CN108525963A - A kind of preparation method of inorganic halogen perovskite thin film - Google Patents
A kind of preparation method of inorganic halogen perovskite thin film Download PDFInfo
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- CN108525963A CN108525963A CN201710116487.3A CN201710116487A CN108525963A CN 108525963 A CN108525963 A CN 108525963A CN 201710116487 A CN201710116487 A CN 201710116487A CN 108525963 A CN108525963 A CN 108525963A
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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 without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of the switching material, e.g. layer deposition
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention discloses a kind of preparation methods of inorganic perovskite thin film.The method is specially：At 80~100 DEG C, in clean hearth electrode surface spraying perovskite precursor liquid CsPbBr3, deposition is had into perovskite CsPbBr3Hearth electrode poor solvent is added dropwise in spin coating, made annealing treatment at 250~300 DEG C, obtain inorganic perovskite thin film.The CsPbBr that the present invention is prepared in spray coating method3Poor solvent is added dropwise in the spin coating process of perovskite thin film, by changing the proportionate relationship of butyric acid and toluene in poor solvent, controls CsPbBr3Grain morphology in film, improves CsPbBr3The stability of film, while it being made to have excellent change resistance performance, it is widely used in memristor field.
Description
Technical field
The invention belongs to microelectronic device preparation fields, are related to a kind of preparation method of inorganic halogen perovskite thin film.
Background technology
Resistive random access memory, abbreviation memristor are to be encouraged based on external voltage and material resistance value is promoted to occur
Change and then record a kind of nonvolatile memory of information.It compares for other memory devices with similar functions, recalls
Device is hindered due to having height to deposit density, and read or write speed is fast, simple in structure, and the retention time is long, and a series of advantage such as low in energy consumption is recognized
To be the contenders of next-generation general-purpose storage.
Inorganic halogen perovskite is due to excellent optical such as high stability and adjustable, efficient luminescence generated by light
Can, by as potential optical gain material and various photoelectric devices, (such as solar photovoltaic device, shines at photodetector
Diode etc.) in luminescent material.Further, since inorganic halogen perovskite can quickly be made by easy low temperature liquid polymerization process
It is standby, the extensive research interest of people is caused, the flow of research of this kind of material is greatly accelerated.Low temperature liquid polymerization process is prepared inorganic
The number of drawbacks such as vacancy, interstitial atom are frequently present of in perovskite thin film, and these defects based on utilization material itself to being lacked
It falls into for the resistance switch memory based on drift, is then intrinsic innate advantage.
There are still some problems for current inorganic perovskite film preparing technology, and that for example reports recently passes through low temperature liquid polymerization process
(Ye Wu,et al.,Capping CsPbBr3with ZnO to improve performance and stability of
perovskite memristors；Nano Research) the inorganic perovskite thin film for preparing there is that crystallite dimension is small, crystal grain
The problems such as crystallinity is poor, consistency is inadequate and the stability of film is poor.So far, the system of single inorganic perovskite thin film
Standby technology cannot still meet current performance indicator demand.
Invention content
Present invention aims at a kind of preparation method of inorganic halogen perovskite thin film is provided, the method is in spraying legal system
Standby CsPbBr3Poor solvent is added dropwise in the spin coating process of perovskite thin film, by changing butyric acid and toluene in poor solvent
Proportionate relationship controls CsPbBr3Grain morphology in film, improves CsPbBr3The stability of film influences the photoelectricity of material
Performance makes it have excellent change resistance performance.
Realize that the technical solution of the object of the invention is as follows：
A kind of preparation method of inorganic perovskite thin film, includes the following steps：
At 80~100 DEG C, in clean hearth electrode surface spraying perovskite precursor liquid CsPbBr3, deposition is had into calcium titanium
Mine CsPbBr3Hearth electrode poor solvent is added dropwise in spin coating, made annealing treatment at 250~300 DEG C, obtain inorganic calcium titanium
Mine film, the poor solvent are the mixed solvent of toluene or toluene and butyric acid.
Preferably, the solvent used in the perovskite precursor liquid is N, N- dimethylformamides (DMF).
Preferably, the hearth electrode is FTO or ITO electro-conductive glass.
Preferably, the rotating speed when spin coating is 1000~4000rpm, and spin-coating time is 8s~1min.
Preferably, the annealing time is 10~15min.
