CN105154854A - Method for preparing load type ZnO nano-particles through molecular layer deposition - Google Patents
Method for preparing load type ZnO nano-particles through molecular layer deposition Download PDFInfo
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- CN105154854A CN105154854A CN201510652083.7A CN201510652083A CN105154854A CN 105154854 A CN105154854 A CN 105154854A CN 201510652083 A CN201510652083 A CN 201510652083A CN 105154854 A CN105154854 A CN 105154854A
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Abstract
A method for preparing load type ZnO nano-particles through molecular layer deposition comprises the following steps: mixing a carrier with ethanol, dispersing the mixture into a uniform suspension liquid, coating the uniform suspension liquid on the surface of sheet glass, leading isocyanate pulses into an MLD reaction chamber body, then leading in a zinc precursor to ensure that a monomolecular layer reaction is carried out on the surface of the carrier in sequence to obtain a base material on which the surface is deposited with a zincky organic-inorganic composite film, treating the base material in air, oxygen, hydrogen or an inert atmosphere at 250 to 900 DEG C for 1 to 2 hours, so as to remove the organic part from the zincky organic-inorganic composite film, and obtain the composite material of which the surface of the base material is deposited with ZnO nano-particles. The method has the advantages that the sizes of the prepared ZnO nano-particles are controllable, and the dispersion of the ZnO nano-particles is uniform.
Description
Technical field
The invention belongs to a kind of method that molecular-layer deposition prepares loading type ZnO nano particle.
Background technology
Nano zine oxide (1-100 nanometer) is a kind of novel high function fine inorganic material, the granular of its crystal grain causes the change of Electronic Structure and crystalline structure, thus produce the features such as surface effects, quantum size effect, macroscopical tunnel effect, high-clarity and the polymolecularity that macroscopical zinc oxide do not have, be with a wide range of applications in short wavelength light electrical equipment, varistor, gas sensor, solar cell, biomaterial, catalysis, weaving and medicine and other fields and receive much concern.
The preparation method of nano zine oxide has multiple, as vapour deposition process, oxidation style, template, such as CN101498051A disclose a kind of electrochemistry anodic oxidation and prepare zinc oxide nano array.Chinese patent CN103058264A and CN103966662A discloses and utilizes chemical Vapor deposition process to induce the grown above silicon ZnO nano array scribbling crystal seed.Patent CN103351021A discloses the method for a kind of hydrothermal oxidization legal system for nano zine oxide, and particle scale is greater than 50 nanometers.The micella that patent CN103739003A is formed with methylsulfonic acid type tensio-active agent is for template, and circumfluence method has prepared the Zinc oxide nanoparticle of dumbbell shaped.The Zinc oxide nanoparticle that patent CN103641153A then utilizes butylamine water heat transfer surface irregularity spherical.Although above method can prepare nano zine oxide, operation is various, preparation cost is high and easily pollute, and cannot prepare at the equally distributed nano zine oxide of various matrix surface.Therefore, the method developing surperficial controlled synthesis nano zine oxide is the problem that those skilled in the art need solution badly.
Summary of the invention
For prior art above shortcomings, the object of the invention is to utilize the method that molecular-layer deposition (MolecularLayerDeposition, MLD) preparation scale is controlled, disperse homogeneous loading type ZnO nano particle.
Molecular-layer deposition is that a kind of molecule rank prepares polymkeric substance or inorganic-organic polymer thin film technique.Utilize the film of molecular-layer deposition conformal on matrix surface uniform deposition, the film Zinc oxide nanoparticle that controlled acquisition yardstick is different after low-temperature heat treatment that organic moiety is different.
The technical solution used in the present invention, is characterized in that comprising the steps:
(1) by carrier and ethanol blending dispersion uniformly suspension, the concentration of sample controls at 0.01-1.0g/ml, be coated in glass sheet surface, be placed in molecular-layer deposition vacuum reaction cavity after evaporate to dryness, the temperature of cavity controls at 30-200 DEG C, be optimized for 60-150 DEG C, chamber pressure is 10-200Pa, is 1/5-1/10min by the volume ratio of carrier gas and vacuum reaction cavity
-1pass into carrier gas to cavity, in deposition process, carrier gas flux is fixed;
(2) make it, at carrier successively surface, unimolecular layer reaction occurs to reactant pulse in MLD reaction cavity
A () passes into isocyanic ester to sediment chamber's pulse, burst length 0.1-5 second, and feel suffocated reaction 1-40 second, isocyanic ester is adsorbed on carrier surface, then purges 10-120 second under vacuum;
B () pulse passes into zinc precursor and occurs to insert surperficial half-reaction, burst length 0.01-1 second, feel suffocated reaction 1-30 second, final vacuum blowing down sweep 10-120 and remove surface physics absorption raw material second;
C () pulse passes into isocyanic ester and surperficial zinc species generation surface reaction, burst length 0.1-5 second, and feel suffocated reaction 1-40 second, isocyanic ester is adsorbed on carrier surface, purges 10-200 and remove surface physics absorption raw material second under vacuum;
D () pulse passes into polyamine and surperficial isocyano and generates urea, burst length 0.01-2 second, then feels suffocated reaction 1-30 second, purges 10-120 and remove surface physics absorption raw material second under vacuum;
E () is repeated c-d step and is regulated urea element length;
F () repeating step a-e step controls inorganic-organic hybrid film thickness, hybridized film is deposited on carrier surface;
(3) surface deposition that step (2) obtained processes 1-2h containing the base material of zinc organic/inorganic composite film in air, oxygen, hydrogen or inert atmosphere at 250-900 DEG C, removing, containing the organic moiety in zinc Organic inorganic film, can obtain the matrix material of substrate material surface deposited oxide zinc nanoparticles.
Body material described in above-mentioned steps (1) is silicon chip, carbon nanotube, carbon fiber, Graphene, SBA-15, gama-alumina, and there are the various materials in hydroxyl, defect or strong physical adsorption site on the surface such as cupric oxide, metal or titanium dioxide.
In above-mentioned steps (1), rare gas element is nitrogen, argon gas or helium.
Zinc precursor described in above-mentioned steps (2) is zinc ethyl, n-propyl zinc, sec.-propyl zinc, normal-butyl zinc, isobutyl-zinc or benzyl zinc etc.
In above-mentioned steps (2), polyamine is quadrol, C2-C10 aromatic series or aliphatic polyamine;
In above-mentioned steps (2), isocyanic ester is vulcabond or C4-C12 multicomponent isocyanate.
In above-mentioned steps (2), (c) and (d) step multiplicity are 1-20 time, and (b)-(f) deposition cycle multiplicity is 10-1000 time.
Compared with prior art, the invention has the advantages that: provide a kind of molecular-layer deposition method preparing loaded nano zinc oxide, process is simple and easy to control, gained zinc oxide yardstick is little and distribute homogeneous, part nitrating Zinc oxide nanoparticle can also be obtained, can the particle scale of controlled oxidization zinc and deployment conditions by adjustment organic moiety length, multiple fields such as photochemical catalysis, sensing, microelectronics and optics can be widely used in.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of superficial molecular deposition Zn-polyureas hybridized film in embodiment 1;
Fig. 2 is embodiment 1 is carrier by sluggish precipitation gained CNTs(carbon nanotube) transmission electron microscope figure after coated Zn-polyureas hybridized film;
Fig. 3 is the transmission electron microscope figure of the coated CNTs of embodiment 1Zn-polyureas hybridized film gained ZnO/CNTs after Overheating Treatment.
Fig. 4 is embodiment 3Zn-polyureas hybridized film coated Si O
2uV, visible light photo absorption performance figure after Overheating Treatment.
embodiment
Embodiment 1:
(1) by carbon nanotube and ethanol blending dispersion uniformly suspension, the concentration of sample is 0.08g/ml, be coated in glass sheet surface, be placed in molecular-layer deposition vacuum reaction cavity after evaporate to dryness, the temperature of cavity is 100 DEG C, chamber pressure is 50Pa, is 1/8min by the volume ratio of carrier gas and vacuum reaction cavity
-1, in deposition process, carrier gas flux is fixed.
(2) make it, at sample successively surface, unimolecular layer reaction occurs to reactant pulse in MLD reaction cavity.
A () passes into PPDI to sediment chamber's pulse, 1 second raw material burst length, reaction 15 seconds of feeling suffocated, and multicomponent isocyanate is adsorbed on carrier surface, then purges 30 seconds under vacuum;
B () then pulse passes into the surperficial half-reaction of zinc ethyl generation insertion, 0.05 second burst length, reaction 15 seconds of then feeling suffocated, purge 30 seconds removing surface physics absorption raw materials under vacuum;
C () then pulse passes into PPDI and surperficial zinc species generation surface reaction, 1 second burst length, reaction 15 seconds of feeling suffocated, purge 30 seconds removing surface physics absorption raw materials under vacuum;
D () then pulse passes into quadrol and surperficial isocyano generates urea, 0.05 second burst length, reaction 10 seconds of then feeling suffocated, purge 30 seconds removing surface physics absorption raw materials under vacuum;
E () repeating step a-e step 80 hybridized film that circulates is deposited on carbon tube-surface (Fig. 2).
