CN114974341A - Four-state memory based on barium-doped bismuth ferrite system film and preparation method thereof - Google Patents

Four-state memory based on barium-doped bismuth ferrite system film and preparation method thereof Download PDF

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CN114974341A
CN114974341A CN202210618114.7A CN202210618114A CN114974341A CN 114974341 A CN114974341 A CN 114974341A CN 202210618114 A CN202210618114 A CN 202210618114A CN 114974341 A CN114974341 A CN 114974341A
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陈水源
陈阳
霍冠忠
苏超
徐宏宇
叶晴莹
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Abstract

The invention discloses a four-state memory based on a barium-doped bismuth ferrite system film and a preparation method thereof. Firstly, preparing Bi by adopting a sol-gel method 1‑x Ba x FeO 3 A precursor of the material, then adding Bi 1‑ x Ba x FeO 3 Powdering the material precursor and preparing the material into a block target material, and then depositing the block target material on an FTO substrate by a pulse laser deposition method to prepare Bi 1‑x Ba x FeO 3 System of thin film, finally in Bi 1‑x Ba x FeO 3 And plating an electrode on the system film to manufacture a four-state storage unit. The invention prepares Bi by a sol-gel method 1‑x Ba x FeO 3 Precursor of a material such that Bi 1‑x Ba x FeO 3 The component materials are mixedThe mixture is relatively uniform; the barium-doped bismuth ferrite system film deposited by the pulse laser deposition method has the characteristics of good quality, high uniformity, stable material components and the like, effectively ensures the consistency of the components of the obtained film and the target material, and Bi 1‑x Ba x FeO 3 The system thin film four-state memory cell can observe obvious ferromagnetism and ferroelectricity, and the coexistence of the two ferroelectricity enables the four-state memory cell to have four polarization states (+/-P, +/-M) so as to realize nonvolatile four-state memory.

Description

Four-state memory based on barium-doped bismuth ferrite system film and preparation method thereof
Technical Field
The invention belongs to the field of memories, particularly relates to a four-state memory based on a barium-doped bismuth ferrite system film and a preparation method thereof, and particularly relates to a four-state memory based on a Bi 1-x Ba x FeO 3 A method for preparing a four-state memory unit of a system film (wherein x is 0-0.25).
Background
With the continuous development of modern process and computer architecture, the demand for higher integration, higher storage density and higher reliability of memory devices is increasing. Most currently studied are single two-state memories (storing both states 0, 1), and to increase storage density, multi-state memories have emerged that are capable of storing multiple information states in a single memory cell. The implementation of multi-state memories requires that the memory material have multiple different physical states at the same time, and there is therefore a pressing need to find materials that have multiple physical states at room temperature. BiFeO 3 Is a few single-phase multiferroic materials with a plurality of different physical states at room temperature, and the doping of barium can improve the single-phase multiferroic material BiFeO 3 Is ferromagnetic, therefore Bi 1-x Ba x FeO 3 The preparation method of the system film is the basis of the research of the single-phase multiferroic material for the multi-state memory.
Disclosure of Invention
The invention aims to improve the storage density of a memory and overcome the defect of the existing Bi 1-x Ba x FeO 3 The defects of low phase forming rate and insufficient film compactness of a system film preparation process are provided 1-x Ba x FeO 3 A four-state memory of a system film and a preparation method thereof, wherein x is 0-0.25 (0, 0.05, 0.10, 0.15, 0.20, 0.25).
The technical scheme adopted by the invention is as follows:
the invention provides a barium-doped bismuth ferrite system film-based four-state memory and a preparation method thereof, which are used for preparing a film based on Bi 1-x Ba x FeO 3 A four-state memory cell of the system thin film, wherein x is 0, 0.05, 0.10, 0.15, 0.20, 0.25. Firstly, preparing Bi by adopting a sol-gel method 1-x Ba x FeO 3 A precursor of the material, then adding Bi 1-x Ba x FeO 3 Powdering the material precursor and preparing the material into a block target material, and then depositing the block target material on an FTO substrate by a pulse laser deposition method to prepare Bi 1-x Ba x FeO 3 System of thin film, finally in Bi 1-x Ba x FeO 3 And plating an electrode on the system film to form a four-state memory cell. The electrodes are made of a material having good conductivity such as platinum, gold, or silver.
