CN101514475A - Method for preparing lead zirconate titanate-cobalt ferrite thick film - Google Patents
Method for preparing lead zirconate titanate-cobalt ferrite thick film Download PDFInfo
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- CN101514475A CN101514475A CNA2009100469441A CN200910046944A CN101514475A CN 101514475 A CN101514475 A CN 101514475A CN A2009100469441 A CNA2009100469441 A CN A2009100469441A CN 200910046944 A CN200910046944 A CN 200910046944A CN 101514475 A CN101514475 A CN 101514475A
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- cobalt ferrite
- lead zirconate
- zirconate titanate
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- 239000010941 cobalt Substances 0.000 title claims abstract description 47
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 47
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000001652 electrophoretic deposition Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims description 29
- 230000003068 static effect Effects 0.000 claims description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001962 electrophoresis Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000002612 dispersion medium Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000007669 thermal treatment Methods 0.000 claims description 3
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910000510 noble metal Inorganic materials 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 17
- 230000005291 magnetic effect Effects 0.000 abstract description 12
- 230000005684 electric field Effects 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000012776 electronic material Substances 0.000 abstract description 2
- 229910002518 CoFe2O4 Inorganic materials 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 47
- 229910003321 CoFe Inorganic materials 0.000 description 17
- 239000002131 composite material Substances 0.000 description 17
- 238000000151 deposition Methods 0.000 description 10
- 230000008021 deposition Effects 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 9
- 239000011858 nanopowder Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 239000003302 ferromagnetic material Substances 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 230000005690 magnetoelectric effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910002902 BiFeO3 Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000005303 antiferromagnetism Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000000224 chemical solution deposition Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000005323 ferromagnetic ordering Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention relates to the field of electronic material and device, and discloses a method for preparing a lead zirconate titanate-cobalt ferrite thick film. The method comprises the steps: Pb(Zr0.52Ti0.48) O3 powder and CoFe2O4 powder are dispersed into solvent to be made into suspending liquid with even concentration; then, the lead zirconate titanate-cobalt ferrite thick film is prepared by electrophoretic deposition under the condition of constant electric field. The lead zirconate titanate-cobalt ferrite thick film prepared by the method has good electrical property and magnetic property, can be applied for preparing a thick film sensor and a shifter, has the characteristics of simple equipment, low cost, quick film formation, easy adjustment of components and the like, and can be used for preparing film materials in a large scale.
Description
Technical field
The invention belongs to electronic material and devices field, be specifically related to a kind of preparation method of lead zirconate titanate-cobalt ferrite thick film.
Background technology
In recent years, magnetoelectric material is widely used in fields such as magnetic recording, wave filter, transmitter, multilayer chip inductor and quantum computer as the very important functional materials of a class.Magnetoelectric material can be divided into single-phase magnetoelectric material and compound magnetoelectric material.Magnetoelectric effect is antiferromagnetism Cr at low temperatures the earliest
2O
3Be observed in the monocrystalline, in other monocrystalline (as BiFeO3 etc.), also be observed subsequently.But the magnetic electricity performance of monophase materials is very weak, and can only could obviously be observed at low temperatures mostly, and this makes single-phase magnetoelectric material not obtain the application on the actual techniques.People's material of having turned to sight ferroelectric material of compound magnetoelectric material-will have and ferromagnetic material to be composited subsequently.This ferroelectric-ferromagnetic matrix material has ferroelectric phase simultaneously with mutually ferromagnetic, externally presents ferroelectricity and ferromegnetism simultaneously.Except the various performances with single-material, because the coupling between electropolarization and the magnetization, it many new performances such as magnetoelectric effect also can occur.In addition, research at present also finds to utilize the ferroelectric and ferromagnetic ordering coupled character of their intrinsic, not only can determine the magnetic properties of material, also wide application prospect and high researching value be arranged at the magnetic resonance device of making " ideal " gyrator, high-density storage, polymorphic mnemon, electric field controls, the piezoelectric transducer of magnetic field control and the aspects such as pressure Magnetic Sensor of electric field controls.
