CN109346601A - The preparation method of the multiple resistive memristor of full-inorganic perovskite - Google Patents
The preparation method of the multiple resistive memristor of full-inorganic perovskite Download PDFInfo
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- CN109346601A CN109346601A CN201811417769.8A CN201811417769A CN109346601A CN 109346601 A CN109346601 A CN 109346601A CN 201811417769 A CN201811417769 A CN 201811417769A CN 109346601 A CN109346601 A CN 109346601A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000010409 thin film Substances 0.000 claims abstract description 24
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004528 spin coating Methods 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052737 gold Inorganic materials 0.000 claims abstract description 3
- 239000010931 gold Substances 0.000 claims abstract description 3
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 3
- 239000011521 glass Substances 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 12
- 239000010408 film Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004851 dishwashing Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000007751 thermal spraying Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000007921 spray Substances 0.000 description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 8
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 3
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910001411 inorganic cation Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/20—Multistable switching devices, e.g. memristors
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of switching materials, e.g. deposition of layers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of switching materials, e.g. deposition of layers
- H10N70/026—Formation of switching materials, e.g. deposition of layers by physical vapor deposition, e.g. sputtering
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of preparation methods of the multiple resistive memristor of full-inorganic perovskite.The method first uses the method for thermal spraying to prepare perovskite thin film on the substrate surface cleaned up；Then the carry out spin coating of solvent is added dropwise in perovskite thin film after the cooling period, and re-annealing handles to obtain full-inorganic perovskite thin film；Finally coating gold or platinum electrode on full-inorganic perovskite thin film, are made memristor element.The method of the present invention is simple to operation, and the perovskite thin film dense uniform prepared, coverage are good, and defect is few；The memristor function admirable of preparation realizes multiple resistive by adjusting the ratio of methanol in solvent and butyric acid.
Description
Technical field
The invention belongs to optoelectronic film technical fields, are related to a kind of preparation side of multiple resistive memristor of full-inorganic perovskite
Method.
Background technique
Memristor is a kind of nonvolatile memory that information is recorded based on material change in resistance.Compared to similar function
Can storage unit, memristor has many advantages, such as that height deposits that density, read or write speed are fast, structure is simple, the retention time is long and low in energy consumption,
It is considered as the contenders of next-generation general-purpose storage.
Though hybrid inorganic-organic perovskite has the advantages that at low cost, carrier mobility is high, the absorption coefficient of light is big,
Still have many problems urgently to be resolved, especially because in system a large amount of intrinsic defects presence, lead to organic inorganic hybridization calcium
Titanium ore stability of material is poor.Meanwhile it is caused to storage, preparation and equipment operation to the extreme sensitivity of oxygen and moisture
The limitation of equal environment, also limits its practical application in every field.And replace organic group can be with inorganic cation
The stability of material, therefore the nanocrystalline CsPbX of full-inorganic lead halogen perovskite are improved well3(X is halogen) has obtained extensively
General research.
Full-inorganic perovskite material acts not only as light absorbing material and acts in photovoltaic device, is also applied to photoelectricity spy
Survey device, transistor, light emitting diode etc..Recently, it also has been reported that and halide perovskite material is applied to memristor, and obtain
Excellent performance.Document 1 uses CH3NH3PbI1-xClxLow-work voltage, high stable are prepared for as novel memristor material
Memristor device (Yoo, Eun Ji, et al. " the Resistive switching behavior in organic-of property
inorganic hybrid CH3NH3PbI3-xClx perovskite for resistive random access memory
devices."Advanced Materials 27.40(2015):6170-6175.).Document 2 uses the CsPbBr of full-inorganic3
Material adds zinc oxide film, and having prepared ON/OFF ratio is more than 105Device (Wu, Ye, et al. " Capping
CsPbBr3with ZnO to improve performance and stability of perovskite
memristors."Nano Research 10.5(2017):1584-1594.).But there is presently no the high-quality of multistage resistive
Measure the report of memristor.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of the multiple resistive memristor of full-inorganic perovskite.
