CN102838351B - Multiferroic material and preparation method thereof - Google Patents

Multiferroic material and preparation method thereof Download PDF

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Publication number
CN102838351B
CN102838351B CN201210351069.XA CN201210351069A CN102838351B CN 102838351 B CN102838351 B CN 102838351B CN 201210351069 A CN201210351069 A CN 201210351069A CN 102838351 B CN102838351 B CN 102838351B
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preparation
multiferroic material
raw material
temperature
rutile
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CN102838351A (en
Inventor
侯育冬
王赛
朱满康
刘晶冰
王如志
张铭
宋雪梅
汪浩
严辉
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The invention provides a multiferroic material and a preparation method thereof, belonging to the technical field of a multiferroic material. The multiferroic material is in a rutile structure, and has a chemical component of FeTiNbO6. The preparation method of the multiferroic material comprises the following steps of: carrying out ball-milling, mixing and drying on Fe2O3, Nb2O5 and TiO2; placing a mixture in a sealed crucible for pre-burning and then crushing; adding polyvinyl alcohol for pelletizing, and pressing a blank piece after passing through an 80-mesh sieve; and placing the blank piece at a temperature of 700 DEG C for discharging glue, arranging the blank piece in the sealed crucible, sintering at a temperature of 900-1400 DEG C, and keeping the temperature for 2-6 h. The rutile type multiferroic material provided by the invention has the advantages of stable structure, simple preparation method, low cost and easiness of operation.

Description

A kind of multi-iron material and preparation method
Technical field
The present invention relates to a kind of multi-iron material, relate in particular to a kind of rutile-type ferromagnetic-ferroelectric ceramic material and preparation method thereof, belong to multi-iron material technical field.
Background technology
Multi-iron material has multiferroic (as ferromegnetism, ferroelectricity, ferroelasticity etc.), due to its huge potential application foreground, developed into a very important field of research, wherein ferroelectricity and magnetic coexist, and magnetoelectricity tight coupling effect is the central issue of research work.Research for multi-iron material focuses mostly at present in the material of perovskite structure, although these material electric properties are excellent, the multi-iron material of single perovskite structure has seriously limited the commercial applications of multi-iron material in semiconductor microactuator field of electronic devices.
The TiO of rutile structure 2be a kind of broad-band gap (3.05eV) semiconductor material, along c-axis, there is large static dielectric (165-250), in micro-wave dielectric field, have important application.While rutile TiO 2be a kind of typical tendency Ferroelectric body, existing researchist finds titanium dioxide to adulterate, and can make it when retaining structure, bring out its ferroelectric generation.Rutile-type multi-iron material of the present invention is utilizing iron ion and niobium ion that titanium dioxide is adulterated and brought out its ferroelectric while, bring out the generation of its magnetic, become a kind of novel lead-free ferromagnetic-ferroelectric material, be a kind of novel multi-ferroic material with potential researching value.
Summary of the invention
The object of the present invention is to provide a kind of novel rutile-type ferromagnetic-ferroelectric material and preparation method thereof, multi-ferroic material prepared by the method has also shown certain magnetics feature when having certain relaxor ferroelectric.
For achieving the above object, the present invention takes following technical scheme:
A kind of multi-iron material of the present invention, is characterized in that, the stupalith that the iron ion that multi-ferroic material is rutile structure and niobium ion adulterate to titanium dioxide, and chemical constitution formula is: FeTiNbO 6.
The concrete preparation method of multi-iron material of above-mentioned rutile structure, the preparation of employing process for solid phase synthesis is tapped a blast furnace, the titania-doped rutile structure pottery of niobium, comprises the steps:
(1) first by Fe 2o 3, Nb 2o 5and TiO 2, 1:1:2 prepares burden in molar ratio;
(2) material step (1) being prepared is put into ball mill batch mixing, requires to mix, and obtains ball milling material;
(3) raw material mixing in step (2) being put into baking oven dries;
(4) the raw material mixed powder of drying in step (3) is put into airtight crucible, be placed in stove and be warming up to pre-burning at 800 ~ 1200 ℃, soaking time is 2 ~ 6h;
(5) block step (4) being obtained grinds in mortar, adds the polyvinyl alcohol of 1 ~ 5wt% of this powder weight to carry out granulation, crosses after 80 mesh sieves, is pressed into base sheet under 120 ~ 300Mpa;
(6) base sheet step (5) compacting being obtained carries out being placed in airtight crucible after binder removal at 700 ℃, sintering at 900 ~ 1400 ℃, insulation 2 ~ 6h.
Compared with prior art, the present invention has following beneficial effect:
(1) rutile-type multi-iron material of the present invention is utilizing iron ion and niobium ion that titanium dioxide is adulterated and brought out its ferroelectric while, bring out the generation of its magnetic, become a kind of novel lead-free ferromagnetic-ferroelectric material, be a kind of novel multi-ferroic material with potential researching value.
(2) rutile-type multi-iron material Stability Analysis of Structures of the present invention, preparation method is simple, cost is low, easy handling.
Accompanying drawing explanation
Fig. 1 has provided the synthetic FeTiNbO of embodiment 3 6the XRD figure spectrum of pottery;
Fig. 2 has provided the synthetic FeTiNbO of embodiment 3 6the dielectric temperature spectrum of pottery;
Fig. 3 has provided the synthetic FeTiNbO of embodiment 3 6the magnetic hysteresis loop of pottery.
Embodiment
The present invention is further described with the following Examples, but following examples are not construed as limiting the invention.
Embodiment 1:
The preparation method of the multi-iron material that the present embodiment 1 is a kind of rutile structure, concrete steps are as follows:
(1) first by Fe 2o 3, Nb 2o 5and TiO 2, according to mol ratio, 1:1:2 prepares burden.
(2) material step (1) being prepared is put into ball mill batch mixing, requires to mix, and obtains ball milling material;
(3) raw material mixing in step (2) being put into baking oven dries.
(4) the raw material mixed powder of drying in step (3) is put into airtight crucible, be placed in stove and be warming up to pre-burning at 900 ℃, soaking time is 4h.
(5) block step (4) being obtained grinds in mortar, adds the polyvinyl alcohol of 1 ~ 5wt% of this powder weight to carry out granulation, crosses after 80 mesh sieves, and under 120 ~ 300Mpa, being pressed into diameter degree is the thin stock sheet that 11.5mm, thickness are 0.5 ~ 2mm.
(6) thin stock sheet step (5) compacting being obtained carries out being placed in airtight crucible after binder removal at 700 ℃, and sintering at 1000 ℃ obtains ceramic plate after insulation 5h.
Embodiment 2:
(1) first by Fe 2o 3, Nb 2o 5and TiO 2, according to mol ratio, 1:1:2 prepares burden.
(2) material step (1) being prepared is put into ball mill batch mixing, requires to mix, and obtains ball milling material;
(3) raw material mixing in step (2) being put into baking oven dries.
(4) the raw material mixed powder of drying in step (3) is put into airtight crucible, be placed in stove and be warming up to pre-burning at 1000 ℃, soaking time is 4h.
(5) block step (4) being obtained grinds in mortar, adds the polyvinyl alcohol of 1 ~ 5wt% of this powder weight to carry out granulation, crosses after 80 mesh sieves, and under 120 ~ 300Mpa, being pressed into diameter degree is the thin stock sheet that 11.5mm, thickness are 0.5 ~ 2mm.
(6) thin stock sheet step (5) compacting being obtained carries out being placed in airtight crucible after binder removal at 700 ℃, and sintering at 1100 ℃ obtains ceramic plate after insulation 5h.
Embodiment 3:
(1) Fe 2o 3, Nb 2o 5and TiO 2, according to mol ratio, 1:1:2 prepares burden.
(2) material step (1) being prepared is put into ball mill batch mixing, requires to mix, and obtains ball milling material;
(3) raw material mixing in step (2) being put into baking oven dries.
(4) the raw material mixed powder of drying in step (3) is put into airtight crucible, be placed in stove and be warming up to pre-burning at 1050 ℃, soaking time is 4h.
(5) block step (4) being obtained grinds in mortar, adds the polyvinyl alcohol of 1 ~ 5wt% of this powder weight to carry out granulation, crosses after 80 mesh sieves, and under 120 ~ 300Mpa, being pressed into diameter degree is the thin stock sheet that 11.5mm, thickness are 0.5 ~ 2mm.
(6) thin stock sheet step (5) compacting being obtained carries out being placed in airtight crucible after binder removal at 700 ℃, and sintering at 1125 ℃ obtains ceramic plate after insulation 5h.
Fig. 1 has provided the synthetic FeTiNbO of embodiment 3 6the XRD figure spectrum of pottery;
Fig. 2 has provided the synthetic FeTiNbO of embodiment 3 6the dielectric temperature spectrum of pottery;
Fig. 3 has provided the synthetic FeTiNbO of embodiment 3 6the magnetic hysteresis loop of pottery.

