CN1889209B - A ferroelectric/ferromagnetic two-phase composite film and producing method thereof - Google Patents
A ferroelectric/ferromagnetic two-phase composite film and producing method thereof Download PDFInfo
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- CN1889209B CN1889209B CN200610052569A CN200610052569A CN1889209B CN 1889209 B CN1889209 B CN 1889209B CN 200610052569 A CN200610052569 A CN 200610052569A CN 200610052569 A CN200610052569 A CN 200610052569A CN 1889209 B CN1889209 B CN 1889209B
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- 239000002131 composite material Substances 0.000 title claims description 43
- 230000005294 ferromagnetic effect Effects 0.000 title claims description 40
- 238000000034 method Methods 0.000 title abstract description 12
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 22
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940046892 lead acetate Drugs 0.000 claims abstract description 11
- 229940078494 nickel acetate Drugs 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims description 23
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims description 21
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000003618 dip coating Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000011065 in-situ storage Methods 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 230000005611 electricity Effects 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 abstract 1
- 229910003264 NiFe2O4 Inorganic materials 0.000 abstract 1
- 229910003781 PbTiO3 Inorganic materials 0.000 abstract 1
- WPJZFFADBPUEOC-UHFFFAOYSA-K butan-1-olate titanium(4+) trihydroxide Chemical compound CCCCO[Ti](O)(O)O WPJZFFADBPUEOC-UHFFFAOYSA-K 0.000 abstract 1
- 239000011365 complex material Substances 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 230000005389 magnetism Effects 0.000 abstract 1
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical group [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 61
- 239000000203 mixture Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 12
- 238000003980 solgel method Methods 0.000 description 9
- 239000010409 thin film Substances 0.000 description 9
- 239000012692 Fe precursor Substances 0.000 description 8
- 229910003271 Ni-Fe Inorganic materials 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 230000005291 magnetic effect Effects 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000005621 ferroelectricity Effects 0.000 description 2
- 239000003302 ferromagnetic material Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 230000005690 magnetoelectric effect Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of ferrum-electricity /ferrum-magnetism biphase complex film on the Si base plate. The ferrum-electricity phase is PbTiO3 and the ferrum-magnetism phase is NiFe2O4. Thepreparation method is as follow. Prepare the sol pioneer with the solute of lead acetate, titanic acid butyl ester, nickel acetate and ferric nitrate and the solvent of acetic acid and glycola methylether. Plate the film on the Si base plate with the method of dipping and pulling and heat treat at different temperatures. The process is simple and the cost is low. The ferrum-electricity /ferrum-magnetism complex material formed by sol-gel let two phases compound uniformly in the molecule level. It increases the contact area and magnetism electricity coefficient. The preparation technique of the ferrum-electricity /ferrum-magnetism film by sol-gel is compatible with the semiconductor molectron technic. The multifunctional circuit, component and system with large scale semiconductor molectron and ferrum-electricity /ferrum-magnetism complex film has great supplication prospect.
Description
Technical field
The present invention relates to the ferroelectric ferromagnetic composite film technical field, specially refer to a kind of sol-gel method in-situ preparing lead titanates-Ni ferrite laminated film and preparation method thereof.
Background technology
Along with mobile communication and fast development of computer technology, various electronic equipments become gradually Highgrade integration, miniaturization, multifunction and responseization fast.Because the Highgrade integration and the miniaturization of electronic equipment make that the electronic jamming of electric room is more and more serious, thereby need more anti-electromagnetic interference (EMI) filter to be distributed on the narrow and small day by day circuit board.So produced a contradiction, i.e. contradiction between the wilderness demand of the miniaturization of electronic equipment and integrated and electromagnetic interface filter.Because present passive filter is made up of discrete electric capacity and inductance element, really integrated presses for a kind of material and has electric capacity and inductance two specific characters simultaneously, and to have ferroelectricity and ferromagnetic material simultaneously in mutually be rarely found same, so ferroelectric/ferromagnetic composite material just arises at the historic moment.
