CN110713350B - Preparation method of one-dimensional nano silicon dioxide - Google Patents
Preparation method of one-dimensional nano silicon dioxide Download PDFInfo
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- CN110713350B CN110713350B CN201911008246.2A CN201911008246A CN110713350B CN 110713350 B CN110713350 B CN 110713350B CN 201911008246 A CN201911008246 A CN 201911008246A CN 110713350 B CN110713350 B CN 110713350B
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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
- C03C17/23—Oxides
- C03C17/245—Oxides by deposition from the vapour phase
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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
- C03C2217/21—Oxides
- C03C2217/213—SiO2
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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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/152—Deposition methods from the vapour phase by cvd
Abstract
The invention relates to a preparation method of one-dimensional nano silicon dioxide, which comprises the following steps: respectively containing a silicon source and ammonia water in two containers for later use; preparing a glass slide as a growth substrate, and cleaning and drying the glass slide for later use; placing a container containing a silicon source and ammonia water and the dried glass slide in a vacuum dryer, sealing and vacuumizing, placing the vacuum dryer in a thermostat, and preserving at constant temperature; taking out the vacuum drier from the thermostat, cooling to room temperature, taking out the glass slide from the vacuum drier, wherein the film on the surface of the glass slide is one-dimensional nano silicon dioxide; the prepared one-dimensional nano silicon dioxide consists of amorphous silicon dioxide with the diameter of 46-53 nm, and the one-dimensional nano silicon dioxide has hydrophobicity. Compared with the prior art, the method has the advantages of simple preparation method, low requirement on equipment, high synthesis efficiency and the like.
Description
Technical Field
The invention belongs to the field of nano materials and preparation thereof, and particularly relates to a preparation method of one-dimensional nano silicon dioxide.
Background
The one-dimensional nano material is an important component of future nano electronic devices and optoelectronic devices, and has good prospects in academic research and practical application. The silicon dioxide nano-rod and the silicon dioxide nano-wire are important materials in one-dimensional nano-materials. At present, the method for preparing the one-dimensional nano silicon dioxide mainly comprises the following steps: a hydrothermal method, a sol-gel technology, a template removing method, a high-temperature chemical vapor deposition method and the like are combined. In these methods, the preparation of the silica nanorods and silica nanowires is generally performed under the conditions of atmospheric pressure or low vacuum and a growth temperature of more than 1000 ℃, or complicated processes of template preparation, template removal, special process drying and the like are required. The growth environment under such conditions limits the improvement of quality and performance of the silica nanorods and nanotubes, and brings many difficulties to the study of the growth mechanism; meanwhile, the growth method is limited by instruments and environment, and cannot be widely popularized and used.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of one-dimensional nano silicon dioxide, which has the advantages of mild preparation conditions, simple preparation process and convenient adjustment of product size.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of one-dimensional nano silicon dioxide comprises the following steps:
preparation of the silicon dioxide nanorod synthetic raw material: respectively containing a silicon source and ammonia water in two containers for later use;
preparing a one-dimensional nano silicon dioxide growth substrate: preparing a glass slide as a growth substrate, and cleaning and drying the glass slide for later use;
growing the one-dimensional nano silicon dioxide by a chemical vapor deposition method: placing a container containing a silicon source and ammonia water and the dried glass slide in a vacuum dryer, sealing and vacuumizing, placing the vacuum dryer in a thermostat, and preserving at constant temperature; and taking the vacuum drier out of the thermostat, cooling to room temperature, and taking the glass slide out of the vacuum drier, wherein the film on the surface of the glass slide is the one-dimensional nano silicon dioxide.
The silicon source is methyl-trimethoxy silane; the purity can be chosen to be 98%.
The mass concentration of the ammonia water is 25-28%.
The temperature of the vacuum dryer stored in the thermostat at constant temperature is 25-102 ℃, and preferably 100 ℃.
The preservation time of the vacuum dryer in a constant temperature box for constant temperature preservation is 1-24 hours, preferably 6 hours.
And the container for containing the silicon source and the ammonia water is arranged at the bottom of the vacuum drier, and the dried glass slide is arranged on a porcelain plate of the vacuum drier.
