CN103178208A - Nano particle thin film with resistance variation storage characteristics and preparation method thereof - Google Patents
Nano particle thin film with resistance variation storage characteristics and preparation method thereof Download PDFInfo
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- CN103178208A CN103178208A CN2013100692883A CN201310069288A CN103178208A CN 103178208 A CN103178208 A CN 103178208A CN 2013100692883 A CN2013100692883 A CN 2013100692883A CN 201310069288 A CN201310069288 A CN 201310069288A CN 103178208 A CN103178208 A CN 103178208A
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Abstract
The invention belongs to the technical field of semiconductors and particularly relates to a nano particle thin film with resistance variation storage characteristics and a preparation method thereof. The nano particle thin film comprises at least one layer of a metal oxide nano particle thin film, or one layer of a metal oxide nano particle thin film doped with metallic elements, or combination of the two. The nano particle thin film is 50-1000mm in thickness, 1-3V in threshold voltage, 100-900 in switch ratio and at least 10 in switch repeatability. The preparation method includes: using a sol gel method to prepare sol, performing alkali treatment to the sol to obtain nano particles, and coating the nano particles on a substrate. The nano particle thin film is low in defect, good in compactness, high in smoothness, low in particle size, high in density, even in distribution, good in resistance state converting stability, and applicable to non-volatile storages.
Description
Technical field
The invention belongs to technical field of semiconductors, be specifically related to a kind of nanoparticulate thin films with resistance-change memory characteristic and preparation method thereof.
Background technology
Currently marketed nonvolatile memory is take flash memory (Flash Memory) as main flow, but along with requiring less thinner for device size in industrial production, in the process that volume constantly dwindles, flash memory presents the shortcomings such as operating voltage is excessive, service speed slow, endurance is good not and fall short of memory time that cause due to excessively thin tunnel oxide.Desirable non-volatility memorizer should possess the characteristics such as operating voltage is low, simple in structure, non-destructive reads, service speed fast, memory time (Retention) is long, device area is little, fatigue properties (Endurance) are good.
Resistive random asccess memory (RRAM) is a kind of nonvolatile memory (NVM) that comes records store data information based on change in resistance.In recent years, because it has high density, high-speed and low-power consumption, the NVM device in the middle of the development of memory in occupation of consequence more and more.Along with the storage component part size dwindle and to low-voltage and low-power dissipation, superintegrated requirement, non-volatile nanocrystalline resistance-variable storing device is subject to researcher's favor day by day.
The material system of RRAM comprises at present: organic polymer, as polyimides (PI), AIDCN and CuTCNQ etc.; Complicated oxide is as Pr
1-xCa
xMnO
3And La
0.7Ca
0.3MnO
3, perovskite material SrTiO
3And SrZrO
3Deng; Simple Dyadic transition group metallic oxide is as the oxide of Cu, Ti, Ni, Ta, Hf, Nb etc.The advantages such as compared to other material with complex, Dyadic transition group metallic oxide has simple in structure, easily makes, and the resistance window is large become the study hotspot in numerous materials.
with respect to thin-film memory, nanocrystalline resistance-variable storing device has the little integrated height of yardstick and stores the advantages such as low-power consumption with height, but study at present the more two-dimensional nanostructure resistive characteristics such as nano wire and nanotube that are, paper " Memory and Threshold Resistance Switching in Ni/NiO Core Shell Nanowires " (Nano Lett for example, 2011, the resistive characteristic of the high density nano-array device of 11:4601-4606) reporting, paper " Metal – Insulator Transition in Au-NiO-Ni Dual Schottky Nanojunctions " (Nanotechnology, 2009, the electrochemical deposition method of 20:455203) reporting prepares the NiO nano wire, its preparation method is complicated, cost is high, because microstructure is limit, research to its resistive characteristic limits to some extent, and the device stores performance of making is good not, can't be directly used at present industrial nanometer storing device, this is a great problem that needs to be resolved hurrily.
Summary of the invention
Problem for the prior art existence, the invention provides a kind of nanoparticulate thin films with resistance-change memory characteristic and preparation method thereof, purpose is when effectively dwindling the storage component part size, can also reduce the leakage phenomenon in storing process, can directly apply to memory as a kind of change resistance layer.