Realize that the technical solution of the object of the invention is as follows:
The preparation method of the multiple resistive memristor of full-inorganic perovskite, includes the following steps:
Step 1, at 100~150 DEG C, CsPbBr is sprayed in the substrate surface cleaned up3Precursor solution prepares calcium titanium
Mine film；
Step 2, the film of step 1 is subjected to spin coating, solvent is added dropwise in spin coating process and carries out dissolution recrystallization, described is molten
The volume ratio of methanol and butyric acid is 100:0~100:5 in agent；
Step 3, the film after spin coating heats at 200~250 DEG C, is made annealing treatment, and it is thin to obtain full-inorganic perovskite
Film；
Step 4, one layer of gold or platinum electrode are plated on full-inorganic perovskite thin film, are obtained the multiple resistive of full-inorganic perovskite and are recalled
Hinder device.
Preferably, in step 1, the substrate successively uses dish washing liquid, and water dries up after ethyl alcohol, acetone ultrasonic cleaning, ultraviolet
Processing 10~15 minutes.
Preferably, in step 1, the substrate is FTO electro-conductive glass.
Preferably, in step 1, the CsPbBr3Precursor solution is CsPbBr3N,N-Dimethylformamide (DMF)
Or dimethyl sulfoxide (DMSO) solution.
Preferably, in step 2, spin speed 2000rpm.
Preferably, in step 4, annealing temperature is 200~250 DEG C.
Preferably, in step 4, annealing time is 2 hours.
Compared with the existing technology, the present invention has the following advantages:
(1) the method for the present invention is simple to operation, methanol and fourth is added dropwise in the processing recrystallized by solvent in the third step
The mixed solvent of acid, is prepared for the good full-inorganic perovskite thin film of even compact, coverage；
(2) present invention can realize the multiple resistive of memristor by adjusting the ratio of methanol and butyric acid.
Detailed description of the invention
Fig. 1 is CsPbBr prepared by embodiment 13The scanning electron microscope (SEM) photograph of perovskite thin film.
Fig. 2 is CsPbBr prepared by embodiment 23The scanning electron microscope (SEM) photograph of perovskite thin film.
Fig. 3 is CsPbBr prepared by embodiment 33The scanning electron microscope (SEM) photograph of perovskite thin film.
Fig. 4 is CsPbBr prepared by embodiment 43The scanning electron microscope (SEM) photograph of perovskite thin film.
Fig. 5 is CsPbBr prepared by comparative example 13The X-ray diffractogram of perovskite thin film.
Fig. 6 is the CsPbBr of different embodiments preparation3The multiple resistive curve of perovskite thin film.
Specific embodiment
The present invention will be described in detail in the following with reference to the drawings and specific embodiments.
Embodiment 1
1) start to be cleaned by ultrasonic FTO electro-conductive glass piece (thickness about 1mm) 20 minutes with dish washing liquid, it may on surface to remove
Existing organic and inorganic spot；Then it is rinsed again with a large amount of tap water；It is clear that FTO is finally put into ultrasound in deionized water
It washes 20 minutes；Above-mentioned clean FTO electro-conductive glass is put into dehydrated alcohol and is cleaned by ultrasonic about 20 minutes, to remove surface residual
Organic impurities, this step repeat multipass；Again by FTO electro-conductive glass ultrasonic cleaning about 20 minutes in acetone, further remove
Remove the organic impurities of surface residual；It is taken from acetone and goes out FTO substrate respectively, placed it in UV ozone cleaning machine, cleaning 30
Minute；The hearth electrode material is the SnO for adulterating fluorine2Transparent conducting glass (SnO2: F), referred to as FTO.
2) CsPbBr of 0.25mol/L is configured3Perovskite precursor solution, 70 DEG C of heating stirrings for 24 hours.
3) washed FTO electro-conductive glass piece is placed on warm table, 100 DEG C of heating spray perovskite precursor solution, spray
Complete cooling.
4) substrate is placed on spin coating instrument, the methanol solution of 500 μ l is added dropwise at 2000rpm, spin coating 1 minute, then exists
It anneals 2 hours at 250 DEG C.
The perovskite thin film of preparation is analyzed and characterized, Fig. 1 is perovskite thin film scanning electron microscope prepared by embodiment 1
Shape appearance figure, perovskite crystal grain is in apparent graininess in figure, and the planarization of film is not high.