In the chemical vapor deposition growth process of the one-dimensional nano silicon dioxide, the vacuum degree of the vacuum drier is-0.05 to-0.10 Mpa.
The cleaning and drying method specifically comprises the steps of placing the glass slide in ethanol, carrying out ultrasonic cleaning, and then blowing by using nitrogen.
The length of the prepared one-dimensional nano silicon dioxide is adjusted by the storage time of the vacuum dryer in the thermostat.
The one-dimensional nano-silica prepared by the preparation method is composed of amorphous silica with the diameter of 46-53 nm and has hydrophobicity.
The invention adopts a very simple glass vacuum dryer as reaction equipment, takes cheap methyl-trimethoxy silane and ammonia water as a silicon source and a catalyst respectively, and prepares large-area one-dimensional nano silicon dioxide by taking a milder environment of 100 ℃ as reaction temperature under the condition of no strict requirement on vacuum degree.
In order to successfully synthesize the silicon dioxide nano-rod, the speed of chemical vapor deposition, particularly suitable raw materials and suitable reaction temperature need to be controlled, so the invention optimizes the technological parameters of the preparation process, particularly the selection of a silicon source and a catalyst, preferably a methyl-trimethoxy silane silicon source and ammonia water as catalysts, because the methyl-trimethoxy silane contains a hydrophobic methyl group and three hydrolyzable methoxy groups. A proper amount of methyl can provide hydrophobicity for the obtained material, and the hydrolyzable methyl can be hydrolyzed into silicon hydroxyl under the catalysis of ammonia water, so that dehydration condensation reaction is carried out to form a network structure of silicon-oxygen-silicon; meanwhile, the steam of the methyl-trimethoxy silane is nontoxic and cannot cause harm to human qi. The ammonia water is taken as a catalyst mainly considering the safety and the volatility: the ammonia water is weak in alkalinity and cannot damage instruments and substrates, and the characteristic of easy volatilization of the ammonia water is beneficial to catalyzing hydrolysis and polycondensation of the methyl-trimethoxy silane in a gaseous state. The use of other silicon sources, such as tetraethyl orthosilicate, trimethylchlorosilane, ethoxytrimethylsilane, etc., has several disadvantages. For example, the reaction product is non-hydrophobic, the reactant vapors are toxic, flammable, pungent, and the like.
The reaction temperature is 100 ℃, if the reaction temperature is too high, the reactant methyl-trimethoxy silane can boil, so that liquid splashes to the surface of the substrate, and the microscopic morphology of a sample is damaged; if the reaction temperature is too low, the hydrolysis product of methyl-trimethoxysilane may be condensed into a solid in the space before moving to the substrate surface, and silica cannot be formed on the substrate. The reaction temperature in the invention can not only avoid the boiling phenomenon of methyl-trimethoxy silane, but also deposit the silicon dioxide nano liquid drop on the surface of the substrate at the fastest speed.
Compared with the prior art, the invention has the following advantages:
(1) the raw materials are cheap, the preparation conditions are mild, and the preparation process is easy to realize: the invention successfully prepares large-area one-dimensional nano silicon dioxide at the reaction temperature of 100 ℃ by using simple equipment and cheap materials;
(2) the invention provides a new chemical vapor deposition technology, provides a new method for preparing one-dimensional silicon dioxide at a lower temperature on the premise of not having strict vacuum degree requirement, can obtain more kinds of one-dimensional nano materials with unique performance by utilizing the method, and has high synthesis efficiency and wide application range;
(3) the size of the one-dimensional silicon dioxide is easy to control, and the growth length of the one-dimensional nano silicon oxide can be strictly controlled by changing the time of chemical vapor deposition, so that the one-dimensional nano silicon oxide grows into longer silicon dioxide nanowires from shorter silicon dioxide nanorods;
(4) the hydrophobic one-dimensional nano-silica has application prospect in the field of self-cleaning.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus used in the production process of the present invention;
FIG. 2 is a photograph of one-dimensional nanosilica in example 1;
FIG. 3 is a scanning electron micrograph of one-dimensional nanosilica in example 1;
FIG. 4 is a physical diagram of one-dimensional nano-silica in example 2;
FIG. 5 is a scanning electron micrograph of one-dimensional nanosilica in example 2;
FIG. 6 is a photograph of the hydrophobic angle of one-dimensional nanosilica in example 2;
in the figure, 1 is methyl-trimethoxy silane, 2 is ammonia water, 3 is a glass slide, 4 is a glass vacuum drier, and 5 is a porcelain plate.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
In the following examples, the respective raw materials were commercially available raw materials, and the purity was of analytical grade unless otherwise specified.