Preferably, the volume fraction of the in the mixed solvent of the toluene and butyric acid, butyric acid is 1%~5%.
Compared with prior art, the present invention having following remarkable advantage：
(1) spray coating method prepares CsPbBr3After perovskite thin film, poor solvent is added dropwise in spin coating process, it not only can be so as to
The perovskite thin film of big crystal grain is prepared promptly, and significantly improves its stability；
(2) by controlling the proportionate relationship of toluene and butyric acid in poor solvent, regulate and control the CsPbBr finally prepared3It is thin
Grain morphology in film, and then influence the photoelectric properties of material；
(3) perovskite thin film made from has thicker change resistance layer, and more capture sites are had in preparation process and (are lacked
Fall into) it generates, more capture site (defect) is easier to capture the carrier generated by electric pulse excitation, to make system obtain
Excellent change resistance performance is obtained, resistive ratio is up to 103~105。
Description of the drawings
Fig. 1 is CsPbBr prepared by conventional spray paint method3The scanning electron microscope shape appearance figure of (poor solvent is not added dropwise).
Fig. 2 is that embodiment 1 prepares CsPbBr3The scanning electron microscope shape appearance figure of film (1mL toluene is added dropwise).
Fig. 3 is that embodiment 2 prepares CsPbBr3Film (is added dropwise 1m butyric acid and toluene Mixed Solvent, wherein butyric acid content is
1%) scanning electron microscope shape appearance figure.
Fig. 4 is that embodiment 3 prepares CsPbBr3Film (is added dropwise 1m butyric acid and toluene Mixed Solvent, wherein butyric acid content is
3%) scanning electron microscope shape appearance figure.
Fig. 5 is that embodiment 4 prepares CsPbBr3Film (is added dropwise 1m butyric acid and toluene Mixed Solvent, wherein butyric acid content is
5%) scanning electron microscope shape appearance figure.
Fig. 6 is that embodiment 5 prepares CsPbBr3Film (is added dropwise 1m butyric acid and toluene Mixed Solvent, wherein butyric acid content is
5%) scanning electron microscope shape appearance figure.
Fig. 7 is that comparative example prepares CsPbBr3(1m butyric acid, toluene Mixed Solvent is added dropwise, wherein butyric acid content is in film
20%) scanning electron microscope shape appearance figure.
Fig. 8 is the CsPbBr prepared based on embodiment 1,2,3,43The resistive curve graph of the memristor storage unit of film.
Specific implementation mode
The present invention will be described in detail in the following with reference to the drawings and specific embodiments.
Embodiment 1
(1) cleaning of hearth electrode：Liquid detergent is cleaned by ultrasonic FTO electro-conductive glass piece (thickness about 1mm) 20 minutes, removes surface
On organic and inorganic spot, then rinsed, FTO electro-conductive glass pieces be put into deionized water ultrasonic with a large amount of tap water
Cleaning, which is put into after twenty minutes in absolute ethyl alcohol, to be cleaned by ultrasonic 20 minutes, and the organic impurities of surface residual is removed, this step repeats more
Time.Later by FTO electro-conductive glass piece ultrasonic cleaning 20 minutes in acetone, the organic impurities of surface residual is further removed,
It after acetone cleaning, places it in UV ozone cleaning machine, cleans 30 minutes.FTO is the SnO for adulterating fluorine2Transparent conducting glass
(SnO2：F).
(2)CsPbBr3The preparation of perovskite precursor liquid storing liquid：It is 1 in molar ratio:1 by CsBr and PbBr2It is dissolved in DMF
In, it is stirred to react at 70 DEG C 12 hours, prepares the CsPbBr of 1M3Perovskite precursor liquid storing liquid.
(3) it sprays：The FTO substrates cleaned up are placed in the heating plate of 100 DEG C of constant temperature, by 200 μ L perovskite forerunners
Storing liquid is dissolved in the DMF of 800 μ L, and perovskite precursor liquid is obtained after being sufficiently stirred, by spraying equipment by perovskite precursor liquid
It is sprayed on FTO substrates, one layer of perovskite thin film is deposited on substrate.
