom ratio, be pressed into diameter and be 1～10 centimetre, thickness is the cake of 0.5～20 millimeters thick, wherein institute's applied pressure is 1～100MP; Put into the electric furnace sintering then, its temperature under 1500 degrees centigrade, the zinc oxide target that sintering obtained mixing in 14 hours; Doping elements can also be aluminium, gallium, indium, and wherein the atomic ratio of zinc atom and doped chemical is between 0.5% to 5%.High-quality MgB 2Film is installed on the interior chip bench of pulsed laser deposition equipment vacuum chamber, with molecular pump vacuum chamber is extracted into 1 * 10 -4The vacuum that Pa is above, simultaneously substrate being heated to temperature is 450 ℃;
3. open excimer pulse laser, with energy be 150 the milli burnt 248nm excimer pulsed laser focus on the zinc oxide target, the bombardment zinc oxide target, deposit, 35 millimeters of ranges, sedimentation time 80 minutes obtains the magnesium diboride film thickness in 600 nanometers, and the ZnO film thickness of growing on boronation magnesium film is at the ZnO/MgB of 600 nanometers 2Heterojunction
Embodiment 3.
Preparation high-quality ZnO/MgB 2Heterojunction material:
1. at first, the high-quality preparation MgB of preparation 2Film adopts sputtering method to prepare high-quality boron film, is extracted into 10 in that boron film and 1 magnesium that restrains are enclosed in vacuum then -5Handkerchief, volume are 1050 degrees centigrade of sintering one hour in 6 cubic centimetres of quartz ampoules, make the reaction of magnesium steam and boron, and the 5nm that obtains rising and falling, thickness are 1200nm high-quality MgB 2Film.
2. be equipped with the doping zinc-oxide target with the pressure sintering legal system, is the Zinc oxide powder of high-purity (purity is 99.9%-99.999%) and purity that 99.999% aluminium oxide powder fully mixes in zinc and 1: 0.03 ratio of al atomic ratio, be pressed into diameter and be 1～10 centimetre, thickness is the cake of 0.5～20 millimeters thick, wherein institute's applied pressure is 1～100MP; Put into the electric furnace sintering then, its temperature is under 1000 degrees centigrade, and sintering obtained the zinc oxide target that aluminium mixes in 10 hours, and is installed on the interior target position of pulsed laser deposition equipment vacuum chamber; High-quality MgB 2Film is installed on the interior chip bench of pulsed laser deposition equipment vacuum chamber, with molecular pump vacuum chamber is extracted into 5 * 10 -4The vacuum that Pa is above, simultaneously substrate being heated to temperature is 450 ℃;
3. open excimer pulse laser, with energy be 350 the milli burnt 248nm excimer pulsed laser focus on the zinc oxide target, the bombardment zinc oxide target, deposit, range 30-50 millimeter, sedimentation time 120 minutes obtains the magnesium diboride film thickness at 1.2 microns, and the ZnO film thickness of growing on boronation magnesium film is at 1.2 microns ZnO/MgB 2Heterojunction material.
Embodiment 4.
Preparation high-quality ZnO/MgB 2Heterojunction material:
1. at first, the high-quality preparation MgB of preparation 2Film adopts the pulse laser method to prepare high-quality boron film, then the magnesium of boron film and 0.5 gram is enclosed in vacuum and is extracted into 10 -3Handkerchief, volume are that sintering kept 1100 degrees centigrade of temperature 40 minutes in 3 cubic centimetres of quartz ampoules, make the reaction of magnesium steam and boron, and obtaining surface smoothness is that 5nm, thickness are 500nm high-quality MgB 2Film.
2. be equipped with the high-purity zinc oxide target with the pressure sintering legal system, high-quality MgB 2Film is installed on the interior chip bench of magnetron sputtering deposition equipment vacuum chamber, with molecular pump vacuum chamber is extracted into 5 * 10 -4The vacuum that Pa is above, simultaneously substrate being heated to temperature is 450 ℃.
3. opening shielding power supply, is that 30 kilovolts accelerating voltage quickens argon ion, the bombardment zinc oxide target with energy, deposit 50 millimeters of ranges, sedimentation time 50 minutes, obtain the magnesium diboride film thickness in 500 nanometers, the ZnO film thickness of growing on boronation magnesium film is at the ZnO/MgB of 600 nanometers 2Heterojunction.