Example 1
A preparation method of one-dimensional nano silicon dioxide comprises the following steps:
(1) preparation of the silicon source and catalyst for chemical vapor deposition to occur: methyl-trimethoxy silane with the purity of 98% is used as a silicon source, ammonia water with the concentration of 25% is used as a catalyst, and the materials are respectively placed in two small beakers according to the volume ratio of 1:1 for later use.
(2) Preparing a one-dimensional nano silicon dioxide growth substrate: the method comprises the following steps of using a common glass slide as a growth substrate, firstly ultrasonically cleaning the glass slide by using ethanol, and then blow-drying the glass slide by using nitrogen with the purity of 99.9% for later use.
(3) Growing the one-dimensional nano silicon dioxide by a chemical vapor deposition method: as shown in FIG. 1, a small beaker containing methyl-trimethoxysilane 1 and ammonia water 2 is placed at the bottom of a glass vacuum drier 4, a cleaned glass slide 3 is placed on the upper surface of a porcelain plate 5 of the glass vacuum drier 4, the glass vacuum drier 4 is sealed and vacuumized, the vacuum degree is-0.10 Mpa, and then the glass vacuum drier is placed in a thermostat at the temperature of 100 ℃ for preservation for 6 hours.
(4) And taking the glass vacuum drier out of the thermostat, cooling to room temperature, and taking the glass slide out of the glass vacuum drier, wherein the film on the surface of the glass slide is the silicon dioxide nano-rod.
The device adopted in the embodiment is a simple and easily-obtained glass vacuum dryer as shown in fig. 1, and is not modified or upgraded, so that the preparation method of the embodiment has low requirements on preparation equipment and is easy for industrial production.
As shown in FIG. 2, the silica nanorods obtained in example 1 could not be observed with the naked eye; therefore, the silicon dioxide nanorods grown on the glass slide do not influence the original transparency of the glass slide.
As shown in FIG. 3, the silica nanorods obtained in example 1 have a nanorod structure with a diameter of 46-53 nm and a length of 46-239 nm.
Example 2
A preparation method of one-dimensional nano silicon dioxide comprises the following steps:
(1) preparation of the silicon source and catalyst for chemical vapor deposition to occur: methyl-trimethoxy silane with the purity of 98% is used as a silicon source, ammonia water with the concentration of 28% is used as a catalyst, and the materials are respectively placed in two small beakers according to the volume ratio of 1:1 for later use.
(2) Preparing a one-dimensional nano silicon dioxide growth substrate: the method comprises the following steps of using a common glass slide as a growth substrate, firstly ultrasonically cleaning the glass slide by using ethanol, and then blow-drying the glass slide by using nitrogen with the purity of 99.9% for later use.
(3) Growing the one-dimensional nano silicon dioxide by a chemical vapor deposition method: placing a small beaker containing a silicon source and a catalyst at the bottom of a glass vacuum dryer, placing a cleaned glass slide on the upper surface of a porcelain plate of the glass vacuum dryer, sealing the glass vacuum dryer, vacuumizing to a vacuum degree of-0.1 Mpa, and then placing the glass vacuum dryer in a thermostat at the temperature of 100 ℃ for storage for 12 hours.
(4) And taking the glass vacuum dryer out of the thermostat, cooling to room temperature, and taking the glass slide out of the glass vacuum dryer, wherein the film on the surface of the glass slide is the silicon dioxide nanowire.
As shown in fig. 4, the silica nanowires obtained in example 2 were not observed with the naked eye; therefore, the silicon dioxide nanorods grown on the glass slide do not influence the original transparency of the glass slide.
