CN109192855B - BEFMO/ZnO composite heterojunction with resistance switching effect and preparation method thereof - Google Patents

BEFMO/ZnO composite heterojunction with resistance switching effect and preparation method thereof Download PDF

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CN109192855B
CN109192855B CN201811089163.6A CN201811089163A CN109192855B CN 109192855 B CN109192855 B CN 109192855B CN 201811089163 A CN201811089163 A CN 201811089163A CN 109192855 B CN109192855 B CN 109192855B
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谈国强
刘云
郭美佑
薛敏涛
任慧君
夏傲
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Shaanxi University of Science and Technology
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Abstract

The invention provides a device with electricityThe BEFMO/ZnO composite heterojunction with the switch-resistant effect and the preparation method thereof comprise a lower layer film and an upper layer film which are compounded together; the chemical formula of the lower layer film is ZnO, and the lower layer film has a hexagonal wurtzite structure; the upper film has a chemical formula of Bi0.9Er0.1Fe0.99Mn0.01O3A twisted rhombohedral perovskite structure, space group R3 c. The preparation method comprises the following steps: preparing ZnO precursor solution; spin-coating ZnO precursor solution on an FTO/Glass substrate, baking, and annealing to obtain a crystalline ZnO film; preparing BEFMO precursor solution, spinning and coating the BEFMO precursor solution on a crystalline ZnO film, baking and annealing to obtain the BEFMO/ZnO composite heterojunction. The BEFMO/ZnO composite heterojunction provided by the invention shows a good resistance switching effect.

Description

BEFMO/ZnO composite heterojunction with resistance switching effect and preparation method thereof
Technical Field
The invention belongs to the field of functional materials, and relates to a BEFMO/ZnO composite heterojunction with a resistance switching effect and a preparation method thereof.
Background
Multiferroic bismuth ferrite BiFeO3The (BFO) material is the only multiferroic material which has ferroelectricity and ferromagnetism at room temperature at present, has excellent ferroelectric and magnetoelectric coupling characteristics, and has wide application prospect in the fields of novel non-volatile memory devices, multifunctional sensing devices, spinning electronic devices, photovoltaic devices and the like. The bismuth ferrite-based resistive random access memory combines the advantages of a ferroelectric memory and a resistive random access memory, realizes high and low resistance state switching by regulating interface potential barrier and carrier transport characteristics through the reversal of ferroelectric polarization, and shows unique advantages instead of regulating resistive behavior through defects.
The BFO has the advantage of high-speed reading and writing because the polarization reversal is fast under the external electric field. However, BiFeO3The bismuth element in the film is easy to volatilize and part of Fe3+To Fe2+Causes more oxygen vacancies to be generated in the thin film, resulting in BiFeO3The film has serious electric leakage phenomenon and larger coercive field, is difficult to polarize and is difficult to obtain a higher remanent polarization value, so the resistance change mechanism is often different from an ideal resistance change structure regulated by ferroelectric polarization, and the resistance change characteristic of the actual bismuth ferrite is limited.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the BEFMO/ZnO composite heterojunction with the resistance switching effect and the preparation method thereof, and the prepared BEFMO/ZnO composite heterojunction has good ferroelectric property and good resistance switching effect.
The invention is realized by the following technical scheme:
a BEFMO/ZnO composite heterojunction with resistance switching effect comprises a lower layer film and an upper layer film which are compounded together; the chemical formula of the lower layer film is ZnO, and the lower layer film has a hexagonal wurtzite structure; the upper film has a chemical formula of Bi0.9Er0.1Fe0.99Mn0.01O3A twisted rhombohedral perovskite structure, space group R3 c.
Preferably, the switching ratio R of the high and low resistance statesHRS/RLRSIs 4.62 to 74.76.
Preferably, the remanent polarization value P is 40-50V under the magnetic field of 1kHz and the voltager27 to 40 mu C/cm2Rectangular degree of hysteresis loop Rsq0.99-1.05, and the coercive field strength is 384-466 kV/cm.