Claims (7)

1. ZnO/MgB 2Heterojunction material is included in growth one deck MgB on the substrate 2Film is characterized in that, at MgB 2Growth layer of ZnO film, wherein MgB on the film 2Film thickness is in 10 nanometers～10 micron; ZnO film thickness is in 10 nanometers～10 micron.
2. one kind prepares ZnO/MgB 2The method of heterojunction material may further comprise the steps and carries out:
1). at first adopt conventional made membrane equipment and prepared MgB 2Pioneer's boron film: preparation thickness is 10 nanometers～10 micron MgB on magnesium oxide or white stone substrate 2Pioneer's boron film;
2). and then the MgB that step 1) is prepared 2The magnesium of pioneer's boron film and 0.1～3.0 gram is enclosed in the quartz ampoule, and this quartz ampoule volume is 1～10 cubic centimetre, and quartz ampoule is evacuated down to 10 -3～10 -5The Pa rear enclosed is placed on sintering in the Muffle furnace, and temperature is 700～1200 ℃, and making magnesium steam and boron reaction time is 40-60 minute, obtains MgB 2Film;
3). the zinc oxide target of oxygenerating zinc target or doping: Zinc oxide powder or doping zinc-oxide powder be pressed into diameter be 1～10 centimetre, thickness is the cake of 0.5～20 millimeters thick, wherein institute's applied pressure is 10～100MPa; Put into the electric furnace sintering then, its sintering temperature is under 900～1500 ℃, and sintering obtained the zinc oxide target of zinc oxide target or doping in 4～48 hours, and is installed on the interior target position of pulsed laser deposition equipment vacuum chamber; Again step 2) preparation MgB 2Film is installed on the interior chip bench of pulsed laser deposition equipment vacuum chamber, with molecular pump vacuum chamber is extracted into 1 * 10 -3～5 * 10 -8The vacuum of Pa is simultaneously with the MgB on the chip bench 2It is 150 ℃-600 ℃ that film is heated to temperature;
4). opening excimer pulse laser, is that the burnt excimer pulsed laser to 450 milli Jiao of 120 millis focuses on zinc oxide target or the doping zinc-oxide target bombardment zinc oxide target or doping zinc-oxide target with energy, deposit, range 30-50 millimeter sedimentation time 10-200 minute, obtains ZnO/MgB 2Heterojunction.
3. by the described preparation of claim 2 ZnO/MgB 2The method of heterojunction material is characterized in that, described conventional made membrane prepared MgB 2Pioneer's boron film comprises: prepare MgB with pulse laser system embrane method, chemical vapour deposition technique, sputtering method, physical vaporous deposition or supersonic spraying 2Pioneer's boron film.
4. by the described preparation of claim 2 ZnO/MgB 2The method of heterojunction material is characterized in that, described doping zinc-oxide powder comprises: the atomic ratio by zinc in zinc oxide and doped chemical boron, aluminium, gallium or indium is preparation in 1: 0.005～1: 0.05.
5. by the described preparation of claim 2 ZnO/MgB 2The method of heterojunction material is characterized in that, described preparation MgB 2The raw material of pioneer's boron film and the purity of magnesium are 99.9-99.9999%.
6. by the described preparation of claim 2 ZnO/MgB 2The method of heterojunction material is characterized in that, the MgB for preparing in the described step 1) 2The surface undulation of pioneer's boron film is less than 50nm.
7. by the described preparation of claim 4 ZnO/MgB 2The method of heterojunction material is characterized in that, the purity of the oxide that described boron, aluminium, gallium or indium are formed is 99.9-99.9999%.
CNB2005101078269A 2005-09-30 2005-09-30 Production of ZnO/mgB heterojunction material Expired - Fee Related CN100459179C (en)

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* Cited by examiner, † Cited by third party
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CN105097983B (en) * 2015-07-23 2017-04-12 武汉大学 Heterojunction near-infrared photosensitive sensor and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08139361A (en) * 1994-11-08 1996-05-31 Toshiba Corp Compound semiconductor light emitting device
CN1400674A (en) * 2002-08-05 2003-03-05 浙江大学 Preparation method of zinc oxide UV photodetector prototype device
US20050116263A1 (en) * 2002-06-06 2005-06-02 Rutgers, The State University of New Jersey and Multifunctional biosensor based on zno nanostructures

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08139361A (en) * 1994-11-08 1996-05-31 Toshiba Corp Compound semiconductor light emitting device
US20050116263A1 (en) * 2002-06-06 2005-06-02 Rutgers, The State University of New Jersey and Multifunctional biosensor based on zno nanostructures
CN1400674A (en) * 2002-08-05 2003-03-05 浙江大学 Preparation method of zinc oxide UV photodetector prototype device

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