CN107673401A - A kind of preparation method of nanoscale ZnS films - Google Patents
A kind of preparation method of nanoscale ZnS films Download PDFInfo
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- CN107673401A CN107673401A CN201711011927.5A CN201711011927A CN107673401A CN 107673401 A CN107673401 A CN 107673401A CN 201711011927 A CN201711011927 A CN 201711011927A CN 107673401 A CN107673401 A CN 107673401A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/287—Chalcogenides
- C03C2217/288—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
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- Organic Chemistry (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)
- Inorganic Chemistry (AREA)
- Electroluminescent Light Sources (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of nanoscale ZnS films.Using soluble zinc salt, ammoniacal liquor, thiocarbamide as raw material, using glass as substrate, by strictly controlling the concentration of each raw material, hydro-thermal reaction is carried out between 150 180 DEG C, the reaction time is 20 40min, obtains nano level film of the thickness between 80 160nm.The temperature and time of hydro-thermal reaction is controlled by crossing, can regulate and control to obtain the nanoscale ZnS films of different-thickness, so as to meet different requirements.The preparation method of nanoscale ZnS films disclosed by the invention, raw materials used simple and easy to get, method and step is few, easily operated, obtained nanoscale ZnS film qualities are good, and thickness is small, and production cost is low, equipment requirement is relatively low, simple and easy to do, has higher application value.
Description
Technical field
The invention belongs to field of film preparation, and in particular to a kind of preparation method of nanoscale ZnS films.
Background technology
Zinc sulphide is a kind of direct wide bandgap semiconductor materials, and band gap width reaches 3.5~3.7eV, is had excellent glimmering
Luminous effect and luminescence generated by light function, it has been widely used for luminescence generated by light, electroluminescent and cathodoluminescence as luminescent material
Device, and photocatalytic device, solar cell and many other photoelectric devices can also be applied to, therefore grinding on ZnS
Study carefully by people's extensive concern.
ZnS films, it is for a kind of visible and infrared region most important thin-film material.In visual field, its often with low folding
Penetrate that the fluoride of rate is combined, it is then often combined with the semi-conducting material of high index of refraction in infrared region, it is visible and infrared to form
The various optical filters in area.In addition, ZnS films are also widely used for the window element of infrared region.
Chemical vapour deposition technique and physical vaporous deposition are usually used in preparing ZnS films.
But when ZnS thin-film depositions are when on room temperature substrate, its film layer fastness is often very poor；If it is deposited on 150 ~ 200
DEG C substrate on, film layer after deposit toasts 4 ~ 8h at 250 ~ 300 DEG C in atmosphere, then film layer firmness is significantly changed
It is kind, if implementing Ions Bombardment also can obtain similar result.But ZnS films, in dry air, its refractive index is with the time
Increase and increase, film can soften in malaria.
In view of this, it is desirable to provide a kind of method for preparing ZnS films, and its thickness is adjusted as needed, such as obtain thickness
Degree is in nano level ZnS films.
The content of the invention
It is an object of the invention to provide a kind of preparation method of nanoscale ZnS films, meet the use need to ultra-thin ZnS films
Ask.
Technical scheme is as follows：
A kind of preparation method of nanoscale ZnS films, comprises the following steps：
（1）Soluble zinc salt, ammoniacal liquor, thiocarbamide are dissolved in deionized water reaction solution is made, then add hydrothermal reaction kettle
In；
（2）The glass substrate of wash clean is put into the hydrothermal reaction kettle, the glass substrate slant setting, with the water
The bottom surface angle of thermal response kettle is controlled between 40-60 degree；
（4）The hydrothermal reaction kettle is heated, between controlling reaction temperature is 150-180 DEG C, reaction time 20-40min；
（5）The ZnS films being deposited in the glass substrate are gently separated, are then cleaned by ultrasonic, naturally dry；
Wherein, the concentration of soluble chromic salts described in the reaction solution is 5-8mmol/L, and the concentration of the thiocarbamide is 50-
100mmol/L, the ammonia concn are 150mmol/L；
The thickness of the nanoscale ZnS films is 80-160nm.
Further, the soluble zinc salt is the one or more in zinc sulfate, zinc acetate, zinc chloride.