Ferroelectric/ferromagnetic composite material is a kind of new material with magnetoelectricity translation function, by two kinds of monophase materialses--and ferroelectric phase is composited through certain method mutually with ferromagnetic.Because it has ferroelectric phase simultaneously with mutually ferromagnetic, so externally present ferroelectricity and ferromagnetism simultaneously, and because the coupling between electric polarization and the magnetization, make ferroelectric/ferromagnetic composite material under externally-applied magnetic field, cause crystal deformation, this deformation makes crystal electric polarization occur again, produce so-called magnetoelectric effect, magnetic-electric coefficient (dE/dH)=magnetostriction coefficient (dX/dH) * piezoelectric modulus (dE/dX).Utilize magnetoelectric effect, ferroelectric/ferromagnetic composite material can be used on the magnetoelastic transducer spare.Because ferroelectric material has the magnetic hysteresis loss of big electric hysteresis loss and ferromagnetic material, makes ferroelectric/ferromagnetic composite material have the loss characteristics of these two kinds of materials concurrently, thereby can develop anti-electromagnetic interference device.Moreover this composite material has electric capacity and inductance two specific characters simultaneously, can reduce the consumption of circuit board space by its filter of developing, thereby can replace present passive filter, realizes miniaturization.Because the peculiar property of ferroelectric/ferromagnetic composite material, all there is extensive and important purposes in fields such as its circuit measuring at microwave regime, ultra-high-tension power transmission line, broadband magnetic detection, magnetic sensors, thereby the research of ferroelectric/ferromagnetic composite material more and more causes attention both domestic and external.
The preparation of ferroelectric/ferromagnetic composite material all is to utilize traditional ceramic post sintering method or sol-gel method earlier usually, prepare ferroelectric phase respectively with mutually ferromagnetic, guaranteeing under the condition that two-phase does not react the complex sintered one-tenth block of two-phase or making ferroelectric phase and the ferromagnetic stratified material that alternates then, people had done a large amount of research to this in recent years, and had obtained the higher block of material of magnetic-electric coefficient and alternately arranged stratified material.Though this preparation method two-phase need be prepared separately and row control is compound, relatively simple and economical again.2003, people such as S.Mazumder are at Materials Research Bulletin (Mazumder S, BattacharyyaG S.Materials Research Bulletin, 38 (2) (2003), P303-310) publish an article on, successfully use oxide powder at 1000 ℃ of following pre-burning 3h, be pressed into sheet then and prepare PbTiO at 1200 ℃ of following sintering 3h in-situ methods
3-Co (Fe
xTi
yCo
z) O
4Composite ceramics, compare with traditional preparation method, ferroelectric/ferromagnetic composite material that original position forms can reach the mixing on the microcosmic more, thereby ferroelectric phase is contacted with ferromagnetic remaining mutually, can make magnetic-electric coefficient higher. but with this composite material of powder precursor in-situ preparing, two-phase can only reach the mixing of ceramic particle yardstick, and can not reach the contact of microcosmic more such as molecular scale. because the sol-gel method reaches the compound uniformity on molecular scale can guarantee preferably the time, by sol-gel method original position compound then be expected to preparation on small scale more evenly compound and on microcosmic, keep more accessible ferroelectric/ferromagnetic composite diphase material, be particularly suitable for preparing two-phase composite film simultaneously, only under the condition of minimum micron dimension, may reach mixing equably at thickness own, magnetic electricity performance is better brought into play. Chinese patent CN1778761 discloses with softening method and has successfully prepared ferroelectric-ferromagnetic two-phase composite granule, but along with the progress of film preparing technology and the developing of application, particularly the technology of preparing of ferroelectric-ferromagnetic film can be compatible mutually with the semiconductor integrated circuit technology, make the ferroelectric of developmental research collection semiconductor large scale integrated circuit and ferroelectric ferromagnetic composite film, ferromagnetic, magneto-electric coupled etc. all multi-functional in the multifunctional circuit of one, device and system, have more tempting prospect, thereby successfully exploitation directly utilize the compound preparation high-performance of sol-gel method original position ferroelectric/ferromagnetic composite diphase material, particularly thin-film material have prior meaning.