The preparation method of the BEFMO/ZnO composite heterojunction with the resistance switching effect is characterized by comprising the following steps of:
step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring to obtain a ZnO precursor solution;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 280-300 ℃ after glue spreading to obtain a dry film, and annealing at 550-580 ℃ to obtain a crystalline ZnO film;
step 3, after the crystalline ZnO film is cooled, repeating the step 2 on the crystalline ZnO film to reach a preset thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O、Er(NO3)3·6H2O、Fe(NO3)3·9H2O、C4H6MnO4·4H2Dissolving O in the mixture of ethylene glycol monomethyl ether and acetic anhydride according to the molar ratio of 0.95:0.10:0.99:0.01, stirring uniformly,obtaining BEFMO precursor solution;
step 5, spin-coating BEFMO precursor solution on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 180-200 ℃ after glue homogenizing to obtain a dry film, and annealing at 530-550 ℃ to obtain the crystalline BEFMO film;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach a preset thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Preferably, the concentration of the metal ions in the ZnO precursor solution in the step 1 is 0.5-0.6 mol/L.
Preferably, the total concentration of metal ions in the BEFMO precursor solution in the step 4 is 0.2-0.3 mol/L.
Preferably, the volume ratio of ethylene glycol monomethyl ether to ethanolamine in the ZnO precursor solution is (30-32): 1; the volume ratio of ethylene glycol monomethyl ether to acetic anhydride in the BEFMO precursor liquid is (2.9-3.2): 1.
Preferably, the glue homogenizing rotation speed in the step 2 and the step 5 is 3800-4000 r/min, and the glue homogenizing time is 12-15 s.
Preferably, the baking time after the glue homogenizing in the step 2 is 15-20 min, and the baking time after the glue homogenizing in the step 5 is 5-10 min.
Preferably, the annealing time in the step 2 is 45-60 min, and the annealing time in the step 5 is 8-15 min.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the BEFMO/ZnO composite heterojunction, rare earth element Er and transition metal element Mn are selected for A, B bit co-doping of BFO, the doping can effectively reduce the content of oxygen vacancies and defects, the leakage current density in the thin film is reduced, and therefore the ferroelectricity of the thin film is improved. ZnO belongs to a wide-bandgap direct band-gap semiconductor at normal temperature, the bandgap is about 3.37eV, and zinc oxide is used as a wide-range semiconductor material and has been applied to a Thin-film transistor (TFT) as a channel material. The ferroelectric film/semiconductor heterojunction is constructed by the BEFMO composite ZnO semiconductor, the ZnO film belongs to an N-type semiconductor, the transport characteristic of an N-type carrier is reflected, and a p-N-like junction can be formed by the ZnO film and a BFO with p-type conduction. The polarization direction and the polarization strength of the ferroelectric layer are regulated and controlled by controlling the external voltage, so that carriers at an interface in the semiconductor layer are depleted or accumulated due to mutual coupling between the ferroelectric layer and the semiconductor layer, the carriers (defects and a large amount of space charges) can generate an intermediate transition layer at the interface of the composite film, and the heterojunction generates different local conductance states, so that the heterojunction can be switched between high and low resistance states, more obvious resistance change behavior is formed, and a good resistance switching effect is shown. In addition, the requirement of diversification effect in practical application, the application of single BFO is limited. In order to improve the resistance change property of bismuth ferrite, the bismuth ferrite film is subjected to oxide compounding, and the bismuth ferrite material shows enhanced resistance change property and mainly comes from enhanced ferroelectric property and resistance change mechanisms such as oxygen vacancy introduction and the like.
Further, the high-low resistance state switching ratio R under the positive electric fieldHRS/RLRSIs 4.62-74.76, which shows that the material has good resistance switching effect.
Furthermore, the BEFMO/ZnO composite heterojunction varies in a voltage range of 40-50V, and the remanent polarization value is 27-40 mu C/cm2The electric hysteresis loop has a rectangular degree of Rsq1.05, so that it has stable ferroelectricity with the change of the applied voltage.
