CN110707211B - Preparation method of cerium oxide memristor film - Google Patents
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- CN110707211B CN110707211B CN201910934567.9A CN201910934567A CN110707211B CN 110707211 B CN110707211 B CN 110707211B CN 201910934567 A CN201910934567 A CN 201910934567A CN 110707211 B CN110707211 B CN 110707211B
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 113
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 21
- 108010025899 gelatin film Proteins 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 230000001678 irradiating effect Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 239000010408 film Substances 0.000 claims description 54
- 239000010409 thin film Substances 0.000 claims description 33
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 17
- CVBUKMMMRLOKQR-UHFFFAOYSA-N 1-phenylbutane-1,3-dione Chemical compound CC(=O)CC(=O)C1=CC=CC=C1 CVBUKMMMRLOKQR-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims 1
- 238000001935 peptisation Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 8
- 229910003437 indium oxide Inorganic materials 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 description 12
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 9
- 230000008859 change Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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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
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
- H10N70/883—Oxides or nitrides
- H10N70/8833—Binary metal oxides, e.g. TaOx
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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
- H10N70/011—Manufacture or treatment of multistable switching devices
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Abstract
The invention discloses a preparation method of a cerium oxide memristor film, which is implemented according to the following steps: step 1, preparing cerium oxide sol; step 2, adopting a dipping-pulling method, taking cerium oxide sol as a raw material, pulling the cerium oxide gel film on an indium oxide (ITO) substrate at room temperature by using a pulling machine, drying the cerium oxide gel film at room temperature, then carrying out heat treatment at 300-700 ℃, and cooling to obtain the cerium oxide film; and 3, irradiating the cerium oxide film obtained in the step 2 by using ultraviolet rays to obtain the cerium oxide memristor film. The preparation method of the cerium oxide memristor film has the advantages of low preparation cost, simple process, easiness in control and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of a microelectronic material resistance random access memory film, and particularly relates to a preparation method of a cerium oxide memristor film.
Background
As a next-generation nonvolatile memory, memristor thin-film materials are being widely researched due to the advantages of simple structure, good compatibility, fast read-write speed, high durability, low energy consumption, low cost and the like.
In the present stage, for the memristor thin-film device, an oxygen vacancy type resistance change memory material is taken as a main research object and is mainly used for improving the resistance change performance of the memristor thin-film device so as to ensure that the memristor thin-film device has good voltage stability during working.
Disclosure of Invention
The invention aims to provide a preparation method of a cerium oxide memristor film, which is used for improving the performance of a memristor film device.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the cerium oxide memristor film is implemented according to the following steps:
and 3, irradiating the cerium oxide film obtained in the step 2 by using ultraviolet rays to obtain the cerium oxide memristor film.
The technical proposal of the invention also has the following characteristics,
in the step 1, preparing cerium oxide sol specifically includes: the method comprises the steps of mixing cerium nitrate, benzoylacetone and absolute ethyl alcohol according to a molar ratio of 1.
In the step 1, the obtained cerium oxide is peptized and stirred for 6 to 8 hours at room temperature, and then aged for 24 hours.
In the step 2, the heat treatment is performed under an oxygen atmosphere.
In the step 2, the time for the heat treatment is 20min.
In the step 3, an ultraviolet LED light source with power of 30W is used for irradiating the cerium oxide film, the wavelength of the ultraviolet LED light source is 365nm, the irradiation distance is 2 cm, and the irradiation time is 2 hours.
The invention has the beneficial effects that: the preparation method of the cerium oxide memristor film has the advantages of low preparation cost, simple process, easiness in control and the like, the preparation efficiency of the cerium oxide memristor film is improved, and the prepared cerium oxide memristor film has good resistance reversal characteristics.
Drawings
Fig. 1 is an Atomic Force Microscope (AFM) two-dimensional photograph of the surface of a cerium oxide memristor thin film prepared in example 1 of the present disclosure;
FIG. 2 is an Atomic Force Microscope (AFM) two-dimensional photograph of the surface of a cerium oxide memristor thin film prepared in example 2 of the present disclosure;
FIG. 3 is an Atomic Force Microscope (AFM) two-dimensional photograph of the surface of a nano-cerium oxide memristor thin film prepared in example 3 of the present disclosure;
FIG. 4 is an X-ray photoelectron spectroscopy (XPS) full spectrum of a cerium oxide memristor thin film prepared in example 3 of the present disclosure;
FIG. 5 is a Ce3d spectrum of X-ray photoelectron spectroscopy (XPS) of a cerium oxide memristor thin film prepared in example 3 of the present disclosure;
FIG. 6 is a graph showing the result of a contact angle test of the cerium oxide thin film prepared in example 3 before irradiation with ultraviolet light;
FIG. 7 is a graph showing the results of a contact angle test after irradiation of the cerium oxide thin film prepared in example 3;
FIG. 8 is a plot of the current-voltage characteristics (I-V) of a cerium oxide memristor thin-film device fabricated from a cerium oxide device thin-film in example 3 of the present disclosure.