At present, magnetic electric compound material mainly contains three kinds of structures: particle is compound, and stratiform is compound and column is compound.Compound is ferroelectric, and ferromagnetic material mainly contains: BaTiO
3, Pb (Zr, Ti) O
3, CoFe
2O
4, NiFe
2O
4Deng.The ferroelectric-ferromagnetic film composite material is compared the advantage of many uniquenesses with compound bulk material: 1. ferroelectric phase can be regulated in small scope with being connected with ferromagnetic mutually compound, realizes the coupling of two-phase on nanoscale.2. the magneto-electric coupled coefficient of film heterojunction structure is higher.The preparation method of film composite material mainly comprises pulsed laser deposition, sol-gel method, radio frequency sputtering method, chemical solution deposition.
Thick-film material is compared with thin-film material, and it has lower surface stress, strong magnetic, electrical characteristic and resistance of aging.Therefore, preparation has certain thickness ferroelectric-ferromagnetic thick film material has become important research work at present.In the preparation technology of thick film, electrophoretic deposition is that people institute extensively adopts with advantages such as its film-forming apparatus are simple, the film forming area is big, device shape is unrestricted.Up to the present, it is fewer to adopt electrophoretic deposition method to prepare the report of ferroelectric-ferromagnetic composite thick film.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of lead zirconate titanate-cobalt ferrite thick film.
Know-why of the present invention:
Electrophoretic deposition method of the present invention is to utilize electrophoresis to move phenomenon, that is: colloidal particle or particle are done directed moving in dispersion medium under External Electrical Field, reaches the process that coagulation takes place behind the electrode base material and form the micelle structure of comparatively dense.
For achieving the above object, the present invention is achieved through the following technical solutions:
The preparation method of lead zirconate titanate-cobalt ferrite thick film specifically may further comprise the steps:
1) earlier with Pb (Zr
0.52Ti
0.48) O
3Powder, CoFe
2O
4Powder mixes and is scattered in makes suspension in the dispersion medium;
2) electrode is placed in the suspension, keeps two-plate parallel;
3) under permanent current field condition, electrophoretic deposition obtains thick film;
4) electrophoresis being finished afterwards, the gained thick film waits static pressure to handle;
5) will make ferroelectric-ferromagnetic thick film through the thick film thermal treatment under hot environment that waits static pressure to handle.
In the step 1), Pb (Zr
0.52Ti
0.48) O
3The ratio that powder accounts for the powder total mole number is 10%～90%, and described powder total mole number is Pb (Zr
0.52Ti
0.48) O
3Powder and CoFe
2O
4The mole number sum of powder.
In the step 1), the particle size range of described Pb-based lanthanumdoped zirconate titanates powder and cobalt ferrite nano-powder is 60-80nm.
In the step 1), described dispersion medium is: propyl carbinol or methyl ethyl diketone are preferably propyl carbinol.
Step 2) in, described electrode is the noble metal platinum gold electrode, perhaps is coated with the alumina substrate of high temperature resistant electrode.
Permanent current field condition in the step 3) is meant constant voltage or galvanostatic conditions.Preferably, continuous current/constant voltage remains on 1-10 μ A.
Processing such as static pressure such as grade in the step 4) is meant goods is placed in the airtight container that apply each to equal pressure to goods, under the highly compressed effect, goods are able to moulding and densification.Preferable, the pressure range that waits static pressure is 100-200MPa.
Heat treated temperature in the step 5) is 700 ℃～1100 ℃, and heat treatment time is 30-60min.
The thickness of the lead zirconate titanate-cobalt ferrite thick film in the step 5) is 5-10 μ m.
Lead zirconate titanate-cobalt ferrite thick film of the present invention, compare with the ferroelectric-ferromagnetic thick film of routine, the composite thick film that belongs to two kinds of powder co-production, have good electrical properties and magnetic property, can be applicable to prepare thick film sensor, shifter, it is simple to have equipment, cost is low, film forming is fast, component is easy to characteristics such as adjustment, but the mass preparation mould material.
Description of drawings
Fig. 1 is the lead zirconate titanate-cobalt ferrite thick film Pb (Zr of embodiment 1 composite deposition preparation
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 4: 1 o'clock X ray diffracting spectrum (XRD).
Fig. 2 is the lead zirconate titanate-cobalt ferrite thick film Pb (Zr of embodiment 1 composite deposition preparation
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 4: 1 o'clock the polarizability and the graph of a relation of extra electric field.
Fig. 3 is the lead zirconate titanate-cobalt ferrite thick film Pb (Zr of embodiment 1 composite deposition preparation
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 4: 1 o'clock the specific magnetising moment and the graph of a relation of externally-applied magnetic field.