Further, step（4）In, in reaction temperature one regularly, by controlling the reaction time to control the nanoscale ZnS
The thickness of film, specially as the reaction time extends, the thickness increase of the nanoscale ZnS films.
Further, step（4）In, in the timing of reaction time one, the nanoscale ZnS is controlled by controlling reaction temperature
The thickness of film, specially with the rise of reaction temperature, the thickness increase of the nanoscale ZnS films.
Further, step is worked as（4）Middle reaction temperature is 160 DEG C, when the reaction time is 30min, obtained nanoscale ZnS
The thickness of film is between 110-130nm.
The present invention is raw material with simple soluble zinc salt, ammoniacal liquor, thiocarbamide, and nanoscale ZnS films are prepared using hydro-thermal method,
By strictly controlling the concentration of each raw material, nano level film is obtained, the temperature and time for controlling hydro-thermal reaction is crossed, can regulate and control
The nanoscale ZnS films of different-thickness are obtained, so as to meet different requirements.
Technical scheme, raw materials used simple and easy to get, method and step is few, easily operated, obtained nanoscale ZnS
Film quality is good, and thickness is small, and production cost is low, and equipment requirement is relatively low, simple and easy to do, has higher application value.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine in any way.
This specification（Including any accessory claim, summary）Disclosed in any feature, unless specifically stated otherwise,
Replaced by other equivalent or with similar purpose alternative features.I.e., unless specifically stated otherwise, each feature is a series of
An example in equivalent or similar characteristics.
Embodiment 1
A kind of preparation method of nanoscale ZnS films, comprises the following steps：
（1）Zinc chloride, ammoniacal liquor, thiocarbamide are dissolved in deionized water reaction solution is made, chlorination zinc concentration in reaction solution
For 5mmol/L, the concentration of thiocarbamide is 50mmol/L, ammonia concn 150mmol/L, is then added in hydrothermal reaction kettle；
（2）The glass substrate of wash clean is put into the hydrothermal reaction kettle, the glass substrate slant setting, with the water
The bottom surface angle of thermal response kettle is controlled at 40 degree；
（4）The hydrothermal reaction kettle is heated, controlling reaction temperature is 150 DEG C, reaction time 20min；
（5）The ZnS films being deposited in the glass substrate are gently separated, are then cleaned by ultrasonic, naturally dry.
The thickness of obtained nanoscale ZnS films is 80nm or so.
Embodiment 2
A kind of preparation method of nanoscale ZnS films, comprises the following steps：
（1）Zinc sulfate, ammoniacal liquor, thiocarbamide are dissolved in deionized water reaction solution is made, chlorination zinc concentration in reaction solution
For 6mmol/L, the concentration of thiocarbamide is 70mmol/L, ammonia concn 150mmol/L, is then added in hydrothermal reaction kettle；
（2）The glass substrate of wash clean is put into the hydrothermal reaction kettle, the glass substrate slant setting, with the water
The bottom surface angle of thermal response kettle is controlled at 50 degree；
（4）The hydrothermal reaction kettle is heated, controlling reaction temperature is 160 DEG C, reaction time 30min；
（5）The ZnS films being deposited in the glass substrate are gently separated, are then cleaned by ultrasonic, naturally dry.
The thickness of obtained nanoscale ZnS films is 120nm or so.
Embodiment 3
A kind of preparation method of nanoscale ZnS films, comprises the following steps：
（1）Zinc acetate, zinc chloride, ammoniacal liquor, thiocarbamide are dissolved in deionized water reaction solution is made, zinc chloride in reaction solution
Concentration be 8mmol/L, the concentration of thiocarbamide is 100mmol/L, ammonia concn 150mmol/L, then adds hydrothermal reaction kettle
In；
（2）The glass substrate of wash clean is put into the hydrothermal reaction kettle, the glass substrate slant setting, with the water
The bottom surface angle of thermal response kettle is controlled at 60 degree；
（4）The hydrothermal reaction kettle is heated, controlling reaction temperature is 180 DEG C, reaction time 40min；
（5）The ZnS films being deposited in the glass substrate are gently separated, are then cleaned by ultrasonic, naturally dry.
The thickness of obtained nanoscale ZnS films is 160nm or so.
