CN108545754A - A kind of preparation method of nanometer titanium dioxide silicon ball - Google Patents
A kind of preparation method of nanometer titanium dioxide silicon ball Download PDFInfo
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- CN108545754A CN108545754A CN201810674615.0A CN201810674615A CN108545754A CN 108545754 A CN108545754 A CN 108545754A CN 201810674615 A CN201810674615 A CN 201810674615A CN 108545754 A CN108545754 A CN 108545754A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- 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
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
- C01P2004/51—Particles with a specific particle size distribution
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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
Abstract
The present invention is a kind of preparation method of nanometer titanium dioxide silicon ball.A kind of preparation method of nanometer titanium dioxide silicon ball, including：(1) nanometer titanium dioxide silicon ball suspension is prepared：Using high-shear mixer, under the rotating speed of 10000 22000r/min, ammonium hydroxide, ethyl orthosilicate and alcoholic solution is mixed, nanometer titanium dioxide silicon ball suspension is obtained；(2) nanometer titanium dioxide silicon ball is detached：By nanometer titanium dioxide silicon ball suspension centrifuge washing, sediment is dried, the nanometer titanium dioxide silicon ball is obtained.A kind of preparation method of nanometer titanium dioxide silicon ball of the present invention, preparation time is relatively short, and 10 20min of stirring can be obtained Nano-meter SiO_2 prepared by hydrolysis2Ball；And it is not necessarily to template, simplifies preparation process, template is removed without high-temperature roasting, has saved cost；Nano-meter SiO_2 can also can be controlled by controlling the conditions such as rotating speed, temperature2The grain size of ball, to meet under different situations to Nano-meter SiO_22The demand of spherolite diameter can be applied in fields such as catalysis, stabilizer, reinforcing agent, additive, biology.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of preparation method of nanometer titanium dioxide silicon ball.
Background technology
Silica (SiO2) there is good mechanical strength, thermal stability and chemical inertness, it is ground all the time in science
Study carefully and plays extremely important role with industrial technical field.Currently, SiO2The preparation of ball mainly uses teos hydrolysis
Method, in order to control SiO2Spherolite diameter be added template, by commonly hydrolyze or high temperature hydro-thermal method prepare, then removed by high-temperature roasting
Template is removed, evenly dispersed Nano-meter SiO_2 is then obtained2Ball, this method is time-consuming (general whipping process needs 2h or so), and at
This is slightly higher.
In view of this, the present invention proposes a kind of Nano-meter SiO_2 at low cost, preparation time is short2The preparation method of ball.
Invention content
The purpose of the present invention is to provide a kind of preparation method of nanometer titanium dioxide silicon ball, which uses high shear
Technology avoids the use of template, solves in existing preparation method Nano-meter SiO_2 in order to control2Spherolite diameter is added template and makes
At cost is higher and the longer problem of preparation time.
To achieve the goals above, used technical solution is：
A kind of preparation method of nanometer titanium dioxide silicon ball, including：
(1) nanometer titanium dioxide silicon ball suspension is prepared：Using high-shear mixer, in the rotating speed of 10000-22000r/min
Under, ammonium hydroxide, ethyl orthosilicate and alcoholic solution are mixed, nanometer titanium dioxide silicon ball suspension is obtained；
(2) nanometer titanium dioxide silicon ball is detached：By nanometer titanium dioxide silicon ball suspension centrifuge washing, sediment is dried, institute is obtained
State nanometer titanium dioxide silicon ball.
Further, the step (1) is specially：
Prepare precursor liquid：Ethyl orthosilicate is added in alcoholic solution, and is uniformly mixed, precursor liquid is obtained；
Prepare nanometer titanium dioxide silicon ball suspension：Ammonium hydroxide is added in precursor liquid and is mixed, nanometer titanium dioxide silicon ball is obtained
Suspension.
