CN104671755B - Preparation method of magneto-electric coupling multi-ferroic material BiMn3Cr4O12 - Google Patents
Preparation method of magneto-electric coupling multi-ferroic material BiMn3Cr4O12 Download PDFInfo
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- CN104671755B CN104671755B CN201510069601.2A CN201510069601A CN104671755B CN 104671755 B CN104671755 B CN 104671755B CN 201510069601 A CN201510069601 A CN 201510069601A CN 104671755 B CN104671755 B CN 104671755B
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Abstract
The invention discloses a magneto-electric coupling multi-ferroic material and a preparation method thereof. A chemical formula of the novel magneto-electric coupling multi-ferroic material is BiMn3Cr4O12. The method for preparing the novel magneto-electric coupling multi-ferroic material BiMn3Cr4O12 comprises the following steps: mixing Bi2O3, Mn2O3 and Cr2O3 of which the purities are more than 99.9% according to a molar ratio of 1:3:4, and then fully grinding and screening; filling screened raw materials into gold capsules or platinum capsules and compacting; and performing solid-phase reaction at high temperature and high pressure. The novel magneto-electric coupling multi-ferroic material BiMn3Cr4O12 disclosed by the invention has weak ferromagnetic spin orders, relatively large dielectric constants and electric dipolar polarization strength as well as relatively high critical temperature, and has good application prospects in the fields of spin electronic devices and multi-state memory devices.
Description
Technical field
The present invention relates to material science is and in particular to a kind of magneto-electric coupled multi-ferroic material bimn3cr4o12Preparation
Method.
Background technology
Magneto-electric coupled multi-ferroic material (magnetoelectric coupling multiferroics) refers to have simultaneously
There are ferroelectricity and the compound of long-range magnetic order, and ferroelectricity and magnetic order have stronger coupling effect.This kind of material can
To realize the mutual regulation and control of electricity and magnetic, for example, electric polarization state is regulated and controled by magnetic field, magnetized state, therefore magnetic are regulated and controled by electric field
Being electrically coupled multi-ferroic material is a kind of Multifunction material, has in fields such as spintronics, multiple-state storage, electromagnetic sensors
It is widely applied prospect.
In transition metal oxide, electric polarization does not need d electronics to participate in, and long-range magnetic order needs the participation of d electronics.
Therefore, ferroelectricity and long-range magnetic order are difficult to coexist in same material system and mutually regulation and control in principle.However,
People find that some special magnetic structures can break the inversion symmetry of some material systems, thus producing spin recently
The electric polarization leading in order, i.e. so-called magnetoelectricity many iron coupling effect.At present, there is the material system of magneto-electric coupled many iron effect
Still very limited, significantly restrict research and the application of this novel effect.
Content of the invention
In view of this, the present invention proposes a kind of magneto-electric coupled multi-ferroic material bimn3cr4o12With and preparation method thereof.
In a first aspect, the invention provides a kind of magneto-electric coupled multi-ferroic material, described novel magnetic power couples multiferroic
The chemical formula of material is bimn3cr4o12.
In second aspect, the invention provides a kind of magneto-electric coupled multi-ferroic material bimn3cr4o12Preparation method, bag
Include:
It is higher than 99.9% bi purity2o3、mn2o3And cr2o3It is fully ground after 1:3:4 mixing in molar ratio, screen；
Garbled raw material is loaded gold or platinum capsule and is compacted；
HTHP solid phase reaction.
Preferably, the device of described HTHP solid phase reaction is cubic hinge press or two grades of propulsion press of 6-8 type.
Preferably, the pressure of described HTHP solid phase reaction be 6-10gpa, temperature be 900-1300 DEG C, HTHP
Reaction time is 10-60 minute.
Preferably, a diameter of 2-10mm of described gold or platinum capsule, length is 2-10mm, and wall thickness is 1-2mm.
Bimn proposed by the present invention3cr4o12It is a kind of new magneto-electric coupled multi-ferroic material, it has weak ferromagnetic spin
Sequence, larger dielectric constant and galvanic couple polarization intensity, and higher critical-temperature, in spin electric device, multi-state memory
There is good application prospect in the fields such as part.
