CN104593733A - Pulsed laser deposition preparation method for copper-doped zinc oxide nanorod - Google Patents
Pulsed laser deposition preparation method for copper-doped zinc oxide nanorod Download PDFInfo
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Abstract
The invention discloses a pulsed laser deposition preparation method for a copper-doped zinc oxide nanorod, relates to a deposition method for a gas-sensitive nano material, and aims to solve problems that an existing method for preparing the copper-doped zinc oxide nanorod is various in chemical raw material types, complex in reaction process and likely to introduce impurities. The pulsed laser deposition preparation method comprises the following steps: 1, preparing a copper-doped zinc oxide ceramic target material; 2, performing ablation on the target material through pulsed laser to obtain a seed crystal layer; III, performing laser ablation on the target material for 20-120 minutes to obtain a copper-doped zinc oxide nano structure. According to the pulsed laser deposition preparation method, a pulsed laser deposition method is adopted to prepare the copper-doped zinc oxide nanorod, the used raw materials are simple, only two raw materials are needed, production is performed in a vacuum cavity, sample crystal quality is high, impurities are avoided, and the controllability of the doped component is good. The pulsed laser deposition preparation method belongs to the preparation field of the copper-doped zinc oxide nanorod.
Description
Technical field
The present invention relates to a kind of air-sensitive depositing nano-materials method.
Background technology
Zinc oxide is traditional gas sensitive, to ethanol, NH
3, NO
xgood air-sensitive response is had Deng gas, and recent years is along with the progress of science and technology and industrial expansion, hydrogen sulfide is in a large amount of use of industrial circle, and hydrogen sulfide is a kind of poisonous, there is corrosive gas, even if be exposed in the hydrogen sulfide of very low concentrations (<20ppm) several hours can produce quite serious harm to human body and Industrial products equally.And pure zinc oxide nano material is due to the restriction of material property itself, to the gas not well response of low concentration hydrogen sulfide, need just to respond hydrogen sulfide in higher temperature (about 300 DEG C), suitability greatly reduces the using value of pure zinc oxide material to hydrogen sulfide sensing.Recent years, people are shown by research, the zinc oxide nano rod of Copper-cladding Aluminum Bar has good air-sensitive to respond to hydrogen sulfide, the nano zinc oxide material that but people prepare Copper-cladding Aluminum Bar generally adopts the wet chemical methods such as hydro-thermal [Li T, Fan H M, Yi J B, HerngT S, Ma Y W, Huang X L, Xue J M and Ding J, 2010, J.Mater.Chem., 20, 5756-5762] and Chinese invention patent [Li Ying etc., copper doped zinc oxide meets the hydrothermal preparing process of lithium iron phosphate positive material, application number: 201110187303.5], raw material time prepared by wet chemical method is more, step is more complicated, and in the solution of chemical reaction, easily introduce impurity.
Summary of the invention
The present invention will solve the existing method preparing copper doped zinc oxide nanometer rod to have that chemical feedstocks kind is many, reaction process is complicated, easily introduces the problem of impurity, and provides a kind of pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod.
The pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod carries out according to following steps:
One, preparation mix copper zinc oxide ceramic target: by purity be 99.9% cupric oxide powder and Zinc oxide powder be 1:(9-99 according to mol ratio) ratio ball milling 24h, at 600-700 DEG C of pre-burning 4-8 hour, make that diameter is 30-50mm, thickness is the disk of 3mm again at the pressure of 20-30MPa, at 1000-1200 DEG C, sinter 4-8 hour subsequently, obtain mixing copper zinc oxide ceramic target;
Two, substrate is cleaned: to substrate according to acetone ultrasonic cleaning 5min ~ 20min, with deionized water ultrasonic cleaning 5min ~ 20min and be for 1 time one-period with each ultrasonic cleaning of the order of methyl alcohol ultrasonic cleaning 5min ~ 20min, in 2 ~ 3 cycles of repeated washing, namely obtain the substrate after cleaning;
Three, the copper zinc oxide ceramic target of mixing step one obtained loads pulsed laser deposition rotation target position, substrate after step 2 being cleaned is fixed on can on rotation sample carrier, and substrate after cleaning with mix copper zinc oxide ceramic target and settle in opposite directions, the substrate after cleaning and the distance of mixing between copper zinc oxide ceramic target are 20mm ~ 100mm;
Four, the vacuum tightness being evacuated to vacuum chamber reaches 1 × 10
-3pa, passes into buffer gas, and controlling buffer gas flow is 1sccm ~ 100sccm;
Five, first regulating underlayer temperature to 400-500 DEG C, is 0.1J/cm at laser energy density
2~ 100J/cm
2, laser pulse width is 25ns, frequency is 1Hz ~ 50Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of oxygen is adopt krypton fluoride excimer laser to carry out laser ablation 1-20min to mixing copper zinc oxide ceramic target under the condition of 0.1-100Pa, obtains inculating crystal layer;
Six, then raising underlayer temperature to 600-750 DEG C, is 0.1J/cm at laser energy density
2~ 100J/cm
2, laser pulse width is 25ns, frequency is 1Hz ~ 50Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of argon gas is 10-1000Pa, the pressure of oxygen is carry out laser ablation 20-120min under the condition of 0-100Pa, must mix copper zinc oxide nano rod;
Seven, after step 6 terminates, stop molecular pump, then stop mechanical pump, open the purging valve of mechanical pump bottom, and pass into buffer gas to normal pressure in vacuum chamber, substrate obtains copper doped zinc oxide nanometer rod;
Substrate described in step 2 is silicon chip, glass, silicon-dioxide or gold,platinized silicon chip;
Buffer gas described in step 4 is the mixed gas of one or more in oxygen, nitrogen, argon gas.
Beneficial effect of the present invention is:
1, the present invention adopts pulsed laser deposition preparation to mix copper zinc oxide nano rod, and use raw material simple, only need two kinds of raw materials, and produce in the vacuum chamber, can not introduce any impurity, generating period is short, is only 3h-4h;
2, the present invention can reach different doping ratios by regulating cupric oxide in target from the ratio of zinc oxide, easy to prepare.
What 2, prepared by the present invention mixes copper zinc oxide nano rod, and diameter Distribution is at 50-200nm; Length distribution is at 500-6000nm, and thinner diameter and larger fineness ratio make to mix copper zinc oxide nano rod and have large specific surface area, first can promote its luminous power, secondly can all have good response to the hydrogen sulfide in wider concentration range.
3, realize detecting the room temperature of hydrogen sulfide, copper doped zinc oxide nanometer rod prepared by PLD is owing to having good crystalline network, and the introducing of Copper-cladding Aluminum Bar, namely good detection can be realized to the hydrogen sulfide of 15ppm concentration Long contact time being produced to harm to human body in room temperature, and response recovers rapidly, to improve and mix copper zinc oxide range of application.
Accompanying drawing explanation
Fig. 1 is the SEM front elevation of copper doped zinc oxide nanometer rod prepared by experiment one;
Fig. 2 is the SEM side elevational view of copper doped zinc oxide nanometer rod prepared by experiment one;
Fig. 3 is the XRD figure of copper doped zinc oxide nanostructure prepared by experiment one;
Fig. 4 is the EDS power spectrum of copper doped zinc oxide nanostructure prepared by experiment three;
Fig. 5 be experiment three prepare copper doped zinc oxide nanometer rod room temperature to the spectral response figure of 15ppm hydrogen sulfide, in figure
for passing into spectrogram before hydrogen sulfide,
for passing into spectrogram after hydrogen sulfide,
for spectrogram after discharge hydrogen sulfide.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the pulsed laser deposition preparation method of present embodiment copper doped zinc oxide nanometer rod carries out according to following steps:
One, preparation mix copper zinc oxide ceramic target: by purity be 99.9% cupric oxide powder and Zinc oxide powder be 1:(9-99 according to mol ratio) ratio ball milling 24h, at 600-700 DEG C of pre-burning 4-8 hour, make that diameter is 30-50mm, thickness is the disk of 3mm again at the pressure of 20-30MPa, at 1000-1200 DEG C, sinter 4-8 hour subsequently, obtain mixing copper zinc oxide ceramic target;
Two, substrate is cleaned: to substrate according to acetone ultrasonic cleaning 5min ~ 20min, with deionized water ultrasonic cleaning 5min ~ 20min and be for 1 time one-period with each ultrasonic cleaning of the order of methyl alcohol ultrasonic cleaning 5min ~ 20min, in 2 ~ 3 cycles of repeated washing, namely obtain the substrate after cleaning;