Further, in the step (1), the volume ratio of the ethyl orthosilicate and alcoholic solution is 2-5:500-800；
The volume ratio of the ammonium hydroxide and precursor liquid is 0-10:80；
Further, in the step (1), the mass fraction of alcohol is not less than 70% in the alcoholic solution；
Further, the alcohol in the alcoholic solution is any one in methanol, ethyl alcohol, propyl alcohol.
Further, the step (1) prepares in nanometer titanium dioxide silicon ball suspension, and the mixing time is 10-
20min。
Further, the step (1) prepares in nanometer titanium dioxide silicon ball suspension, and the mixing time is
15min, whipping temp are 10-50 DEG C.
Further, in the step (2), the washing solution is alcoholic solution.
Further, in the step (2), the centrifuge washing rotating speed is 3000-8000r/min.
Further, in the step (2), the drying temperature is 100 DEG C, time 0.5-12h.
Compared with prior art, the beneficial effects of the present invention are：
1, the preparation method of a kind of nanometer titanium dioxide silicon ball of the present invention, method is simple, and preparation time is relatively short,
Stirring 10-20min can be obtained Nano-meter SiO_2 prepared by hydrolysis2Ball.
2. a kind of preparation method of nanometer titanium dioxide silicon ball of the present invention is not necessarily to template, simplifies preparation process,
Template is removed without high-temperature roasting, has saved cost.
3, the preparation method of a kind of nanometer titanium dioxide silicon ball of the present invention, can be by controlling the items such as rotating speed, temperature
Part can control Nano-meter SiO_22The grain size of ball, to meet under different situations to Nano-meter SiO_22The demand of spherolite diameter, can be in catalysis, steady
Determine the application of the fields such as agent, reinforcing agent, additive, adsorbent, photoelectricity, biology.
Description of the drawings
Fig. 1 is Nano-meter SiO_2 prepared by the embodiment of the present invention 12The transmission electron microscope picture of ball；
Fig. 2 is Nano-meter SiO_2 prepared by the embodiment of the present invention 22The transmission electron microscope picture of ball；
Fig. 3 is Nano-meter SiO_2 prepared by the embodiment of the present invention 32The transmission electron microscope picture of ball；
Fig. 4 is Nano-meter SiO_2 prepared by the embodiment of the present invention 42The transmission electron microscope picture of ball；
Fig. 5 is Nano-meter SiO_2 prepared by 1-4 of the embodiment of the present invention2The grain size distribution of ball.
Specific implementation mode
In order to which the present invention is further explained, a kind of preparation method of nanometer titanium dioxide silicon ball, reaches expected goal of the invention, with
Lower combination preferred embodiment, to a kind of preparation method of the nanometer titanium dioxide silicon ball proposed according to the present invention, specific embodiment party
Formula, structure, feature and its effect are described in detail as after.In the following description, different " embodiment " or " embodiment " refers to
It is not necessarily the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any suitable forms
Combination.
Before elaborating a kind of preparation method of nanometer titanium dioxide silicon ball of the present invention, it is necessary to being referred in the present invention
Raw material and method etc. be described further, to reach better effect.
Ethyl orthosilicate (TEOS), molecular formula are Si (OC2H5)4, molecular weight 208.33 is colourless liquid, slightly gas
Taste, -77 DEG C of fusing point, 165-169 DEG C of boiling point are slightly soluble in water, are dissolved in ethyl alcohol, ether, stablize in the presence of no moisture, when distillation regardless of
Solution, can be miscible with ethyl alcohol and ether, is slightly soluble in benzene, is practically insoluble in water, but can gradually be water dispersible into silica.The present embodiment
The middle reagent specification used is pure to analyze.
The water used in the embodiment of the present invention is RO water.
In the application using high-shear mixer can high-speed stirred, make ammonium hydroxide mixed with precursor liquid evenly, reduction gas
Liquid two-phase resistance to mass tranfer.
