CN110203940A - Load the preparation method of the hollow mesoporous silicon oxide micro-nano ball of more metallic particles - Google Patents
Load the preparation method of the hollow mesoporous silicon oxide micro-nano ball of more metallic particles Download PDFInfo
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- CN110203940A CN110203940A CN201910561733.5A CN201910561733A CN110203940A CN 110203940 A CN110203940 A CN 110203940A CN 201910561733 A CN201910561733 A CN 201910561733A CN 110203940 A CN110203940 A CN 110203940A
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- 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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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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
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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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Abstract
The present invention provides a kind of preparation methods of hollow mesoporous silicon oxide micro-nano ball for loading more metallic particles comprising following steps: using the method for the ion sputtering metal material different in the surface spraying plating of the template ball of Monolayer Dispersion, obtaining Janus particle;Using sol-gel method, one layer of mesoporous silicon oxide is grown in obtained Janus particle surface;Calcining, removes removing template, and the metal layer of mesoporous silicon oxide inner surface is dispersed into multiple little particles to get the hollow mesoporous silicon oxide micro-nano ball of internal more metallic particles is arrived at the same time.Using technical solution of the present invention, method is simple, and the universality with element selection can realize the accurate control of internal metallic particles content according to demand;The excellent properties of its interior metal are not only played well, while unique core-shell structure can carry out effective protection to internal metallic.
Description
Technical field
The invention belongs to field of material technology more particularly to a kind of hollow mesoporous silicon oxide for loading more metallic particles are micro-
The preparation method of nanosphere.
Background technique
The hollow mesoporous silicon oxide micro-nano granules (HMSNPs@metal) for loading more metallics, as multi-component
Nano-hybrid material has good biocompatibility, bigger specific surface area.Meanwhile the multiple metallic particles of cavity inside help
In its special performance of performance.For example carried metal includes Au, Au particle drives in photo-thermal, and biological detection etc. has good
Effect;For example the noble metals such as carried metal Pt, Pd have a wide range of applications in catalytic field, and different metal element is compound
While having double-response property, the effect of " 1+1 > 2 " is often shown.
Currently, have the preparation method of the hollow mesoporous silicon oxide micro-nano granules of the more metallics of some research loads, but
It is substantially preparation process complexity, and does not have the universality of element selection, while internal metallic particles content can not be controlled accurately
System.
Summary of the invention
Against the above technical problems, the invention discloses a kind of hollow mesoporous silicon oxide micro-nanos for loading more metallic particles
The preparation method of rice ball, method is simple, can be by single metal or alloy material inside change and control accurate, to realize
A variety of different applications.
In this regard, the technical solution adopted by the present invention are as follows:
A kind of preparation method for the hollow mesoporous silicon oxide micro-nano ball loading more metallic particles comprising following steps:
Step S1 is obtained using the method for the ion sputtering metal material different in the surface spraying plating of the template ball of Monolayer Dispersion
Janus particle;Wherein, the metal material that different metal materials is two kinds or more.
Step S2 grows one layer of meso-porous titanium dioxide in the Janus particle surface that step S1 is obtained using sol-gel method
Silicon;
Step S3, calcining, removes removing template, and the metal layer of mesoporous silicon oxide inner surface is dispersed into multiple little particles at the same time,
Obtain the hollow mesoporous silicon oxide micro-nano ball of internal more metallic particles.
This technical solution, using the method for ion sputtering in monodispersed template ball (Polystyrene, PS) surface spraying plating
Different metal material (such as Au/Ag/Pt/Pd/Fe).Then the method for utilizing sol-gel, in the Janus particle surface of synthesis
Grow one layer of mesoporous silicon oxide (SiO2).Under the hot environment of calcining, metal layer heat shrinkable is at fine particle, macromolecule
The calcining of template ball removes, to form the granose hollow meso-porous silica core-shell structure of load.In addition to this, pass through adjusting
The ion sputtering spraying plating time, can further control accurate interior metal constituent content (mass percent), to obtain ideal
The hollow meso-hole structure of pattern.
As a further improvement of the present invention, the metal material includes at least two in Au, Ag, Pt, Fe, Pd.
As a further improvement of the present invention, in step S1, plating current < 10 mA of ion sputtering, the spraying plating time is
20-180s。
As a further improvement of the present invention, step S2 is the following steps are included: use Janus of ultrasonic collection step S1
Grain sample, is placed in reaction vessel, and triethanolamine and surfactant is added, and simultaneously ethyl orthosilicate progress is added in heating water bath
Reaction grows one layer of mesoporous silicon oxide on the surface of sample.Further, the temperature of heating water bath is 70 ~ 90 DEG C;Further
Preferably, the temperature of heating water bath is 80 DEG C.