Fig. 4 is the lead zirconate titanate-cobalt ferrite thick film Pb (Zr of embodiment 2 composite depositions preparation
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 1: 1 o'clock X ray diffracting spectrum (XRD).
Fig. 5 is the lead zirconate titanate-cobalt ferrite thick film Pb (Zr of embodiment 2 composite depositions preparation
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 1: 1 o'clock polarizability and the graph of a relation of extra electric field.
Embodiment
Embodiment 1: electrophoretic composite deposition lead zirconate titanate-cobalt ferrite thick film (Pb (Zr on silver-plated alumina substrate
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 4: 1):
A, the chemical feedstocks that is adopted are Pb-based lanthanumdoped zirconate titanates, cobalt ferrite nano-powder, solvent is a propyl carbinol, take by weighing earlier Pb-based lanthanumdoped zirconate titanates, cobalt ferrite nano-powder 0.25g, 0.05g respectively, then powder was stirred 10 minutes in the 60mL butanol solution, ultra-sonic dispersion formed the suspension (suspension concentration is 5g/L) that mixes in 20 minutes again.
B, employed constant current/constant voltage power supply is transferred to constant current state, and keep the constant output value of 5 μ A.
C, the platinum electrode that electrophoretic deposition is used are fixed in the electrophoresis chamber, and the two-plate spacing is 2cm, and it is parallel to remain two-plate in electrophoresis process.
D, two electrodes are connected power supply, keeps that acquisition has certain thickness thick film after 40 minutes.The time of electrophoretic deposition can be controlled according to needed thickness, and thick film thickness and electrophoretic deposition time are proportional approximately.
E, the composite thick film that electrophoretic deposition is obtained take out from electrophoresis solution, treat to wait static pressure 200MPa to handle 5 minutes after film dries in the shade naturally.
The thermal treatment 0.5 hour under 700 ℃ of environment of F, the thick film after will waiting static pressure to handle.Electric performance test adopts the d.c. sputtering method to make Au circular electrode (thickness is about 100nm) at upper surface.
The X-ray diffraction analysis collection of illustrative plates of the lead zirconate titanate-cobalt ferrite thick film that makes as shown in Figure 1, the X-ray diffraction analysis collection of illustrative plates shows that composite thick film presents PZT uhligite phase structure and CFO spinel phase structure, does not have the generation of intermediate product; Lead zirconate titanate-cobalt ferrite thick film (x) Pb (Zr of deposition preparation
0.52Ti
0.48) O
3-(1-x) CoFe
2O
4(x=0.80) polarizability and extra electric field, the graph of a relation of the specific magnetising moment and externally-applied magnetic field such as Fig. 2, shown in Figure 3.As can be seen from Figure 2, prepared lead zirconate titanate-cobalt ferrite composite thick film saturated polarization Ps under room temperature environment is 13.9 μ C/cm
2, remnant polarization Pr is 11.1 μ C/cm
2, coercivity electric field ec is 1038KV/cm.As can be seen from Figure 3 saturation magnetization Ms is 300emu/cm
3, residual magnetization Mr is 101emu/cm
3, coercive field Hc is 804Oe.By above-mentioned data as can be seen, the lead zirconate titanate-cobalt ferrite thick film of present embodiment preparation has excellent magnetism energy more.
The difference of itself and embodiment 1 is Pb (Zr in the lead zirconate titanate-cobalt ferrite thick film of electrophoretic composite deposition
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 1: 1, solvent is a methyl ethyl diketone, the preparation method is identical with embodiment 1, adjusts Pb-based lanthanumdoped zirconate titanates, cobalt ferrite nano-powder quality is respectively 0.17g, 0.13g.
Finally make Pb (Zr
0.52Ti
0.48) O
3-(1-x) CoFe
2O
4(x=0.50) lead zirconate titanate-cobalt ferrite thick film.Electric performance test adopts the d.c. sputtering method to make Au circular electrode (thickness is about 100nm) at upper surface.
The X-ray diffraction analysis collection of illustrative plates of the ferroelectric-magnetoelectricity thick film that makes as shown in Figure 4, the X-ray diffraction analysis collection of illustrative plates shows that thick film presents PZT uhligite phase structure and CFO spinel phase structure, does not have the generation of intermediate product; As can be seen from Figure 5, the lead zirconate titanate-cobalt ferrite composite thick film Pb (Zr of electrophoretic deposition preparation
0.52Ti
0.48) O
3-(1-x) CoFe
2O
4(x=0.50) saturated polarization Ps under room temperature environment is 1.4 μ C/cm
2, remnant polarization Pr is 0.7 μ C/cm
2, coercivity electric field ec is 496KV/cm.
