CN103160146A - Method for microwave-assisted ferrite surface in-situ modification - Google Patents

Method for microwave-assisted ferrite surface in-situ modification Download PDF

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Publication number
CN103160146A
CN103160146A CN2013101153067A CN201310115306A CN103160146A CN 103160146 A CN103160146 A CN 103160146A CN 2013101153067 A CN2013101153067 A CN 2013101153067A CN 201310115306 A CN201310115306 A CN 201310115306A CN 103160146 A CN103160146 A CN 103160146A
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ferrite
microwave
situ
assisted
modification
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CN2013101153067A
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Chinese (zh)
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刘俊亮
张明
张兴凯
张健
杨文盼
***
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Yangzhou University
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Yangzhou University
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Abstract

The invention relates to a method for microwave-assisted ferrite surface in-situ modification. The method adopts the technical scheme of: based on nanoferrite as an initial raw material, mixing with a high polymer material according to the mass ratio of 1:(1-20) on a mixing mill or an internal mixer; paving the obtained nanoferrite-high polymer mixture in a quartz or ceramic tray; and putting in an industrial microwave oven to carry out irradiation treatment, so as to achieve ferrite in-situ modification. According to the method, the defects that the complexity of the process is increased and the implementation difficulty is also increased due to the fact that the third phase materials, such as a surfactant and a silane coupling agent, need to be introduced to modify inorganic functional bodies in the physical modification or chemical modification in the prior art are solved. A local overheat area is formed on the surface of the ferrite because of microwave absorption under the micro-wave irradiation condition, so that the organic polymer achieves in-situ modification on the ferrite surface, and the compatibility of the inorganic ferrite and organic polymer matrix can be improved.

