CN106191985B - A kind of preparation method of stainless steel surface nanometic zinc oxide rod array - Google Patents

A kind of preparation method of stainless steel surface nanometic zinc oxide rod array Download PDF

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CN106191985B
CN106191985B CN201610503250.6A CN201610503250A CN106191985B CN 106191985 B CN106191985 B CN 106191985B CN 201610503250 A CN201610503250 A CN 201610503250A CN 106191985 B CN106191985 B CN 106191985B
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solution
stainless steel
steel surface
zinc oxide
rod array
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CN106191985A (en
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詹玮婷
倪红卫
陈荣生
刘伟
唐书杰
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Wuhan University of Science and Engineering WUSE
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
    • C30B7/105—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes using ammonia as solvent, i.e. ammonothermal processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer

Abstract

The present invention relates to a kind of preparation methods of stainless steel surface nanometic zinc oxide rod array.Its technical solution is: being first successively cleaned by ultrasonic stainless steel in dehydrated alcohol and distilled water, dries up, immerses in mixed solution, it is irradiated 1 ~ 5 time in micro-wave oven, the time irradiated every time is 0.5 ~ 10min, and the interval time irradiated every time is 5 ~ 10s to get stainless steel surface nanometic zinc oxide rod array.The mixed solution is the mixed solution of zinc ion solution, ammonium ion solution and graphene oxide solution, wherein: zinc ion solution concentration is 0.001 ~ 0.1mol/L, the concentration of ammonium ion solution is 0.001 ~ 0.1mol/L, and the concentration of graphene oxide is 0.01 ~ 2g/L.Present invention process is simple, quick, environmental-friendly and low in cost；The photocatalysis of prepared stainless steel surface nanometic zinc oxide rod array and photoelectrochemical behaviour are excellent, and the pattern and microstructure of nanostructure are controllable, be firmly combined with substrate, corrosion resistance is strong and hardness is high.