(4) spin coating and annealing：Above-mentioned FTO substrates are transferred on spin coating instrument and carry out spin coating (1000rpm~8s), and are being revolved
The toluene of 1mL is persistently added dropwise during painting on calcium titanium ore bed, be subsequently placed in 250 DEG C of heating plate carry out annealing 10~
15min。
(5) magnetron sputtering prepares memristor storage unit：Perovskite thin film obtained above is placed in magnetron sputtering reaction
In room, it is evacuated to less than 5 × 10-5Pa each leads into high-purity argon gas as working gas, and operating air pressure 0.2Pa sputters work(
Rate is 65W, and sputtering under room temperature obtains the gold electrode of thickness about 300nm or so, obtains with CsPbBr3Film is change resistance layer
Memristor storage unit.
Fig. 1 is CsPbBr prepared by conventional spray paint method3(poor solvent is not added dropwise) scanning electron microscope (SEM) shape appearance figure, Fig. 2 are
CsPbBr prepared by embodiment 13Film (1mL toluene is added dropwise) scanning electron microscope (SEM) shape appearance figure.Comparison diagram 1 and Fig. 2 are it is found that logical
Cross the CsPbBr prepared to spray coating method3First is added dropwise during the spin coating after spraying in the post-processing of perovskite thin film
Benzene is compared to traditional spray coating method, can prepare the perovskite thin film of crystal grain bigger.In addition, finding after tested (see figure
8), CsPbBr manufactured in the present embodiment3The resistive ratio of perovskite thin film memristor is about 103~105, and it is based on conventional spray paint method
The CsPbBr of preparation3The resistive of film memristor is than only 20~100, CsPbBr made from the present embodiment3Perovskite thin film has
More excellent change resistance performance.
Embodiment 2
(1) cleaning of hearth electrode is the same as embodiment 1.
(2)CsPbBr3The preparation of perovskite precursor liquid storing liquid is the same as embodiment 1.
(3) spraying is the same as embodiment 1.
(4) spin coating and annealing：Above-mentioned FTO substrates are transferred on spin coating instrument and carry out spin coating (4000rpm~1min), and
The toluene and butyric acid mixed solvent (wherein the content of butyric acid is 1%) of 1mL is persistently added dropwise during spin coating on calcium titanium ore bed,
Then it places it in and carries out 10~15min of annealing in 250 DEG C of heating plate.
(5) magnetron sputtering prepares memristor storage unit：Perovskite thin film obtained above is placed in magnetron sputtering reaction
In room, it is evacuated to less than 5 × 10-5Pa each leads into high-purity argon gas as working gas, and operating air pressure 0.2Pa sputters work(
Rate is 65W, and sputtering under room temperature obtains the gold electrode of thickness about 300nm or so, obtains with CsPbBr3Film is change resistance layer
Memristor storage unit.
The perovskite thin film of preparation is analyzed and characterized：Fig. 3 is that present example 2 prepares CsPbBr3Film scanning
Electronic Speculum (SEM) shape appearance figure；The CsPbBr by being prepared to spray coating method is found after comparison3The post-processing of perovskite thin film is being sprayed
Toluene, the butyric acid mixed solution (wherein the content of butyric acid is 1%) of 1mL are added dropwise during spin coating after painting, not only may be used
To prepare the perovskite thin film of crystal grain bigger, and gradually changed from three-dimensional block crystal grain to accurate two-dimentional crystal grain.In addition, through surveying
Examination finds (see Fig. 8), the CsPbBr prepared based on the optimization method3The high low-resistance ratio of perovskite thin film memristor is about 104With
On.
Embodiment 3
(1) cleaning of hearth electrode is the same as embodiment 1.
(2)CsPbBr3The preparation of perovskite precursor liquid storing liquid is the same as embodiment 1.
(3) spraying is the same as embodiment 1.
(4) spin coating and annealing：Above-mentioned FTO substrates are transferred on spin coating instrument and carry out spin coating (1000rpm~8s), and are being revolved
The toluene and butyric acid mixed solvent (wherein the content of butyric acid is 3%) of 1mL is persistently added dropwise during painting on calcium titanium ore bed, so
It places it in afterwards and carries out 10~15min of annealing in 250 DEG C of heating plate.
(5) magnetron sputtering prepares memristor storage unit：Perovskite thin film obtained above is placed in magnetron sputtering reaction
In room, it is evacuated to less than 5 × 10-5Pa each leads into high-purity argon gas as working gas, and operating air pressure 0.2Pa sputters work(
Rate is 65W, and sputtering under room temperature obtains the gold electrode of thickness about 300nm or so, obtains with CsPbBr3Film is change resistance layer
Memristor storage unit.
