CN110204216A - A kind of ZnO nano-band and preparation method thereof - Google Patents

A kind of ZnO nano-band and preparation method thereof Download PDF

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Publication number
CN110204216A
CN110204216A CN201910560639.8A CN201910560639A CN110204216A CN 110204216 A CN110204216 A CN 110204216A CN 201910560639 A CN201910560639 A CN 201910560639A CN 110204216 A CN110204216 A CN 110204216A
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band
zno nano
zno
preparation
glass substrate
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杨为家
刘俊杰
刘铭全
何鑫
陈柏桦
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Wuyi University
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Wuyi University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23Oxides
    • C03C17/245Oxides by deposition from the vapour phase
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/21Oxides
    • C03C2217/216ZnO
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/71Photocatalytic coatings
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/15Deposition methods from the vapour phase
    • C03C2218/151Deposition methods from the vapour phase by vacuum evaporation
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/17Deposition methods from a solid phase
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/30Aspects of methods for coating glass not covered above
    • C03C2218/31Pre-treatment
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/30Aspects of methods for coating glass not covered above
    • C03C2218/32After-treatment

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

The present invention provides a kind of ZnO nano-band and preparation method thereof, the ZnO nano-band includes glass, and it is evenly distributed on the ZnO nano-band on glass, preparation method includes the cleaning of glass, the preparation of precursor thin-film and high annealing, the present invention has the characteristics that preparation process is simple, good dispersion, Preparation equipment of the present invention is mature simultaneously, has interests to reduce production cost.In addition, ZnO nano-band dispersibility prepared by the present invention is preferably, there are interests to increase the specific surface area of nano material.The present invention prepares ZnO nano-band and has a good application prospect in fields such as photocatalytic degradation, gas sensings.

