CN107399738A - A kind of method that magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials - Google Patents

A kind of method that magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials Download PDF

Info

Publication number
CN107399738A
CN107399738A CN201710684802.2A CN201710684802A CN107399738A CN 107399738 A CN107399738 A CN 107399738A CN 201710684802 A CN201710684802 A CN 201710684802A CN 107399738 A CN107399738 A CN 107399738A
Authority
CN
China
Prior art keywords
magnetic field
nanostructured materials
hollow
mesoporous nanostructured
kinkendal effect
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710684802.2A
Other languages
Chinese (zh)
Other versions
CN107399738B (en
Inventor
盛志高
卞跃成
丁伟
胡林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hefei Institutes of Physical Science of CAS
Original Assignee
Hefei Institutes of Physical Science of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hefei Institutes of Physical Science of CAS filed Critical Hefei Institutes of Physical Science of CAS
Priority to CN201710684802.2A priority Critical patent/CN107399738B/en
Publication of CN107399738A publication Critical patent/CN107399738A/en
Application granted granted Critical
Publication of CN107399738B publication Critical patent/CN107399738B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a kind of method that magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials, during hollow/mesoporous nanostructured materials are prepared using Kinkendal Effect, hydro-thermal reaction step therein is carried out under additional magnetic field condition.The present invention is substantially reduced using Kinkendal Effect from solid nanostructures material to the transformation time of hollow/mesoporous nanostructured materials at a lower temperature using externally-applied magnetic field; there is huge Benefit Value for reducing reaction preparation cost, meet the current saving energy and the development topic of environmental protection.

Description

A kind of magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials Method
Technical field
The present invention relates to field of nanometer technology, more particularly to a kind of magnetic field modulation Kinkendal Effect prepare it is hollow/mesoporous The method of nano structural material.
Background technology
Ke Kendaer(Kirkendall)Effect is a kind of classical method for synthesizing hollow/meso-porous nano structure, It is widely used in the synthesis of various hollow nano/Mesoporous Spheres.The various hollow nano structures synthesized by this method are widely used, It is widely applied in neighborhoods such as nanocatalyst, nano-reactor, drug delivery, electrode material, optical materials.Current system Standby this method generally requires high temperature again, reacts for a long time.This undoubtedly improves business and prepares cost.And magnetic field is as a species The thermodynamic parameter of temperature, pressure etc. is similar to, substantial amounts of physics and chemical process are all had a major impact.And magnetic field is to material Effect be by a kind of contactless mode, it is simple to operate.In addition with the fast development of society, shortage of resources and ring Border problem becomes increasingly conspicuous, and by shortening the reaction time, reduces reaction cost, increasingly becomes industrial active demand.
Generally, hollow/meso-porous nano structure function material is accordingly synthesized using Ke Kendaer to be required in high temperature, React for a long time.Ke Kendaer(Kirkendall)Effect relates generally to the diffusion couple with different diffusion coefficients, is mutually expanding In scattered process, internal core layer material is more than the speed that outside Shell Materials inwardly spread to the speed of external diffusion, is expanding Internal in scattered process to gradually form hole, last hole polymerize to form a big internal cavities.The present invention is to be based on nanometer Structural material passes through Ke Kendaer(Kirkendall)During effect is converted into hollow/mesoporous nanostructured materials, pass through The auxiliary of externally-applied magnetic field, promote above-mentioned conversion process.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided prepared by a kind of magnetic field modulation Kinkendal Effect The method of hollow/mesoporous nanostructured materials.
The present invention is achieved by the following technical solutions:
A kind of method that magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials, it is characterised in that utilizing During Kinkendal Effect prepares hollow/mesoporous nanostructured materials, reactions steps therein are in additional magnetic field condition Lower progress.
The method that described magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials, including following tool Body step:
(1)Nano structural material is pre-processed to form precursors or nano structural material directly is dispersed in into liquid phase reactor In thing, formation can form hollow or mesoporous nanostructured materials reaction systems using Kinkendal Effect;
(2)Hollow or mesoporous nanostructured materials reaction systems can be formed by what is obtained outside using Kinkendal Effect Add and synthetic reaction is carried out in magnetic field, obtain hollow/mesoporous nanostructured materials.
The nano structural material is metal or inorganic non-metallic nano structural material.
The size of the nano structural material is 50-500nm.
Described externally-applied magnetic field is steady magnetic field or alternating magnetic field.
The intensity of the steady magnetic field is no more than 10T.
The nano structural material is nano silicon particles, and the liquid phase reactor thing is deionized water.
The preprocess method is that air atmosphere lower part aoxidizes at 800-1000 DEG C by nano silicon particles.
Described synthetic reaction condition is 180-200 DEG C, 5-10h.
It is an advantage of the invention that:
During hollow/mesoporous nanostructured materials are prepared using Kinkendal Effect, externally-applied magnetic field can promote nucleocapsid The mutual diffusion process of material, so as to accelerate the formation of inner void.
The present invention is to utilize externally-applied magnetic field at a lower temperature, substantially reduces and is received using Kinkendal Effect from solid Transformation time of the rice structural material to hollow/mesoporous nanostructured materials.This has huge effect for reducing reaction preparation cost Benefit value.Meet the current saving energy and the development topic of environmental protection.
Brief description of the drawings
Fig. 1 is the schematic diagram for preparing hollow nano/mesoporous nanostructured materials using Kinkendal Effect under magnetic field.1 Represented respectively within the same reaction time with 2, during no magnetic field, obtained nano structural material structure microscopic appearance is shown in 1, has During magnetic field, the obtained microcosmic appearance of nano structural material is shown in 2.
Fig. 2 is the equipment figure for preparing hollow nano/mesoporous nanostructured materials using Kinkendal Effect under magnetic field. Wherein 1 represents superconducting magnet cold head, and 2 represent 10 T superconducting magnet, and 3 represent stainless steel autoclave, and 4 represent the water cooling of heating furnace Layer, 5 represent the temperature control of heating furnace, and 6 represent whole heating furnace.
Fig. 3 is the transmission electron microscope of sample(TEM)Picture.
Embodiment
Embodiment
First by nano silicon particles in tube furnace in 800 DEG C, air atmosphere lower part oxidation, in the table of nano silicon particles Face forms one layer of thin oxide layer, obtains predecessor of the nano silicon particles after partial oxidation as hydro-thermal reaction, then passes through Supersound process is dispersed in deionized water by the nano silicon particles after the partial oxidation, adds and is served as a contrast with polytetrafluoroethylene (PTFE) In the stainless steel autoclave at bottom, seal, then stainless steel autoclave is put into heater, finally equipped with stainless after packaged The heater of steel autoclave is put into steady magnetic field under the conditions of 1T in 180 DEG C of hydro-thermal reaction 5h, and another preparation identical presoma is molten Liquid reacts 5h and 24h respectively under without magnetic field, carries out TEM tests to obtained sample, as a result as shown in Figure 3.
Fig. 3 is transmission electron microscope (TEM) picture of sample.Left side figure and middle graph are the conditions in no magnetic field Under in 180 DEG C respectively react 5h, 24h after sample topography.Right side figure be in steady magnetic field under the conditions of 1T 180 DEG C reaction 5h after sample topography.It can be seen that final result is all that of obtaining hollow shell structure, and in same temperature Under degree, the mesopore size that reaction 5h is obtained in 1T steady magnetic fields is both greater than the nano structural material for being not added with magnetic field reaction 5h Mesopore size.By Fig. 3 contrast, the Ke Kendaer that magnetic field accelerates mesoporous nanostructured materials is demonstrated from the real space Effect.
By the way that the test result of above-described embodiment is analyzed, it is known that the presence in magnetic field is to meso-porous nano material There is acceleration effect in Kinkendal Effect, help to shorten at a lower temperature using Kinkendal Effect from solid nano junction Transformation time of the structure material to hollow/mesoporous nanostructured materials.