A kind of nanoparticulate thin films with resistance-change memory characteristic of the present invention, be have the metal oxide nanoparticles film of one deck structure at least, doped with the metal oxide nanoparticles film of metallic element or composite nanoparticle film both, its thickness is 50-1000nm, the threshold voltage of film is 1-3V, on-off ratio is 100 ~ 900, and switch is repeatable for being at least 10 times; Described metal oxide is: TiO
2, ZrO
2, Nb
2O
5, Al
2O
3, SnO
2, one or more in ZnO, NiO form in any proportion, the metallic element of described doping is one or more in Ag, Li, Ru, Eu, La, Ce, Cu, and the doping ratio of metallic element is metallic element in molar ratio: metal oxide=(1 ~ 30): 100.
Preparation method with nanoparticulate thin films of resistance-change memory characteristic of the present invention carries out according to following steps:
(1) adopt sol-gal process to prepare respectively metal oxide sol or doped with the metal-oxide composite sol of metallic element; Described metal oxide is TiO
2, ZrO
2, Nb
2O
5, Al
2O
3, SnO
2, one or more in ZnO, NiO; Described doped metallic elements is one or more in Ag, Li, Ru, Eu, La, Ce, Cu, and the doping ratio of metallic element is metallic element in molar ratio: metal oxide=(1 ~ 30): 100;
(2) splash into respectively ammoniacal liquor or sodium hydroxide solution in the colloidal sol that makes, regulate pH value to 8-13, water bath with thermostatic control 8-12h under 80 ℃ of conditions obtains nanoparticle sol;
(3) nanoparticle sol is put into centrifuge centrifugal with the speed of 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing, obtain the metal oxide nanoparticles of heterogeneity or doped with the metal oxide nanoparticles of metallic element;
(4) select silicon chip or ITO as substrate, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinse with absolute ethyl alcohol, dry on heating platform afterwards;
(5) nano particle that obtains is scattered in absolute ethyl alcohol, be spin-coated on successively on substrate according to variety classes, in 80 ℃ of drying and processing 20-30min, finally obtain thickness and be the metal oxide nanoparticles film with one deck structure at least of 50-1000nm, doped with the metal oxide nanoparticles film of metallic element or composite nanoparticle film both.
Compared with prior art, characteristics of the present invention and beneficial effect are:
(1) it is high that the nanoparticulate thin films defective that is applied to non-volatility memorizer of the present invention's preparation is less, compactness reaches smoothness well; Nano particle is less, density is high and be evenly distributed.
(2) the prepared nanoparticulate thin films threshold voltage ranges of the present invention is at 1-3V, and switch can reach two orders of magnitude, and the switch repeatability is more than 10 times, and resistance state conversion stability better.
(3) preparation method of the present invention adopts sol-gal process and low temperature immersion method, and depositing device is simple, cost is low, film composition easy to control.
Description of drawings
Fig. 1 is the process chart that the present invention prepares nanoparticulate thin films;
Fig. 2 is the voltage-current characteristic testing apparatus figure that the present invention prepares nanoparticulate thin films;
Fig. 3 is the nanoparticulate thin films I-V characteristic curve of the embodiment of the present invention 1 preparation, the scanning direction be 0V →-4V → 4V → 0V, change low resistance state at-1V left and right film, i.e. ON state, film transforms back into high-impedance state when being scanned up to the 1V left and right, i.e. OFF state;
Fig. 4 is 9 scan round I-V curves of nanoparticulate thin films of the embodiment of the present invention 1 preparation;
Fig. 5 is transmission electron microscope (TEM) picture of the prepared nano particle of the embodiment of the present invention 1;
Fig. 6 is atomic force microscope (AFM) shape appearance figure of the prepared nanoparticulate thin films of the embodiment of the present invention 1;
Fig. 7 is the X-ray micro-zone analysis (EDS) of the prepared nanoparticulate thin films of the embodiment of the present invention 1.
Embodiment
The embodiment of the present invention adopts sol-gal process to prepare metal oxide and doped with the method for the metal oxide of metallic element at application number is: open in 201110329169.8 patent.