The perovskite thin film of preparation is analyzed and characterized：Fig. 4 is that present example 3 prepares CsPbBr3Film scanning
Electronic Speculum (SEM) shape appearance figure；The CsPbBr by being prepared to spray coating method is found after comparison3The post-processing of perovskite thin film is being sprayed
Toluene, the butyric acid mixed solution (wherein the content of butyric acid is 5%) of 1mL are added dropwise during spin coating after painting, not only may be used
To prepare the perovskite thin film of crystal grain bigger, and more obvious showing from three-dimensional block crystal grain to accurate two-dimentional crystal grain turns
Become.In addition, find (see Fig. 8) after tested, the CsPbBr prepared based on the optimization method3The high low-resistance of perovskite thin film memristor
Ratio is about 105More than.
Embodiment 4
(1) cleaning of hearth electrode is the same as embodiment 1.
(2)CsPbBr3The preparation of perovskite precursor liquid storing liquid is the same as embodiment 1.
(3) spraying is the same as embodiment 1.
(4) spin coating and annealing：Above-mentioned FTO substrates are transferred on spin coating instrument and carry out spin coating (1000rpm~8s), and are being revolved
The toluene and butyric acid mixed solvent (wherein the content of butyric acid is 5%) of 1mL is persistently added dropwise during painting on calcium titanium ore bed, so
It places it in afterwards and carries out 10~15min of annealing in 250 DEG C of heating plate.
(5) magnetron sputtering prepares memristor storage unit：Perovskite thin film obtained above is placed in magnetron sputtering reaction
In room, it is evacuated to less than 5 × 10-5Pa each leads into high-purity argon gas as working gas, and operating air pressure 0.2Pa sputters work(
Rate is 65W, and sputtering under room temperature obtains the gold electrode of thickness about 300nm or so, obtains with CsPbBr3Film is change resistance layer
Memristor storage unit.
The perovskite thin film of preparation is analyzed and characterized：Fig. 5 is that present example 4 prepares CsPbBr3Film scanning
Electronic Speculum (SEM) shape appearance figure；The CsPbBr by being prepared to spray coating method is found after comparison3The post-processing of perovskite thin film is being sprayed
Toluene, the butyric acid mixed solution (wherein the content of butyric acid is 5%) of 1mL are added dropwise during spin coating after painting, not only may be used
To prepare the perovskite thin film of crystal grain bigger, and completely by two dimensional crystal subject to the transformation of three-dimensional block crystal grain.In addition,
Find (see Fig. 8) after tested, the CsPbBr prepared based on the optimization method3The high low-resistance ratio of perovskite thin film memristor about exists
105More than.
Embodiment 5
(1) cleaning of hearth electrode is the same as embodiment 1.
(2)CsPbBr3The preparation of perovskite precursor liquid storing liquid is the same as embodiment 1.
(3) spraying is the same as embodiment 1.
(4) spin coating and annealing：Above-mentioned FTO substrates are transferred on spin coating instrument and carry out spin coating (1000rpm~8s), and are being revolved
The toluene and butyric acid mixed solvent (wherein the content of butyric acid is 5%) of 1mL is persistently added dropwise during painting on calcium titanium ore bed, so
It places it in afterwards and carries out 10~15min of annealing in 300 DEG C of heating plate.
(5) magnetron sputtering prepares memristor storage unit：Perovskite thin film obtained above is placed in magnetron sputtering reaction
In room, it is evacuated to less than 5 × 10-5Pa each leads into high-purity argon gas as working gas, and operating air pressure 0.2Pa sputters work(
Rate is 65W, and sputtering under room temperature obtains the gold electrode of thickness about 300nm or so, obtains with CsPbBr3Film is change resistance layer
Memristor storage unit.
The perovskite thin film of preparation is analyzed and characterized：Fig. 6 is that present example 5 prepares CsPbBr3Film scanning
Electronic Speculum (SEM) shape appearance figure；The CsPbBr by being prepared to spray coating method is found after comparison3The post-processing of perovskite thin film is being sprayed
The toluene and butyric acid mixed solution (wherein the content of butyric acid is 5%) of 1mL, Yi Ji are added dropwise during spin coating after painting
Change the temperature of annealing within the temperature range of being given above, three-dimensional block crystal grain equally may be implemented and turn to quasi- two dimensional crystal
Become.