Claims (1)

1. a preparation method for multi-iron material, is characterized in that, comprises the steps:
(1) Fe 2o 3, Nb 2o 5and TiO 2, according to mol ratio, 1:1:2 prepares burden;
(2) material step (1) being prepared is put into ball mill batch mixing, requires to mix, and obtains ball milling material;
(3) raw material mixing in step (2) being put into baking oven dries;
(4) the raw material mixed powder of drying in step (3) is put into airtight crucible, be placed in stove and be warming up to pre-burning at 1050 ℃, soaking time is 4h;
(5) block step (4) being obtained grinds in mortar, adds the polyvinyl alcohol of 1～5wt% of this powder weight to carry out granulation, crosses after 80 mesh sieves, and under 120～300Mpa, being pressed into diameter is the thin stock sheet that 11.5mm, thickness are 0.5～2mm;
(6) thin stock sheet step (5) compacting being obtained carries out being placed in airtight crucible after binder removal at 700 ℃, and sintering at 1125 ℃ obtains ceramic plate after insulation 5h.
CN201210351069.XA 2012-09-19 2012-09-19 Multiferroic material and preparation method thereof Expired - Fee Related CN102838351B (en)

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CN104177076B (en) * 2014-08-14 2016-04-13 华中科技大学 A kind of Al 3+doping Bi 2fe 4o 9multiferroic stupalith and preparation method thereof
CN105293585B (en) * 2015-12-01 2016-11-30 福建江夏学院 A kind of iron titanate nano-powder of zinc-nickel doping and preparation method thereof

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CN101186496A (en) * 2007-11-27 2008-05-28 西安交通大学 Low-temperature sintering Ti-base microwave medium ceramic material and preparation thereof

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CN101186496A (en) * 2007-11-27 2008-05-28 西安交通大学 Low-temperature sintering Ti-base microwave medium ceramic material and preparation thereof

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Title
Rohini Mani等.Dielectric properties of some MM′O4 and MTiM′O6 (M=Cr,Fe,Ga;M′=Nb,Ta,Sb) rutile-type oxides.《Journal of Solid State Chemistry》.2010,第183卷(第6期),第1380–1387页. *

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