Wherein Bi 1-x Ba x FeO 3 The preparation method of the system film comprises the following steps:
step 1: preparation of Bi by sol-gel method 1-x Ba x FeO 3 A precursor of the material is prepared,
step 2: adding Bi 1-x Ba x FeO 3 The material precursor is powdered and made into a block target material,
and step 3: depositing the bulk target material on an FTO substrate by a pulse laser deposition method to obtain Bi 1-x Ba x FeO 3 A film.
Further, the preparation of Bi by a sol-gel method 1-x Ba x FeO 3 The material used in the material precursor comprises a bismuth source material, a barium source material, an iron source material, a solvent A, a solvent B and a complexing agent, wherein the bismuth source material, the barium source material, the iron source material, the solvent A, the solvent B and the complexing agent respectively correspond to bismuth nitrate, barium nitrate, ferric nitrate, deionized water, ethylene glycol and citric acid.
Further, in the step 1Preparation of Bi by sol-gel method 1-x Ba x FeO 3 The material precursor specifically comprises the following steps:
1. accurately weighing bismuth nitrate, barium nitrate and ferric nitrate according to the mass ratio of cationic substances in the chemical formula of 1-x: x:1, sequentially adding a proper amount of ethylene glycol, and stirring until the materials are completely dissolved to obtain a reddish brown transparent solution A;
2. mixing citric acid with
Figure BDA0003674086450000021
(wherein m is mass, n is amount of substance, x is 0, 0.05, 0.10, 0.15, 0.20, 0.25, amount ratio of citric acid to metal cation is 1.2: 1) accurately weighing, adding appropriate amount of deionized water, and stirring to completely dissolve to obtain transparent solution B;
3. slowly adding the solution A into the solution B (the sequence can not be changed, so that the citric acid solution is in an excessive state in the system in the whole operation process), fully and uniformly mixing to obtain a solution C, and placing the solution C into a water bath kettle at the temperature of 80-85 ℃ for water bath stirring to make the solution C viscous to obtain a red brown wet gel;
4. drying the wet gel in a 120 ℃ blast drying oven for 2-3 days to obtain loose and porous reddish brown xerogel, removing organic matters at 400 ℃ to obtain Bi 1-x Ba x FeO 3 Material precursor powder a.
Furthermore, the dosage of the glycol is determined according to the dissolution of the bismuth source material, the barium source material and the iron source material, but the quantitative concentration of the bismuth nitrate substance cannot be lower than 1mol/L, namely c Bismuth nitrate ≥1mol/L。
Furthermore, the dosage of the deionized water is determined according to the dissolution condition of the complexing agent.
Further, Bi 1-x Ba x FeO 3 The method comprises the following steps of calcining material precursor powder A at a high temperature to prepare a block target material:
1. the dried Bi was placed in an agate mortar 1-x Ba x FeO 3 Grinding the material precursor powder A into fine powder B;
2. pressing the powder B on a tablet press by using a metal die to form a cylindrical target material with the diameter of 30mm and the thickness of 2-3 mm, wherein the pressure intensity is 25 MPa;
3. placing the cylindrical target material in a muffle furnace at 625 ℃ for rapid annealing for 10min to obtain Bi 1-x Ba x FeO 3 A bulk target.
Further, Bi is deposited by pulse laser deposition 1-x Ba x FeO 3 The deposition of the bulk target on the FTO substrate specifically comprises the following steps:
1. the Bi is added 1-x Ba x FeO 3 Respectively placing the block target material and the FTO substrate at proper positions of a target position and a substrate disc, fixing, closing the vacuum cavity, and sequentially starting the mechanical pump and the molecular pump to vacuumize the vacuum cavity;
2. when the vacuum degree of the vacuum chamber reaches 10 -4 When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 9 Pa;
3. setting the temperature of an FTO substrate in a vacuum chamber to be 620-630 ℃, and covering the FTO substrate by using a baffle;
4. setting the voltage of a pulse laser to be 19-20 kV, setting the frequency to be 1Hz, and performing pre-striking for a time determined according to the actual condition of the surface of the target material;
5. setting the energy of a pulse laser to be 340-360 mJ and the frequency to be 4Hz, removing the baffle, starting deposition, slowly introducing air to atmospheric pressure after the deposition is finished, preserving the heat in situ for 1-1.2 h, and cooling to room temperature to prepare Bi 1-x Ba x FeO 3 A film.