Summary of the invention
The object of the present invention is to provide a kind of sol-gel of utilization method original position form molecular scale ferroelectric uniformly/ferromagnetic two-phase composite film and preparation method thereof.
Of the present invention ferroelectric/ferromagnetic two-phase composite film is a generated in-situ ferroelectric phase and ferromagnetic two-phase composite film mutually on the Si substrate, ferroelectric phase wherein is PbTiO
3Phase, ferromagnetic is NiFe mutually
2O
4Phase.
Of the present invention ferroelectric/preparation method of ferromagnetic two-phase composite film, its step is as follows:
1) lead acetate dissolves in acetate, and controlled concentration is heated to dissolving at 60 ℃～100 ℃ in 2mol/L～5mol/L scope, obtain the solution first;
2) butyl titanate dissolves in EGME, and controlled concentration is stirred to and mixes in 1mol/L～5mol/L scope, obtains solution second;
3) nickel acetate dissolves in EGME, controls its concentration in 0.2mol/L～0.5mol/L scope, maintains the temperature at 60 ℃～100 ℃ and adds thermal agitation and make its whole dissolvings, obtains solution third;
4) ferric nitrate dissolves in EGME, controls its concentration in 0.2mol/L～0.5mol/L scope, maintains the temperature at 60 ℃～100 ℃ and adds thermal agitation and make its whole dissolvings, obtains the solution fourth;
5) above-mentioned first, second, third, four kinds of solution of fourth are mixed, be stirred to evenly, controlling wherein, Pb, Ti, four kinds of component concentrations of Ni, Fe are respectively: Pb:0.18mol/L～0.02mol/L, Ti:0.18mol/L～0.02mol/L, Ni:0.02mol/L～0.18mol/L, Fe:0.02mol/L～0.18mol/L obtains precursor colloidal sol;
6) colloidal sol that uses step 5) to prepare with dip-coating method coating on the Si substrate, then at 550 ℃～950 ℃ following heat treatment 0.5h～2h, obtains ferroelectric (PbTiO
3)/ferromagnetic (NiFe
2O
4) two-phase composite film.
The present invention compares the useful effect that has with background technology:
1, with sol-gel method original position form ferroelectric/ferromagnetic phase composite materials can so that ferroelectric phase with ferromagnetic evenly compound on molecular scale, thereby can form yardstick only at the two-phase composite film of micron dimension;
2, form ferroelectric/ferromagnetic composite film with sol-gel method original position, make ferroelectric phase with ferromagnetic mutually can be evenly compound on molecular scale, therefore can more keep in touch on the small scale, increase contact area greatly, make magnetic-electric coefficient higher;
3, the technology of preparing of sol-gel method original position ferroelectric-ferromagnetic film can be compatible mutually with the semiconductor integrated circuit technology, feasible exploitation integrates all multi-functional multifunctional circuits, device and the system such as ferroelectric, ferromagnetic, magneto-electric coupled of semiconductor large scale integrated circuit and ferroelectric ferromagnetic composite film, has the better application prospect.
4, sol-gel method original position ferroelectric/the ferromagnetic composite film preparing technique process is simple, with low cost, has good market prospects.
Description of drawings
Fig. 1 is a prepared complex phase film schematic diagram on the Si substrate, and (1) is the Si substrate among the figure, and (2) are PbTiO
3Phase, (3) are NiFe
2O
4Phase;
Fig. 2 be of the present invention ferroelectric/the XRD curve of ferromagnetic two-phase composite film, in the curve ◆, ▲ represent PbTiO respectively
3Phase and NiFe
2O
4The XRD peak position of phase;
Fig. 3 is the SEM photo of laminated film of the present invention.
Embodiment
Embodiment 1:
Lead acetate is dissolved in acetate, and butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, and its concentration is respectively: 5mol/L, 4mol/L, 0.1mol/L and 0.1mol/L.Four kinds of solution mix then, obtain Pb-Ti-Ni-Fe precursor colloidal sol, and the molar concentration of four kinds of components is respectively: 0.18mol/L, 0.18mol/L, 0.02mol/L and 0.04mol/L.With dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 750 ℃ of following heat treatment 1h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.The complex phase film that generates on the Si substrate is seen accompanying drawing 1.The composition of complex phase film is seen accompanying drawing 2 curves 1.As seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.