The application can control Nano-meter SiO_2 by controlling the conditions such as rotating speed, temperature2The grain size of ball, concrete principle be,
During preparing nanometer titanium dioxide silicon ball suspension：(1) temperature is relatively low, and ethyl orthosilicate (TEOS) hydrolysis is slower, is formed
SiO2Spherolite diameter is smaller；Temperature is higher, and ethyl orthosilicate (TEOS) hydrolysis is very fast, forms SiO2Spherolite diameter is larger.(2) stirring speed
Degree is higher, and mass transfer rate is higher, is conducive to ethyl orthosilicate (TEOS) hydrolysis.(3) ammonia volume is less, ethyl orthosilicate
(TEOS) hydrolysis is relatively slow or is unable to complete hydrolysis, the Nano-meter SiO_2 hydrolyzed2Ball is smaller；Ammonia volume is more, ethyl orthosilicate
(TEOS) hydrolysis is very fast, the Nano-meter SiO_2 hydrolyzed2Ball is larger.
After having understood above-mentioned raw materials and method etc., below in conjunction with specific embodiment to a kind of nano-silica of the present invention
The preparation method of SiClx ball is further described in detail：
Embodiment 1.
Concrete operation step is as follows：
(1) precursor liquid is prepared：Second alcohol and water is pressed 7：3 mass ratio mixing, it is molten to obtain the ethyl alcohol that mass fraction is 70%
Liquid；Then 500 μ L ethyl orthosilicates (TEOS) are added in the ethanol solution of 80mL, are uniformly mixed, obtain precursor liquid.
(2) nanometer titanium dioxide silicon ball suspension is prepared：80mL precursor liquids are placed in high-shear mixer to be stirred, are added
5mL ammonium hydroxide stirs under conditions of 30 DEG C of water-bath, rotating speed 10000r/min, after stirring 5min, it can be seen that nano silicon dioxide
Appearance, stir 15min after, reaction terminates, and obtains nanometer titanium dioxide silicon ball suspension.Contain in nanometer titanium dioxide silicon ball suspension
Nanometer titanium dioxide silicon ball.
(3) nanometer titanium dioxide silicon ball is detached：By nanometer titanium dioxide silicon ball suspension under the rotating speed of 6000r/min, use
Ethanol solution centrifuge washing 1 time, then puts the precipitate in air dry oven, and dry 12h, obtains powdered at 100 DEG C
The nanometer titanium dioxide silicon ball.
Fig. 1 is Nano-meter SiO_2 prepared by the embodiment of the present invention 12The transmission electron microscope picture of ball, as seen from the figure, sample are spherical, are in
Normal distribution, average grain diameter is at 60 nanometers.
Embodiment 2.
The concrete operation step of embodiment 2 is same as Example 1, the difference is that, it is high the step of embodiment 2 in (2)
The rotating speed of shear mixer is 13000r/min.
Fig. 2 is Nano-meter SiO_2 prepared by the embodiment of the present invention 12The transmission electron microscope picture of ball, as seen from the figure, sample are spherical, are in
Normal distribution.
Embodiment 3.
The concrete operation step of embodiment 3 is same as Example 1, the difference is that, it is high the step of embodiment 3 in (2)
The rotating speed of shear mixer is 16000r/min.
Fig. 3 is Nano-meter SiO_2 prepared by the embodiment of the present invention 12The transmission electron microscope picture of ball, as seen from the figure, sample are spherical, are in
Normal distribution.
Embodiment 4.
The concrete operation step of embodiment 4 is same as Example 1, the difference is that, it is high the step of embodiment 4 in (2)
The rotating speed of shear mixer is 19000r/min.
Fig. 4 is Nano-meter SiO_2 prepared by the embodiment of the present invention 12The transmission electron microscope picture of ball, as seen from the figure, sample are spherical, are in
Normal distribution.