Further, Bi is produced 1-x Ba x FeO 3 The deposition time of the film is adjusted according to the thickness of the film to be prepared, and the growth rate of the film is about 95-105nm/h (different preparation environments are changed).
Furthermore, the FTO substrate belongs to conductive glass, the softening temperature is not lower than 700 ℃, and the reduction rate of the conductivity of the conductive layer is not higher than 50% at the temperature of 625 +/-10 ℃ and in a normal temperature state.
The invention adopts the technical scheme that the barium ion part is usedThe bismuth ion in the bismuth ferrite is replaced and the Bi is adjusted 1-x Ba x FeO 3 Preparation of Bi from the ratio of metal cations in the material 1-x Ba x FeO 3 The system thin film (wherein x is 0, 0.05, 0.10, 0.15, 0.20, 0.25), utilize ferroelectric comprehensive test system, comprehensive measurement system of Physical Property (PPMS) to carry on the ferroelectric, ferromagnetic performance test to the said memory cell, find it has good ferroelectricity, ferromagnetism, two kinds of ferroelectricity coexist make it have four polarization states (± P, ± M), to realize the four-state memory of the non-volatility; because the sol-gel method can realize uniform doping on the molecular level and the required temperature is low, the system powder prepared by the sol-gel method has small grain diameter and high uniformity; finally depositing by a pulse laser deposition method to obtain Bi 1-x Ba x FeO 3 The film obtained by the method has high deposition rate, short test period and uniform prepared film. The method of the invention can prepare a Bi-based material 1-x Ba x FeO 3 Storage unit for four-state storage of system film, prepared Bi 1-x Ba x FeO 3 The system film has high phase purity, can accurately control the stoichiometry, and has good ferroelectricity and ferromagnetism.
Drawings
The invention is described in further detail below with reference to the accompanying drawings and the detailed description;
FIG. 1 shows that the present invention is based on Bi 1-x Ba x FeO 3 A flow diagram of a preparation method of a four-state storage unit of a system film;
FIG. 2 shows Bi-based compounds obtained by the present method 1-x Ba x FeO 3 A system thin film material storage unit and an XRD (X-ray diffraction) pattern thereof;
FIG. 3 shows Bi-based compounds obtained by the present method 1-x Ba x FeO 3 A hysteresis loop of the system film material storage unit at room temperature;
FIG. 4 shows Bi-based films obtained by the present method 1-x Ba x FeO 3 The system thin film material memory cell has a hysteresis loop at room temperature.
Detailed Description
As shown in one of fig. 1 to 4, the invention discloses a four-state memory based on a barium-doped bismuth ferrite system film and a preparation method thereof, which are used for preparing a storage unit of the four-state memory, and the preparation method comprises the following steps:
1) preparation of Bi by sol-gel method 1-x Ba x FeO 3 Material precursor
The materials used in the step comprise a bismuth source material, a barium source material, an iron source material, a solvent A, a solvent B and a complexing agent, wherein the bismuth source material, the barium source material, the iron source material, the solvent A, the solvent B and the complexing agent respectively correspond to bismuth nitrate, barium nitrate, ferric nitrate, deionized water, ethylene glycol and citric acid. The specific steps are as follows:
1-1) accurately weighing bismuth nitrate, barium nitrate and ferric nitrate according to the mass ratio of cationic substances in the chemical formula of 1-x: x:1, sequentially adding a proper amount of ethylene glycol, and stirring until the materials are completely dissolved to obtain a red brown transparent solution A;
1-2) mixing citric acid
Figure BDA0003674086450000041
(wherein m is mass, n is amount of substance, x is 0, 0.05, 0.10, 0.15, 0.20, 0.25, amount ratio of citric acid to metal cation is 1.2: 1) accurately weighing, adding appropriate amount of deionized water, and stirring to completely dissolve to obtain transparent solution B;
1-3) slowly adding the solution A into the solution B (the sequence can not be changed, so that the whole operation process keeps the citric acid solution in an excessive state in the system), fully and uniformly mixing to obtain a solution C, and placing the solution C into a water bath kettle at 80 ℃ for water bath stirring to make the solution C viscous to obtain a red brown wet gel;
1-4) placing the wet gel in a 120 ℃ blast drying oven for drying for 2-3 days to obtain loose and porous red brown xerogel, and removing organic matters at 400 ℃ to obtain Bi 1-x Ba x FeO 3 Material precursor powder a.