Be by liquid gallium indium microdrop technique, film sample to be carried out volt-ampere (I-V) characteristic test in the embodiment of the present invention, the electrology characteristic of checking film is by size and the film morphology of transmission electron microscope and AFM Analysis nano particle.
Further illustrate the specific embodiment of the present invention by embodiment, but be not only to be confined to embodiment, it is pure that in the embodiment of the present invention, chemical reagent used is analysis.
A kind of nanoparticulate thin films with resistance-change memory characteristic, the thickness that is one deck structure are the Eu-Ru codope nickel tin composite nanoparticle film of 50-1000nm, and the threshold voltage of film is 2V, and on-off ratio is 900, and switch is repeatable for being at least 10 times.
Its preparation method is:
(1) the employing sol-gal process prepares the metal-oxide composite sol doped with metallic element: take 1.19 to 1.20g Ni (CH
3COO)
24H
2O is dissolved in the 24mL absolute ethyl alcohol, adds 0.069 to 0.070g RuCl after stirring 20 min under the water bath condition of 60 ℃
33H
2Then O continues to stir 60 min, obtains the nickel oxide colloidal sol of Ru doping, Ni in colloidal sol
2+Concentration is 0.2 mol/L, Ni in colloidal sol
2+With Ru
3+Mol ratio be 100:7;
Take 0.36 to 0.37g SnCl when stirring
22H
2O is dissolved in the 8mL absolute ethyl alcohol, adds 0.113 to 0.114g Eu (NO after stirring 20min under the water bath condition of 60 ℃
3)
36H
2Then O continues to stir 60min, obtains the tin ash colloidal sol of Eu doping, Sn in colloidal sol
4+Concentration is 0.2mol/L, Sn
2+With Eu
3+Mol ratio be 100:7;
Mix at last two kinds of colloidal sols and stir 1h under the water bath condition of 60 ℃, obtain the nickel tin complex sol of Ru-Eu codope, with its still aging 24h in air;
(2) splash into ammoniacal liquor in the colloidal sol that makes, regulate pH value to 8, water bath with thermostatic control 8h under 80 ℃ of conditions obtains nanoparticle sol;
(3) nanoparticle sol is put into centrifuge centrifugal with 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing;
(4) selecting ITO is substrate, and substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinses with absolute ethyl alcohol, dries on heating platform afterwards;
(5) the Eu-Ru codope nickel tin composite nanoparticle that obtains is scattered in absolute ethyl alcohol, and be spin-coated on the ITO substrate, in 80 ℃ of drying and processing 20min, obtaining thickness is the Eu-Ru codope nickel tin composite nanoparticle film of 50-1000nm, and it is carried out voltage-current characteristic test, as Fig. 2-shown in Figure 4, the threshold voltage that can find out film is 2V, its switch repeatability is good, is at least 10 times, and on-off ratio is 900 after tested; Its TEM and AFM picture such as Fig. 5, shown in Figure 6, as can be seen from the figure the particle diameter of single nano particle is about 10 to 30nm, and the compactness of film is better, and nano particle is evenly distributed.
A kind of nanoparticulate thin films with resistance-change memory characteristic is Ag doping SnO
2The double-decker film of nanoparticulate thin films and Li doping zinc oxide nanometer particle Film laminated, thickness is 300-700nm, and the threshold voltage of film is 1V, and on-off ratio is 800, and switch is repeatable for being at least 10 times.