As a further improvement of the present invention, the surfactant is cetyl trimethyl ammonium.
As a further improvement of the present invention, the dosage of triethanolamine is the 5 ~ 10% of template ball quality, the surface-active
The dosage of agent is the 10 ~ 20% of template ball quality, and the amount of each mg template ball of the dosage of the ethyl orthosilicate is 0.04 ~ 0.2 μ L.
As a further improvement of the present invention, it in step S1, using biopolymer nanoparticles PS as template, is added dropwise in slide
The upper template ball for forming Monolayer Dispersion.
As a further improvement of the present invention, in step S3, the temperature of calcining is 450 DEG C -550 DEG C.
As a further improvement of the present invention, the inside of the hollow mesoporous silicon oxide micro-nano ball of internal more metallic particles
Metallic particles content Y is adjusted by ion sputtering spraying plating time X, the numerical relation of the two are as follows: Y=0.23X+0.31.
Compared with prior art, the invention has the benefit that
Using technical solution of the present invention, the hollow structure of load different metal is prepared using ion sputtering and chemically grown,
Simultaneously can accuracy controlling its interior metal content, method is simple, the universality with element selection, can realize according to demand in
The accurate control of portion's metallic particles content;The excellent properties of its interior metal, while unique nucleocapsid knot are not only played well
Structure can carry out effective protection to internal metallic;And the equipment used is simple, and it is easy to operate, it can be widely used in and urge
Change, bio-sensing, the fields such as drug release.
Detailed description of the invention
Fig. 1 is a kind of stream of the preparation method for the hollow mesoporous silicon oxide micro-nano ball for loading more metallic particles of the present invention
Journey schematic diagram.
Fig. 2 is the transmission electron microscope picture of the hollow mesoporous silicon oxide micro-nano ball obtained the different spraying plating times of the invention;Its
In, it is a) spraying plating time 40s, c for spraying plating time 20s, b)) it is spraying plating time 80s's.Fig. 3 is different spraying platings of the invention
Time corresponds to two point atom chart of percentage comparisons.
Fig. 4 is the hollow mesoporous silicon dioxide nano of the more metallic particles of load under the different sputtering Au/Pt times of the invention
The transmission electron microscope picture of particle;Wherein a) two kinds of spraying plating Au/Pt different element times are 40/20 s respectively;B) difference spraying plating Au/Pt
Two kinds of different element times be 40/30 s, c) respectively two kinds of difference element times of spraying plating Au/Pt be 40/40 s.
Fig. 5 is the EDX and mapping of the bimetallic hollow mesoporous silica nano-particle of spraying plating Au/Pt of the invention
Analysis chart.
Specific embodiment
Preferably embodiment of the invention is described in further detail below.
A kind of preparation method for the hollow mesoporous silicon oxide micro-nano ball loading more metallic particles, as shown in Figure 1, it is wrapped
Include following steps:
Step S1 regard 50 mg biopolymer nanoparticles (PS) as template first, is added dropwise on slide and guarantees Monolayer Dispersion knot
Structure.By the method for ion sputtering, wherein at least two kinds of different metals, the time such as spraying plating Au, Ag, Pt, Fe, Pd are set as 20-
180 s, plating current < 10 mA.
Step S2, ultrasound collect sample and are placed in three-necked flask, and the triethanolamine (TEOA) of 4 mg, 5-10 mg table is added
Face activating agent: cetyl trimethyl ammonium (CTAB), be added after heating water bath under the conditions of heating (80 DEG C) it is a certain amount of just
Silester (TEOS) (2-10 μ L) grows one layer of mesoporous silicon oxide on surface.
Step S3 completely removes PS template ball, the gold of spraying plating at the same time by Muffle furnace calcining sample within a certain period of time
Category layer, which can dissolve, is dispersed into multiple little particles, can form the hollow mesoporous silicon oxide micro-nano ball of internal more metallic particles.
In step S3, the temperature of calcining is 450 DEG C -550 DEG C.
Using same method, by control different metal ions sputtering time and TEOS additive amount, two layers of spraying plating or
Two layers or more of metal material, to achieve the purpose that interior metal alloying and control thickness of shell.
In the following, by controlling different metal ions sputtering time, containing different metal using the above method to adjust inside
The mesoporous silicon oxide hollow core-shell structure of content.By taking spraying plating monometallic particle as an example, regulate and control spraying plating time 20 s, 40s and
Transmission electron microscope (TEM) characterization of 80 s, obtained mesoporous silicon oxide micro-nano ball are as shown in Figure 2.As it can be seen that with the spraying plating time
Increase, the metal in mesoporous silicon oxide micro-nano ball increases.
In addition, being characterized for the metal nucleocapsid particles under the different spraying plating times, and by elemental analysis to its inside
Metallic particles content is counted, and it is as shown in Figure 3 to obtain curve graph, it can be deduced that following relationship: Y=0.23X+0.31 (R2=
0.99935).Wherein, X is the spraying plating time, and Y is internal metallic particles percentage composition.It can be sprayed by this relationship with quantitative description
The proportionate relationship of time and interior metal content are plated, while hollow mesoporous silicon core-shell structure loading content controllable precise can be synthesized
Metal nanoparticle.
In addition to this, we attempt to carry out the alloying of different metal, and two kinds of spraying plating Au/Pt different element times are respectively
(40/20 s, 40/30 s, 40/40 s), and transmission electron microscope picture is as shown in Figure 4, it is seen then that obtains surface clearly nucleocapsid knot
Structure.EDX the and mapping analysis chart of the bimetallic hollow mesoporous silica nano-particle of spraying plating Au/Pt is as shown in Figure 5.
By above-mentioned experimental result as it can be seen that by regulating and controlling bimetallic sputtering time, so that the ratio of interior metal is adjusted,
Realize the inner alloy of hollow mesoporous silica nano-particle load different metal, while can controllable precise tenor.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (9)
1. a kind of preparation method for the hollow mesoporous silicon oxide micro-nano ball for loading more metallic particles, which is characterized in that it is wrapped
Include following steps:
Step S1 is obtained using the method for the ion sputtering metal material different in the surface spraying plating of the template ball of Monolayer Dispersion
Janus particle;
Step S2 grows one layer of mesoporous silicon oxide in the Janus particle surface that step S1 is obtained using sol-gel method;
Step S3, calcining, removes removing template, and the metal layer of mesoporous silicon oxide inner surface is dispersed into multiple little particles at the same time,
Obtain the hollow mesoporous silicon oxide micro-nano ball of internal more metallic particles.
2. the preparation method of the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load according to claim 1,
It is characterized by: the metal material includes at least two in Au, Ag, Pt, Fe, Pd.
3. the preparation method of the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load according to claim 2,
It is characterized by: plating current < 10 mA of ion sputtering, the spraying plating time is 20-180s in step S1.
4. the preparation method of the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load according to claim 1,
It is characterized by: step S2 the following steps are included: using ultrasonic collection step S1 Janus particulate samples, be placed in reaction and hold
In device, it is added triethanolamine and surfactant, heating water bath is simultaneously added ethyl orthosilicate and is reacted, raw on the surface of sample
Long one layer of mesoporous silicon oxide.
5. the preparation method of the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load according to claim 4,
It is characterized by: the surfactant is cetyl trimethyl ammonium.
6. the preparation method of the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load according to claim 4,
It is characterized by: the dosage of triethanolamine is the 5 ~ 10% of template ball quality, the dosage of the surfactant is template ball quality
10 ~ 20%, the amount of each mg template ball of the dosage of the ethyl orthosilicate is 0.04 ~ 0.2 μ L.
7. the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load described in any one according to claim 1 ~ 6
Preparation method, it is characterised in that: the internal metallic particles of the hollow mesoporous silicon oxide micro-nano ball of internal more metallic particles contain
It measures Y to adjust by ion sputtering spraying plating time X, the numerical relation of the two are as follows: Y=0.23X+0.31.
8. the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load described in any one according to claim 1 ~ 6
Preparation method, it is characterised in that: in step S1, using biopolymer nanoparticles PS as template, dropwise addition forms single layer on slide
The template ball of dispersion.
9. the hollow mesoporous silicon oxide micro-nano ball of the more metallic particles of load described in any one according to claim 1 ~ 6
Preparation method, it is characterised in that: in step S3, the temperature of calcining is 450 ~ 550 DEG C.
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CN114534685A (en) * | 2022-02-22 | 2022-05-27 | 广东邦普循环科技有限公司 | Silicon-aluminum-iron composite material and preparation method and application thereof |
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CN114534685B (en) * | 2022-02-22 | 2023-09-12 | 广东邦普循环科技有限公司 | Silicon-aluminum-iron composite material and preparation method and application thereof |
GB2621299A (en) * | 2022-02-22 | 2024-02-07 | Guangdong Brunp Recycling Technology Co Ltd | Silicon-aluminum-iron composite material, and preparation method therefor and application thereof |
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