Embodiment 2
1) start to be cleaned by ultrasonic FTO electro-conductive glass piece (thickness about 1mm) 20 minutes with dish washing liquid, it may on surface to remove
Existing organic and inorganic spot；Then it is rinsed again with a large amount of tap water；It is clear that FTO is finally put into ultrasound in deionized water
It washes 20 minutes；Above-mentioned clean FTO electro-conductive glass is put into dehydrated alcohol and is cleaned by ultrasonic about 20 minutes, to remove surface residual
Organic impurities, this step repeat multipass；Again by FTO electro-conductive glass ultrasonic cleaning about 20 minutes in acetone, further remove
Remove the organic impurities of surface residual；It is taken from acetone and goes out FTO substrate respectively, placed it in UV ozone cleaning machine, cleaning 30
Minute；The hearth electrode material is the SnO for adulterating fluorine2Transparent conducting glass (SnO2: F), referred to as FTO.
2) CsPbBr of 0.25mol/L is configured3Perovskite precursor solution, 70 DEG C of heating stirrings for 24 hours.
3) washed FTO electro-conductive glass piece is placed on warm table, 100 DEG C of heating spray perovskite precursor solution, spray
Complete cooling.
4) substrate is placed on spin coating instrument, the methanol of 500 μ l is added dropwise at 2000rpm: butyric acid volume ratio is the mixed of 100:1
Solution is closed, spin coating 1 minute, is then annealed 2 hours at 250 DEG C.
The perovskite thin film of preparation is analyzed and characterized, Fig. 2 is perovskite thin film scanning electron microscope prepared by embodiment 2
Shape appearance figure, perovskite crystal grain starts to change to sheet in figure, and flatness is got higher.
Embodiment 3
1) start to be cleaned by ultrasonic FTO electro-conductive glass piece (thickness about 1mm) 20 minutes with dish washing liquid, it may on surface to remove
Existing organic and inorganic spot；Then it is rinsed again with a large amount of tap water；It is clear that FTO is finally put into ultrasound in deionized water
It washes 20 minutes；Above-mentioned clean FTO electro-conductive glass is put into dehydrated alcohol and is cleaned by ultrasonic about 20 minutes, to remove surface residual
Organic impurities, this step repeat multipass；Again by FTO electro-conductive glass ultrasonic cleaning about 20 minutes in acetone, further remove
Remove the organic impurities of surface residual；It is taken from acetone and goes out FTO substrate respectively, placed it in UV ozone cleaning machine, cleaning 30
Minute；The hearth electrode material is the SnO for adulterating fluorine2Transparent conducting glass (SnO2: F), referred to as FTO.
2) CsPbBr of 0.25mol/L is configured3Perovskite precursor solution, 70 DEG C heating stirring 24 hours.
3) washed FTO electro-conductive glass piece is placed on warm table, 100 DEG C of heating spray perovskite precursor solution, spray
Complete cooling.
4) substrate is placed on spin coating instrument, the methanol of 500 μ l is added dropwise at 2000rpm: butyric acid volume ratio is the mixed of 100:3
Solution is closed, spin coating 1 minute, then annealed at 250 DEG C 2h.
The perovskite thin film of preparation is analyzed and characterized, Fig. 3 is perovskite thin film scanning electron microscope prepared by embodiment 3
Shape appearance figure, the transformation of perovskite sheet of particles stratiform is further obvious in figure, and film flatness further increases.
Embodiment 4
1) start to be cleaned by ultrasonic FTO electro-conductive glass piece (thickness about 1mm) 20 minutes with dish washing liquid, it may on surface to remove
Existing organic and inorganic spot；Then it is rinsed again with a large amount of tap water；It is clear that FTO is finally put into ultrasound in deionized water
It washes 20 minutes；Above-mentioned clean FTO electro-conductive glass is put into dehydrated alcohol and is cleaned by ultrasonic about 20 minutes, to remove surface residual
Organic impurities, this step repeat multipass；Again by FTO electro-conductive glass ultrasonic cleaning about 20 minutes in acetone, further remove
Remove the organic impurities of surface residual；It is taken from acetone and goes out FTO substrate respectively, placed it in UV ozone cleaning machine, cleaning 30
Minute；The hearth electrode material is the SnO for adulterating fluorine2Transparent conducting glass (SnO2: F), referred to as FTO.