Its preparation method is:
(1) the employing sol-gal process prepares the metal-oxide composite sol doped with metallic element: take 2.16 to 2.17g Zn (CH
3COO)
22H
2O is dissolved in the 24mL absolute ethyl alcohol, adds the LiCl of 0.05-0.06g after stirring 20 min under the water bath condition of 60 ℃, then continues to stir 60min, obtains the zinc oxide colloidal sol of Li doping, Zn in colloidal sol
2+Concentration is 0.4 mol/L, Zn
2+With Li
+Mol ratio be 100:17;
Take 2.16 to 2.17g SnCl when stirring
22H
2O is dissolved in the 24mL absolute ethyl alcohol, adds 0.02 to 0.03g AgNO after stirring 20min under the water bath condition of 60 ℃
3, then continue to stir 60min, obtain the tin ash colloidal sol of Ag doping, Sn in colloidal sol
4+Concentration is 0.4mol/L, Sn
4+With Ag
+Mol ratio be 100:1;
With two kinds of colloidal sols still aging 24h in air;
(2) splash into respectively sodium hydroxide solution in two kinds of colloidal sols that make, regulate pH value to 10, respectively at water bath with thermostatic control 10h under 80 ℃ of conditions, obtain two kinds of different nanoparticle sols;
(3) respectively two kinds of nanoparticle sols are put into centrifuge centrifugal with 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing, obtain Li doping zinc oxide nanometer particle and Ag doping SnO
2Nano particle;
(4) selecting silicon chip is substrate, and substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinses with absolute ethyl alcohol, dries on heating platform afterwards;
(5) with the Li doping zinc oxide nanometer particle and the Ag doping SnO that obtain
2Nano particle is scattered in respectively in absolute ethyl alcohol, and SnO first adulterates Ag
2Nano particle is spin-coated on silicon chip, and then spin coating Li doping zinc oxide nanometer particle, be placed in drying and processing 25min on 80 ℃ of heating platforms, the final approximately double-decker nanoparticulate thin films of 300-700nm of thickness that forms, the threshold voltage of film is 1V after testing, its switch repeatability is good, is at least 10 times, and on-off ratio is 800 after tested.
A kind of nanoparticulate thin films with resistance-change memory characteristic is NiO/TiO
2The nanoparticulate thin films of/NiO sandwich, thickness are 600-1000nm, and the threshold voltage of film is 3V, and on-off ratio is 500, and switch is repeatable for being at least 10 times.
Its preparation method is:
(1) the employing sol-gal process prepares the metal-oxide composite sol doped with metallic element: take 1.19 to 1.20g Ni (CH
3COO)
24H
2O is dissolved in the 24mL absolute ethyl alcohol, stirs 60 min under the water bath condition of 60 ℃, obtains nickel oxide colloidal sol, Ni in colloidal sol
2+Concentration is 0.2 mol/L;
Take 18ml Ti (OC when stirring
4O
9)
4, be dissolved in the 24mL absolute ethyl alcohol, stir 60min under the water bath condition of 60 ℃, obtain TiO 2 sol, Ti in colloidal sol
4+Concentration is 0.2mol/L;
With two kinds of colloidal sols still aging 24h in air;
(2) splash into respectively sodium hydroxide solution in two kinds of colloidal sols that make, regulate pH value to 13, respectively at water bath with thermostatic control 12h under 80 ℃ of conditions, obtain two kinds of different nanoparticle sols;
(3) respectively two kinds of nanoparticle sols are put into centrifuge centrifugal with 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing, obtain NiO nanoparticle and titanium dioxide nano-particle;
(4) selecting silicon chip is substrate, and substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinses with absolute ethyl alcohol, dries on heating platform afterwards;
(5) with the NiO nano particle and the TiO that obtain
2Nano particle is scattered in absolute ethyl alcohol, and presses NiO, TiO
2, NiO order successively be spin-coated on silicon chip, form the approximately sandwich of 600-1000nm of thickness, be placed in drying and processing 30min on 80 ℃ of heating platforms, finally obtain the composite nanoparticle film, after testing, the threshold voltage of film is 3V, and its switch repeatability is good, be at least 10 times, on-off ratio is 500 after tested.
Embodiment 4
A kind of nanoparticulate thin films with resistance-change memory characteristic is the niobium zinc composite nanoparticle film of the copper doping of single layer structure, and thickness is 50-300nm, and the threshold voltage of film is 2.5V, and on-off ratio is 300, and switch is repeatable for being at least 10 times.
Its preparation method is:
(1) the employing sol-gal process prepares the metal-oxide composite sol doped with metallic element: take 0.6 to 0.7g Nb (C
2H
5O)
5, be dissolved in the 24mL absolute ethyl alcohol, stir 20min under the water bath condition of 60 ℃, obtain niobium oxide colloidal sol, Nb in colloidal sol
2+Concentration is 0.2 mol/L;
Take 4.38 to 4.39g Zn (CH when stirring
3COO)
22H
2O is dissolved in the 24mL absolute ethyl alcohol, stirs 20min under the water bath condition of 60 ℃, obtains zinc oxide colloidal sol, Zn in colloidal sol
2+Concentration is 0.8mol/L;
With two kinds of colloidal sols by volume 4:1 mix and add 0.2 to 0.3g Cu (NO
3)
23H
2O continues to stir 30min, obtains the niobium zinc complex sol of copper doping, and the mol ratio of Zn and Cu is 100:5, at last mixed sols is placed in air ageing 24h;
(2) splash into ammoniacal liquor in the colloidal sol that makes, regulate pH value to 13, water bath with thermostatic control 12h under 80 ℃ of conditions obtains the niobium zinc nanoparticle sol that copper adulterates;
(3) nanoparticle sol is put into centrifuge centrifugal with 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing, obtain the niobium zinc nano particle of copper doping;
(4) selecting ITO is substrate, and substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinses with absolute ethyl alcohol, dries on heating platform afterwards;
(6) the niobium zinc composite nanoparticle that the copper that obtains is adulterated is scattered in absolute ethyl alcohol, and be spin-coated on the ITO substrate, thickness is 50-300nm approximately, be placed in drying and processing 20min on 80 ℃ of heating platforms, after testing, the threshold voltage of film is 2.5V, and its switch repeatability is good, be at least 10 times, on-off ratio is 300 after tested.
A kind of nanoparticulate thin films with resistance-change memory characteristic is the La doped with Al
2O
3Nanoparticulate thin films, the Ce ZrO that adulterates
2The compound structure film of nanoparticulate thin films and NiO nanoparticulate thin films, thickness are 600-1000nm, and the threshold voltage of film is 2 V, and on-off ratio is 100, and switch is repeatable for being at least 10 times.
(1) the employing sol-gal process prepares the metal-oxide composite sol doped with metallic element: take 3.6 to 3.7g Al (NO
3)
39H
2O is dissolved in the 24mL absolute ethyl alcohol, adds the La (NO of 1.5-4.6g after stirring 20 min under the water bath condition of 60 ℃
3)
36H
2Then O continues to stir 60min, obtains the alumina sol of La doping, Al in colloidal sol
3+Concentration is 0.4 mol/L, and the mol ratio of Al and La is 100:30;
Take 3.1 to 3.2g ZrOCl when stirring
28H
2O is dissolved in the 24mL absolute ethyl alcohol, adds 0.3 to 0.4g Ce (NO after stirring 20min under the water bath condition of 60 ℃
3)
26H
2Then O continues to stir 60min, obtains the zirconia sol of Ce doping, Zr in colloidal sol
4+Concentration is 0.4mol/L, and the mol ratio of Zr and Ce is 100:7;
With two kinds of colloidal sols still aging 24h in air;
Take 1.19 to 1.20g Ni (CH
3COO)
24H
2O is dissolved in the 24mL absolute ethyl alcohol, stirs 60 min under the water bath condition of 60 ℃, obtains nickel oxide colloidal sol, Ni in colloidal sol
2+Concentration is 0.2 mol/L.
(2) splash into respectively ammoniacal liquor in three kinds of colloidal sols that make, regulate pH value to 8, water bath with thermostatic control 8h under 80 ℃ of conditions obtains three kinds of nanoparticle sols;
(3) three kinds of nanoparticle sols are put into respectively centrifuge centrifugal with 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing, obtain the La doped with Al
2O
3Nano particle, the Ce ZrO that adulterates
2Nano particle and NiO nano particle;
(4) selecting ITO is substrate, and substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinses with absolute ethyl alcohol, dries on heating platform afterwards;
(5) with the La doped with Al that obtains
2O
3Nano particle, the Ce ZrO that adulterates
2Nano particle and NiO nano particle are scattered in respectively in absolute ethyl alcohol, first with the La doped with Al
2O
3Nano particle is spin-coated on the ITO substrate, rear spin coating Ce doping ZrO
2Nano particle, spin coating NiO nano particle forms laminated construction again, thickness is 600-1000nm approximately, be placed in drying and processing 20min on 80 ℃ of heating platforms, finally obtain the nanoparticulate thin films of composite construction, after testing, the threshold voltage of film is 2V, its switch repeatability is good, is at least 10 times, and on-off ratio is 100 after tested.