The difference of itself and embodiment 1 is Pb (Zr in the lead zirconate titanate-cobalt ferrite thick film of electrophoretic composite deposition
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 1: 9, the preparation method is identical with embodiment 1, adjusts Pb-based lanthanumdoped zirconate titanates, cobalt ferrite nano-powder quality is respectively 0.04g, 0.26g.
Finally make Pb (Zr
0.52Ti
0.48) O
3-(1-x) CoFe
2O
4(x=0.10) lead zirconate titanate-cobalt ferrite thick film.
The difference of itself and embodiment 1 is Pb (Zr in the lead zirconate titanate-cobalt ferrite thick film of electrophoretic composite deposition
0.52Ti
0.48) O
3With CoFe
2O
4Mol ratio be 9: 1, the preparation method is identical with embodiment 1, adjusts Pb-based lanthanumdoped zirconate titanates, cobalt ferrite nano-powder quality is respectively 0.28g, 0.02g.
Finally make Pb (Zr
0.52Ti
0.48) O
3-(1-x) CoFe
2O
4(x=0.90) lead zirconate titanate-cobalt ferrite thick film.
Claims (10)
1, a kind of preparation method of lead zirconate titanate-cobalt ferrite thick film comprises the steps:
1) earlier PZT powder, cobalt ferrite powder are mixed and be scattered in and make suspension in the dispersion medium;
2) electrode is placed in the suspension, keeps two-plate parallel;
3) under permanent current field condition, electrophoretic deposition obtains thick film;
4) electrophoresis being finished afterwards, the gained thick film waits static pressure to handle;
5) will make lead zirconate titanate-cobalt ferrite thick film through the thick film thermal treatment under hot environment that waits static pressure to handle.
2, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1 is characterized in that, the ratio that PZT powder described in the step 1) accounts for the powder total mole number is 10%～90%.
3, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1 is characterized in that, the particle size range of PZT powder described in the step 1) and cobalt ferrite powder is 60-80nm.
4, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1 is characterized in that, dispersion medium described in the step 1) is propyl carbinol or methyl ethyl diketone.
5, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1 is characterized in that step 2) described in electrode be the noble metal platinum gold electrode, perhaps be coated with the alumina substrate of high temperature resistant electrode.
6, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1 is characterized in that, permanent current field condition is meant constant voltage or galvanostatic conditions described in the step 3).
7, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1, it is characterized in that, wait static pressure to handle described in the step 4) to be meant goods are placed in the airtight container, applying pressure range to goods is that each of 100-200Mpa is to equal pressure.
8, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1 is characterized in that, heat treated temperature described in the step 5) is 700 ℃～1100 ℃, and heat treatment time is 30-60 minute.
9, the preparation method of lead zirconate titanate-cobalt ferrite thick film as claimed in claim 1 is characterized in that, the thickness of lead zirconate titanate-cobalt ferrite thick film described in the step 5) is 5-10 μ m.
10, a kind of lead zirconate titanate-cobalt ferrite thick film is made by the described preparation method of arbitrary claim among the claim 1-9.
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|---|---|---|---|
| CNA2009100469441A CN101514475A (en) | 2009-03-03 | 2009-03-03 | Method for preparing lead zirconate titanate-cobalt ferrite thick film |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531595A (en) * | 2011-12-23 | 2012-07-04 | 常州大学 | Preparation method for 0-3 compound multiple-ferrite ceramic of cobalt ferrite and lead lanthanum zironate titanate |
| CN110923747A (en) * | 2019-12-09 | 2020-03-27 | 中国石油大学(华东) | Preparation method of bismuth ferrite photocatalytic film electrodeposition |
-
2009
- 2009-03-03 CN CNA2009100469441A patent/CN101514475A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531595A (en) * | 2011-12-23 | 2012-07-04 | 常州大学 | Preparation method for 0-3 compound multiple-ferrite ceramic of cobalt ferrite and lead lanthanum zironate titanate |
| CN110923747A (en) * | 2019-12-09 | 2020-03-27 | 中国石油大学(华东) | Preparation method of bismuth ferrite photocatalytic film electrodeposition |
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Application publication date: 20090826 |