Description

A kind of preparation method of stainless steel surface nanometic zinc oxide rod array
Technical field
The invention belongs to stainless steel surface nano stick array technique fields.It is related to a kind of stainless steel surface zinc oxide nano rod The preparation method of array.
Background technique
Zinc oxide as semiconductor material research with prepare long-standing, with the development of nanometer material science, ZnO is received The research of rice array has started new upsurge.ZnO nano material is in electroluminescent, solar battery, photocatalysis and sensor etc. Field has with important application.However, the preparation and application of ZnO nano material need to be suitble to industry there is also some problems The preparation process of production and suitable substrate material are to adapt to rugged environment.Stainless steel material has superior corrosion-resistant Property, wearability and obdurability, adapt to more severe pollution environment, meanwhile, there is good workability, stability, lead Electrical property and thermal conductivity are conducive to the photocatalysis efficiency for improving ZnO nano material.Currently, the method for preparing zinc-oxide film has gold Belong to organic chemical vapor deposition, molecular beam epitaxy, pulse laser deposition, electrochemical deposition etc., these methods all exist respective Disadvantage, if equipment needed for the methods of Metallo-Organic Chemical Vapor deposition, molecular beam epitaxy, pulse laser deposition is expensive, at high cost, Substrate is required harsh；The growth time as needed for electrochemical deposition method is longer, generally at two more than hour, gained nanostructure Poor orientation.
Microwave-hydrothermal method microwave can realize that " penetration " of body phase adds by the dielectric loss of heating object confrontation microwave Heat, so that heated material can reach the height of hundreds if not thousands of degrees Celsius in the very short time (even moment) Temperature.Therefore, microwave heating show heating efficiency it is high, without thermal inertia, energy conservation and it is quick the advantages that, can easily realize quickly Heating or the large-scale production of high frequency time, while microwave process can force the substance in microwave field according to the movement side of microwave To being moved, nano material is made to tend to ordering, directionality is good.But the premise of this ordering oriented growth is by base Material surface carries out paving crystal seed film process, promotes nano material crystalline growth using crystal seed fast nucleation.Spreading crystal seed film process is one The process of a long-time repeatedly, substantially prolongs nano material preparation process, is unfavorable for industrialization promotion.
Summary of the invention
The present invention is directed to overcome defect in prior art, it is therefore an objective to provide a kind of simple and effective, environmental-friendly and at low cost Honest and clean stainless steel surface prepares the preparation method of nanometic zinc oxide rod array.The stainless steel surface zinc oxide nano prepared with this method The compound with regular structure of rice stick array is orderly, photocatalysis and photoelectrochemical behaviour are excellent, be firmly combined with substrate, corrosion resistance is strong and hard Degree is high.
To achieve the above object, the technical solution adopted by the present invention is that: first by stainless steel successively in dehydrated alcohol and distillation Be cleaned by ultrasonic in water, dry up, immerse mixed solution in, micro-wave oven irradiate 1~5 time, the time irradiated every time be 0.5~ 10min, the interval time irradiated every time are 5~10s to get stainless steel surface nanometic zinc oxide rod array.
The mixed solution is the mixed solution of zinc ion solution, ammonium ion solution and graphene oxide solution, in which: zinc Solion concentration is 0.001~0.1mol/L, and the concentration of ammonium ion solution is 0.001~0.1mol/L, graphene oxide Concentration is 0.01~2g/L；The pH value of the mixed solution is 8~10.
The zinc ion solution is one of solution of zinc sulfate, zinc nitrate solution and liquor zinci chloridi.
The ammonium ion solution is one of hexa solution, ammonium hydroxide and urea liquid.
The size of graphene oxide is 1nm~10 μm in the graphene oxide solution, and the number of plies is 1~30 layer.
The micro-wave oven is general commercial micro-wave oven or is industrial micro-wave oven, and the output power of the micro-wave oven is 50 ~500W.
By adopting the above scheme, compared with prior art, the present invention having the advantage that
1) short, simple production process the time required to preparation process of the invention, it is high-efficient；Required instrument and equipment investment It is few；Raw materials used cheap, utilization rate is high, without environmental pollution, is suitable for batch production.
2) microwave-hydrothermal method that the present invention uses belongs to non-linear process, can be to large area and complex-shaped stainless steel Product carry out nanosizing processing.
3) technological parameter of the invention accurately controls, by changing reaction time, reaction temperature, irradiation intensity and solution Concentration can adjust the pattern, composition and microstructure of ZnO nano-rod array, and directionality is good, reproducible.
4) stainless steel surface nanometic zinc oxide rod array produced by the present invention is based on graphene oxide film layer, with stainless base steel Material binding force is strong, and attachment is uniformly secured, and no obscission, corrosion resistance is strong, and hardness is high.
5) stainless steel surface the nanometic zinc oxide rod array produced by the present invention, (100mW under simulated solar irradiation irradiation cm-2) density of photocurrent be 1 × 10-4~3 × 10-4A·cm-2, and the photoelectric current of ZnO nano-rod array made from commonsense method Density is 1 × 10-6~2 × 10-5A·cm-2；90% (irradiation 60min) or more is reached to the photocatalytic activity of rhodamine B, and The degradation rate of ZnO nano-rod array made from commonsense method is 57%.The result shows that stainless steel surface zinc-oxide nano obtained Stick array has excellent photocatalysis and photoelectrochemical behaviour.