Brief description
By the description to the embodiment of the present invention referring to the drawings, the above-mentioned and other purpose of the present invention, feature and
Advantage will be apparent from, in the accompanying drawings:
Fig. 1 shows the magneto-electric coupled multi-ferroic material bimn of embodiment 1 preparation3cr4o12Xrd collection of illustrative plates；
Fig. 2 shows the bimn of embodiment 1 preparation3cr4o12Magnetic susceptibility and the curve that varies with temperature of specific heat；
Fig. 3 shows the bimn of embodiment 1 preparation3cr4o12Dielectric constant with temperature change curve；
Fig. 4 shows the bimn of embodiment 1 preparation3cr4o12The curve that varies with temperature of polarization intensity；
Fig. 5 shows the bimn of embodiment 1 preparation3cr4o12Electric hysteresis loop；And
Fig. 6 shows the bimn of embodiment 1 preparation3cr4o12Hysteresis curve.
Specific embodiment
Below in the detailed description of the present invention, detailed describe some specific detail sections.To art technology
For personnel, the description of part can also understand the present invention completely without these details.In order to avoid obscuring the essence of the present invention,
Known method, process, flow process, element and circuit do not describe in detail.Unless the context clearly requires otherwise, otherwise entirely illustrate
Book and the similar words such as " inclusion " in claims, "comprising" should be construed to the implication comprising rather than exclusive or exhaustive
Implication；That is, being the implication of " including but not limited to ".
The present invention relates to have the magneto-electric coupled multi-ferroic material bimn of ferroelectricity and long-range magnetic order simultaneously3cr4o12And
Its preparation method.As a preferred embodiment of the present invention, bimn proposed by the present invention3cr4o12Can be by following steps
Preparation:
It is higher than 99.9% bi purity2o3、mn2o3And cr2o3It is fully ground after 1:3:4 mixing in molar ratio, then pass through
200 mesh sieve screenings；Garbled raw material is loaded gold or platinum capsule being compacted, wherein, described gold or platinum capsule straight
Footpath is 2-10mm, and length is 2-10mm, and wall thickness is 1-2mm；Capsule is placed in cubic hinge press or two grades of propulsion press of 6-8 type,
Setting pressure is 6-10gpa, temperature is 900-1300 DEG C, makes the raw material reaction time at high temperature under high pressure in gold or platinum capsule
For 10-60 minute.
Below based on embodiment, present invention is described, but the present invention is not restricted to these embodiments.
Embodiment 1:
It is higher than 99.9% bi purity2o3、mn2o3And cr2o3Pass through after being fully ground after 1:3:4 mixing in molar ratio
200 mesh sieve screenings；Garbled raw material is loaded gold or platinum capsule being compacted, wherein, described gold or platinum capsule straight
Footpath is 10mm, and length is 10mm, and wall thickness is 2mm；Gold or platinum capsule are placed in cubic hinge press or two grades of propulsion pressures of 6-8 type
Machine, setting pressure is 8gpa, temperature is 1050 DEG C, and the reaction time is 30 at high temperature under high pressure to make the raw material in gold or platinum capsule
Minute.
Fig. 1 shows the novel magnetic power coupling multi-ferroic material bimn of embodiment 1 preparation3cr4o12Xrd collection of illustrative plates.Pass through
Novel magnetic power couples multi-ferroic material bimn3cr4o12Xrd collection of illustrative plates can obtain prepare bimn3cr4o12Belong to a position to stand in order
Square structure of double perovskite, belongs to im-3 space group, and lattice parameter is
Fig. 2 shows the bimn of embodiment 1 preparation3cr4o12Magnetic susceptibility and the curve that varies with temperature of specific heat.Wherein,
The measurement process of null field cooling (zero field cooled, zfc) of magnetic susceptibility, lowers the temperature, so in the case of being not added with magnetic field first
Rise the magnetic susceptibility of temperature measurement sample afterwards under externally-applied magnetic field h, have the measurement process of field cooling (field cooled, fc), first
Lower the temperature under externally-applied magnetic field h, under externally-applied magnetic field h, then rise the magnetic susceptibility of temperature measurement sample.From bimn3cr4o12Magnetic susceptibility with
Bimn can be obtained than heating curve3cr4o12There are two antiferromagnetic phase transformations, corresponding antiferromagnetic phase transition temperature respectively may be about tn1=
120k and tn2=40k.
Fig. 3 shows the bimn of embodiment 1 preparation3cr4o12Dielectric constant with temperature change curve.As shown in figure 3,
Reduce with temperature, dielectric constant is gradually increased, and reaches maximum near 140k and form wider peak, particularly in tn2Attached
The variation tendency of nearly dielectric constant has a significantly change, imply that the coupling of magnetic dielectric property.