The method for preparing the BFO and ZnO film has a plurality of methods at present, compared with other methods, the method has the advantages that the chemical process of the sol-gel method adopted by the invention is simpler, the cost of equipment and maintenance is lower, the uniform doping on the molecular level is easy to realize, and the thickness of the film can be effectively controlled. The BEFMO/ZnO composite heterojunction is prepared by the good composition of the ferroelectric layer and the semiconductor layer, and the prepared composite heterojunction is good in uniformity.
Drawings
FIG. 1 is an XRD pattern of a BEFMO/ZnO composite heterojunction prepared according to the present invention;
FIG. 2 is a leakage current diagram of a BFO/ZnO composite heterojunction and a BEFMO/ZnO composite heterojunction prepared by the present invention;
FIG. 3 is a graph of the ratio of high to low resistivity state change of BFO/ZnO composite heterojunction and BEFMO/ZnO composite heterojunction prepared by the present invention;
FIG. 4 is a hysteresis loop plot of a BEFMO/ZnO composite heterojunction prepared in accordance with the present invention;
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The BEFMO/ZnO composite heterojunction with the resistance switching effect is a double-layer film and comprises a lower layer film and an upper layer film which are compounded together, wherein the lower layer film is a ZnO crystalline film and has a hexagonal wurtzite structure; the upper film is Bi0.9Er0.1Fe0.99Mn0.01O3(BEFMO for short) crystalline film, distorted rhombohedral perovskite structure, space group R3 c.
The BEFMO/ZnO composite heterojunction with the resistance switching effect generates a Bi-Er-Mn-Zn-rich intermediate transition layer at the interface of the BEFMO/ZnO due to defects and a large amount of space charges, and has a high-low resistance state switching ratio R under a positive electric fieldHRS/RLRSThe composite heterojunction has a resistance switching effect of 4.62-74.76.
Under the voltage of 40-50V, the remanent polarization value P of the BEFMO/ZnO composite heterojunctionr27 to 40 mu C/cm2Rectangular degree of hysteresis loop RsqThe coercive field strength is 384-466 kV/cm, and the heterojunction has good ferroelectricity.
The preparation method of the BEFMO/ZnO composite heterojunction comprises the following steps:
step 1: c is to be4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring to obtain a ZnO precursor solution;
step 2: spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 280-300 ℃ after spin-coating to obtain a dry film, and annealing at 550-580 ℃ to obtain a crystalline ZnO film;
and step 3: after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
and 4, step 4: adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O、C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring to obtain BEFMO precursor solution;
and 5: spin-coating BEFMO precursor solution on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 180-200 ℃ after glue spreading to obtain a dry film, and annealing at 530-550 ℃ to obtain the crystalline BEFMO film;
step 6: and (5) after the crystalline BEFMO film is naturally cooled, repeating the step (5) on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
The total concentration of metal ions in the ZnO precursor solution in the step 1 is 0.5-0.6 mol/L.
The total concentration of metal ions in the BEFMO precursor solution in the step 4 is 0.2-0.3 mol/L.
The volume ratio of ethylene glycol monomethyl ether to ethanolamine in the ZnO precursor solution is (30-32) to 1; the volume ratio of ethylene glycol monomethyl ether to acetic anhydride in the BEFMO precursor liquid is (2.9-3.2): 1; the time for uniform stirring in the step 1 is 1.5-2 h.
Cleaning the FTO/glass substrate before the step 2, then irradiating under ultraviolet light, and spin-coating ZnO precursor solution; and 5, before the step, carrying out ultraviolet irradiation treatment on the ZnO crystalline film, and then spin-coating BEFMO precursor solution.
The glue homogenizing rotating speed in the step 2 and the step 5 is 3800-4000 r/min, and the glue homogenizing time is 12-15 s.
The baking time after the glue homogenizing in the step 2 and the step 5 is 15-20 min and 5-10 min respectively.
The annealing time in the step 2 is 45-60 min, and the annealing time in the step 5 is 8-15 min.