Three, the copper zinc oxide ceramic target of mixing step one obtained loads pulsed laser deposition rotation target position, substrate after step 2 being cleaned is fixed on can on rotation sample carrier, and substrate after cleaning with mix copper zinc oxide ceramic target and settle in opposite directions, the substrate after cleaning and the distance of mixing between copper zinc oxide ceramic target are 20mm ~ 100mm;
Four, the vacuum tightness being evacuated to vacuum chamber reaches 1 × 10
-3pa, passes into buffer gas, and controlling buffer gas flow is 1sccm ~ 100sccm;
Five, first regulating underlayer temperature to 400-500 DEG C, is 0.1J/cm at laser energy density
2~ 100J/cm
2, laser pulse width is 25ns, frequency is 1Hz ~ 50Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of oxygen is adopt krypton fluoride excimer laser to carry out laser ablation 1-20min to mixing copper zinc oxide ceramic target under the condition of 0.1-100Pa, obtains inculating crystal layer;
Six, then raising underlayer temperature to 600-750 DEG C, is 0.1J/cm at laser energy density
2~ 100J/cm
2, laser pulse width is 25ns, frequency is 1Hz ~ 50Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of argon gas is 10-1000Pa, the pressure of oxygen is carry out laser ablation 20-120min under the condition of 0-100Pa, must mix copper zinc oxide nano rod;
Seven, after step 6 terminates, stop molecular pump, then stop mechanical pump, open the purging valve of mechanical pump bottom, and pass into buffer gas to normal pressure in vacuum chamber, substrate obtains copper doped zinc oxide nanometer rod;
Substrate described in step 2 is silicon chip, glass, silicon-dioxide or gold,platinized silicon chip;
Described substrate and the distance of mixing between copper zinc oxide ceramic target are by handwheel free adjustment;
Buffer gas described in step 4 is the mixed gas of one or more in oxygen, nitrogen, argon gas.
When buffer gas described in present embodiment is mixed gas between each composition for arbitrarily than.
Embodiment two: present embodiment and embodiment one sinter unlike being 1050-1150 DEG C in temperature in step one.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two are 40-60mm unlike being substrate and the distance of mixing between copper zinc oxide ceramic target described in step 3.Other is identical with one of embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are unlike first regulating underlayer temperature to 420-460 DEG C in step 5.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four are 1.2-6J/cm unlike the laser energy density described in step 5
2.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are 10-15min unlike the laser ablation time described in step 5.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are unlike then raising underlayer temperature in step 6 to 620-720 DEG C.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven are 60-100min unlike laser ablation time in step 6.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight are 1-10Pa unlike the pressure of the oxygen described in step 6.Other is identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine are 100-150Pa unlike the pressure of the argon gas described in step 6, the pressure of oxygen is 0Pa.Other is identical with one of embodiment one to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
The pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod carries out according to following steps:
One, copper zinc oxide ceramic target is mixed in preparation: be 99.9% cupric oxide powder and purity by purity be 99.9% Zinc oxide powder be the ratio ball milling 24h of 1:99 according to mol ratio, 700 DEG C of pre-burnings 4 hours, make that diameter is 30mm, thickness is the disk of 3mm again at the pressure of 20MPa, at 1150 DEG C, sintering makes its shaping and densification for 6 hours subsequently, obtains mixing copper zinc oxide ceramic target;
Two, substrate is cleaned: to substrate according to acetone ultrasonic cleaning 10min, with deionized water ultrasonic cleaning 10min and be for 1 time one-period with each ultrasonic cleaning of the order of methyl alcohol ultrasonic cleaning 10min, in 2 cycles of repeated washing, namely obtain the substrate after cleaning;
Three, the copper zinc oxide ceramic target of mixing step one obtained loads pulsed laser deposition rotation target position, substrate after step 2 being cleaned is fixed on can on rotation sample carrier, and substrate after cleaning with mix copper zinc oxide ceramic target and settle in opposite directions, the substrate after cleaning and the distance of mixing between copper zinc oxide ceramic target are 40mm;
Four, the vacuum tightness being evacuated to vacuum chamber reaches 1 × 10
-3pa, passes into buffer gas, and controlling buffer gas flow is 50sccm;
Five, first regulating underlayer temperature to 450 DEG C, is 1.5J/cm at laser energy density
2, laser pulse width is 25ns, frequency is 8Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of oxygen is adopt krypton fluoride excimer laser to carry out laser ablation 10min to mixing copper zinc oxide ceramic target under the condition of 5Pa, obtains inculating crystal layer;
Six, then raising underlayer temperature to 700 DEG C, is 1.5J/cm at laser energy density
2, laser pulse width is 25ns, frequency is 8Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of argon gas is 120Pa, the pressure of oxygen is carry out laser ablation 60min under the condition of 0Pa, must mix copper zinc oxide nano rod;
Seven, after step 6 terminates, stop molecular pump, then stop mechanical pump, open the purging valve of mechanical pump bottom, and pass into buffer gas to normal pressure in vacuum chamber, substrate obtains copper doped zinc oxide nanometer rod;
Substrate described in step 2 is silicon chip;
Buffer gas described in step 4 is oxygen.
