CN105206710B - The preparation method of the ferroelectric thin film with texture - Google Patents
The preparation method of the ferroelectric thin film with texture Download PDFInfo
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- CN105206710B CN105206710B CN201510689332.XA CN201510689332A CN105206710B CN 105206710 B CN105206710 B CN 105206710B CN 201510689332 A CN201510689332 A CN 201510689332A CN 105206710 B CN105206710 B CN 105206710B
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- 239000010409 thin film Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 22
- 239000006249 magnetic particle Substances 0.000 claims description 17
- 238000004549 pulsed laser deposition Methods 0.000 claims description 7
- 238000000224 chemical solution deposition Methods 0.000 claims description 6
- 238000003980 solgel method Methods 0.000 claims description 6
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 238000001451 molecular beam epitaxy Methods 0.000 claims description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 241000209094 Oryza Species 0.000 claims 2
- 239000010408 film Substances 0.000 abstract description 29
- 230000000694 effects Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 description 9
- 238000000151 deposition Methods 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- 229910002902 BiFeO3 Inorganic materials 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000011553 magnetic fluid Substances 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- 229910002518 CoFe2O4 Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000013087 polymer photovoltaic Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- H01L31/18—
-
- H01L31/02363—
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- H01L31/032—
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention discloses a kind of preparation method of the ferroelectric thin film with texture, which it is critical only that and prepares magnetic nano chain first on film-forming carrier, then ferroelectric thin film is grown on the magnetic nano chain again, using the invention has the beneficial effects as follows by changing the size in magnetic field, direction, gradient magnitude with regard to the length of controllable nano-magnetic chain, thickness and orientation so as to reach the texture and purity of control ferrite film, preparation method is simple, and effect is good.
Description
Technical field
The invention belongs to technical field of semiconductor, and in particular to a kind of preparation side of the ferroelectric thin film with texture
Method.
Background technology
Energy crisis is the great difficult problem that our times various countries face, develop regenerative resource be alleviate the problem it is effective
Approach, in numerous regenerative resources, solar energy because its have the advantages that aboundresources, it is widely distributed, clean it is clean enjoy
Favor, photovoltaic generation are a kind of principal modes for developing solar energy, and its principle is to make photovoltaic cell using photovoltaic effect,
The luminous energy of the sun is converted into into electric energy, photovoltaic cell is broadly divided into silicon, CIS, GaAs, cadmium telluride and polymer photovoltaic
Battery etc., existing industrial thin-film solar cells have that conversion efficiency is low, stability is poor, production cost is higher etc. and lack
Point, wants change disadvantage mentioned above, can pass through to improve the preparation technology and technical parameter of film, or improve utilizing for light and imitate
Rate, the problems such as first method faces R＆D cycle length, high cost, technical difficulty, therefore improves the utilization ratio of light and just seems
It is very necessary, want to improve the utilization rate of sunshine, by improving absorptivity of the film to sunshine, and film can be increased
Thickness can accomplish this point, but film is thicker, will certainly reduce the stability of solar cell, while can also increase photoproduction load
Stream recombination rate, reduce conversion efficiency, and prepare mass, possess specific texture, relatively low defect, higher purity
The film of (high principal phase ratio) is the effective means for solving this difficult problem, the film with texture can strengthen the absorption of light and not
As for the compound of photo-generated carrier is affected, so as to play a part of to improve photoelectric transformation efficiency, therefore how to prepare with spy
Determine texture, highly purified solar battery thin film and just seem very necessary.
Prepare at present the method for film mainly include sol-gel process (Sol-Gel), chemical solution deposition (CSD),
Chemical gaseous phase depositing process (CVD), pulse laser sediment method (PLD), molecular beam epitaxy (MBE) and magnetically controlled sputter method
(Magnetron Sputtering), no matter which kind of method, is all first to prepare film, then film is sintered or anneals
Process, but these methods are all difficult to obtain the film with specific texture.
The content of the invention
To solve above technical problem, the invention discloses a kind of preparation method of the ferroelectric thin film with specific texture.