As shown in FIG. 5, the silica nanowires obtained in example 2 have nanowire-like structures with diameters of 46-53 nm and lengths of more than 500 nm.
As shown in fig. 6, the silica nanowires obtained in example 2 have better hydrophobicity.
Example 3
A preparation method of one-dimensional nano silicon dioxide comprises the following steps:
(1) preparation of the silicon source and catalyst for chemical vapor deposition to occur: methyl-trimethoxy silane with the purity of 98% is used as a silicon source, ammonia water with the concentration of 25% is used as a catalyst, and the materials are respectively placed in two small beakers according to the volume ratio of 1:1 for later use.
(2) Preparing a one-dimensional nano silicon dioxide growth substrate: the method comprises the following steps of using a common glass slide as a growth substrate, firstly ultrasonically cleaning the glass slide by using ethanol, and then blow-drying the glass slide by using nitrogen with the purity of 99.9% for later use.
(3) Growing the one-dimensional nano silicon dioxide by a chemical vapor deposition method: as shown in FIG. 1, a small beaker containing methyl-trimethoxysilane 1 and ammonia water 2 is placed at the bottom of a glass vacuum drier 4, a cleaned glass slide 3 is placed on the upper surface of a porcelain plate 5 of the glass vacuum drier 4, the glass vacuum drier 4 is sealed and vacuumized, the vacuum degree is-0.05 Mpa, and then the glass vacuum drier is placed in a thermostat at the temperature of 25 ℃ for 24 hours.
(4) And taking the glass vacuum dryer out of the thermostat, cooling to room temperature, taking the glass slide out of the glass vacuum dryer, wherein the film on the surface of the glass slide is the silicon dioxide nano rod, and the obtained silicon dioxide nano wire is in a nano rod-shaped structure with the diameter of 46-53 nm and the length of 72 nm.
Example 4
A preparation method of one-dimensional nano silicon dioxide comprises the following steps:
(1) preparation of the silicon source and catalyst for chemical vapor deposition to occur: methyl-trimethoxy silane with the purity of 98% is used as a silicon source, ammonia water with the concentration of 25% is used as a catalyst, and the materials are respectively placed in two small beakers according to the volume ratio of 1:1 for later use.
(2) Preparing a one-dimensional nano silicon dioxide growth substrate: the method comprises the following steps of using a common glass slide as a growth substrate, firstly ultrasonically cleaning the glass slide by using ethanol, and then blow-drying the glass slide by using nitrogen with the purity of 99.9% for later use.
(3) Growing the one-dimensional nano silicon dioxide by a chemical vapor deposition method: as shown in figure 1, a small beaker containing methyl-trimethoxy silane 1 and ammonia water 2 is placed at the bottom of a glass vacuum dryer 4, a cleaned glass slide 3 is placed on the upper surface of a porcelain plate 5 of the glass vacuum dryer 4, the glass vacuum dryer 4 is sealed and vacuumized, the vacuum degree is-0.05 Mpa, and then the glass vacuum dryer is placed in a thermostat at the temperature of 102 ℃ for storage for 1 hour.
(4) And taking the glass vacuum dryer out of the thermostat, cooling to room temperature, taking the glass slide out of the glass vacuum dryer, wherein the film on the surface of the glass slide is the silicon dioxide nano rod, and the obtained silicon dioxide nano wire is in a nano rod-shaped structure with the diameter of 46-53 nm and the length of 80 nm.