Claims (9)

1. a kind of method that magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials, it is characterised in that in profit During preparing hollow/mesoporous nanostructured materials with Kinkendal Effect, synthetic reaction step therein is in additional magnetic Carried out under field condition.
2. a kind of magnetic field modulation Kinkendal Effect according to claim 1 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that including step in detail below:
(1)Nano structural material is pre-processed to form precursors or nano structural material directly is dispersed in into liquid phase reactor In thing, formation can form hollow or mesoporous nanostructured materials reaction systems using Kinkendal Effect;
(2)Hollow or mesoporous nanostructured materials reaction systems can be formed by what is obtained outside using Kinkendal Effect Add and synthetic reaction is carried out in magnetic field, obtain hollow/mesoporous nanostructured materials.
3. a kind of magnetic field modulation Kinkendal Effect according to claim 2 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that the nano structural material is metal or inorganic nonmetallic nanometer material.
4. a kind of magnetic field modulation Kinkendal Effect according to claim 2 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that the size of the nano structural material is 50-500nm.
5. a kind of magnetic field modulation Kinkendal Effect according to claim 2 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that described externally-applied magnetic field is steady magnetic field or alternating magnetic field.
6. a kind of magnetic field modulation Kinkendal Effect according to claim 5 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that the intensity of the steady magnetic field is not more than 10T.
7. a kind of magnetic field modulation Kinkendal Effect according to claim 2-6 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that the nano structural material is nano silicon particles, and the liquid phase reactor thing is deionized water.
8. a kind of magnetic field modulation Kinkendal Effect according to claim 7 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that the preprocess method is that air atmosphere lower part aoxidizes at 800-1000 DEG C by nano silicon particles.
9. a kind of magnetic field modulation Kinkendal Effect according to claim 7 prepares hollow/mesoporous nanostructured materials Method, it is characterised in that described synthetic reaction condition is 180-200 DEG C, 5-10h.
CN201710684802.2A 2017-08-11 2017-08-11 Method for preparing hollow/mesoporous nano-structure material by magnetic field modulation Cokendall effect Active CN107399738B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710684802.2A CN107399738B (en) 2017-08-11 2017-08-11 Method for preparing hollow/mesoporous nano-structure material by magnetic field modulation Cokendall effect