Therefore, present invention process is simple, fast and effective, environmental-friendly and low in cost；Prepared stainless steel surface oxygen Photocatalysis and the photoelectrochemical behaviour for changing zinc nanometer stick array are excellent, and the pattern and microstructure of nanostructure be controllable and substrate It is firmly combined, corrosion resistance is strong and hardness is high.
Specific embodiment
Below with reference to embodiment, the invention will be further described, not to the limitation of its protection scope.
It is first that technical parameter Unify legislation involved in present embodiment is as follows to avoid repeating:
The size of graphene oxide is 1nm~10 μm in the graphene oxide solution, and the number of plies is 1~30 layer.
Embodiment 1
A kind of preparation method of stainless steel surface nanometic zinc oxide rod array.First by stainless steel successively in dehydrated alcohol and steaming Be cleaned by ultrasonic in distilled water, dry up, immerse mixed solution in, micro-wave oven irradiate 1~2 time, the time irradiated every time be 0.5~ 1min, the interval time irradiated every time are 5~10s to get stainless steel surface nanometic zinc oxide rod array.
The mixed solution is the mixed solution of zinc ion solution, ammonium ion solution and graphene oxide solution, in which: zinc Solion concentration is 0.001~0.005mol/L, and the concentration of ammonium ion solution is 0.001~0.005mol/L, graphite oxide The concentration of alkene is 0.01~0.05g/L；The pH value of the mixed solution is 8~10.
The zinc ion solution is zinc nitrate solution.
The ammonium ion solution is ammonium hydroxide.
The micro-wave oven is industrial micro-wave oven, and the output power of the micro-wave oven is 400~500W.
Embodiment 2
A kind of preparation method of stainless steel surface nanometic zinc oxide rod array.First by stainless steel successively in dehydrated alcohol and steaming Be cleaned by ultrasonic in distilled water, dry up, immerse mixed solution in, micro-wave oven irradiate 2~3 times, the time irradiated every time be 1~ 3min, the interval time irradiated every time are 5~10s to get stainless steel surface nanometic zinc oxide rod array.
The mixed solution is the mixed solution of zinc ion solution, ammonium ion solution and graphene oxide solution, in which: zinc Solion concentration is 0.005~0.01mol/L, and the concentration of ammonium ion solution is 0.005~0.01mol/L, graphene oxide Concentration be 0.05~0.1g/L；The pH value of the mixed solution is 8~10.
The zinc ion solution is liquor zinci chloridi.
The ammonium ion solution is hexa solution.
The micro-wave oven is general commercial micro-wave oven, and the output power of the micro-wave oven is 200~400W.
Embodiment 3
A kind of preparation method of stainless steel surface nanometic zinc oxide rod array.First by stainless steel successively in dehydrated alcohol and steaming Be cleaned by ultrasonic in distilled water, dry up, immerse mixed solution in, micro-wave oven irradiate 3~4 times, the time irradiated every time be 3~ 7min, the interval time irradiated every time are 5~10s to get stainless steel surface nanometic zinc oxide rod array.
The mixed solution is the mixed solution of zinc ion solution, ammonium ion solution and graphene oxide solution, in which: zinc Solion concentration is 0.01~0.05mol/L, and the concentration of ammonium ion solution is 0.01~0.05mol/L, graphene oxide Concentration is 0.1~1g/L；The pH value of the mixed solution is 8~10.
The zinc ion solution is solution of zinc sulfate.
The ammonium ion solution is urea liquid.
The micro-wave oven is general commercial micro-wave oven, and the output power of the micro-wave oven is 100~200W.
Embodiment 4
A kind of preparation method of stainless steel surface nanometic zinc oxide rod array.First by stainless steel successively in dehydrated alcohol and steaming Be cleaned by ultrasonic in distilled water, dry up, immerse mixed solution in, micro-wave oven irradiate 4~5 times, the time irradiated every time be 7~ 10min, the interval time irradiated every time are 5~10s to get stainless steel surface nanometic zinc oxide rod array.
The mixed solution is the mixed solution of zinc ion solution, ammonium ion solution and graphene oxide solution, in which: zinc Solion concentration is 0.05~0.1mol/L, and the concentration of ammonium ion solution is 0.05~0.1mol/L, graphene oxide it is dense Degree is 1~2g/L；The pH value of the mixed solution is 8~10.
The zinc ion solution is zinc nitrate solution.
The ammonium ion solution is ammonium hydroxide.
The micro-wave oven is general commercial micro-wave oven, and the output power of the micro-wave oven is 50~100W.
Present embodiment compared with prior art, has the advantage that
1) short, simple production process the time required to the preparation process of present embodiment, it is high-efficient；Required instrument is set Standby small investment；Raw materials used cheap, utilization rate is high, without environmental pollution, is suitable for batch production.
2) microwave-hydrothermal method that present embodiment uses belongs to non-linear process, can be to large area and complex-shaped Stainless steel products carries out nanosizing processing.
3) technological parameter of present embodiment accurately controls, by changing reaction time, reaction temperature, irradiation by force Degree and solution concentration, can adjust the pattern, composition and microstructure of ZnO nano-rod array, directionality is good, reproducible.
4) stainless steel surface nanometic zinc oxide rod array made from present embodiment is based on graphene oxide film layer, with Stainless steel substrate binding force is strong, and attachment is uniformly secured, and no obscission, corrosion resistance is strong, and hardness is high.
5) stainless steel surface nanometic zinc oxide rod array made from present embodiment, under simulated solar irradiation irradiation (100mW·cm-2) density of photocurrent be 1 × 10-4~3 × 10-4A·cm-2, and ZnO nano-rod array made from commonsense method Density of photocurrent be 1 × 10-6~2 × 10-5A·cm-2；90% (irradiation is reached to the photocatalytic activity of rhodamine B More than 60min), and the degradation rate of ZnO nano-rod array made from commonsense method is 57%.The result shows that stainless steel obtained Surface oxidation zinc nanometer stick array has excellent photocatalysis and photoelectrochemical behaviour.
Therefore, present embodiment simple process, fast and effective, environmental-friendly and low in cost；Prepared is stainless The photocatalysis of steel surface nanometic zinc oxide rod array and photoelectrochemical behaviour are excellent, and the pattern and microstructure of nanostructure can It controls, be firmly combined with substrate, corrosion resistance is strong and hardness is high.