Embodiment 2:
Lead acetate is dissolved in acetate, and butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, and its concentration is respectively: 4mol/L, 5mol/L, 0.2mol/L and 0.2mol/L.Four kinds of solution mix then, obtain Pb-Ti-Ni-Fe precursor colloidal sol, and the molar concentration of four kinds of components is respectively: 0.18mol/L, 0.18mol/L, 0.02mol/L and 0.04mol/L.With dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 950 ℃ of following heat treatment 0.5h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.The composition of complex phase film is seen accompanying drawing 2 curves 2.As seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.
Embodiment 3:
Lead acetate is dissolved in acetate, and butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, and its concentration is respectively: 4mol/L, 4mol/L, 0.2mol/L and 0.2mol/L.Four kinds of solution mix then, obtain Pb-Ti-Ni-Fe precursor colloidal sol, and the molar concentration of four kinds of components is respectively: 0.14mol/L, 0.14mol/L, 0.06mol/L and 0.06mol/L.With dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 550 ℃ of following heat treatment 2h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.The composition of complex phase film is seen accompanying drawing 2 curves 3.As seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.
Embodiment 4:
Lead acetate is dissolved in acetate, and butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, and its concentration is respectively: 4mol/L, 3mol/L, 0.2mol/L and 0.2mol/L.Four kinds of solution mix then, obtain Pb-Ti-Ni-Fe precursor colloidal sol, and the molar concentration of four kinds of components is respectively: 0.14mol/L, 0.14mol/L, 0.06mol/L and 0.06mol/L.With dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 650 ℃ of following heat treatment 1.2h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.The composition of complex phase film is seen accompanying drawing 2 curves 4.As seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.
Embodiment 5:
Lead acetate is dissolved in acetate, butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, its concentration is respectively: 3mol/L, 3mol/L, 0.3mol/L and 0.3mol/L. four kinds of solution then mix, obtain Pb-Ti-Ni-Fe precursor colloidal sol, the molar concentration of four kinds of components is respectively: 0.1mol/L, 0.1mol/L, 0.1mol/L and 0.2mol/L. dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 600 ℃ of following heat treatment 1.5h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.The composition of complex phase film and morphology analysis are seen accompanying drawing 2 curves 5, and as seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.Its pattern is seen accompanying drawing 3 (a).
Embodiment 6:
Lead acetate is dissolved in acetate, and butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, and its concentration is respectively: 3mol/L, 3mol/L, 0.4mol/L and 0.4mol/L.Four kinds of solution mix then, obtain Pb-Ti-Ni-Fe precursor colloidal sol, and the molar concentration of four kinds of components is respectively: 0.1mol/L, 0.1mol/L, 0.1mol/L and 0.2mol/L.With dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 800 ℃ of following heat treatment 1.5h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.The composition of complex phase film and morphology analysis are seen accompanying drawing 2 curves 6, and as seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.Its pattern is seen accompanying drawing 3 (b).
Embodiment 7:
Lead acetate is dissolved in acetate, and butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, and its concentration is respectively: 3mol/L, 2mol/L, 0.4mol/L and 0.4mol/L.Four kinds of solution mix then, obtain Pb-Ti-Ni-Fe precursor colloidal sol, and the molar concentration of four kinds of components is respectively: 0.1mol/L, 0.1mol/L, 0.1mol/L and 0.2mol/L.With dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 850 ℃ of following heat treatment 1.5h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.The composition of complex phase film and morphology analysis are seen accompanying drawing 2 curves 7, and as seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.Its pattern is seen accompanying drawing 3 (c).
Embodiment 8:
Lead acetate is dissolved in acetate, and butyl titanate, nickel acetate and ferric nitrate are dissolved in EGME respectively, and its concentration is respectively: 2mol/L, 1mol/L, 0.5mol/L and 0.5mol/L.Four kinds of solution mix, and obtain Pb-Ti-Ni-Fe precursor colloidal sol, and the molar concentration of four kinds of components is respectively: 0.06mol/L, 0.06mol/L, 0.14mol/L and 0.28mol/L.With dip-coating method plated film on the Si substrate, the Si substrate level that plates film is placed in the air dries, obtain the thin film precursor body, it at 750 ℃ of following heat treatment 0.8h, is obtained PbTiO
3/ NiFe
2O
4Two-phase composite film.Accompanying drawing 2 curves 8 are seen in the constituent analysis of complex phase film.As seen from the figure, the film that generates under this example condition is PbTiO
3, NiFe
2O
4Two-phase.
Claims (2)
1. ferroelectric/ferromagnetic two-phase composite film is characterized in that generated in-situ ferroelectric phase and ferromagnetic two-phase composite film mutually on the Si substrate, and ferroelectric phase wherein is PbTiO
3Phase, ferromagnetic is NiFe mutually
2O
4Phase.
2. according to claim 1 ferroelectric/preparation method of ferromagnetic two-phase composite film, it is characterized in that step is as follows:
1) lead acetate dissolves in acetate, and controlled concentration is heated to dissolving at 60 ℃～100 ℃ in 2mol/L～5mol/L scope, obtain the solution first;
2) butyl titanate dissolves in EGME, and controlled concentration is stirred to and mixes in 1mol/L～5mol/L scope, obtains solution second;
3) nickel acetate dissolves in EGME, controls its concentration in 0.2mol/L～0.5mol/L scope, maintains the temperature at 60 ℃～100 ℃ and adds thermal agitation and make its whole dissolvings, obtains solution third;
4) ferric nitrate dissolves in EGME, controls its concentration in 0.2mol/L～0.5mol/L scope, maintains the temperature at 60 ℃～100 ℃ and adds thermal agitation and make its whole dissolvings, obtains the solution fourth;
5) above-mentioned first, second, third, four kinds of solution of fourth are mixed, be stirred to evenly, controlling wherein, Pb, Ti, four kinds of component concentrations of Ni, Fe are respectively: Pb:0.18mol/L～0.02mol/L, Ti:0.18mol/L～0.02mol/L, Ni:0.02mol/L～0.18mol/L, Fe:0.02mol/L～0.18mol/L obtains precursor colloidal sol;
6) colloidal sol that uses step 5) to prepare with dip-coating method coating on the Si substrate, then at 550 ℃～950 ℃ following heat treatment 0.5h～2h, obtains ferroelectric/ferromagnetic two-phase composite film.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101090024B (en) * | 2007-04-29 | 2010-12-15 | 湘潭大学 | La rear earth ion doped-bismuth titanate spinel ferrite ferroelectric ferromagnetic composite film preparation method |
| CN101538711B (en) * | 2009-03-20 | 2010-12-08 | 同济大学 | Method for preparing ferroelectricicity-ferromagnetic composite thick film by combination of electrophoretic deposition and sol-gel |
| CN102879289A (en) * | 2012-09-26 | 2013-01-16 | 中国人民解放军装甲兵工程学院 | Preparation method of PbTiO3 intelligent coating and PbTiO3 intelligent coating |
| CN109037435B (en) * | 2018-08-29 | 2021-11-05 | 郑州轻工业学院 | Preparation method of magnetoelectric nanocomposite based on biological-assisted self-assembly |
| CN110228822A (en) * | 2019-05-17 | 2019-09-13 | 华中科技大学 | A kind of Ferromagnetic/Antiferromagnetic hetero-junctions and its preparation with exchange bias effect |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580322A (en) * | 2004-05-15 | 2005-02-16 | 华中科技大学 | Method for preparing strontium-barium titanate ferroelectric film |
| CN1262514C (en) * | 2004-08-19 | 2006-07-05 | 南京大学 | Magnetoelectric composite film and its preparation method |
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|---|---|---|---|---|
| CN1580322A (en) * | 2004-05-15 | 2005-02-16 | 华中科技大学 | Method for preparing strontium-barium titanate ferroelectric film |
| CN1262514C (en) * | 2004-08-19 | 2006-07-05 | 南京大学 | Magnetoelectric composite film and its preparation method |
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| Title |
|---|
| JP平11-286774A 1999.10.19 |
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