The number of layers of the crystalline ZnO film is 5-8, and the number of layers of the crystalline BEFMO film is 8-13.
Specific examples are as follows.
Example 1
Step 1, mixingC4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.5mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 300 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 550 ℃ for 60min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.3mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 200 ℃ for 8min after glue homogenizing to obtain a dry film, and annealing at 550 ℃ for 10min to obtain the crystalline BEFMO film;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 2
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.5mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating the ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 300 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 550 ℃ for 60min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.3mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 200 ℃ for 8min after glue homogenizing to obtain a dry film, and annealing at 530 ℃ for 15min to obtain the crystalline BEFMO film;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 3
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.5mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 280 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 560 ℃ for 60min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.3mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 200 ℃ for 8min after glue homogenizing to obtain a dry film, and annealing at 550 ℃ for 10min to obtain the crystalline BEFMO film;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 4
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.5mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 300 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 550 ℃ for 60min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.2mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 180 ℃ for 8min after glue homogenizing to obtain a dry film, and annealing at 550 ℃ for 10min to obtain the crystalline BEFMO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 5
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.6mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 300 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 580 ℃ for 50min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.3mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 200 ℃ for 8min after glue homogenizing to obtain a dry film, and annealing at 550 ℃ for 10min to obtain the crystalline BEFMO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 6
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.6mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 31: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 280 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 560 ℃ for 60min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.3mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 2.9: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 200 ℃ for 8min after glue homogenizing to obtain a dry film, and annealing at 550 ℃ for 10min to obtain the crystalline BEFMO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 7
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.52mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 32: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 285 ℃ for 15min after glue spreading to obtain a dry film, and annealing at 555 ℃ for 45min to obtain a crystalline ZnO film; the spin rate of spin coating is 3800r/min, the spin coating time is 12 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.22mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 185 ℃ for 5min after glue homogenizing to obtain a dry film, and annealing at 535 ℃ for 8min to obtain the crystalline BEFMO film; the spin rate of the spin coating is 3800r/min, and the spin coating time is 12 s;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 8
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.54mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film for 16min at 290 ℃ after glue spreading to obtain a dry film, and annealing for 50min at 560 ℃ to obtain a crystalline ZnO film; the spin rate of the spin coating is 3900r/min, and the spin coating time is 13 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.24mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3.1: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 190 ℃ for 6min after glue homogenizing to obtain a dry film, and annealing at 540 ℃ for 10min to obtain the crystalline BEFMO film; the spin rate of the spin coating is 3900r/min, and the spin coating time is 13 s;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 9
Step 1, adding C4H6O4Zn·2H2Dissolving O in the mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain ZnO precursor solutionThe concentration of the medium metal ions is 0.56mol/L, and the volume ratio of ethylene glycol monomethyl ether to ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 295 ℃ for 18min after glue spreading to obtain a dry film, and annealing at 570 ℃ for 55min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 14 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.26mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3.2: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 195 ℃ for 9min after glue homogenizing to obtain a dry film, and annealing at 545 ℃ for 12min to obtain the crystalline BEFMO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 14 s;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Example 10