FIG. 9 is a voltage-current characteristic (I-V) curve of a cerium oxide memristor thin-film device fabricated from a cerium oxide memristor thin-film in example 7 of the present disclosure.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and detailed description.
A preparation method of a cerium oxide memristor film is implemented according to the following steps:
And preparing a top electrode, namely putting the cerium oxide memristor thin film sample into a sputtering instrument, fixing a Mask plate (Mask), then opening a power supply of the sputtering instrument, exhausting air, and sputtering the top electrode when the vacuum degree reaches 1 × 10-3 Pa. The sputtering target material is Pt, the purity is 99.9%, and the sputtering time is 5 minutes. The sputtered Pt layer is a top electrode of the cerium oxide memristor film, and the preparation of the nano cerium oxide film memristor unit is completed, so that the resistance change performance can be tested and researched.
Example 1
A preparation method of a cerium oxide memristor film is implemented according to the following steps:
Example 2
A preparation method of a cerium oxide memristor film is implemented according to the following steps:
Example 3
A preparation method of a cerium oxide memristor film is implemented according to the following steps:
As shown in fig. 1, microscopic studies of the thin surface of the cerium oxide memristor prepared from example 1 were performed using an Atomic Force Microscope (AFM) with a scan area of 2 x 2um 2 The cerium oxide film heat treated at 300 deg.c is heat treated in oxygen atmosphere to volatilize organic matter and form obvious grains of size smaller than 200nm and size homogeneous, and the microscopic surface has surface undulation of 52.94nm.
As shown in FIG. 2, the thin surface of the cerium oxide memristor prepared in example 2 was microscopically studied using an Atomic Force Microscope (AFM) with a scan area of 2 x 2um 2 The cerium oxide film heat-treated at 500 ℃ was subjected to heat treatment in an oxygen atmosphere, and had significant particle formation, a particle size of about 200nm was small and uniform, and surface waviness in a microscopic form of 24.86nm was reduced as compared with the cerium oxide film in example 1.
As shown in FIG. 3, the thin surface of the cerium oxide memristor prepared in example 3 was microscopically studied using an Atomic Force Microscope (AFM) with a scan area of 2 x 2um 2 Scan area of 2 x 2um 2 The cerium oxide film heat-treated at 700 ℃ has obvious particle formation and obviously reduced particle size through heat treatment in an oxygen atmosphere, so that nano-scale particles are formed, the size is about 100nm and is uniform, and the surface of the cerium oxide film in a microscopic form fluctuates by 22.17nm.
FIG. 4 is an X-ray photoelectron spectroscopy (XPS) survey of the nano-cerium oxide memristor thin film prepared in example 3 of the present invention, in which six peaks appear, and the peaks respectively correspond to Ce3d 5/2 And Ce3d 3/2 Spin orbit fracture. Indicates that Ce exists in the cerium oxide memristor film at the same time 3+ And Ce 4+ Two valence states.
FIG. 5 is a Ce3d spectrum of an X-ray photoelectron spectroscopy (XPS) of a cerium oxide memristor thin film prepared in example 3 of the present invention, in which the peak is formed by fitting three peaks, the peak No. 1 is lattice oxygen, i.e., the binding energy of Ce-O bonds, and the peak No. 2 is oxygen adsorbed on the surface of the thin film, i.e., -OH, H 2 O, etc., corresponding to peak No. 3Is an oxygen vacancy, and therefore, the doped titanium oxide film respectively contains Ce3d and O1s in the detection depth range of the X-ray photoelectron spectroscopy.