To it, electron microscope scanning and X-ray diffraction analysis are carried out to copper doped zinc oxide nanometer rod prepared by experiment one, Fig. 1 is the SEM front elevation of copper doped zinc oxide nanometer rod prepared by experiment one, as can be seen from the figure the copper doped zinc oxide nanometer rod of a preparation is tested, diameter 80-120nm, length 5000-6000nm, Fig. 2 are the SEM side elevational view of copper doped zinc oxide nanometer rod prepared by experiment one.Fig. 3 is the XRD figure of copper doped zinc oxide nanometer rod prepared by experiment one, is as can be seen from the figure ZnO crystal structure diffraction peak, illustrates that copper is all mixed with in the crystal of ZnO.
Experiment two:
The pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod carries out according to following steps:
One, copper zinc oxide ceramic target is mixed in preparation: be 99.9% cupric oxide powder and purity by purity be 99.9% Zinc oxide powder be the ratio ball milling 24h of 1:19 according to mol ratio, 650 DEG C of pre-burnings 4 hours, make that diameter is 30mm, thickness is the disk of 3mm again at the pressure of 20MPa, at 1100 DEG C, sinter 6 hours subsequently, obtain mixing copper zinc oxide ceramic target;
Two, substrate is cleaned: to substrate according to acetone ultrasonic cleaning 10min, with deionized water ultrasonic cleaning 10min and be for 1 time one-period with each ultrasonic cleaning of the order of methyl alcohol ultrasonic cleaning 10min, in 3 cycles of repeated washing, namely obtain the substrate after cleaning;
Three, the copper zinc oxide ceramic target of mixing step one obtained loads pulsed laser deposition rotation target position, substrate after step 2 being cleaned is fixed on can on rotation sample carrier, and substrate after cleaning with mix copper zinc oxide ceramic target and settle in opposite directions, the substrate after cleaning and the distance of mixing between copper zinc oxide ceramic target are 40mm;
Four, the vacuum tightness being evacuated to vacuum chamber reaches 1 × 10
-3pa, passes into buffer gas, and controlling buffer gas flow is 50sccm;
Five, first regulating underlayer temperature to 450 DEG C, is 1.5J/cm at laser energy density
2, laser pulse width is 25ns, frequency is 10Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of oxygen is adopt krypton fluoride excimer laser to carry out laser ablation 10min to mixing copper zinc oxide ceramic target under the condition of 5Pa, obtains inculating crystal layer;
Six, then raising underlayer temperature to 700 DEG C, is 1.5J/cm at laser energy density
2, laser pulse width is 25ns, frequency is 8Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of argon gas is 120Pa, the pressure of oxygen is carry out laser ablation 60min under the condition of 1Pa, must mix copper zinc oxide nano rod;
Seven, after step 6 terminates, stop molecular pump, then stop mechanical pump, open the purging valve of mechanical pump bottom, and pass into buffer gas to normal pressure in vacuum chamber, substrate obtains copper doped zinc oxide nanometer rod;
Substrate described in step 2 is silicon chip;
Buffer gas described in step 4 is oxygen.