Description

A kind of ZnO nano-band and preparation method thereof
Technical field
The present invention relates to technical field of nano material, especially a kind of ZnO nano-band and preparation method thereof.
Background technique
Zinc oxide (ZnO) is a kind of third generation semiconductor material, it has, and forbidden bandwidth is larger, chemical stability is good, raw The many merits such as object compatibility is good, preparation method is simple, the wide Eg=3.37eV of forbidden band at room temperature, exciton confinement 60meV can be can reach, the 25meV much higher than GaN, thus receive the favor of researcher.Especially, it is received when zinc oxide is made into When rice material, because of its unique bulk effect, quantum size effect, skin effect, tunnel-effect, piezoelectric effect and photocatalysis Property etc., so that nano zinc oxide material is expected to play positive effect in fields such as optics, electricity, biomedicines.Therefore, oxygen The controllable preparation for changing zinc nano material is always a hot spot of zone material research.
Zinc oxide nano sheet is an emphasis of current research.Existing research shows that Zinc oxide nano sheet is dropped in photocatalysis The fields such as solution organic pollutant, gas sensing, biosensor have shown extremely excellent performance, before wide application Scape.
Currently, the method for preparing Zinc oxide nano sheet is more, mainly hydro-thermal method.Hydro-thermal method technique is relatively easy, cost It is cheap, thus be widely used.However, the formula that current hydro-thermal method prepares Zinc oxide nano sheet is complex, and portion Divide the growth cycle longer (more than 5 hours) or microwave-assisted of hydro-thermal method.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of ZnO nano-band and preparation method thereof, which has preparation The characteristics of simple process, good dispersion.
The technical solution of the present invention is as follows: a kind of ZnO nano-band, including glass substrate and is distributed on a glass substrate ZnO nano belt, the width of the ZnO nano belt are 160-300nm.
Further, the size of the glass substrate is 2*2cm-4 inches.
The present invention also provides a kind of preparation methods of ZnO nano-band, comprising the following steps:
S1), glass substrate is cleaned, is dried up using ethyl alcohol, deionized water ultrasonic glass cleaning 3-5 times, and using air gun;
S2), the glass substrate cleaned up is transferred in high vacuum coating equipment by the preparation of precursor thin-film, and ZnO powder is uniformly placed in tungsten boat, and then air pressure is extracted into less than or equal to 5 × 10-3Pa;Then within 5-10min Evaporation current is slowly risen into 100-140A, 10-20min is deposited, amorphous ZnO forerunner can be obtained on a glass substrate Body thin film;
S3), the precursor thin-film prepared is transferred in annealing furnace by high annealing, with 4-10 DEG C/min of rate It is warming up to 500-600 DEG C, 60-120 minutes is kept the temperature, equally distributed ZnO nano-band can be obtained on glass.
Further, step S1) in, the size of the glass substrate is 2*2cm-4 inches.
Further, step S2) in, the purity of the ZnO powder is greater than 99.9%.
Further, step S3) in, the width of the ZnO nano-band is 160-300nm.
Further, the present invention prepares ZnO nano-band and is mainly used in photocatalytic degradation, gas-sensitive detector.
The invention has the benefit that
1, Preparation equipment of the present invention is mature, simple process, has interests to reduce production cost.
2, the present invention prepares ZnO nano-band dispersibility preferably, has interests to increase the specific surface area of nano material.
3, the present invention prepares ZnO nano-band and has a good application prospect in fields such as photocatalytic degradation, gas sensings.
Detailed description of the invention
Fig. 1 is low power scanning electron microscope (SEM) figure of ZnO nano-band prepared by the embodiment of the present invention 1;
Fig. 2 is high power scanning electron microscope (SEM) figure of ZnO nano-band prepared by the embodiment of the present invention 1;
Fig. 3 is X-ray diffraction (XRD) map of ZnO nano-band prepared by the embodiment of the present invention 1;
Fig. 4 is the absorption map of the photocatalytic degradation methylene blue of ZnO nano-band prepared by the embodiment of the present invention 1.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing:
Embodiment 1
A kind of preparation method of ZnO nano-band, comprising the following steps:
S1), glass substrate is cleaned, is dried up using ethyl alcohol, deionized water ultrasonic glass cleaning 3 times, and using air gun;
S2), the glass substrate cleaned up is transferred in high vacuum coating equipment by the preparation of precursor thin-film, and The ZnO powder that purity is 99.9% or more is uniformly placed in tungsten boat, and then air pressure is extracted into less than 5 × 10-3Pa;Then exist Evaporation current is slowly risen into 140A within 10min, 10min is deposited, before amorphous ZnO being obtained on a glass substrate Drive body thin film;
S3), the precursor thin-film prepared is transferred in annealing furnace by high annealing, with 10 DEG C/min of rate liter Temperature keeps the temperature 60 minutes, equally distributed ZnO nano-band can be obtained on glass to 600 DEG C.
Fig. 1 and Fig. 2 is the low power and high power scanning electron microscope (SEM) figure of ZnO nano-band manufactured in the present embodiment, from In Fig. 1 as can be seen that ZnO nano-band occupy very biggish area, and distribution uniform, from figure 2 it can be seen that sample by ZnO nano-band composition has preferable dispersibility, width 160-250nm.
Fig. 3 is X-ray diffraction (XRD) map of ZnO nano-band manufactured in the present embodiment, be can be seen that from map Occur stronger ZnO (002) diffraction maximum at 34.5 °, faint ZnO occurs at 31.5 °, 36.1 ° and 47.7 ° (100), (101) and (102) diffraction maximum, thus illustrates, growth nanobelt is ZnO.
Fig. 4 is the absorption map of the photocatalytic degradation methylene blue of ZnO nano-band manufactured in the present embodiment, can from map To find out, after the photocatalytic degradation of 2h, the trap of methylene blue is reduced to 0.81 by original 1.97, thus says Bright, ZnO nano-band has the function of preferable photocatalytic degradation.
Embodiment 2
A kind of preparation method of ZnO nano-band, comprising the following steps:
S1), glass substrate is cleaned, is dried up using ethyl alcohol, deionized water ultrasonic glass cleaning 4 times, and using air gun;
S2), the glass substrate cleaned up is transferred in high vacuum coating equipment by the preparation of precursor thin-film, and The ZnO powder that purity is 99.9% or more is uniformly placed in tungsten boat, and then air pressure is extracted into less than 5 × 10-3Pa;Then exist Evaporation current is slowly risen into 100A within 8min, 20min is deposited, before amorphous ZnO being obtained on a glass substrate Drive body thin film;
S3), the precursor thin-film prepared is transferred in annealing furnace by high annealing, with 4 DEG C/min of rate liter Temperature keeps the temperature 120 minutes, equally distributed ZnO nano-band can be obtained on glass to 500 DEG C.
Embodiment 3
A kind of preparation method of ZnO nano-band, comprising the following steps:
S1), glass substrate is cleaned, is dried up using ethyl alcohol, deionized water ultrasonic glass cleaning 5 times, and using air gun;
S2), the glass substrate cleaned up is transferred in high vacuum coating equipment by the preparation of precursor thin-film, and The ZnO powder that purity is 99.9% or more is uniformly placed in tungsten boat, and then air pressure is extracted into less than 5 × 10-3Pa;Then exist Evaporation current is slowly risen into 120A within 6min, 15min is deposited, before amorphous ZnO being obtained on a glass substrate Drive body thin film;
S3), the precursor thin-film prepared is transferred in annealing furnace by high annealing, with 7 DEG C/min of rate liter Temperature keeps the temperature 100 minutes, equally distributed ZnO nano-band can be obtained on glass to 550 DEG C.
Embodiment 4
A kind of preparation method of ZnO nano-band, comprising the following steps:
S1), glass substrate is cleaned, is dried up using ethyl alcohol, deionized water ultrasonic glass cleaning 5 times, and using air gun;
S2), the glass substrate cleaned up is transferred in high vacuum coating equipment by the preparation of precursor thin-film, and The ZnO powder that purity is 99.9% or more is uniformly placed in tungsten boat, and then air pressure is extracted into less than 5 × 10-3Pa;Then exist Evaporation current is slowly risen into 130A within 6min, 20min is deposited, before amorphous ZnO being obtained on a glass substrate Drive body thin film;
S3), the precursor thin-film prepared is transferred in annealing furnace by high annealing, with 5 DEG C/min of rate liter Temperature keeps the temperature 80 minutes, equally distributed ZnO nano-band can be obtained on glass to 580 DEG C.
The above embodiments and description only illustrate the principle of the present invention and most preferred embodiment, is not departing from this Under the premise of spirit and range, various changes and improvements may be made to the invention, these changes and improvements both fall within requirement and protect In the scope of the invention of shield.