The cerium oxide memristor thin film prepared in example 3 was subjected to ultraviolet light irradiation process treatment using a surface contact angle measuring instrument, and surface contact angle studies were performed on the surfaces before and after ultraviolet light irradiation, respectively. Fig. 6 is a graph showing the result of a contact angle test of the cerium oxide thin film prepared in example 3 before irradiation of ultraviolet light, using deionized water as a test liquid, and having a contact angle of 67.7 °. Because the cerium oxide film has better photocatalysis, the technical scheme of the invention adopts an ultraviolet light irradiation method to improve the oxygen vacancy defect on the surface of the cerium oxide film, thereby improving the resistance change performance of the cerium oxide film. The cerium oxide film prepared in example 3 was used for high-power ultraviolet LED light source irradiation with a wavelength of 365nm, a power of 30W, an irradiation distance of 2 cm, and an irradiation time of 2 hours. Fig. 7 is a contact angle test result graph of the cerium oxide film prepared in example 3 after irradiation, the adopted test liquid is deionized water, the contact angle is 13.5 °, and obviously the contact angle of the surface of the cerium oxide memristor film after irradiation by an ultraviolet light source is obviously reduced.
An electrical tester was used to test the ceria memristor thin film device made of the ceria memristor thin film in example 3, and fig. 8 is an I-V curve of the ceria memristor thin film device. The heterojunction has complete bipolar resistance transition characteristics. It can be seen that the cerium oxide memristor thin-film device has a condition that the resistance is obviously suddenly changed when the voltage is in the range of 2-2.5V, however, the sudden change condition is not very stable, the cerium oxide memristor thin-film device is changed from a high resistance state to a low resistance state, namely, a SET process occurs, and the low resistance state is stably maintained in subsequent tests. When reverse voltage is applied, the resistance is changed from a low resistance state to a high resistance state when the voltage is-1.8V, namely, a RESET RESET process occurs, and the performance of the high resistance state is kept in subsequent tests. An electricity tester is used for testing a cerium oxide memristor thin-film device made of the cerium oxide memristor thin film in the embodiment 3, fig. 9 is an I-V curve of the cerium oxide memristor thin film obtained after ultraviolet light source irradiation, the heterojunction has complete bipolar resistance transition characteristics, the condition that the resistance of the cerium oxide memristor thin-film device is obviously suddenly changed when the voltage is 0.91V can be seen, the cerium oxide memristor thin-film device is changed from a high resistance state to a low resistance state, namely an SET process occurs, and the low resistance state is stably maintained in subsequent tests; when reverse voltage is applied, the resistance is changed from a low resistance state to a high resistance state when the voltage is-1.00V, namely, a RESET RESET process occurs, and the performance of the high resistance state is kept in subsequent tests.
After the cerium oxide memristor film is irradiated by an ultraviolet light source, the resistance conversion performance is obviously improved, the SET voltage and the RESET voltage are obviously reduced, and the stability of a cerium oxide memristor film device made of the cerium oxide memristor film is better. The method is mainly characterized in that more oxygen vacancies are generated on the surface of the cerium oxide memristor film in the irradiation process, so that the migration probability of the oxygen vacancies is increased; the oxygen vacancy has small resistance along with the movement of the electric field direction, so that the SET voltage and the RESET voltage of the device are both small, low power consumption is realized, and the good resistance transition characteristic is shown.
Claims (4)
1. A preparation method of a cerium oxide memristor film is characterized by comprising the following steps:
step 1, preparing cerium oxide sol; stirring the obtained cerium oxide peptization at room temperature for 6h to 8h, and then aging for 24h;
step 2, adopting a dipping-pulling method, taking cerium oxide sol as a raw material, pulling the cerium oxide gel film on an ITO substrate at room temperature by using a pulling machine, drying the cerium oxide gel film at room temperature, then carrying out heat treatment at 300-700 ℃, and cooling to obtain the cerium oxide film; the preparation of the cerium oxide sol specifically comprises the following steps: taking absolute ethyl alcohol as a solvent, cerium nitrate as a precursor and benzoylacetone as a chemical modifier, mixing the cerium nitrate, the benzoylacetone and the absolute ethyl alcohol according to a molar ratio of 1;
and 3, irradiating the cerium oxide film obtained in the step 2 by using ultraviolet rays to obtain the cerium oxide memristor film.
2. The method for preparing the cerium oxide memristor thin film according to claim 1, wherein in the step 2, the heat treatment is performed under an oxygen atmosphere.
3. The method for preparing the cerium oxide memristor thin film according to claim 1, wherein in the step 2, the time of the heat treatment is 20min.
4. The method for preparing the cerium oxide memristor film according to claim 1, wherein in the step 3, the cerium oxide film is irradiated by using an ultraviolet LED light source with power of 30W, the wavelength of the ultraviolet LED light source is 365nm, the irradiation distance is 2 cm, and the irradiation time is 2h.
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