In the embodiment of the invention, the large-area one-dimensional nano silicon dioxide is successfully prepared at the reaction temperature of 100 ℃ by using simple equipment and cheap materials. The invention provides a new chemical vapor deposition technology, provides a new method for preparing one-dimensional silicon dioxide at a lower temperature in a large scale on the premise of not having strict vacuum degree requirement, can obtain more kinds of one-dimensional nano materials with unique performance by utilizing the method, provides a new thought for the research of the one-dimensional nano materials, and has important significance for the research of the growth mechanism of the one-dimensional nano materials. The prepared one-dimensional nano silicon dioxide with hydrophobicity has application prospect in the field of self-cleaning.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A preparation method of one-dimensional nano silicon dioxide is characterized by comprising the following steps:
preparation of the silicon dioxide nanorod synthetic raw material: respectively containing a silicon source and ammonia water in two containers for later use; the silicon source is methyl-trimethoxy silane;
preparing a one-dimensional nano silicon dioxide growth substrate: preparing a glass slide as a growth substrate, and cleaning and drying the glass slide for later use;
growing the one-dimensional nano silicon dioxide by a chemical vapor deposition method: placing a container containing a silicon source and ammonia water and the dried glass slide in a vacuum dryer, sealing and vacuumizing, placing the vacuum dryer in a thermostat, and preserving at constant temperature; and taking the vacuum drier out of the thermostat, cooling to room temperature, and taking the glass slide out of the vacuum drier, wherein the film on the surface of the glass slide is the one-dimensional nano silicon dioxide.
2. The method for preparing one-dimensional nano silicon dioxide according to claim 1, wherein the mass concentration of the ammonia water is 25-28%.
3. The method for preparing one-dimensional nano silica according to claim 1, wherein the temperature of the vacuum dryer maintained at constant temperature in the thermostat is 25-102 ℃.
4. The method for preparing one-dimensional nanosilicon dioxide as claimed in claim 3, wherein the temperature of the vacuum dryer maintained at constant temperature in the thermostat is 100 ℃.
5. The method for preparing one-dimensional nano silica according to claim 1, wherein the vacuum dryer is kept in a thermostat for 1-24 hours.
6. The method for preparing one-dimensional nano-silica according to claim 1, wherein the container containing the silicon source and the ammonia water is placed at the bottom of a vacuum dryer, and the dried glass slide is placed on a porcelain plate of the vacuum dryer.
7. The method for preparing one-dimensional nano silicon dioxide according to claim 1, wherein the vacuum degree of a vacuum drier is-0.05 to-0.10 MPa in the chemical vapor deposition growth process of the one-dimensional nano silicon dioxide.
8. The method for preparing one-dimensional nano silica as claimed in claim 1, wherein the cleaning and drying method comprises placing a glass slide in ethanol, ultrasonically cleaning the glass slide, and drying the glass slide with nitrogen.
9. The method of claim 1, wherein the length of the one-dimensional nanosilica is adjusted by maintaining the vacuum dryer in a thermostat.
10. The one-dimensional nano-silica prepared by the preparation method of claim 1 is characterized by consisting of amorphous silica with the diameter of 46-53 nm, and the one-dimensional nano-silica has hydrophobicity.
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| CN103050640A (en) * | 2013-01-29 | 2013-04-17 | 哈尔滨工业大学 | Preparation method of nanorod with zinc oxide nano-particle/silicon dioxide composite structure |
| CN103923645A (en) * | 2014-05-05 | 2014-07-16 | 吉林大学 | Method for preparing one-dimensional SiO2:Eu<3+>, Gd<3+> nano luminescent material with controllable morphology |
| CN106587079A (en) * | 2016-12-30 | 2017-04-26 | 湖北工程学院 | One-dimensional SiO2 nano material and preparation method thereof |
| KR101972056B1 (en) * | 2017-08-29 | 2019-04-25 | 강원대학교산학협력단 | Synthesis of Silica Nanowires Using Amorphous Silicon |
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| CN103050640A (en) * | 2013-01-29 | 2013-04-17 | 哈尔滨工业大学 | Preparation method of nanorod with zinc oxide nano-particle/silicon dioxide composite structure |
| CN103923645A (en) * | 2014-05-05 | 2014-07-16 | 吉林大学 | Method for preparing one-dimensional SiO2:Eu<3+>, Gd<3+> nano luminescent material with controllable morphology |
| CN106587079A (en) * | 2016-12-30 | 2017-04-26 | 湖北工程学院 | One-dimensional SiO2 nano material and preparation method thereof |
| KR101972056B1 (en) * | 2017-08-29 | 2019-04-25 | 강원대학교산학협력단 | Synthesis of Silica Nanowires Using Amorphous Silicon |
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