Technical scheme is as follows：
A kind of preparation method of the ferroelectric thin film with texture, which it is critical only that
Rice chain, then ferroelectric thin film is grown on the magnetic nano chain, thus prepared ferroelectric thin film has specific texture.
Further, above-mentioned magnetic nano chain is prepared according to following steps：
Step one, prepare magnetic particle；
Step 2, the magnetic particle is dispersed in base fluid forms magnetic liquid；
Step 3, the magnetic liquid is injected into the film-forming carrier, magnetic field is applied to the magnetic liquid, then to liquid
Body carries out heated baking, and drying obtains the magnetic nano chain.
Above-mentioned magnetic particle is nano-scale magnetic particulate.
Above-mentioned magnetic particle is ferrite.
Above-mentioned film-forming carrier is provided with liquid cell, and the magnetic liquid is injected in the liquid cell.
Ferroelectric thin film is grown on the magnetic nano chain and adopts sol-gel process, chemical solution deposition, chemical gaseous phase
Any one in the methods such as sedimentation, pulsed laser deposition, molecular beam epitaxy, magnetron sputtering method.
Beneficial effect：
Using the invention has the beneficial effects as follows, can just regulate and control nanometer by changing the size in magnetic field, direction, gradient magnitude
The length of magnetic chain, thickness and orientation, then on the basis of nano-magnetic chain prepare ferroelectric thin film, just can obtain with texture
Ferroelectric thin film, the ferroelectric thin film prepared with the method has certain texture, purity high, and preparation method is simple, and effect is good.
Description of the drawings
I-V curve figures of the Fig. 1 for control group I；
I-V curve figures of the Fig. 2 for test group I；
I-V curve figures of the Fig. 3 for control group II；
I-V curve figures of the Fig. 4 for test group II；
I-V curve figures of the Fig. 5 for control group III；
I-V curve figures of the Fig. 6 for test group III.
Specific embodiment
With reference to embodiment, the invention will be further described.
A kind of preparation method of the ferroelectric thin film with texture, arranges liquid cell first on film-forming carrier, then prepares
Nano magnetic particle, the nano magnetic particle of the preparation is dispersed in base fluid and forms nano-magnetic fluid, will be obtained
The nano-magnetic fluid inject in the liquid cell, magnetic field is applied to the liquid cell, heating baking is carried out to liquid then
Roasting, drying obtains magnetic nano chain, then on the magnetic nano chain grows ferroelectric thin film.
Above-mentioned nano magnetic particle be ferrite, on the magnetic nano chain grow ferroelectric thin film method be colloidal sol-
Gel method, chemical solution deposition, chemical vapour deposition technique, pulsed laser deposition, molecular beam epitaxy or magnetron sputtering method
In any one.
With reference to test example and accompanying drawing, the invention will be further described.
The nano magnetic particle is with CoFe2O4(it is abbreviated as：CFO as a example by).
First, by 100ml concentration for 0.04mol/L FeCl3·6H2O and 100ml concentration is 0.02mol/L Co
(NO3)2·6H2Add 500ml concentration for the NaOH of 0.35mol/L after O mixing, mixed liquor is heated to into boiling then, while soon
Speed is stirred, and removes natural sedimentation, the H (NO) of 1mol/L is used after fully precipitating after keeping boiling 1min3Cleaning sediment is until heavy
Starch pH value is 7, the CFO nano magnetic particles required for then obtain cleaning products therefrom Jing after the operation such as dehydration, dry.
According to demand, the CFO nano magnetic particles of certain mass are uniformly dispersed in certain density silicone oil, to match somebody with somebody
It is 5% to put volume fraction, and as a example by cumulative volume is for the CFO magnetic liquids of 100ml, required CFO nano magnetic particles volume is 5ml,
Its density is about 6g/cm3, then the quality for needing CFO nano magnetic particles is 30g, and the concentration of oleic acid is 2%, then need to measure
The oleic acid of 2ml, then the volume of silicone oil is 93ml, the 30g CFO nano magnetic particles for weighing is added in the oleic acid of 2ml, is carried out
Shake, is then uniformly dispersed in 93ml silicone oil, puts in the vial or other containers of good seal, shakes on shaking table
Surpass 1 hour in about 1 hour or ultrasonic wave, obtain CFO nano-magnetic solution.