2) configure 0.25mol/L CsPbBr3 perovskite precursor solution, 70 DEG C of heating stirrings for 24 hours.
3) washed FTO electro-conductive glass piece is placed on warm table, 100 DEG C of heating spray perovskite precursor solution, spray
Complete cooling.
4) substrate is placed on spin coating instrument, the methanol of 500 μ l is added dropwise at 2000rpm: butyric acid volume ratio is the mixed of 100:5
Solution is closed, spin coating 1 minute, is then annealed 2 hours at 250 DEG C.
The perovskite thin film of preparation is analyzed and characterized, Fig. 4 is perovskite thin film scanning electron microscope prepared by embodiment 4
Shape appearance figure, perovskite particle is thoroughly changed into sheet in figure, and flatness is also higher.
Comparative example 1
This comparative example is substantially the same manner as Example 1, unique the difference is that the ratio of methanol and butyric acid is 100:20.Fig. 5 is
CsPbBr prepared by comparative example 13The X-ray diffractogram of perovskite thin film, as can be seen from the figure under these conditions, not
Perovskite Phase is formed, illustrates that the ratio of methanol and butyric acid is more than that 100:5 can make Perovskite Phase decompose, memristor can not be prepared
Device device.
Claims (7)
1. the preparation method of the multiple resistive memristor of full-inorganic perovskite, which comprises the steps of:
Step 1, at 100~150 DEG C, CsPbBr is sprayed in the substrate surface cleaned up3It is thin to prepare perovskite for precursor solution
Film；
Step 2, the film of step 1 is subjected to spin coating, solvent is added dropwise in spin coating process and carries out dissolution recrystallization, in the solvent
The volume ratio of methanol and butyric acid is 100:0~100:5；
Step 3, the film after spin coating heats at 200~250 DEG C, is made annealing treatment, and full-inorganic perovskite thin film is obtained；
Step 4, one layer of gold or platinum electrode are plated on full-inorganic perovskite thin film, obtain the multiple resistive memristor of full-inorganic perovskite
Device.
2. preparation method according to claim 1, which is characterized in that in step 1, the substrate successively uses dish washing liquid,
Water dries up, ultraviolet processing 10~15 minutes after ethyl alcohol, acetone ultrasonic cleaning.
3. preparation method according to claim 1, which is characterized in that in step 1, the substrate is FTO electro-conductive glass.
4. preparation method according to claim 1, which is characterized in that in step 1, the CsPbBr3Precursor solution is
CsPbBr3DMF or DMSO solution.
5. preparation method according to claim 1, which is characterized in that in step 2, spin speed 2000rpm.
6. preparation method according to claim 1, which is characterized in that in step 4, annealing temperature is 200~250 DEG C.
7. preparation method according to claim 1, which is characterized in that in step 4, annealing time is 2 hours.
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| CN110379921A (en) * | 2019-07-25 | 2019-10-25 | 陕西科技大学 | A kind of flexible multi-state resistive memory and one step solwution method preparation method based on full-inorganic perovskite thin film |
| CN110690345A (en) * | 2019-08-30 | 2020-01-14 | 深圳大学 | Light-operated memristor and preparation method thereof |
| CN111200177A (en) * | 2020-02-28 | 2020-05-26 | 南京信息工程大学 | Lead-halogen perovskite light-driven charging electrode and preparation method thereof |
| CN112382726A (en) * | 2020-10-09 | 2021-02-19 | 西北工业大学 | Photoelectric coupling perovskite memristor for neuromorphic calculation and preparation method |
| CN112820824A (en) * | 2021-01-05 | 2021-05-18 | 华中科技大学 | Perovskite memristor and preparation method thereof |
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| CN110379921A (en) * | 2019-07-25 | 2019-10-25 | 陕西科技大学 | A kind of flexible multi-state resistive memory and one step solwution method preparation method based on full-inorganic perovskite thin film |
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| CN112820824A (en) * | 2021-01-05 | 2021-05-18 | 华中科技大学 | Perovskite memristor and preparation method thereof |
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