Claims (5)

1. a kind of preparation method of stainless steel surface nanometic zinc oxide rod array, it is characterised in that the preparation method is: first will Stainless steel is successively cleaned by ultrasonic in dehydrated alcohol and distilled water, and drying is immersed in mixed solution, irradiates 1~5 in micro-wave oven Secondary, the time irradiated every time is 0.5~10min, and the interval time irradiated every time is 5~10s to get stainless steel surface zinc oxide Nanometer stick array；
The mixed solution is the mixed solution of zinc ion solution, ammonium ion solution and graphene oxide solution, in which: zinc ion Solution concentration is 0.001~0.1mol/L, and the concentration of ammonium ion solution is 0.001~0.1mol/L, the concentration of graphene oxide For 0.01~2g/L；The pH value of the mixed solution is 8~10.
2. the preparation method of stainless steel surface nanometic zinc oxide rod array as described in claim 1, it is characterised in that the zinc Solion is one of solution of zinc sulfate, zinc nitrate solution and liquor zinci chloridi.
3. the preparation method of stainless steel surface nanometic zinc oxide rod array as described in claim 1, it is characterised in that the ammonia Solion is one of hexa solution, ammonium hydroxide and urea liquid.
4. the preparation method of stainless steel surface nanometic zinc oxide rod array as described in claim 1, it is characterised in that the oxygen The size of graphene oxide is 1nm~10 μm in graphite alkene solution, and the number of plies is 1~30 layer.
5. the preparation method of stainless steel surface nanometic zinc oxide rod array as described in claim 1, it is characterised in that described micro- Wave furnace is general commercial micro-wave oven or is industrial micro-wave oven, and the output power of the micro-wave oven is 50~500W.
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CN103212421A (en) * 2013-03-01 2013-07-24 北京化工大学常州先进材料研究院 Preparation method of nano-grade electro-catalyst based on graphene
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CN104549281A (en) * 2015-02-04 2015-04-29 中国科学技术大学 Active graphene-metal oxide composite photocatalyst and preparation method and application thereof
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Publication number Priority date Publication date Assignee Title
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KR101128880B1 (en) * 2011-06-23 2012-03-26 홍상휘 Method for manufacturing highgrade zinc oxide
CN102921416A (en) * 2012-11-05 2013-02-13 江苏大学 Nano composite photocatalytic material and method for preparing same
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