Electrode base sheet will be prepared as film-forming carrier, electrode base sheet surrounding and top pass through AB glue or 502 glue
(or the film that other materials are done, this film decomposition temperature should be less than ferroelectric material, with 500 degrees Celsius to be pasted with plastic tab
Below it is preferred), electrode base sheet and plastic tab form the liquid cell, and CFO nano-magnetic solution is injected into the liquid cell
In, the magnetic field of 500Gs is applied along the direction parallel to substrate to the liquid cell, makes CFO nano magnetic particles exist along magnetic direction
CFO nano-magnetic chains are formed on substrate, is maintained magnetic field constant by the square heated baking containing CFO nano-magnetic chains, is dried
After remove magnetic field, be put into 500 DEG C or 800 DEG C of high-temperature calcinations, make other in square in addition to substrate and CFO nano-magnetic chains
Material is decomposed, and finally obtains the CFO nano-magnetic chains with texture.
Finally, with sol-gel process, chemical solution deposition, chemical vapour deposition technique, pulsed laser deposition, molecule
Any one in the methods such as beam epitaxy methods, magnetron sputtering method prepares ferroelectric thin on the CFO nano-magnetic chains with texture
Film.
Following experimental group is set：
Control group I：On the substrate for preparing bottom electrode, BiFeO is prepared with traditional pulse laser deposition3Film, it is right
The BiFeO3Film is carried out after vacuum annealing again in the BiFeO3Film preparation Top electrode.
Test group I：On the substrate for preparing bottom electrode, the CFO nano-magnetics with texture are prepared according to said method
Chain, prepares BiFeO with pulsed laser deposition on CFO nano-magnetic chains3Film, then in the BiFeO3Electricity in film preparation
Pole.
Control group II：On the substrate for preparing bottom electrode, BaTiO is prepared with traditional pulse laser deposition3Film, it is right
The BaTiO3Film is carried out after vacuum annealing again in the BaTiO3Film preparation Top electrode.
Test II：On the substrate for preparing bottom electrode, the CFO nano-magnetics with texture are prepared according to said method
Chain, prepares BaTiO with pulsed laser deposition on CFO nano-magnetic chains3Film, then in the BaTiO3Electricity in film preparation
Pole.
Control group III：On the substrate for preparing bottom electrode, pzt thin film is prepared with traditional pulse laser deposition, to institute
State after pzt thin film carries out vacuum annealing Top electrode is prepared in the pzt thin film again.
Test III：On the substrate for preparing bottom electrode, the CFO nano-magnetics with texture are prepared according to said method
Chain, prepares pzt thin film on CFO nano-magnetic chains with pulsed laser deposition, then prepares Top electrode in the pzt thin film.
Two gauge outfits of 2400 digital sourcemeters of Keithley (Keithley) are connected on into ferroelectric thin film obtained in above each group
On upper and lower electrode, laser is opened, laser is that wavelength is the green glow of 532nm, is irradiated on film surface along Top electrode direction,
Tested.
The survey of the ferroelectric thin film that control group I, test group I, control group II, test group II, control group III, test group III are obtained
Test result is respectively as shown in figures 1 to 6.
As depicted in figs. 1 and 2, it can be seen that compare with control group I, BiFeO obtained in test group I3The photoelectric current of film
With photoconductive effect all compared with BiFeO obtained in conventional method3Film is big.
As shown in Figure 3 and Figure 4, it can be seen that compare with control group II, BaTiO obtained in test group II3The photoelectricity of film
Stream and photoconductive effect are all compared with BaTiO obtained in conventional method3Film is big.
As shown in Figure 5 and Figure 6, it can be seen that compare with control group III, the photoelectric current of pzt thin film obtained in test group III and
Photoconductive effect is all big compared with pzt thin film obtained in conventional method.