Wherein the dosage of the ethylene glycol is determined according to the dissolution conditions of the bismuth source material, the barium source material and the iron source material,but the mass concentration of the substance of bismuth nitrate cannot be less than 1mol/L, i.e. c Bismuth nitrate Not less than 1 mol/L. The deionized water is used according to the dissolving condition of the complexing agent.
2) Adding Bi 1-x Ba x FeO 3 The material precursor is powdered and made into a block target material, which comprises the following specific steps:
2-1) drying the Bi with agate mortar 1-x Ba x FeO 3 Grinding the material precursor powder A into fine powder B;
2-2) pressing the powder B into a cylindrical target material with the diameter of 30mm and the thickness of 2-3 mm on a tablet press by using a metal die, wherein the pressure intensity is 25 MPa;
2-3) placing the cylindrical target material in a muffle furnace at 625 ℃ for rapid annealing for 10min to obtain Bi 1-x Ba x FeO 3 A bulk target.
3) Depositing the bulk target material on an FTO substrate by a pulse laser deposition method to obtain Bi 1-x Ba x FeO 3 The film is specifically as follows:
3-1) adding Bi 1-x Ba x FeO 3 Respectively placing the block target and the FTO substrate at proper positions of a target position and a substrate disc, fixing, closing the vacuum cavity, and sequentially starting the mechanical pump and the molecular pump to vacuumize the vacuum cavity;
the FTO substrate belongs to conductive glass, the softening temperature is not lower than 700 ℃, and the reduction rate of the conductivity of the conductive layer is not higher than 50% at the temperature of about 625 +/-10 ℃ and in a normal temperature state;
3-2) when the vacuum degree of the vacuum chamber reaches 10 -4 When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 9 Pa;
3-3) setting the temperature of an FTO substrate in a vacuum chamber to be 625 ℃, wherein the FTO substrate is covered by a baffle;
3-4) setting the voltage of the pulse laser to be 19kV, setting the frequency to be 1Hz, and performing pre-striking for a time determined according to the actual condition of the surface of the target material;
3-5) setting the energy of the pulse laser at 350mJ and the frequency at 4Hz, removing the baffle plate, starting deposition, slowly introducing air to atmospheric pressure after the deposition is finished,preserving heat for 1h in situ, cooling to room temperature to obtain Bi 1-x Ba x FeO 3 A film.
Wherein Bi is produced 1-x Ba x FeO 3 The deposition time of the film is adjusted according to the thickness of the film to be prepared, and the growth rate of the film is about 95-105nm/h (different preparation environments are changed).
4) In Bi 1-x Ba x FeO 3 And plating an electrode on the system film to manufacture a four-state storage unit.

Claims (10)

1. Based on Bi 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: firstly, preparing Bi by adopting a sol-gel method 1-x Ba x FeO 3 A precursor of the material, then adding Bi 1-x Ba x FeO 3 Powdering the material precursor and preparing the material into a block target material, and then depositing the block target material on an FTO substrate by a pulse laser deposition method to prepare Bi 1-x Ba x FeO 3 System of thin film, finally in Bi 1-x Ba x FeO 3 And plating an electrode on the system film to manufacture a four-state storage unit.