Experiment three:
The pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod carries out according to following steps:
One, copper zinc oxide ceramic target is mixed in preparation: be 99.9% cupric oxide powder and purity by purity be 99.9% Zinc oxide powder be the ratio ball milling 24h of 1:9 according to mol ratio, 600 DEG C of pre-burnings 4 hours, make that diameter is 30mm, thickness is the disk of 3mm again at the pressure of 20MPa, at 1050 DEG C, sinter 6 hours subsequently, obtain mixing copper zinc oxide ceramic target;
Two, substrate is cleaned: to substrate according to acetone ultrasonic cleaning 10min, with deionized water ultrasonic cleaning 10min and be for 1 time one-period with each ultrasonic cleaning of the order of methyl alcohol ultrasonic cleaning 10min, in 3 cycles of repeated washing, namely obtain the substrate after cleaning;
Three, the copper zinc oxide ceramic target of mixing step one obtained loads pulsed laser deposition rotation target position, substrate after step 2 being cleaned is fixed on can on rotation sample carrier, and substrate after cleaning with mix copper zinc oxide ceramic target and settle in opposite directions, the substrate after cleaning and the distance of mixing between copper zinc oxide ceramic target are 40mm;
Four, the vacuum tightness being evacuated to vacuum chamber reaches 1 × 10
-3pa, passes into buffer gas, and controlling buffer gas flow is 50sccm;
Five, first regulating underlayer temperature to 450 DEG C, is 1.5J/cm at laser energy density
2, laser pulse width is 25ns, frequency is 8Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of oxygen is adopt krypton fluoride excimer laser to carry out laser ablation 10min to mixing copper zinc oxide ceramic target under the condition of 5Pa, obtains inculating crystal layer;
Six, then raising underlayer temperature to 700 DEG C, is 1.5J/cm at laser energy density
2, laser pulse width is 25ns, frequency is 8Hz, mix that copper zinc oxide ceramic target rotational velocity is 15r/min, substrate rotational velocity is 20r/min, the pressure of argon gas is 120Pa, the pressure of oxygen is carry out laser ablation 60min under the condition of 10Pa, must mix copper zinc oxide nano rod;
Seven, after step 6 terminates, stop molecular pump, then stop mechanical pump, open the purging valve of mechanical pump bottom, and pass into buffer gas to normal pressure in vacuum chamber, substrate obtains copper doped zinc oxide nanometer rod;
Substrate described in step 2 is silicon chip, glass, silicon-dioxide or gold,platinized silicon chip;
Buffer gas described in step 4 is the mixed gas in nitrogen, argon gas, the volume ratio of two kinds of gases be arbitrarily than.
To it, EDS energy spectrum analysis is carried out to copper doped zinc oxide nanometer rod prepared by experiment three, Fig. 4 is the EDS power spectrum of copper doped zinc oxide nanometer rod prepared by experiment three, can find out and have Zn element and Cu element to exist simultaneously, find that Cu element accounts for Zn through calculating, 13.9% of the total amount of Cu element, substantially with in target 10% the content of Cu element corresponding.Fig. 5 is the spectrum sensing to hydrogen sulfide of copper doped zinc oxide nanometer rod prepared by experiment three, as can be seen from the figure, the zinc oxide nanowire rod mixing copper has good response to the hydrogen sulfide of 15ppm concentration, total spectral intensity change is about 70%, can find out that at room temperature preparation is mixed copper zinc oxide nano rod and had good spectral response characteristic to hydrogen sulfide.