Claims (5)
1. a kind of preparation method of nanoscale ZnS films, it is characterised in that the described method comprises the following steps：
（1）Soluble zinc salt, ammoniacal liquor, thiocarbamide are dissolved in deionized water reaction solution is made, then add hydrothermal reaction kettle
In；
（2）The glass substrate of wash clean is put into the hydrothermal reaction kettle, the glass substrate slant setting, with the water
The bottom surface angle of thermal response kettle is controlled between 40-60 degree；
（4）The hydrothermal reaction kettle is heated, between controlling reaction temperature is 150-180 DEG C, reaction time 20-40min；
（5）The ZnS films being deposited in the glass substrate are gently separated, are then cleaned by ultrasonic, naturally dry；
Wherein, the concentration of soluble chromic salts described in the reaction solution is 5-8mmol/L, and the concentration of the thiocarbamide is 50-
100mmol/L, the ammonia concn are 150mmol/L；
The thickness of the nanoscale ZnS films is 80-160nm.
A kind of 2. preparation method of nanoscale ZnS films according to claim 1, it is characterised in that the soluble Zn
Salt is the one or more in zinc sulfate, zinc acetate, zinc chloride.
A kind of 3. preparation method of nanoscale ZnS films according to claim 1, it is characterised in that step（4）In,
The timing of reaction temperature one, by controlling the reaction time to control the thickness of the nanoscale ZnS films, specially with the reaction time
Extend, the thickness increase of the nanoscale ZnS films.
A kind of 4. preparation method of nanoscale ZnS films according to claim 1, it is characterised in that step（4）In,
The timing of reaction time one, the thickness of the nanoscale ZnS films is controlled by controlling reaction temperature, specially with reaction temperature
Rise, the nanoscale ZnS films thickness increase.
5. the preparation method of a kind of nanoscale ZnS films according to claim 1, it is characterised in that work as step（4）In it is anti-
It is 160 DEG C to answer temperature, and when the reaction time is 30min, the thickness of obtained nanoscale ZnS films is between 110-130nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711011927.5A CN107673401A (en) | 2017-10-25 | 2017-10-25 | A kind of preparation method of nanoscale ZnS films |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711011927.5A CN107673401A (en) | 2017-10-25 | 2017-10-25 | A kind of preparation method of nanoscale ZnS films |
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| CN107673401A true CN107673401A (en) | 2018-02-09 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557719A (en) * | 2004-01-19 | 2004-12-29 | 上海交通大学 | Method for preparing zine sulfide nanometer material with orientation arrangement nano-tubes |
| CN1996623A (en) * | 2005-12-28 | 2007-07-11 | 中国科学院大连化学物理研究所 | II-VI family semiconductor thin film used for the photovoltaic cell |
| CN103496736A (en) * | 2013-09-18 | 2014-01-08 | 中山大学 | ZnS nano-crystalline film and preparation method and application thereof |
| CN104018137A (en) * | 2014-06-13 | 2014-09-03 | 北京四方继保自动化股份有限公司 | Method for preparing ZnS film by chemical bath reaction |
| CN105070664A (en) * | 2015-09-04 | 2015-11-18 | 台州学院 | Optoelectronic device ZnO/ZnS heterojunction nano-array film preparing method |
-
2017
- 2017-10-25 CN CN201711011927.5A patent/CN107673401A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557719A (en) * | 2004-01-19 | 2004-12-29 | 上海交通大学 | Method for preparing zine sulfide nanometer material with orientation arrangement nano-tubes |
| CN1996623A (en) * | 2005-12-28 | 2007-07-11 | 中国科学院大连化学物理研究所 | II-VI family semiconductor thin film used for the photovoltaic cell |
| CN103496736A (en) * | 2013-09-18 | 2014-01-08 | 中山大学 | ZnS nano-crystalline film and preparation method and application thereof |
| CN104018137A (en) * | 2014-06-13 | 2014-09-03 | 北京四方继保自动化股份有限公司 | Method for preparing ZnS film by chemical bath reaction |
| CN105070664A (en) * | 2015-09-04 | 2015-11-18 | 台州学院 | Optoelectronic device ZnO/ZnS heterojunction nano-array film preparing method |
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Application publication date: 20180209 |