(3) surface deposition step (2) obtained containing the base material of zinc organic/inorganic composite film in air atmosphere in 300 DEG C of stove process 2h, removing, containing the organic moiety in zinc Organic inorganic film, can obtain the matrix material of substrate material surface deposited oxide zinc nanoparticles.Transmissioning electric mirror test nano granular of zinc oxide yardstick is 5nm, and content is 7wt%.
Embodiment 2:
(1) by Graphene and ethanol blending dispersion uniformly suspension, the concentration of sample is 0.1g/ml, be coated in glass sheet surface, be placed in molecular-layer deposition vacuum reaction cavity after evaporate to dryness, the temperature of cavity is 80 DEG C, chamber pressure is 60Pa, is 1/10min by the volume ratio of carrier gas and vacuum reaction cavity
-1, in deposition process, carrier gas flux is fixed.
(2) make it, at sample successively surface, unimolecular layer reaction occurs to reactant pulse in MLD reaction cavity.
A () passes into tolylene diisocyanate to sediment chamber, 2 seconds burst lengths, reaction 20 seconds of feeling suffocated, and multicomponent isocyanate is adsorbed on carrier surface, then purges 35 seconds under vacuum;
B () then pulse passes into the surperficial half-reaction of methyl zinc generation insertion, 0.05 second burst length, reaction 15 seconds of then feeling suffocated, purge 30 seconds removing surface physics absorption raw materials under vacuum;
C () then pulse passes into tolylene diisocyanate and surperficial zinc species generation surface reaction, 2 seconds burst lengths, reaction 20 seconds of feeling suffocated, purge 35 seconds removing surface physics absorption raw materials under vacuum;
D () then pulse passes into Putriscine and surperficial isocyano generates urea, 0.05 second burst length, reaction 10 seconds of then feeling suffocated, purge 30 seconds removing surface physics absorption raw materials under vacuum;
E () repeats c-d step 2 time;
F () repeating step a-e step 120 time obtains the coated sample of hybridized film.
(3) surface deposition that step (2) obtained containing the Graphene of zinc organic/inorganic composite film in argon gas in 350 DEG C of process 2h, removing is containing the organic moiety in zinc Organic inorganic film, can obtain the matrix material of graphenic surface deposited oxide zinc nanoparticles, graphenic surface Zinc oxide particles yardstick is 3nm.
Embodiment 3:
(1) by silicon-dioxide and ethanol blending dispersion uniformly suspension, sample concentration is 0.5g/ml, by suspension in glass sheet surface, be placed in molecular-layer deposition vacuum reaction cavity after evaporate to dryness, the temperature of cavity is 120 DEG C, chamber pressure is 40Pa, is 1/6min by the volume ratio of carrier gas and vacuum reaction cavity
-1, in deposition process, carrier gas flux is fixed.
(2) make it, at sample successively surface, unimolecular layer reaction occurs to reactant pulse in MLD reaction cavity.
A () passes into diphenylmethanediisocyanate to sediment chamber, 1.5 seconds burst lengths, reaction 10 seconds of feeling suffocated, and multicomponent isocyanate is adsorbed on carrier surface, then purges 40 seconds under vacuum;
B () then pulse passes into the surperficial half-reaction of sec.-propyl zinc generation insertion, 0.2 second burst length, reaction 15 seconds of then feeling suffocated, purge 35 seconds removing surface physics absorption raw materials under vacuum;
C () then pulse passes into diphenylmethanediisocyanate and surperficial zinc species generation surface reaction, 1.5 seconds burst lengths, reaction 20 seconds of feeling suffocated, purge 35 seconds removing surface physics absorption raw materials under vacuum;
D () then pulse passes into Ursol D and surperficial isocyano generates urea, 0.06 second burst length, reaction 15 seconds of then feeling suffocated, purge 35 seconds removing surface physics absorption raw materials under vacuum;
E () repeats c-d step 1 time;
F () repeating step a-e step 60 time obtains the coated sample of hybridized film.