Claims (7)

1. a kind of ZnO nano-band, it is characterised in that: including the ZnO nano-band of glass substrate and distribution on a glass substrate Layer, the width of the ZnO nano belt are 160-300nm.
2. ZnO nano-band according to claim 1, it is characterised in that: the size of the glass substrate is 2*2cm-4 English It is very little.
3. a kind of method for being used to prepare ZnO nano-band of any of claims 1 or 2, feature is satisfied with certainly, including following step It is rapid: S1), cleaning glass substrate, using ethyl alcohol, deionized water ultrasonic glass cleaning 3-5 time, and using air gun drying;
S2), the glass substrate cleaned up is transferred in high vacuum coating equipment by the preparation of precursor thin-film, and in tungsten ZnO powder is uniformly placed on boat, and then air pressure is extracted into less than or equal to 5 × 10-3Pa;Then within 5-10min slowly Evaporation current rises to 100-140A, 10-20min is deposited, it is thin amorphous ZnO precursor can be obtained on a glass substrate Film;
S3), the precursor thin-film prepared is transferred in annealing furnace by high annealing, is heated up with 4-10 DEG C/min of rate To 500-600 DEG C, 60-120 minutes are kept the temperature, equally distributed ZnO nano-band can be obtained on glass.
4. the preparation method of ZnO nano-band according to claim 3, it is characterised in that: step S1) in, the glass The size of substrate is 2*2cm-4 inches.
5. the preparation method of ZnO nano-band according to claim 3, it is characterised in that: step S2) in, the ZnO powder Purity be greater than 99.9%.
6. the preparation method of ZnO nano-band according to claim 3, it is characterised in that: step S3) in, the ZnO receives The width of rice band is 160-300nm.
7. a kind of application of the ZnO nano-band using the preparation of claim 3-6 the method, it is characterised in that: the ZnO receives Rice band is mainly used in photocatalytic degradation, gas-sensitive detector.
CN201910560639.8A 2019-06-26 2019-06-26 A kind of ZnO nano-band and preparation method thereof Pending CN110204216A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101182030A (en) * 2007-11-27 2008-05-21 华东师范大学 ZnO nano strip material and preparation method thereof
CA2619361C (en) * 2005-08-25 2015-10-20 University Of Washington Super-low fouling sulfobetaine and carboxybetaine materials and related methods
CN107492583A (en) * 2017-08-08 2017-12-19 淮阴工学院 A kind of preparation method of the UV sensor based on zinc oxide nano-belt
CN109665558A (en) * 2019-01-02 2019-04-23 吉林师范大学 A kind of preparation method of cellular single crystal ZnO nanobelt photocatalyst film
TW201946319A (en) * 2018-03-20 2019-12-01 澳大利亞商印製能源技術有限公司 Supercapacitors having frustules

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2619361C (en) * 2005-08-25 2015-10-20 University Of Washington Super-low fouling sulfobetaine and carboxybetaine materials and related methods
CN101182030A (en) * 2007-11-27 2008-05-21 华东师范大学 ZnO nano strip material and preparation method thereof
CN107492583A (en) * 2017-08-08 2017-12-19 淮阴工学院 A kind of preparation method of the UV sensor based on zinc oxide nano-belt
TW201946319A (en) * 2018-03-20 2019-12-01 澳大利亞商印製能源技術有限公司 Supercapacitors having frustules
CN109665558A (en) * 2019-01-02 2019-04-23 吉林师范大学 A kind of preparation method of cellular single crystal ZnO nanobelt photocatalyst film

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Title
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黄圣恩: "以电子束蒸镀氧化锌薄膜制作紫外光侦测器之研究", 《屏东大学应用物理系博硕士论文》 *

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Application publication date: 20190906