2. The Bi-based material of claim 1 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: the material used for the electrodes is platinum, gold or silver.
3. The Bi-based material of claim 1 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: x is 0 to 0.25.
4. The Bi-based material of claim 3 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: x is 0, 0.05, 0.10, 0.15, 0.20, 0.25.
5. According toA Bi-based material according to claim 1 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: preparation of Bi by sol-gel method 1-x Ba x FeO 3 The material used in the material precursor comprises a bismuth source material, a barium source material, an iron source material, a solvent A, a solvent B and a complexing agent, wherein the bismuth source material, the barium source material, the iron source material, the solvent A, the solvent B and the complexing agent respectively correspond to bismuth nitrate, barium nitrate, ferric nitrate, deionized water, ethylene glycol and citric acid.
6. The Bi-based material of claim 5 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: preparation of Bi by sol-gel method 1-x Ba x FeO 3 The material precursor specifically comprises the following steps:
1) accurately weighing bismuth nitrate, barium nitrate and ferric nitrate according to the mass ratio of cationic substances in the chemical formula of 1-x: x:1, adding a proper amount of ethylene glycol, and stirring until the materials are completely dissolved to obtain a solution A;
2) mixing citric acid with
Figure FDA0003674086440000011
Accurately weighing, adding deionized water, and stirring until the deionized water is completely dissolved to obtain a solution B;
3) slowly adding the solution A into the solution B, fully and uniformly mixing to obtain a solution C, and putting the solution C into a water bath kettle at the temperature of 80-85 ℃ for water bath stirring to obtain wet gel;
4) drying the wet gel in a blast drying oven at 120 ℃ to obtain dry gel, removing organic matters to obtain Bi 1- x Ba x FeO 3 Material precursor powder a.
7. The Bi-based material of claim 1 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: adding Bi 1-x Ba x FeO 3 Material precursor is powdered and made into block target materialThe method specifically comprises the following steps:
1) adding Bi 1-x Ba x FeO 3 Grinding the material precursor powder A into fine powder B;
2) pressing the powder B into a cylindrical target material on a tablet press by using a metal die;
3) placing the cylindrical target material in a muffle furnace for rapid annealing to obtain Bi 1-x Ba x FeO 3 A bulk target.
8. The Bi-based material of claim 1 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: depositing a bulk target material on an FTO substrate by a pulse laser deposition method to prepare Bi 1-x Ba x FeO 3 The system film specifically comprises the following steps:
1) adding Bi 1-x Ba x FeO 3 Respectively placing the block target material and the FTO substrate at proper positions of a target position and a substrate disc, fixing, closing the vacuum cavity, and sequentially starting the mechanical pump and the molecular pump to vacuumize the vacuum cavity;
2) when the vacuum degree of the vacuum chamber reaches 10 -4 When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 9 Pa;
3) setting the temperature of an FTO substrate in a vacuum chamber to be 620-630 ℃, and covering the FTO substrate by using a baffle;
4) setting the voltage of a pulse laser to be 19-20 kV, setting the frequency to be 1Hz, and performing pre-striking for a time determined according to the actual condition of the surface of the target material;
5) setting the energy of a pulse laser to be 350-360 mJ and the frequency to be 4Hz, removing a baffle, starting deposition, slowly introducing air to atmospheric pressure after the deposition is finished, preserving the temperature in situ, and cooling to room temperature to prepare Bi 1-x Ba x FeO 3 And (5) a system film.
9. The Bi-based material of claim 8 1-x Ba x FeO 3 The preparation method of the four-state memory of the system film is characterized by comprising the following steps: the FTO substrate isThe softening temperature of the conductive glass is not lower than 700 ℃, and the reduction rate of the conductivity of the conductive layer is not higher than 50% at the temperature of about 625 +/-10 ℃ and under the normal temperature state.
10. Bi-based material obtained by the production method according to any one of claims 1 to 9 1-x Ba x FeO 3 A thin film four-state memory.
CN202210618114.7A 2022-06-01 2022-06-01 Four-state memory based on barium-doped bismuth ferrite system film and preparation method thereof Pending CN114974341A (en)

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