Description

A kind of method that microwave-assisted ferrite surface in situ is modified
Technical field
The invention belongs to surface and interface control technique in organic-inorganic nano function complex function, specially refer to a kind of method that microwave-assisted ferrite surface in situ is modified.
Background technology
The organic-inorganic nano functional composite material has had sound, light, electricity, magnetic, thermal characteristics and the organic materials lightweight of inorganic materials excellence, the characteristics of toughness concurrently, makes it at photosensor, in electronic component and sensor Advanced Equipment, good application prospect is arranged.For the organic-inorganic nano functional materials, realize that its high-performance, multifunction are the trend of future development, this not only depends on the performance that consists of matrix material each component self, and is usually also closely bound up with the interfacial property that is connected between matrix and functive.Control for the interface roughly can be divided into two levels: 1) improve the consistency between organic phase and inorganic phase; 2) construct the novel organic-inorganic interfacial structure, should, the former is the basis of realizing that organic and inorganic is compound, can realize that possibly material is in qualitative breakthrough and the latter is more.
Before the present invention, be intended to improve the consistency between organic phase and inorganic phase, the inorganic functional body is realized that finishing and modification are a kind of important approach, generally can adopt physics or chemical process that the inorganic functional filling surface is modified, on purpose change inorganic functional surface character, to improve the dispersiveness of inorganic phase in organic matrix.But, all these methods, no matter physically modified or chemical modification all need to introduce third phase material such as tensio-active agent, and silane coupling agents etc. are realized modification to the inorganic functional body, not only increase to a certain extent the complicacy of technique, and increased the difficulty of implementing.For this reason, how to realize that the relative inorganic functional body of organic matrix carries out the finishing of original position, this maybe can become a kind of surface treatment method of novelty, and be needs a urgent difficult problem that solves always.
Summary of the invention
The object of the invention is to overcome defects, develop a kind of method that microwave-assisted ferrite surface in situ is modified.
Technical scheme of the present invention is:
A kind of method that microwave-assisted ferrite surface in situ is modified, its major technique step is as follows:
(1) take nanometer ferrite as starting raw material,, mix on mixing roll or Banbury mixer according to mass ratio 1: 1~20 with macromolecular material;
(2) gained ferrite-macromolecule mixture is tiled in quartz or ceramic tray, is placed in industrial microwave oven and carries out radiation treatment, namely realizes the ferrite in-situ surface finishing.
The present invention is intended to realize that inorganic nano ferrite surface high-molecular in-situ modifies to improve inorganic nanoparticles and macromolecule matrix consistency, reaches organic-inorganic nano compound.Based on this, proposed to utilize nanometer ferrite self absorbing property, under microwave exposure, ferrite surface formation local superheating is regional, makes the near surface polymer soften viscosity flow, realizes the method that inorganic iron oxysome surface in situ is modified.
Advantage of the present invention and effect are to utilize dexterously the local superheating zone of inhaling ripple due to ferrite self and forming on the surface under the microwave exposure condition, make organic polymer realize in-situ modification to the ferrite surface, can improve the consistency of inorganic iron oxysome and organic polymer matrix, provide a kind of novel method for realizing that organic-inorganic nano is compound, and efficient, the preparation of wideband suction wave height molecule based composite material are had good pushing effect.
Method provided by the present invention has the characteristics such as thinking novelty, suitability be strong, is embodied in:
1, utilize ferrite self absorbing property, adopt microwave-assisted to make it to form local superheating near ferrite regional, to realize that macromolecule matrix to the modification of ferrite particle surface in situ, has greatly improved the consistency at interface between inorganic functional body and macromolecule matrix;
2, the present invention does not relate to third phase such as tensio-active agent, and adding of coupling agent etc. reduced the difficulty of finishing, has equipment simple, easy to operate, and the characteristics such as with low cost have represented extremely strong practicality and using value;
3, method provided by the present invention also can prepare the median surface Compatibility improvement and regulate and control to play positive reference function inorganic-organic composite material.
Other concrete advantages of the present invention and effect will go on to say below.
Description of drawings
Fig. 1---the transmission electron microscope photo schematic diagram that microwave-assisted hexagonal strontium ferrite particle surface of the present invention is modified.
Fig. 2---the stereoscan photograph schematic diagram that microwave-assisted hexagonal strontium ferrite particle surface of the present invention is modified.
Embodiment
Concrete thought of the present invention is:
Take the nanometer ferrite powder as starting raw material, carry out blend with appropriate polymer; Under microwave exposure, nanometer ferrite absorbs microwave and is converted into heat energy, in ferrite near surface zone formation local superheating zone, this makes the macromolecular chain softening viscosity flow under the effect of heat that is present in ferrite near surface zone, and even cracking activation, and it is surperficial to spread over the ferrite nanometer particle with high-ratio surface energy, realize that macromolecule matrix modifies the ferrite surface in situ, improve the interface compatibility between inorganic iron ferrite nano particle and macromolecule matrix, lay a good foundation for realizing that further ferrite and macromolecule matrix are nano combined.
The below exemplifies specific embodiment and is illustrated.
Embodiment 1:
(1) be that to adopt hexagonal strontium ferrite powder and macromolecular material in this example be that in this example, employing butylbenzene rubber mass ratio is 1: 3 according to the starting raw material nanometer ferrite, mixing on mixing roll, reach hexagonal strontium ferrite superfine powder and evenly mix with the butylbenzene rubber, get the blend sample;
(2) gained blend sample is put in quartzy pallet, be placed in industrial microwave oven, proportion is 2.45GHz, irradiation power 600W, irradiation time 10min, under microwave exposure, hexagonal strontium ferrite ultra-fine grain strong absorption microwave energy changes heat energy into, promotes the macromolecular chain fracture of its near zone, realize inorganic magnetic particle surface in-situ modification, i.e. sample.
The starting raw material nanometer ferrite must have good absorbing property, can comprise that hexagonal M type ferrite is BaFe 12O 19, SrFe 12O 19And element doping modifier; Hexagonal W type ferrite is BaFe 16O 27And element doping modifier; Hexagonal Z-iron oxysome is Ba 3Fe 24O 41And the element doping modifier, and spinel type ferrite is MFe 2O 4, wherein, M=Mn, Zn, Cu, Ni, Mg, Co and element doping modifier thereof, particle size is at 10nm~1 μ m.
The TEM photo of the sample for preparing is as shown in Figure 1: inorganic iron oxysome powder surface obviously is enclosed with one deck polymer substance, has realized under microwave-assisted, and the surface in situ of ferrite particle is modified.
Embodiment 2:
(1) be 1: 19 according to hexagonal strontium ferrite powder and powder butylbenzene rubber mass ratio, it is mixed on ball mill.
(2) gained blend sample, be put in quartzy pallet, be placed in industrial microwave oven, proportion is 2.45GHz, irradiation power 700W, irradiation time 15min, under microwave exposure, hexagonal strontium ferrite ultra-fine grain strong absorption microwave energy changes heat energy into, promote the macromolecular chain fracture of its near zone, realize inorganic magnetic particle surface in-situ modification.
All the other are with embodiment 1.
The SEM photo of the sample for preparing is as shown in Figure 2: in figure, white dot is inorganic ferrite powder, and its surface obviously has material to coat, and the profile of ferrite particle is comparatively round and smooth, has realized under microwave-assisted, and the surface in situ of ferrite particle is modified.
Embodiment 3:
(1) be 1: 20 according to hexagonal strontium ferrite powder and powder butylbenzene rubber mass ratio, it is mixed on ball mill.
(2) gained blend sample, be put in quartzy pallet, be placed in industrial microwave oven, proportion is 2.45GHz, irradiation power 700W, irradiation time 15min, under microwave exposure, hexagonal strontium ferrite ultra-fine grain strong absorption microwave energy changes heat energy into, promote the macromolecular chain fracture of its near zone, realize inorganic magnetic particle surface in-situ modification.
All the other are with embodiment 1.
Embodiment 4:
(1) be 1: 1 according to hexagonal strontium ferrite powder and powder butylbenzene rubber mass ratio, it is mixed on ball mill.
(3) gained blend sample, be put in quartzy pallet, be placed in industrial microwave oven, proportion is 2.45GHz, irradiation power 700W, irradiation time 15min, under microwave exposure, hexagonal strontium ferrite ultra-fine grain strong absorption microwave energy changes heat energy into, promote the macromolecular chain fracture of its near zone, realize inorganic magnetic particle surface in-situ modification.
All the other are with embodiment 1.