Comparative example
(1) cleaning of hearth electrode is the same as embodiment 1.
(2)CsPbBr3The preparation of perovskite precursor liquid storing liquid is the same as embodiment 1.
(3) spraying is the same as embodiment 1.
(4) spin coating and annealing：Above-mentioned FTO substrates are transferred on spin coating instrument and carry out spin coating (4000rpm~1min), and
The toluene and butyric acid mixed solvent (wherein the content of butyric acid is 5%) of 1mL is persistently added dropwise during spin coating on calcium titanium ore bed,
Then it places it in and carries out 10~15min of annealing in 250 DEG C of heating plate.
Fig. 7 is CsPbBr prepared by comparative example3Scanning electron microscope (SEM) shape appearance figure of film.Made from Examples 1 to 5
It is found that CsPbBr by being prepared to spray coating method after film comparison3The post-processing of perovskite thin film, i.e. rotation after spraying
The toluene and butyric acid mixed solvent (wherein the content of butyric acid is 20%) of 1mL are added dropwise during painting, finds original CsPbBr3
Structure has been destroyed, and PbI is decomposed into2。
Claims (6)
1. a kind of preparation method of inorganic perovskite thin film, which is characterized in that include the following steps：
At 80~100 DEG C, in clean hearth electrode surface spraying perovskite precursor liquid CsPbBr3, deposition is had into perovskite
CsPbBr3Hearth electrode poor solvent is added dropwise in spin coating, made annealing treatment at 250~300 DEG C, obtain inorganic perovskite
Film, the poor solvent are the mixed solvent of toluene or toluene and butyric acid.
2. preparation method according to claim 1, which is characterized in that the in the mixed solvent of the toluene and butyric acid, fourth
The volume fraction of acid is 1%~5%.
3. preparation method according to claim 1 or 2, which is characterized in that used in the perovskite precursor liquid molten
Agent is N, N- dimethylformamides.
4. preparation method according to claim 1 or 2, which is characterized in that the hearth electrode is FTO or ITO conduction glass
Glass.
5. preparation method according to claim 1 or 2, which is characterized in that rotating speed when the described spin coating is 1000~
4000rpm, spin-coating time are 8s~1min.
6. preparation method according to claim 1 or 2, which is characterized in that the annealing time be 10~
15min。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109346601A (en) * | 2018-11-26 | 2019-02-15 | 南京理工大学 | The preparation method of the multiple resistive memristor of full-inorganic perovskite |
| CN110305660A (en) * | 2019-06-14 | 2019-10-08 | 上海大学 | The preparation method of the quasi- two-dimentional perovskite thin film of low defect based on the induction of methylsulphur acid anion |
| CN111139059A (en) * | 2019-12-19 | 2020-05-12 | 南京理工大学 | Method for improving perovskite quantum dot performance by short-chain alkyl carboxylic acid |
| CN111269716A (en) * | 2020-04-07 | 2020-06-12 | 郑州卓而泰新材料科技有限公司 | Method for in-situ preparation of transition metal doped perovskite quantum dot film |
| CN111628091A (en) * | 2020-06-08 | 2020-09-04 | 西北工业大学 | Method for improving quality of perovskite thin film through solvent bath auxiliary heat treatment |
| CN112038449A (en) * | 2020-08-27 | 2020-12-04 | 上海应用技术大学 | CsPbX prepared by solution spraying method3Film, its preparation and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110305660B (en) * | 2019-06-14 | 2022-07-12 | 上海大学 | Preparation method of low-defect quasi-two-dimensional perovskite film based on methanesulfonic acid anion induction |
| CN111139059A (en) * | 2019-12-19 | 2020-05-12 | 南京理工大学 | Method for improving perovskite quantum dot performance by short-chain alkyl carboxylic acid |
| CN111269716A (en) * | 2020-04-07 | 2020-06-12 | 郑州卓而泰新材料科技有限公司 | Method for in-situ preparation of transition metal doped perovskite quantum dot film |
| CN111628091A (en) * | 2020-06-08 | 2020-09-04 | 西北工业大学 | Method for improving quality of perovskite thin film through solvent bath auxiliary heat treatment |
| CN112038449A (en) * | 2020-08-27 | 2020-12-04 | 上海应用技术大学 | CsPbX prepared by solution spraying method3Film, its preparation and use |
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Application publication date: 20180914 |