Claims (10)
1. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod, is characterized in that the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod carries out according to following steps:
One, preparation mix copper zinc oxide ceramic target: by purity be 99.9% cupric oxide powder and Zinc oxide powder be 1:(9-99 according to mol ratio) ratio ball milling 24h, at 600-700 DEG C of pre-burning 4-8 hour, make that diameter is 30-50mm, thickness is the disk of 3mm again at the pressure of 20-30MPa, at 1000-1200 DEG C, sinter 4-8 hour subsequently, obtain mixing copper zinc oxide ceramic target;
Two, substrate is cleaned: to substrate according to acetone ultrasonic cleaning 5min ~ 20min, with deionized water ultrasonic cleaning 5min ~ 20min and be for 1 time one-period with each ultrasonic cleaning of the order of methyl alcohol ultrasonic cleaning 5min ~ 20min, in 2 ~ 3 cycles of repeated washing, namely obtain the substrate after cleaning;
Three, the copper zinc oxide ceramic target of mixing step one obtained loads pulsed laser deposition rotation target position, substrate after step 2 being cleaned is fixed on can on rotation sample carrier, and substrate after cleaning with mix copper zinc oxide ceramic target and settle in opposite directions, the substrate after cleaning and the distance of mixing between copper zinc oxide ceramic target are 20mm ~ 100mm;
Four, the vacuum tightness being evacuated to vacuum chamber reaches 1 × 10
-3pa, passes into buffer gas, and controlling buffer gas flow is 1sccm ~ 100sccm;
Five, first regulating underlayer temperature to 400-500 DEG C, is 0.1J/cm at laser energy density
2~ 100J/cm
2, laser pulse width is 25ns, frequency is 1Hz ~ 50Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of oxygen is adopt krypton fluoride excimer laser to carry out laser ablation 1-20min to mixing copper zinc oxide ceramic target under the condition of 0.1-100Pa, obtains inculating crystal layer;
Six, then raising underlayer temperature to 600-750 DEG C, is 0.1J/cm at laser energy density
2~ 100J/cm
2, laser pulse width is 25ns, frequency is 1Hz ~ 50Hz, mix that copper zinc oxide ceramic target rotational velocity is 20r/min, substrate rotational velocity is 15r/min, the pressure of argon gas is 10-1000Pa, the pressure of oxygen is carry out laser ablation 20-120min under the condition of 0-100Pa, must mix copper zinc oxide nano rod;
Seven, after step 6 terminates, stop molecular pump, then stop mechanical pump, open the purging valve of mechanical pump bottom, and pass into buffer gas to normal pressure in vacuum chamber, substrate obtains copper doped zinc oxide nanometer rod;
Substrate described in step 2 is silicon chip, glass, silicon-dioxide or gold,platinized silicon chip;
Buffer gas described in step 4 is the mixed gas of one or more in oxygen, nitrogen, argon gas.
2. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod according to claim 1, is characterized in that being 1050-1150 DEG C in temperature in step one sinters.
3. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod according to claim 1 or 2, is characterized in that described in step 3 for substrate and the distance of mixing between copper zinc oxide ceramic target are 40-60mm.
4. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod according to claim 1 or 2, is characterized in that first regulating underlayer temperature to 420-460 DEG C in step 5.
5. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod described in 1 or 2 as requested, is characterized in that the laser energy density described in step 5 is 1.2-6J/cm
2.
6. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod described in 1 or 2 as requested, is characterized in that the laser ablation time described in step 5 is 10-15min.
7. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod described in 1 or 2 as requested, is characterized in that then raising underlayer temperature in step 6 to 620-720 DEG C.
8. the pulsed laser deposition preparation method of copper doped zinc oxide nanometer rod described in 1 or 2 as requested, is characterized in that in step 6, laser ablation time is 60-100min.
9. the pulsed laser deposition preparation method of copper doped zinc oxide nanostructure rod described in 1 or 2 as requested, is characterized in that the pressure of the oxygen described in step 6 is 1-10Pa.
10. the pulsed laser deposition preparation method of copper doped zinc oxide nanostructure rod described in 1 or 2 as requested, it is characterized in that the pressure of the argon gas described in step 6 is 100-150Pa, the pressure of oxygen is 0Pa.
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Cited By (2)
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| CN112111711A (en) * | 2020-08-25 | 2020-12-22 | 深圳大学 | Gallium oxide nanorod, preparation method thereof and photoelectric detector |
| CN114335266A (en) * | 2022-01-27 | 2022-04-12 | 东南大学 | Preparation method of white light Micro-LED based on high-quality Micro-sphere cavity |
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| CN112111711A (en) * | 2020-08-25 | 2020-12-22 | 深圳大学 | Gallium oxide nanorod, preparation method thereof and photoelectric detector |
| CN114335266A (en) * | 2022-01-27 | 2022-04-12 | 东南大学 | Preparation method of white light Micro-LED based on high-quality Micro-sphere cavity |
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