(3) surface deposition that step (2) obtained containing the silicon-dioxide of zinc organic/inorganic composite film in atmosphere in 400 DEG C of process 2h, removing is containing the organic moiety in zinc Organic inorganic film, the matrix material of silica sphere deposited oxide zinc nanoparticles can be obtained, surface oxidation zinc particle scale is 3nm, and this material has good visible absorption performance as shown in Figure 4.
Embodiment 4:
(1) by titanium dioxide and ethanol blending dispersion uniformly suspension, sample concentration is 0.7g/ml, by suspension in glass sheet surface, be placed in molecular-layer deposition vacuum reaction cavity after evaporate to dryness, the temperature of cavity is 180 DEG C, chamber pressure is 90Pa, is 1/5min by the volume ratio of carrier gas and vacuum reaction cavity
-1, in deposition process, carrier gas flux is fixed.
(2) make it, at sample successively surface, unimolecular layer reaction occurs to reactant pulse in MLD reaction cavity.
A () passes into hexamethylene diisocyanate to sediment chamber, 1.5 seconds burst lengths, reaction 10 seconds of feeling suffocated, and multicomponent isocyanate is adsorbed on carrier surface, then purges 30 seconds under vacuum;
B () then pulse passes into the surperficial half-reaction of normal-butyl zinc generation insertion, 0.1 second burst length, reaction 15 seconds of then feeling suffocated, purge 35 seconds removing surface physics absorption raw materials under vacuum;
C () then pulse passes into hexamethylene diisocyanate and surperficial zinc species generation surface reaction, 3 seconds burst lengths, reaction 10 seconds of feeling suffocated, purge 30 seconds removing surface physics absorption raw materials under vacuum;
D () then pulse passes into diethylenetriamine and surperficial isocyano generates urea, 0.1 second burst length, reaction 15 seconds of then feeling suffocated, purge 35 seconds removing surface physics absorption raw materials under vacuum;
E () repeating step a-d step 60 time obtains the coated titanium dioxide of hybridized film.
(3) surface deposition that step (2) obtained containing the silicon-dioxide of zinc organic/inorganic composite film in helium in 600 DEG C of process 2h, removing is containing the organic moiety in zinc Organic inorganic film, can obtain the matrix material of silica sphere deposition carbon dope Zinc oxide nanoparticle, surface oxidation zinc particle scale is 1nm.
In addition, applicant studies discovery, utilize the inventive method can also prepare aluminum oxide, ferric oxide, stannic oxide, manganese oxide, zirconium white and etc. various load metal oxide nano material.The amendment that other foundation technical solution of the present invention are carried out or equivalent replacement, all should be encompassed in the middle of right of the present invention.
Claims (8)
1. molecular-layer deposition prepares a method for loading type ZnO nano particle, it is characterized in that comprising the steps:
(1) by carrier and ethanol blending dispersion uniformly suspension, the concentration of sample controls at 0.01-1.0g/ml, be coated in glass sheet surface, be placed in molecular-layer deposition vacuum reaction cavity after evaporate to dryness, the temperature of cavity controls at 30-200 DEG C, be optimized for 60-150 DEG C, chamber pressure is 10-200Pa, is 1/5-1/10min by the volume ratio of carrier gas and vacuum reaction cavity
-1pass into carrier gas to cavity, in deposition process, carrier gas flux is fixed;
(2) make it, at carrier successively surface, unimolecular layer reaction occurs to reactant pulse in MLD reaction cavity
A () passes into isocyanic ester to sediment chamber's pulse, burst length 0.1-5 second, and feel suffocated reaction 1-40 second, isocyanic ester is adsorbed on carrier surface, then purges 10-120 second under vacuum;
B () pulse passes into zinc precursor and occurs to insert surperficial half-reaction, burst length 0.01-1 second, feel suffocated reaction 1-30 second, final vacuum blowing down sweep 10-120 and remove surface physics absorption raw material second;
C () pulse passes into isocyanic ester and surperficial zinc species generation surface reaction, burst length 0.1-5 second, and feel suffocated reaction 1-40 second, isocyanic ester is adsorbed on carrier surface, purges 10-200 and remove surface physics absorption raw material second under vacuum;
D () pulse passes into polyamine and surperficial isocyano and generates urea, burst length 0.01-2 second, then feels suffocated reaction 1-30 second, purges 10-120 and remove surface physics absorption raw material second under vacuum;
E () is repeated c-d step and is regulated urea element length;
F () repeating step a-e step controls inorganic-organic hybrid film thickness, hybridized film is deposited on carrier surface;
(3) surface deposition that step (2) obtained processes 1-2h containing the base material of zinc organic/inorganic composite film in air, oxygen, hydrogen or inert atmosphere at 250-900 DEG C, removing, containing the organic moiety in zinc Organic inorganic film, can obtain the matrix material of substrate material surface deposited oxide zinc nanoparticles.