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.58mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 280 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 560 ℃ for 58min to obtain a crystalline ZnO film; the spin rate of the spin coating is 3800r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (excess of bismuth nitrate 5%), Er (NO)3)3·6H2O、Fe(NO3)3·9H2O and C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring for 2 hours to obtain BEFMO precursor solution, wherein the concentration of metal ions in the BEFMO precursor solution is 0.28mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BEFMO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet rays, respectively spin-coating the BEFMO precursor liquid on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 200 ℃ for 10min after glue homogenizing to obtain a dry film, and annealing at 550 ℃ for 14min to obtain the crystalline BEFMO film; the spin rate of the spin coating is 3800r/min, and the spin coating time is 15 s;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach the required thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
Comparative example 1
Step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring for 2h to obtain a ZnO precursor solution, wherein the concentration of metal ions in the ZnO precursor solution is 0.5mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the ethanolamine is 30: 1;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 300 ℃ for 20min after glue spreading to obtain a dry film, and annealing at 550 ℃ for 60min to obtain a crystalline ZnO film; the spin rate of the spin coating is 4000r/min, and the spin coating time is 15 s;
step 3, after the crystalline ZnO film is naturally cooled, repeating the step 2 on the crystalline ZnO film to reach the required thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O (bismuth nitrate excess 5%) and Fe (NO)3)3·9H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 1.05:1, and uniformly stirring for 2 hours to obtain a BFO precursor solution, wherein the concentration of metal ions in the BFO precursor solution is 0.3mol/L, and the volume ratio of the ethylene glycol monomethyl ether to the acetic anhydride is 3: 1;
step 5, standing the prepared BFO precursor liquid for 24h, irradiating a ZnO crystalline film for 40min by adopting ultraviolet light, respectively spin-coating the BFO precursor liquid on the crystalline ZnO film to obtain a BFO wet film, baking the wet film at 200 ℃ for 8min after glue spreading to obtain a dry film, and annealing at 550 ℃ for 10min to obtain the crystalline BFO film;
and 6, after the crystalline BFO film is naturally cooled, repeating the step 5 on the BFO film to reach the required thickness, and thus obtaining the BFO/ZnO composite heterojunction.
XRD is adopted to determine the phase composition structure of the BEFMO/ZnO composite film heterojunction; testing the leakage current characteristic of the BEFMO/ZnO composite film heterojunction by using Agilent B2900; and testing the ferroelectric property of the BEFMO/ZnO composite film heterojunction by using a TF2000 ferroelectric analyzer.
FIG. 1 is an XRD pattern of a BEFMO/ZnO composite heterojunction prepared according to example 1 of the present invention and a BFO/ZnO composite heterojunction prepared according to comparative example 1. As can be seen from the figure, the film had (101), (110), (021) and (122) crystal plane diffraction peaks corresponding to 2 θ of 22.5 °, 32 °, 39.5 ° and 57.5 °, and BiFeO3The standard card (JCPDS No.20-0169) is matched with a twisted rhombohedral perovskite structure and a space group R3c, the crystal face diffraction peaks (100), (002) and (101) of the film corresponding to 2 theta (31.5 degrees), 34.5 degrees and 36.5 degrees are matched with the ZnO standard card (JCPDS No.36-1415), the characteristic peak of ZnO is weak and is of a hexagonal wurtzite structure, and the crystallinity of the film after compounding is good.
FIGS. 2 and 3 are graphs of leakage current curves and high-low resistivity state ratio change curves of the BEFMO/ZnO composite film heterojunction prepared in example 1. Defects and a large amount of space charges at the interface of the BEFMO/ZnO composite heterojunction can cause a Bi-Er-Mn-Zn intermediate transition layer to be generated at the interface of the composite film, and the high-low resistance state on-off ratio under the positive electric field can be known from the graphs in FIGS. 2 and 3RHRS/RLRSAt 74.76, the composite film has a resistive switching effect. The BEFMO/ZnO composite heterojunction has larger on-off ratio RHRS/RLRS74.76, the J-E loop of the film becomes wider as Er and Mn ions are doped into the upper BFO layer, namely the resistance change effect is enhanced, which indicates that the interface effect between BEFMO and ZnO layer is enhanced.
FIG. 4 is a hysteresis loop diagram of the BEFMO/ZnO composite heterojunction prepared in example 1, and it can be seen from the hysteresis loop diagram measured at room temperature of 1kHz that the remanent polarization value P of the BEFMO/ZnO heterojunction is within 40-50Vr27 to 40 mu C/cm2Rectangular degree of hysteresis loop RsqThe coercive field strength is 384-446 kV/cm, and the film has good ferroelectricity and stable ferroelectricity along with the change of an external voltage.
The above-described details are further intended to describe the present invention in connection with the particular preferred embodiments thereof, and it is not intended to limit the invention to all or the only embodiments disclosed, and all equivalents and modifications which may occur to those skilled in the art upon reading the present specification are intended to be encompassed by the present claims.