Claims (4)

1. the microwave-assisted ferrite surface in situ method of modifying, its step is as follows:
(1) take nanometer ferrite as starting raw material,, mix on mixing roll or Banbury mixer according to mass ratio 1: 1~20 with macromolecular material;
(2) gained ferrite-macromolecule mixture is tiled in quartz or ceramic tray, is placed in industrial microwave oven and carries out radiation treatment, namely realizes the ferrite in-situ surface finishing.
2. the method for a kind of microwave-assisted ferrite surface in situ modification according to claim 1, is characterized in that in described step (1), the starting raw material nanometer ferrite that adopts comprises that hexagonal M type ferrite is BaFe 12O 19, SrFe 12O 19And element doping modifier; Hexagonal W type ferrite is BaFe 16O 27And element doping modifier; Hexagonal Z-iron oxysome is Ba 3Fe 24O 41And the element doping modifier, and spinel type ferrite is MFe 2O 4, wherein, M=Mn, Zn, Cu, Ni, Mg, Co and element doping modifier thereof, particle size is at 10nm~1 μ m.
3. a kind of microwave-assisted ferrite surface in situ according to claim 1 method of modifying, it is characterized in that in described step (1), the macromolecule matrix that adopts is thermal plastic high polymer, and namely polyethylene, polypropylene, polystyrene and polyvinyl chloride and rubber polymer are natural rubber, styrene-butadiene rubber(SBR), isoprene-isobutylene rubber, terpolymer EP rubber, chloroprene rubber.
4. the method for a kind of microwave-assisted ferrite surface in situ modification according to claim 1, is characterized in that in described step (2), the microwave exposure frequency that adopts is 2.45GHz, irradiation power scope 50~800W, irradiation time 30 seconds to 10 minutes.
CN2013101153067A 2013-04-02 2013-04-02 Method for microwave-assisted ferrite surface in-situ modification Pending CN103160146A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104356646A (en) * 2014-11-24 2015-02-18 扬州大学 Preparation method of ferrite/conductive high-molecular multiphase composite wave-absorbent material
CN105367854A (en) * 2015-12-03 2016-03-02 丁玉琴 Preparation method for nanoscale iron slag-modified styrene-butadiene rubber composite wave-absorbing material
CN107698799A (en) * 2017-10-20 2018-02-16 扬州大学 A kind of method of microwave radiation technology expanded graphite surface polyvinyl chloride in-situ modification