Embodiment 6
A kind of nanoparticulate thin films with resistance-change memory characteristic, the NiO nanoparticulate thin films of individual layer, thickness are 60-200nm, and the threshold voltage of film is 1.5 V, and on-off ratio is 300, and switch is repeatable for being at least 10 times.
Its preparation method is:
(1) take 1.19 to 1.20g Ni (CH
3COO)
24H
2O is dissolved in the 24mL absolute ethyl alcohol, stirs 60 min under the water bath condition of 60 ℃, obtains nickel oxide colloidal sol, Ni in colloidal sol
2+Concentration is 0.2 mol/L;
(2) splash into ammoniacal liquor in the colloidal sol that makes, regulate pH value to 13, water bath with thermostatic control 10h under 80 ℃ of conditions obtains nanoparticle sol;
(3) nanoparticle sol is put into centrifuge centrifugal with 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing, obtain the NiO nano particle;
(4) selecting ITO is substrate, and substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinses with absolute ethyl alcohol, dries on heating platform afterwards;
(5) be scattered in respectively the NiO nano particle that obtains in absolute ethyl alcohol, the NiO nano particle is spin-coated on the ITO substrate forms single layer structure, thickness is 60-200nm approximately, be placed in drying and processing 20min on 80 ℃ of heating platforms, finally obtain the nanoparticulate thin films of composite construction, after testing, the threshold voltage of film is 1.5V, its switch repeatability is good, is at least 10 times, and on-off ratio is 300 after tested.
Claims (3)
1. nanoparticulate thin films with resistance-change memory characteristic, it is characterized in that having the metal oxide nanoparticles film of one deck structure at least, doped with the metal oxide nanoparticles film of metallic element or composite nanoparticle film both, its thickness is 50-1000nm, the threshold voltage of film is 1-3V, on-off ratio is 100 ~ 900, and switch is repeatable for being at least 10 times.
2. a kind of nanoparticulate thin films with resistive characteristic according to claim 1, is characterized in that described metal oxide is: TiO
2, ZrO
2, Nb
2O
5, Al
2O
3, SnO
2, one or more in ZnO, NiO form in any proportion, the metallic element of described doping is one or more in Ag, Li, Ru, Eu, La, Ce, Cu, and the doping ratio of metallic element is metallic element in molar ratio: metal oxide=(1 ~ 30): 100.
3. preparation method with nanoparticulate thin films of resistance-change memory characteristic is characterized in that carrying out according to following steps:
(1) adopt sol-gal process to prepare respectively metal oxide sol or doped with the metal-oxide composite sol of metallic element; Described metal oxide is TiO
2, ZrO
2, Nb
2O
5, Al
2O
3, SnO
2, one or more in ZnO, NiO; Described doped metallic elements is one or more in Ag, Li, Ru, Eu, La, Ce, Cu, and the doping ratio of metallic element is metallic element in molar ratio: metal oxide=(1 ~ 30): 100;
(2) splash into respectively ammoniacal liquor or sodium hydroxide solution in the colloidal sol that makes, regulate pH value to 8-13, water bath with thermostatic control 8-12h under 80 ℃ of conditions obtains nanoparticle sol;
(3) nanoparticle sol is put into centrifuge centrifugal with the speed of 4000r/min, be precipitated thing and supernatant, discard supernatant, with deionized water and absolute ethyl alcohol washing and precipitating thing, obtain the metal oxide nanoparticles of heterogeneity or doped with the metal oxide nanoparticles of metallic element;
(4) select silicon chip or ITO as substrate, substrate is successively cleaned 10min at acetone, absolute ethyl alcohol and deionized water for ultrasonic ripple, then rinse with absolute ethyl alcohol, dry on heating platform afterwards;
(5) nano particle that obtains is scattered in absolute ethyl alcohol, be spin-coated on successively on substrate according to variety classes, in 80 ℃ of drying and processing 20-30min, finally obtain thickness and be the metal oxide nanoparticles film with one deck structure at least of 50-1000nm, doped with the metal oxide nanoparticles film of metallic element or composite nanoparticle film both.
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