Fig. 5 is Nano-meter SiO_2 prepared by 1-4 of the embodiment of the present invention2The grain size distribution of ball, as seen from the figure, rotating speed is to preparing
Nano-meter SiO_22Ball has an impact, and can control Nano-meter SiO_2 by controlling rotating speed2The grain size of ball.
Embodiment 5.
The concrete operation step of embodiment 5 is same as Example 1, the difference is that, the step of embodiment 5 in (2), ammonia
The additive amount of water is 10mL.
Embodiment 6.
The concrete operation step of embodiment 6 is same as Example 1, the difference is that, the step of embodiment 5 in (2), not
Add ammonium hydroxide.
After testing, the average grain diameter for the nanometer titanium dioxide silicon ball that prepared by embodiment 6 is minimum, nanometer prepared by embodiment 1-4
The average grain diameter of silica spheres is taken second place, and the average grain diameter of nanometer titanium dioxide silicon ball prepared by embodiment 5 is maximum, illustrates ammonium hydroxide
Dosage can influence Nano-meter SiO_22The grain size of ball, ammonia volume is less, and ethyl orthosilicate (TEOS) hydrolysis is relatively slow or cannot be complete
Hydrolysis, the Nano-meter SiO_2 hydrolyzed2Ball is smaller；Ammonia volume is more, and ethyl orthosilicate (TEOS) hydrolysis is very fast, and hydrolysis obtains
Nano-meter SiO_22Ball is larger.
Embodiment 7.
The concrete operation step of embodiment 7 is same as Example 1, the difference is that, the step of embodiment 6 in (2), water
The temperature of bath is 10 DEG C.
Embodiment 8.
The concrete operation step of embodiment 8 is same as Example 1, the difference is that, the step of embodiment 6 in (2), water
The temperature of bath is 50 DEG C.
After testing, the average grain diameter for the nanometer titanium dioxide silicon ball that prepared by embodiment 7 is minimum, nanometer prepared by embodiment 1-4
The average grain diameter of silica spheres is taken second place, and the average grain diameter of nanometer titanium dioxide silicon ball prepared by embodiment 8 is maximum, illustrates that temperature can
To influence particle size, temperature is relatively low, and ethyl orthosilicate (TEOS) hydrolysis is slower, forms SiO2Spherolite diameter is smaller；Temperature is higher,
Ethyl orthosilicate (TEOS) hydrolysis is very fast, forms SiO2Spherolite diameter is larger.
Embodiment 9.
Concrete operation step is as follows：
(1) precursor liquid is prepared：Isopropyl alcohol and water is pressed 7：3 mass ratio mixing, obtains the isopropyl that mass fraction is 70%
Alcoholic solution；Then 400 μ L ethyl orthosilicates (TEOS) are added in the aqueous isopropanol of 100mL, are uniformly mixed, obtain forerunner
Liquid.
(2) nanometer titanium dioxide silicon ball suspension is prepared：80mL precursor liquids are placed in high-shear mixer and are stirred, are added
Enter 10mL ammonium hydroxide, high-speed stirred under conditions of 30 DEG C of water-bath, rotating speed 10000r/min, after stirring 5min, it can be seen that nanometer
The appearance of silica, after stirring 20min, reaction terminates, and obtains nanometer titanium dioxide silicon ball suspension.Nanometer titanium dioxide silicon ball suspends
Contain nanometer titanium dioxide silicon ball in liquid.
(3) nanometer titanium dioxide silicon ball is detached：By nanometer titanium dioxide silicon ball suspension under the rotating speed of 3000r/min, use
Ethanol solution centrifuge washing 1 time, then puts the precipitate in air dry oven, and dry 10h, obtains powdered at 100 DEG C
The nanometer titanium dioxide silicon ball.
Embodiment 10.
Concrete operation step is as follows：
(1) precursor liquid is prepared：First alcohol and water is pressed 7：3 mass ratio mixing, it is molten to obtain the methanol that mass fraction is 70%
Liquid；Then 500 μ L ethyl orthosilicates (TEOS) are added in the methanol solution of 80mL, are uniformly mixed, obtain precursor liquid.
(2) nanometer titanium dioxide silicon ball suspension is prepared：80mL precursor liquids are placed under high-shear mixer and are stirred,
High-speed stirred under conditions of 50 DEG C of water-bath, rotating speed 22000r/min, after stirring 5min, it can be seen that nano silicon dioxide goes out
Existing, after stirring 10min, reaction terminates, and obtains nanometer titanium dioxide silicon ball suspension.Contain nanometer in nanometer titanium dioxide silicon ball suspension
Silica spheres.
(3) nanometer titanium dioxide silicon ball is detached：By nanometer titanium dioxide silicon ball suspension under the rotating speed of 8000r/min, use
Methanol solution centrifuge washing 1 time, then puts the precipitate in air dry oven, and dry 0.5h, obtains powdered at 100 DEG C
The nanometer titanium dioxide silicon ball.
Embodiment 11.
Concrete operation step is as follows：
(1) precursor liquid is prepared：Second alcohol and water is pressed 1:0 mass ratio mixing, i.e., using straight alcohol as alcoholic solution；Then will
400 μ L ethyl orthosilicates (TEOS) are added in the ethanol solution of 80mL, are uniformly mixed, are obtained precursor liquid.
(2) nanometer titanium dioxide silicon ball suspension is prepared：80mL precursor liquids are placed in high-shear mixer and are stirred, are added
Enter 5mL ammonium hydroxide, high-speed stirred under conditions of 10 DEG C of water-bath, rotating speed 18000r/min, after stirring 5min, it can be seen that nanometer two
The appearance of silica, after stirring 15min, reaction terminates, and obtains nanometer titanium dioxide silicon ball suspension.Nanometer titanium dioxide silicon ball suspension
In contain nanometer titanium dioxide silicon ball.
(3) nanometer titanium dioxide silicon ball is detached：By nanometer titanium dioxide silicon ball suspension under the rotating speed of 6000r/min, use
Ethanol solution centrifuge washing 1 time, then puts the precipitate in air dry oven, and dry 12h, obtains powdered at 100 DEG C
The nanometer titanium dioxide silicon ball.
A kind of preparation method of nanometer titanium dioxide silicon ball described in 1-11 of the embodiment of the present invention, preparation time is relatively short,
Stirring 10-20min can be obtained Nano-meter SiO_2 prepared by hydrolysis2Ball；And it is not necessarily to template, simplifies preparation process, without height
Temperature roasting removes template, has saved cost；Nano-meter SiO_2 can also can be controlled by controlling the conditions such as rotating speed, temperature2Ball
Grain size, to meet under different situations to Nano-meter SiO_22The demand of spherolite diameter, can catalysis, stabilizer, reinforcing agent, additive,
It applies in the fields such as adsorbent, photoelectricity, biology.
The above is only the preferred embodiment of the embodiment of the present invention, not makees any shape to the embodiment of the present invention
Limitation in formula, the technical spirit of embodiment is to any simple modification, equivalent variations made by above example according to the present invention
With modification, in the range of still falling within technical solution of the embodiment of the present invention.
Claims (10)
1. a kind of preparation method of nanometer titanium dioxide silicon ball, which is characterized in that including：
(1) nanometer titanium dioxide silicon ball suspension is prepared：Using high-shear mixer, under the rotating speed of 10000-22000r/min,
Ammonium hydroxide, ethyl orthosilicate and alcoholic solution are mixed, nanometer titanium dioxide silicon ball suspension is obtained；
(2) nanometer titanium dioxide silicon ball is detached：By nanometer titanium dioxide silicon ball suspension centrifuge washing, sediment is dried, obtains described receive
Rice silica spheres.
2. preparation method according to claim 1, which is characterized in that wherein,
The step (1) is specially：
Prepare precursor liquid：Ethyl orthosilicate is added in alcoholic solution, and is uniformly mixed, precursor liquid is obtained；
Prepare nanometer titanium dioxide silicon ball suspension：Ammonium hydroxide is added in precursor liquid and is mixed, the suspension of nanometer titanium dioxide silicon ball is obtained
Liquid.
3. preparation method according to claim 2, which is characterized in that wherein,
In the step (1), the volume ratio of the ethyl orthosilicate and alcoholic solution is 2-5:500-800；
The volume ratio of the ammonium hydroxide and precursor liquid is 0-10:80.
4. preparation method according to claim 1, which is characterized in that wherein,
In the step (1), the mass fraction of alcohol is not less than 70% in the alcoholic solution.
5. preparation method according to claim 4, which is characterized in that wherein,
Alcohol in the alcoholic solution is any one in methanol, ethyl alcohol, propyl alcohol.
6. preparation method according to claim 2, which is characterized in that wherein,
The step (1) prepares in nanometer titanium dioxide silicon ball suspension, and the mixing time is 10-20min.
7. preparation method according to claim 6, which is characterized in that wherein,
The step (1) prepares in nanometer titanium dioxide silicon ball suspension, and the mixing time is 15min, whipping temp 10-
50℃。
8. preparation method according to claim 1, which is characterized in that wherein,
In the step (2), the washing solution is alcoholic solution.
9. preparation method according to claim 1, which is characterized in that wherein,
In the step (2), the centrifuge washing rotating speed is 3000-8000r/min.
10. preparation method according to claim 1, which is characterized in that wherein, in the step (2), the drying temperature
It is 100 DEG C, time 0.5-12h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110479954A (en) * | 2019-08-19 | 2019-11-22 | 安徽省含山县兴建铸造厂 | A kind of model casting precision casting shell fire resistant covering material |
| CN111517333A (en) * | 2020-05-11 | 2020-08-11 | 石河子大学 | Porous SiO of three-dimensional hierarchical structure2Method for preparing microspheres |
| CN113526515A (en) * | 2021-08-29 | 2021-10-22 | 浙江华飞电子基材有限公司 | Nano spherical silicon micro powder separation and extraction method |
| CN114394602A (en) * | 2021-12-22 | 2022-04-26 | 中国人民解放军陆军军医大学第一附属医院 | Manganese-doped hollow mesoporous silica nanomaterial and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140179A (en) * | 2010-08-05 | 2011-08-03 | 山东轻工业学院 | Method for preparing styrene grafted silicon dioxide superhydrophobic thin film |
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2018
- 2018-06-27 CN CN201810674615.0A patent/CN108545754A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140179A (en) * | 2010-08-05 | 2011-08-03 | 山东轻工业学院 | Method for preparing styrene grafted silicon dioxide superhydrophobic thin film |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110479954A (en) * | 2019-08-19 | 2019-11-22 | 安徽省含山县兴建铸造厂 | A kind of model casting precision casting shell fire resistant covering material |
| CN111517333A (en) * | 2020-05-11 | 2020-08-11 | 石河子大学 | Porous SiO of three-dimensional hierarchical structure2Method for preparing microspheres |
| CN111517333B (en) * | 2020-05-11 | 2023-05-09 | 石河子大学 | Porous SiO of three-dimensional hierarchical structure 2 Method for preparing microsphere |
| CN113526515A (en) * | 2021-08-29 | 2021-10-22 | 浙江华飞电子基材有限公司 | Nano spherical silicon micro powder separation and extraction method |
| CN114394602A (en) * | 2021-12-22 | 2022-04-26 | 中国人民解放军陆军军医大学第一附属医院 | Manganese-doped hollow mesoporous silica nanomaterial and preparation method and application thereof |
| CN114394602B (en) * | 2021-12-22 | 2023-09-22 | 中国人民解放军陆军军医大学第一附属医院 | Manganese-doped hollow mesoporous silica nanomaterial and preparation method and application thereof |
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Application publication date: 20180918 |