In sum, after first magnetic nano chain being prepared on film-forming carrier grow ferroelectric thin film again on the magnetic nano chain
Method can significantly improve the photoelectric property of ferroelectric thin film.
Claims (4)
1. a kind of preparation method of the ferroelectric thin film with texture, it is characterised in that：Magnetic is prepared first on film-forming carrier to receive
Rice chain, then ferroelectric thin film is grown on the magnetic nano chain；
The magnetic nano chain is prepared according to following steps：
Step one, prepare magnetic particle；
Step 2, the magnetic particle is dispersed in base fluid forms magnetic liquid；
Step 3, the magnetic liquid is injected into the film-forming carrier, magnetic field is applied to the magnetic liquid, then liquid is entered
Row heated baking, drying obtain the magnetic nano chain；
The film-forming carrier is provided with liquid cell, and the magnetic liquid is injected in the liquid cell.
2. the preparation method of the ferroelectric thin film with texture according to claim 1, it is characterised in that：The magnetic particle
For nano-scale magnetic particulate.
3. the preparation method of the ferroelectric thin film with texture according to claim 1 and 2, it is characterised in that：The magnetic
Particulate is ferrite.
4. the preparation method of the ferroelectric thin film with texture according to claim 1, it is characterised in that：Receive in the magnetic
Ferroelectric thin film is grown on rice chain adopt sol-gel process, chemical solution deposition, chemical vapour deposition technique, pulsed laser deposition
Any one in method, molecular beam epitaxy, magnetron sputtering method.
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| CN201510689332.XA CN105206710B (en) | 2015-10-22 | 2015-10-22 | The preparation method of the ferroelectric thin film with texture |
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| CN201510689332.XA CN105206710B (en) | 2015-10-22 | 2015-10-22 | The preparation method of the ferroelectric thin film with texture |
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| CN105702762B (en) * | 2016-01-21 | 2017-11-17 | 重庆科技学院 | A kind of method for preparing T-phase bismuth ferrite thin film |
| CN109994315B (en) * | 2019-02-19 | 2021-02-19 | 湖北大学 | Magnetoelectric composite material combined by ferroelectric film of magnetic nano fiber and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1745468A (en) * | 2002-09-30 | 2006-03-08 | 纳米系统公司 | Large-area nanoenabled macroelectronic substrates and uses therefor |
| CN101913867A (en) * | 2010-07-15 | 2010-12-15 | 上海大学 | Low-frequency multiferroic particle magnetic-electric composite material and preparation method thereof |
| CN102856430A (en) * | 2012-07-25 | 2013-01-02 | 常州大学 | Preparation method for bismuth titanate nanowire solar cells |
| CN103949656A (en) * | 2014-04-24 | 2014-07-30 | 山西霍尼韦尔水处理工程有限公司 | Method using ferric chloride to prepare zero-valent iron nanometer particles |
| CN104575658A (en) * | 2014-12-24 | 2015-04-29 | 中山大学 | Magnetic field and application of magnetic nanowires in transparent conductive film as well as transparent conductive film and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7135728B2 (en) * | 2002-09-30 | 2006-11-14 | Nanosys, Inc. | Large-area nanoenabled macroelectronic substrates and uses therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1745468A (en) * | 2002-09-30 | 2006-03-08 | 纳米系统公司 | Large-area nanoenabled macroelectronic substrates and uses therefor |
| CN101913867A (en) * | 2010-07-15 | 2010-12-15 | 上海大学 | Low-frequency multiferroic particle magnetic-electric composite material and preparation method thereof |
| CN102856430A (en) * | 2012-07-25 | 2013-01-02 | 常州大学 | Preparation method for bismuth titanate nanowire solar cells |
| CN103949656A (en) * | 2014-04-24 | 2014-07-30 | 山西霍尼韦尔水处理工程有限公司 | Method using ferric chloride to prepare zero-valent iron nanometer particles |
| CN104575658A (en) * | 2014-12-24 | 2015-04-29 | 中山大学 | Magnetic field and application of magnetic nanowires in transparent conductive film as well as transparent conductive film and preparation method |
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