Fig. 4 shows the bimn of embodiment 1 preparation3cr4o12The added electric field cooling polarization intensity that obtains of measurement with temperature
The curve of change.Just electropolarized appearance can be observed when temperature is reduced to 170k as shown in Figure 4, drop further with temperature
Low electrode intensity is gradually increased, and in tn1Nearby close to saturation.But it is cooled to t furthern2When nearby, electric polarization
Strengthened again, more confirmed tn2Neighbouring magneto-electric coupled many iron behavior and there is larger electric polarization.
Fig. 5 shows the bimn of embodiment 1 preparation3cr4o12Ferroelectric hysteresis loop.As shown in figure 5, the maximum field of extra electric field
It is by force 8.5kv/cm, bimn3cr4o12There is obvious ferroelectricity.In 30k, remanent polarization is 0.045 μ c/cm to temperature2,
Coercive field is 6.0kv/cm；In 75k, remanent polarization is 0.082 μ c/cm to temperature2, coercive field is 5.8kv/cm；Temperature
In 130k, remanent polarization is 0.071 μ c/cm2, coercive field is 5.7kv/cm.Ferroelectric hysteresis loop tests equal table with electric polarization
Bright bimn3cr4o12Characteristic of Electric Polarization Feature occurred more than antiferromagnetic order temperature, and in tn2When obvious magnetic can be observed
It is electrically coupled the behavior of many iron.
Fig. 6 shows the bimn of embodiment 1 preparation3cr4o12Hysteresis curve, temperature be less than 50k when, embodiment 1 is made
Standby bimn3cr4o12Have that weak magnetic is stagnant, imply that the appearance of the weak ferromagnetism that antiferromagnetic order leads to.In temperature it is higher than
During 50k, the bimn of embodiment 1 preparation3cr4o12The intensity of magnetization and externally-applied magnetic field between show good linear dependence and close
System, with corresponding collinearly antiferromagnetic behavior (tn1With tn2Between) or paramagnetic state (tn1More than) it is identical.
Bimn proposed by the present invention3cr4o12It is a kind of novel magnetic power coupling multi-ferroic material, there is weak ferromagnetic ordering, relatively
Big dielectric constant and galvanic couple polarization intensity, have good application prospect in fields such as spin electric device, multiple-state storage devices.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for those skilled in the art
For, the present invention can have various change and change.All any modifications made within spirit and principles of the present invention, etc.
With replacing, improving etc., should be included within the scope of the present invention.
Claims (5)
1. a kind of magneto-electric coupled multi-ferroic material, its chemical formula is bimn3cr4o12.
2. a kind of method of the magneto-electric coupled multi-ferroic material prepared described in claim 1, comprising:
It is higher than 99.9% bi purity2o3、mn2o3And cr2o3It is fully ground after 1:3:4 mixing in molar ratio, screen；
Garbled raw material is loaded gold or platinum capsule and is compacted；
HTHP solid phase reaction.
3. the preparation method of magneto-electric coupled multi-ferroic material according to claim 2 is it is characterised in that described HTHP
The device of solid phase reaction is cubic hinge press or two grades of propulsion press of 6-8 type.
4. the preparation method of magneto-electric coupled multi-ferroic material according to claim 2 is it is characterised in that described HTHP
The pressure of solid phase reaction is 6-10gpa, temperature is 900-1300 DEG C, the high-temperature high-voltage reaction time is 10-60 minute.
5. magneto-electric coupled multi-ferroic material according to claim 2 preparation method it is characterised in that described gold or platinum
A diameter of 2-10mm of capsule, length is 2-10mm, and wall thickness is 1-2mm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06251649A (en) * | 1993-02-24 | 1994-09-09 | Chodendo Hatsuden Kanren Kiki Zairyo Gijutsu Kenkyu Kumiai | Manufacture of ceramic superconducting member |
| JP2005203613A (en) * | 2004-01-16 | 2005-07-28 | Ulvac Japan Ltd | Capacitor, and deposition method of capacitor film |
| CN101260565A (en) * | 2007-12-19 | 2008-09-10 | 清华大学 | Micron-stage sheet-like sodium bismuth titanate crystal and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06251649A (en) * | 1993-02-24 | 1994-09-09 | Chodendo Hatsuden Kanren Kiki Zairyo Gijutsu Kenkyu Kumiai | Manufacture of ceramic superconducting member |
| JP2005203613A (en) * | 2004-01-16 | 2005-07-28 | Ulvac Japan Ltd | Capacitor, and deposition method of capacitor film |
| CN101260565A (en) * | 2007-12-19 | 2008-09-10 | 清华大学 | Micron-stage sheet-like sodium bismuth titanate crystal and preparation method thereof |
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