2. a kind of molecular-layer deposition as claimed in claim 1 prepares the method for loading type ZnO nano particle, it is characterized in that the temperature of cavity in step (1) controls at 60-150 DEG C.
3. a kind of molecular-layer deposition as claimed in claim 1 prepares the method for loading type ZnO nano particle, it is characterized in that the body material described in step (1) is silicon chip, carbon nanotube, carbon fiber, Graphene, SBA-15, gama-alumina, cupric oxide, metal or titanium dioxide.
4. a kind of molecular-layer deposition as claimed in claim 1 prepares the method for loading type ZnO nano particle, it is characterized in that in step (1), rare gas element is nitrogen, argon gas or helium.
5. a kind of molecular-layer deposition as claimed in claim 1 prepares the method for loading type ZnO nano particle, it is characterized in that the zinc precursor described in step (2) is zinc ethyl, n-propyl zinc, sec.-propyl zinc, normal-butyl zinc, isobutyl-zinc or benzyl zinc.
6. a kind of molecular-layer deposition as claimed in claim 1 prepares the method for loading type ZnO nano particle, it is characterized in that in step (2), polyamine is quadrol, C2-C10 aromatic series or aliphatic polyamine.
7. a kind of molecular-layer deposition as claimed in claim 1 prepares the method for loading type ZnO nano particle, it is characterized in that in step (2), isocyanic ester is vulcabond or C4-C12 multicomponent isocyanate.
8. a kind of molecular-layer deposition as claimed in claim 1 prepares the method for loading type ZnO nano particle, it is characterized in that in step (2), (c) and (d) step multiplicity are 1-20 time, (b)-(f) deposition cycle multiplicity is 10-1000 time.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531891A (en) * | 2018-05-18 | 2018-09-14 | 南京工业大学 | A kind of method and application preparing gas filtration film using molecule and technique for atomic layer deposition |
| CN110512189A (en) * | 2019-06-14 | 2019-11-29 | 邱越 | A kind of aperture adjustable porous metal oxide preparation method based on molecular-layer deposition |
| CN111499479A (en) * | 2020-04-14 | 2020-08-07 | 西安近代化学研究所 | Combustion speed regulator for carbon-based zinc oxide composite propellant and low-temperature preparation method thereof |
| CN111816876A (en) * | 2020-06-30 | 2020-10-23 | 南京大学 | Lithium ion battery anode material taking quantum dot @ carbon film as protective layer and preparation method thereof |
| CN115124727A (en) * | 2022-07-08 | 2022-09-30 | 中国科学院山西煤炭化学研究所 | Preparation method of MOF film |
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| CN1377991A (en) * | 2002-01-30 | 2002-11-06 | 吉林大学 | MOCVD equipment and process for growing ZnO film |
| CN104846369A (en) * | 2015-03-30 | 2015-08-19 | 陕西科技大学 | Method for preparing super-hydrophilic and hydrophobic composite nano array interface material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531891A (en) * | 2018-05-18 | 2018-09-14 | 南京工业大学 | A kind of method and application preparing gas filtration film using molecule and technique for atomic layer deposition |
| CN110512189A (en) * | 2019-06-14 | 2019-11-29 | 邱越 | A kind of aperture adjustable porous metal oxide preparation method based on molecular-layer deposition |
| CN111499479A (en) * | 2020-04-14 | 2020-08-07 | 西安近代化学研究所 | Combustion speed regulator for carbon-based zinc oxide composite propellant and low-temperature preparation method thereof |
| CN111499479B (en) * | 2020-04-14 | 2021-11-23 | 西安近代化学研究所 | Combustion speed regulator for carbon-based zinc oxide composite propellant and low-temperature preparation method thereof |
| CN111816876A (en) * | 2020-06-30 | 2020-10-23 | 南京大学 | Lithium ion battery anode material taking quantum dot @ carbon film as protective layer and preparation method thereof |
| CN111816876B (en) * | 2020-06-30 | 2021-11-12 | 南京大学 | Lithium ion battery anode material taking quantum dot @ carbon film as protective layer and preparation method thereof |
| CN115124727A (en) * | 2022-07-08 | 2022-09-30 | 中国科学院山西煤炭化学研究所 | Preparation method of MOF film |
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