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CN1475534A (en) * 2003-07-01 2004-02-18 武汉理工大学 Powder surface imcrowave auxiliary modification method
CN101209861A (en) * 2006-12-25 2008-07-02 石家智 Method for preparing iron oxide nano material by gas separation method
CN101531835A (en) * 2009-04-24 2009-09-16 吉林大学 Wollastonite powder surface wet modification method assisted by microwave
WO2010004814A1 (en) * 2008-07-07 2010-01-14 旭硝子株式会社 Core-shell particle and method for producing core-shell particle
CN101885868A (en) * 2010-07-16 2010-11-17 扬州大学 Method for preparing magnetic rubber from recovered rubber powder
CN102015913A (en) * 2008-04-25 2011-04-13 3M创新有限公司 Process for the surface modification of particles
CN102477117A (en) * 2010-11-22 2012-05-30 大连创达技术交易市场有限公司 Method for in-situ preparation of organic-inorganic composite nanoparticles
CN102503393A (en) * 2011-10-25 2012-06-20 安徽理工大学 Method for preparing high-performance ferrite material with microwave sintering method
CN102976726A (en) * 2012-08-07 2013-03-20 横店集团东磁股份有限公司 Method for preparing ultrathin type ferrite sheet by using microwave sintering

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4129549A (en) * 1975-03-27 1978-12-12 Union Minerale Method of grafting a polymer to filler materials
CN1475534A (en) * 2003-07-01 2004-02-18 武汉理工大学 Powder surface imcrowave auxiliary modification method
CN101209861A (en) * 2006-12-25 2008-07-02 石家智 Method for preparing iron oxide nano material by gas separation method
CN102015913A (en) * 2008-04-25 2011-04-13 3M创新有限公司 Process for the surface modification of particles
WO2010004814A1 (en) * 2008-07-07 2010-01-14 旭硝子株式会社 Core-shell particle and method for producing core-shell particle
CN101531835A (en) * 2009-04-24 2009-09-16 吉林大学 Wollastonite powder surface wet modification method assisted by microwave
CN101885868A (en) * 2010-07-16 2010-11-17 扬州大学 Method for preparing magnetic rubber from recovered rubber powder
CN102477117A (en) * 2010-11-22 2012-05-30 大连创达技术交易市场有限公司 Method for in-situ preparation of organic-inorganic composite nanoparticles
CN102503393A (en) * 2011-10-25 2012-06-20 安徽理工大学 Method for preparing high-performance ferrite material with microwave sintering method
CN102976726A (en) * 2012-08-07 2013-03-20 横店集团东磁股份有限公司 Method for preparing ultrathin type ferrite sheet by using microwave sintering

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104356646A (en) * 2014-11-24 2015-02-18 扬州大学 Preparation method of ferrite/conductive high-molecular multiphase composite wave-absorbent material
CN104356646B (en) * 2014-11-24 2017-07-04 扬州大学 The preparation method of ferrite/conducting polymer multiphase composite wave-suction material
CN105367854A (en) * 2015-12-03 2016-03-02 丁玉琴 Preparation method for nanoscale iron slag-modified styrene-butadiene rubber composite wave-absorbing material
CN107698799A (en) * 2017-10-20 2018-02-16 扬州大学 A kind of method of microwave radiation technology expanded graphite surface polyvinyl chloride in-situ modification

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Application publication date: 20130619