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710684802.2A CN107399738B (en) 2017-08-11 2017-08-11 Method for preparing hollow/mesoporous nano-structure material by magnetic field modulation Cokendall effect

Publications (2)

Publication Number Publication Date
CN107399738A true CN107399738A (en) 2017-11-28
CN107399738B CN107399738B (en) 2020-04-03

Family

ID=60396355

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710684802.2A Active CN107399738B (en) 2017-08-11 2017-08-11 Method for preparing hollow/mesoporous nano-structure material by magnetic field modulation Cokendall effect

Country Status (1)

Country Link
CN (1) CN107399738B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114620737A (en) * 2022-01-19 2022-06-14 中国科学院深圳先进技术研究院 Hollow silicon dioxide and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105839146A (en) * 2016-04-01 2016-08-10 宁夏邦鼎材料与环保科技有限公司 Silicon-germanium solid solution and preparation method and application thereof
KR20160136550A (en) * 2015-05-20 2016-11-30 고려대학교 산학협력단 Method of manufacturing a nano metal oxide particle having a hollow structure

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20160136550A (en) * 2015-05-20 2016-11-30 고려대학교 산학협력단 Method of manufacturing a nano metal oxide particle having a hollow structure
CN105839146A (en) * 2016-04-01 2016-08-10 宁夏邦鼎材料与环保科技有限公司 Silicon-germanium solid solution and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李东刚: "异质金属体系扩散行为和界面反应的强磁场控制研究", 《中国博士学位论文全文数据库工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114620737A (en) * 2022-01-19 2022-06-14 中国科学院深圳先进技术研究院 Hollow silicon dioxide and preparation method and application thereof
CN114620737B (en) * 2022-01-19 2023-09-15 深圳先进电子材料国际创新研究院 Hollow silicon dioxide and preparation method and application thereof

Also Published As

Publication number Publication date
CN107399738B (en) 2020-04-03

Similar Documents

Publication Publication Date Title
Salavati-Niasari et al. Synthesis of lanthanum carbonate nanoparticles via sonochemical method for preparation of lanthanum hydroxide and lanthanum oxide nanoparticles
CN109536137B (en) Phase-change microcapsule with magnetic and photo-thermal conversion characteristics and preparation method thereof
CN105776350B (en) A kind of preparation method of hollow bar-shaped ferroso-ferric oxide and its compound
CN103193273B (en) Preparation method of extra-long manganese dioxide nanowires
CN106115805A (en) The preparation method of nanometer hierarchy cobalt acid nickel/mos2 microsphere
Chen et al. Synthesis of hierarchical transition metal oxyhydroxides in aqueous solution at ambient temperature and their application as OER electrocatalysts
CN109692701A (en) g-C3N4/MoS2Composite photo-catalyst and its one-pot preparation thereof
Ai et al. Study of ZrO2 nanopowders based stearic acid phase change materials
CN104150451A (en) Preparation method for nickel phosphide with hollow core-shell structure
CN107399738A (en) A kind of method that magnetic field modulation Kinkendal Effect prepares hollow/mesoporous nanostructured materials
CN105129849A (en) Flowerlike nano-sized titanium dioxide material and template-free preparation method thereof
CN108440767A (en) It is a kind of that nanometer Au is combined to the new method for preparing Au@MOF composite materials with porous MOF
Tian et al. MoS2‐Based Catalysts for N2 Electroreduction to NH3–An Overview of MoS2 Optimization Strategies
CN107497455A (en) A kind of preparation method and applications of the ultra-thin Bismuth tungstate nano-sheet photochemical catalyst of Determination of Trace Sulfur surface modification
CN104985194B (en) A kind of preparation method at oxide dispersion intensifying iron cobalt nano composite powder end
CN110116017A (en) A kind of azotized carbon nano tube preparation method of copper platinum bimetallic load
Wang et al. Transmission electron microscopy and Raman characterization of copper (I) oxide microspheres composed of nanoparticles
CN109128216A (en) The synthetic method of gold nanoparticle under room temperature
CN108083338B (en) A kind of ion liquid microemulsion thermal synthesis MoS2The preparation method of sub-micron bouquet
CN108996548A (en) A kind of preparation method of orthorhombic phase nano bar-shape molybdenum trioxide
CN104817107B (en) A kind of method of preparing black titanium dioxide B phase and anatase-phase nano particle
CN102531062B (en) Structure-controlling preparation of uniform-thickness ultrathin iron tungstate nanosheet
CN107188216A (en) A kind of preparation method of nanometer spherical cerium group light rare earth oxide
CN108083337A (en) A kind of method that hollow mos2 microsphere is prepared in reverse micro emulsion
CN108977827A (en) Include FeSe2-Co3O4Composite material and preparation method and catalyst and application

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant