CN103121836B - Method for preparing BiFe1-xCrxO3 ferroelectric film by using sol-gel method - Google Patents
Method for preparing BiFe1-xCrxO3 ferroelectric film by using sol-gel method Download PDFInfo
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- CN103121836B CN103121836B CN201210498900.4A CN201210498900A CN103121836B CN 103121836 B CN103121836 B CN 103121836B CN 201210498900 A CN201210498900 A CN 201210498900A CN 103121836 B CN103121836 B CN 103121836B
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- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000003980 solgel method Methods 0.000 title claims abstract description 10
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000004528 spin coating Methods 0.000 claims abstract description 16
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 8
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 230000010287 polarization Effects 0.000 claims description 14
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 230000005684 electric field Effects 0.000 claims description 6
- 230000005291 magnetic effect Effects 0.000 claims description 6
- 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 abstract 2
- 229910002902 BiFeO3 Inorganic materials 0.000 abstract 1
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 abstract 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract 1
- 229910001887 tin oxide Inorganic materials 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000005621 ferroelectricity Effects 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 230000005303 antiferromagnetism Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Inorganic Insulating Materials (AREA)
- Semiconductor Memories (AREA)
Abstract
The invention provides a method for preparing a BiFe1-xCrxO3 ferroelectric film by using a sol-gel method. The method comprises the following steps of: dissolving bismuth nitrate, ferric nitrate and chromic nitrate according to a molar ratio of 1.05: (1-x): x into a mixed solution containing ethylene glycol monomethyl ether, acetic oxide and cholamine, and magnetically stirring to obtain a stable BiFe1-xCrxO3 precursor with the metal ion concentration of 0.003-0.3mol/L, wherein x is equal to 0.00-0.03, and the volume ratio of the ethylene glycol monomethyl ether to the acetic oxide to the cholamine is 14: 5: 1. A film is prepared by spin-coating the BiFe1-xCrxO3 precursor on an FTO (Fluorine-doped Tin Oxide)/glass substrate by using a spin-coating method, and a crystalline BiFe1-xCrxO3 film is obtained by adopting a layer-by-layer annealing process. The method disclosed by the invention has simple requirements on equipment, and experimental conditions are easy to achieve; the prepared film is better in uniformity, and the doping amount is easy to control; and the ferroelectric property of the BiFeO3 film is improved through B-bit Cr doping.
Description
Technical field
The invention belongs to field of functional materials, relate to and prepare BiFe at the FTO/glass substrate surface of functionalization
1-xcr
xo
3the method of film.
Background technology
BiFeO
3there is ferroelectricity and antiferromagnetism, and with weak ferromegnetism, this causes people greatly and studies interest.BiFeO
3have the perovskite structure of distortion, have ferroelectric order (TC=810 DEG C) and G type antiferromagnetic order (TN=380 DEG C) under room temperature, be one of a few single phase multi-iron material simultaneously.BiFeO
3have a wide range of applications in information storage, information storage, image display etc.But, pure phase BiFeO
3there is the problem of large leakage conductance, cause him cannot obtain saturated ferroelectric hysteresis loop and higher residual polarization, thus limit its practical application greatly.
Summary of the invention
A kind of sol-gel method is the object of the present invention is to provide to prepare BiFe
1-xcr
xo
3the method of film, this kind of method can prepare a kind of BiFe
0.98cr
0.02o
3film, to solve large leakage conductance and the low problem of residual polarization.
To achieve these goals, the present invention adopts following technical scheme:
A kind of sol-gel method prepares BiFe
1-xcr
xo
3the method of ferroelectric membranc, comprises the following steps:
Step 1: by Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2o and Cr (NO
3)
39H
2o 1.05: 1-x: x is dissolved in the mixed solution of ethylene glycol monomethyl ether, acetic anhydride and thanomin in molar ratio, obtains the stable BiFe that concentration of metal ions is 0.003 ~ 0.3mol/L after magnetic agitation
1-xcr
xo
3precursor liquid, wherein x=0.00 ~ 0.03, the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 2: adopt spin-coating method spin coating BiFe on FTO/glass substrate
1-xcr
xo
3precursor liquid prepares film, adopts annealing process process layer by layer, obtains crystalline state BiFe
1-xcr
xo
3film.
The present invention further improves and is, x=0.01, x=0.02 or x=0.03 in step 1.
The present invention further improves and is, in step 1, churning time is 3h.
The present invention further improves and is, repeats spin coating and prepare film in step 2, and annealing process process is layer by layer until obtain the film of desired thickness.
The present invention further improves and is, 0 < x≤0.03.
The present invention further improves and is, 0 < x≤0.02.
The present invention further improves and is, 0 < x≤0.01.
The present invention further improves and is, 0.01≤x≤0.03.
The present invention further improves and is, 0.02≤x≤0.03.
The present invention further improves and is, 0.01≤x≤0.02.
Relative to prior art, the present invention has the following advantages:
1. the inventive method selects Cr to carry out the doping of B position, Cr
3+radius is less than Fe
3+, after doping, admittedly be melting into into lattice, can make the approximate bismuth ferrite crystal lattices distortion in perovskite structure originally, structural aberration aggravates, and in film, the rollover number of electricdomain increases, thus improves the ferroelectricity of film.
2. at present for the preparation of BiFeO
3the method of film has a lot, as chemical Vapor deposition process (CVD), magnetron sputtering method (rf magnetron sputtering), deposition of metal organic method (MOD), metal-organic chemical vapor deposition equipment method (MOCVD), liquid phase deposition (LPD), molecular beam epitaxy (MBE), pulsed laser deposition (PLD), sol-gel method (Sol-Gel) etc.Compare additive method, Sol-Gel method due to equipment simple, reaction is easily carried out, temperature of reaction is lower, easy to operate, be suitable for preparing film on large surface and surface in irregular shape, easily realize the Uniform Doped on molecular level, and the advantage such as chemical composition controllable precise and be widely used for preparing ferroelectric material.
3. in the present invention, adopt sol-gel method to prepare BiFeO
3film, is adulterated by B position Cr, and FTO substrate is prepared the BiFe that a kind of Cr adulterates
0.98cr
0.02o
3film, it is in 1kHz frequency, and the saturated polarization recorded under the test electric field of 1181.8kV/cm is 61.05 μ C/cm
2, remnant polarization is 39.50 μ C/cm
2, coercive field is 502.73kV/cm.
4. present device requires simple, and experiment condition easily reaches, and the uniformity of film of preparation is better, and doping can accurately control, and improves the ferroelectric properties of film by Cr doping.
Accompanying drawing explanation
Fig. 1 is BiFe prepared by the present invention
0.98cr
0.02o
3the XRD figure of film;
Fig. 2 is BiFe prepared by the present invention
0.98cr
0.02o
3the SEM figure of film;
Fig. 3 is BiFe prepared by the present invention
0.98cr
0.02o
3the ferroelectric hysteresis loop figure of film.
Embodiment
Embodiment 1
Step 1: by Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2o and Cr (NO
3)
39H
2o is dissolved in the mixed solution of ethylene glycol monomethyl ether, acetic anhydride and thanomin in molar ratio at 1.05: 1.00: 0.00, and obtaining concentration of metal ions after magnetic agitation 3h is stable BiFeO O.003mol/L
3precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 2: adopt spin-coating method spin coating BiFeO on FTO/glass substrate
3precursor liquid prepares film, adopts annealing process process layer by layer, obtains crystalline state BiFeO
3film.
Step 3: at crystalline state BiFeO
30.502mm is prepared in film surface ion sputtering
2au electrode, then 300 DEG C insulation 20min carry out electrode anneal process.
Adopt XRD determining BiFeO
3the thing phase composite structure of film, measures BiFeO with FE-SEM
3the microscopic appearance of film, with the ferroelectric test system and test BiFeO of TF2000
3the ferroelectric properties of film.In 1kHz frequency, the saturated polarization recorded under the test electric field of 454.5kV/cm is 4.73 μ C/cm
2, remnant polarization is 0.86 μ C/cm
2, coercive field is 77.71kV/cm.
Embodiment 2
Step 1: by Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2o and Cr (NO
3)
39H
2o is dissolved in the mixed solution of ethylene glycol monomethyl ether, acetic anhydride and thanomin in molar ratio at 1.05: 0.99: 0.01, obtains the stable BiFe that concentration of metal ions is 0.3mol/L after magnetic agitation 3h
0.99cr
0.01o
3precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 2: adopt spin-coating method spin coating BiFe on FTO/glass substrate
0.99cr
0.01o
3precursor liquid prepares film, adopts annealing process process layer by layer, obtains the BiFe of crystalline state Cr doping
0.99cr
0.01o
3film.
Step 3: at crystalline state BiFe
0.99cr
0.01o
30.502mm is prepared in film surface ion sputtering
2au electrode, then 300 DEG C insulation 20min carry out electrode anneal process.
Adopt XRD determining BiFe
0.99cr
0.01o
3the thing phase composite structure of film, measures BiFe with FE-SEM
0.99cr
0.01o
3the microscopic appearance of film.With the ferroelectric test system and test BiFe of TF2000
0.99cr
0.01o
3the ferroelectric properties of film, in 1kHz frequency, the saturated polarization recorded under the test electric field of 454.5kV/cm is 7.92 μ C/cm
2, remnant polarization is 5.59 μ C/cm
2, coercive field is 519.60kV/cm.
Embodiment 3
Step 1: by Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2o and Cr (NO
3)
39H
2o is dissolved in the mixed solution of ethylene glycol monomethyl ether, acetic anhydride and thanomin in molar ratio at 1.05: 0.98: 0.02, obtains the stable BiFe that concentration of metal ions is 0.1mol/L after magnetic agitation 3h
0.98cr
0.02o
3precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 2: adopt spin-coating method spin coating BiFe on FTO/glass substrate
0.98cr
0.02o
3precursor liquid prepares film, adopts annealing process process layer by layer, obtains the BiFe of crystalline state Cr doping
0.98cr
0.02o
3film.
Step 3: at crystalline state BiFe
0.98cr
0.02o
30.502mm is prepared in film surface ion sputtering
2au electrode, then 300 DEG C insulation 20min carry out electrode anneal process.
Shown in Figure 1, adopt XRD determining BiFe
0.98cr
0.02o
3the thing phase composite structure of film, shown in Figure 2, measure BiFe with FE-SEM
0.98cr
0.02o
3the microscopic appearance of film.Shown in Figure 3, with the ferroelectric test system and test BiFe of TF2000
0.98cr
0.02o
3the ferroelectric properties of film, in 1kHz frequency, the saturated polarization recorded under the test electric field of 1181.8kV/cm is 61.05 μ C/cm
2, remnant polarization is 39.50 μ C/cm
2, coercive field is 502.73kV/cm.
Embodiment 4
Step 1: by Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2o and Cr (NO
3)
39H
2o is dissolved in the mixed solution of ethylene glycol monomethyl ether, acetic anhydride and thanomin in molar ratio at 1.05: 0.97: 0.03, obtains the stable BiFe that concentration of metal ions is 0.2mol/L after magnetic agitation 3h
0.97cr
0.03o
3precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 2: adopt spin-coating method spin coating BiFe on FTO/glass substrate
0.97cr
0.03o
3precursor liquid prepares film, adopts annealing process process layer by layer, obtains the BiFe of crystalline state Cr doping
0.97cr
0.03o
3film.
Step 3: at crystalline state BiFe
0.97cr
0.03o
30.502mm is prepared in film surface ion sputtering
2au electrode, then 300 DEG C insulation 20min carry out electrode anneal process.
Adopt XRD determining BiFe
0.97cr
0.03o
3the thing phase composite structure of film, measures BiFe with FE-SEM
0.97cr
0.03o
3the microscopic appearance of film, with the ferroelectric test system and test BiFe of TF2000
0.97cr
0.03o
3the ferroelectric properties of film.In 1kHz frequency, the saturated polarization recorded under the test electric field of 1181.8kV/cm is 50.79 μ C/cm
2, remnant polarization is 33.06 μ C/cm
2, coercive field is 519.60kV/cm.
Above said content is in conjunction with concrete preferred implementation further description made for the present invention, it not whole or unique embodiment, the conversion of those of ordinary skill in the art by reading specification sheets of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.
Claims (1)
1. a sol-gel method prepares BiFe
1-xcr
xo
3the method of ferroelectric membranc, is characterized in that, comprises the following steps:
Step 1: by Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2o and Cr (NO
3)
39H
2o in molar ratio 1.05:1-x:x is dissolved in the mixed solution of ethylene glycol monomethyl ether, acetic anhydride and thanomin, obtains the stable BiFe that concentration of metal ions is 0.003 ~ 0.3mol/L after magnetic agitation
1-xcr
xo
3precursor liquid, wherein x=0.02, the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14:5:1;
Step 2: adopt spin-coating method spin coating BiFe on FTO/glass substrate
1-xcr
xo
3precursor liquid prepares film, adopts annealing process process layer by layer, obtains crystalline state BiFe
1-xcr
xo
3film; Gained crystalline state BiFe
1-xcr
xo
3film is in 1kHz frequency, and the saturated polarization recorded under the test electric field of 1181.8kV/cm is 61.05 μ C/cm
2, remnant polarization is 39.50 μ C/cm
2, coercive field is 502.73kV/cm;
In step 1, churning time is 3h;
Repeat spin coating in step 2 and prepare film, annealing process process is layer by layer until obtain the film of desired thickness.
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|---|---|---|---|
| CN201210498900.4A CN103121836B (en) | 2012-11-28 | 2012-11-28 | Method for preparing BiFe1-xCrxO3 ferroelectric film by using sol-gel method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210498900.4A CN103121836B (en) | 2012-11-28 | 2012-11-28 | Method for preparing BiFe1-xCrxO3 ferroelectric film by using sol-gel method |
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| Publication Number | Publication Date |
|---|---|
| CN103121836A CN103121836A (en) | 2013-05-29 |
| CN103121836B true CN103121836B (en) | 2015-01-28 |
Family
ID=48453024
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| CN103613372B (en) * | 2013-11-04 | 2015-07-29 | 陕西科技大学 | A kind of low-leakage current BiFeO of Tb, Mn and Cu ternary codoped 3film and preparation method thereof |
| CN103601249B (en) * | 2013-11-04 | 2015-07-29 | 陕西科技大学 | A kind of high remnant polarization and high-k BiFe 0.96-ymn 0.04cr yo 3ferroelectric membranc and preparation method thereof |
| CN103708562B (en) * | 2013-12-20 | 2015-06-24 | 陕西科技大学 | Bi0.90Ho0.10Fe1-XMnXO3 ferroelectric film with high remanent polarization and preparation method thereof |
| CN107342229B (en) * | 2017-07-20 | 2019-12-10 | 广东工业大学 | Amorphous thin film device and manufacturing method thereof |
| CN109809493B (en) * | 2017-11-22 | 2020-08-04 | 清华大学 | Bismuth ferrite room-temperature multiferromagnetic coupling material, preparation method and electronic device |
| CN110501583B (en) * | 2019-04-29 | 2021-09-28 | 南京大学 | Method for calculating crystal lattice orientation and domain turnover angle of polycrystalline ferroelectric material domain |
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Effective date of registration: 20201218 Address after: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd. Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY Effective date of registration: 20201218 Address after: 224000 Qingyang Road (within Qingdun Office), Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (8) Patentee after: Yancheng Qinglong Jinbang water Co.,Ltd. Address before: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd. |
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| CI03 | Correction of invention patent | ||
| CI03 | Correction of invention patent |
Correction item: Patentee|Address Correct: Yancheng Qingdun Jinbang Water Affairs Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8) False: Yancheng Qingyi Jinbang Water Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8) Number: 01-01 Volume: 37 |