Claims (9)

1. The preparation method of the BEFMO/ZnO composite heterojunction with the resistance switching effect is characterized in that the BEFMO/ZnO composite heterojunction with the resistance switching effect comprises a lower layer film and an upper layer film which are compounded together; the chemical formula of the lower layer film is ZnO, and the lower layer film has a hexagonal wurtzite structure; the upper film has a chemical formula of Bi0.9Er0.1Fe0.99Mn0.01O3A twisted rhombus perovskite structure, space group R3 c; high and low resistance state switching ratio RHRS/RLRS4.62 to 74.76;
the method comprises the following steps:
step 1, adding C4H6O4Zn·2H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and ethanolamine, and uniformly stirring to obtain a ZnO precursor solution;
step 2, spin-coating ZnO precursor solution on an FTO/Glass substrate by adopting a spin-coating method to obtain a ZnO wet film, baking the wet film at 280-300 ℃ after glue spreading to obtain a dry film, and annealing at 550-580 ℃ to obtain a crystalline ZnO film;
step 3, after the crystalline ZnO film is cooled, repeating the step 2 on the crystalline ZnO film to reach a preset thickness, and obtaining the ZnO film;
step 4, adding Bi (NO)3)3·5H2O、Er(NO3)3·6H2O、Fe(NO3)3·9H2O、C4H6MnO4·4H2Dissolving O in a mixed solution of ethylene glycol monomethyl ether and acetic anhydride according to a molar ratio of 0.95:0.10:0.99:0.01, and uniformly stirring to obtain BEFMO precursor solution;
step 5, spin-coating BEFMO precursor solution on the crystalline ZnO film to obtain a BEFMO wet film, baking the wet film at 180-200 ℃ after glue homogenizing to obtain a dry film, and annealing at 530-550 ℃ to obtain the crystalline BEFMO film;
and 6, after the crystalline BEFMO film is naturally cooled, repeating the step 5 on the BEFMO film to reach a preset thickness, and thus obtaining the BEFMO/ZnO composite heterojunction.
2. The method for preparing a BEFMO/ZnO composite heterojunction with resistive switching effect as claimed in claim 1, wherein the concentration of metal ions in the ZnO precursor solution in step 1 is 0.5-0.6 mol/L.
3. The method for preparing a BEFMO/ZnO composite heterojunction with resistive switching effect as claimed in claim 1, wherein the total concentration of metal ions in the BEFMO precursor solution in step 4 is 0.2-0.3 mol/L.
4. The method for preparing the BEFMO/ZnO composite heterojunction with the resistance switching effect according to claim 1, wherein the volume ratio of ethylene glycol methyl ether to ethanolamine in the ZnO precursor solution is (30-32): 1; the volume ratio of ethylene glycol monomethyl ether to acetic anhydride in the BEFMO precursor liquid is (2.9-3.2): 1.
5. The method for preparing the BEFMO/ZnO composite heterojunction with the resistance switching effect as claimed in claim 1, wherein the glue spreading rotation speed in the step 2 and the step 5 is 3800-4000 r/min, and the glue spreading time is 12-15 s.
6. The method for preparing the BEFMO/ZnO composite heterojunction with the resistance switching effect as claimed in claim 1, wherein the baking time after glue homogenizing in step 2 is 15-20 min, and the baking time after glue homogenizing in step 5 is 5-10 min.
7. The method for preparing the BEFMO/ZnO composite heterojunction with the resistance switching effect as claimed in claim 1, wherein the annealing time in the step 2 is 45-60 min, and the annealing time in the step 5 is 8-15 min.
8. The BEFMO/ZnO composite heterojunction with the resistance switching effect prepared by the method of claim 1.
9. The BEFMO/ZnO composite heterojunction with resistive switching effect as claimed in claim 8, wherein the remanent polarization P is between 40V and 50V at 1kHz magnetic fieldr27 to 40 mu C/cm2Rectangular degree of hysteresis loop Rsq0.99-1.05, and the coercive field strength is 384-466 kV/cm.
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