CN104103755A - Sodium bismuth titanate thin film system based resistance random access memory and preparation method thereof - Google Patents
Sodium bismuth titanate thin film system based resistance random access memory and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a sodium bismuth titanate thin film system based resistance random access memory and a preparation method thereof. The sodium bismuth titanate thin film system based resistance random access memory comprises a lower electrode, an upper electrode (104) and a sodium bismuth titanate thin film (103) which is arranged between the lower electrode and the upper electrode (104), wherein the sodium bismuth titanate thin film (103) and the upper electrode (104) form into a memory unit. The preparation method of the sodium bismuth titanate thin film system based resistance random access memory comprises generating a conducting oxidizing material layer through a magnetron sputtering method on a glass substrate or directly selecting a commercialized conducting glass substrate with a conducting oxidizing material coating; preparing the sodium bismuth titanate thin film on the conducting oxidizing material coating through a chemical solution deposition method; preparing the upper electrode on the sodium bismuth titanate thin film through a physical method and controlling the shape of the upper electrode through a mask. Compared with the prior art, the sodium bismuth titanate thin film system based resistance random access memory has the advantages of being good in resistance random access effect, simple in preparation method, low in cost and easy to prepare in a large scale and produce in an industrialized mode.
Description
Technical field
The present invention relates to the technical field of non-volatility memorizer, particularly relate to resistance random access memory based on bismuth-sodium titanate thin film system and preparation method thereof.
Background technology
The information technology of high speed development depend on large capacity, at a high speed, nonvolatile information storage technology.Nonvolatile information storage technology, because of its feature of still possessing information data when the power-off, has been widely used in the fields such as computer, automobile and modern industry.Flash memories (Flash Memory) is the non-volatility memorizer of current main flow, but it exists the problems such as operating voltage is high, speed is slow, endurance is poor.Yet the memory technology of the information technology inevitable requirement information of current develop rapidly improves constantly, therefore necessary exploitation low-power consumption, the non-volatility memorizer that speed is fast and the retention time is long.At present, ferroelectric random memory (FeRAM), magnetoresistive RAM (MRAM), resistance random access memory (RRAM) are main candidates.The primary structure of RRAM is " metal-recording medium-metal ".The Resistance states that can control RRAM by applying electric pulse is switched between high-impedance state (HRS) and low resistance state (LRS), thereby realizes writing and wiping of information.That RRAM has advantages of is simple in structure, operating voltage is low, switch speed is fast and the Information preservation time is long, is the study hotspot of current non-volatility memorizer.
The key technology of RRAM work is exactly electroresistance effect, under applying voltage pulse, can change the resistance states of the recording medium of RRAM, and it is switched between high-impedance state (HRS) and low resistance state (LRS).At present, oxide material is as composite perofskite type oxide (Pr
1-xca
xmnO
3, La
1-xca
xmnO
3, Pb (Zr
1-xti
x) O
3, LiNbO
3, SrTiO
3deng) and binary oxide (NiO, TiO
2, ZnO, ZrO
2, SiO
2, CuO etc.) be to study a class material the most widely.
We have also found obvious electroresistance effect in bismuth sodium titanate based thin film system recently.Ca-Ti ore type metatitanic acid bismuth sodium matrix system is a kind of novel oxygen conduction electrolyte.[M.Li, M.J.Pietrowski, R.A.De Souza, H.Zhang, I.M.Reaney, S.N.Cook, J.A.Kilner, D.C.Sinclair, A Family of Oxide Ion Conductors Based on the Ferroelectric Perovskite Na
0.5bi
0.5tiO
3nature Materials2014,13,31-35.] its feature is: 1. the special lattice structure of bismuth-sodium titanate is conducive to the diffusion of oxonium ion in system, 2. by acceptor impurity (as divalence magnesium) thus carry out the doping of titanium position or oxygen vacancy concentration that the means of bismuth position trace bismuth disappearance can increase system improves its oxygen conduction, the component proportion that 3. changes bismuth-sodium titanate system can change its oxygen conduction.In addition Ca-Ti ore type metatitanic acid bismuth sodium, as a kind of ferroelectric material, can regulate and control its ferroelectricity by extra electric field, and this just makes bismuth-sodium titanate system aspect FeRAM, RRAM, have potential using value.The electroresistance effect of finding in this novel oxygen ion conductor of bismuth-sodium titanate thin film system has been expanded the type of RRAM candidate material, for the exploitation of non-volatile resistance random asccess memory provides a kind of new thinking.
Summary of the invention
Object of the present invention is exactly to provide resistance random access memory based on bismuth-sodium titanate thin film system that a kind of preparation method is simple, cost is low and preparation method thereof in order to overcome the defect of above-mentioned prior art existence.
Object of the present invention can be achieved through the following technical solutions: a kind of resistance random access memory based on bismuth-sodium titanate thin film system, it is characterized in that, comprise bottom electrode, top electrode, and the bismuth-sodium titanate base film arranging between bottom electrode and top electrode, wherein bismuth-sodium titanate base film and top electrode form a memory cell.
Described bottom electrode is comprised of the conductive oxide coating of glass substrate and setting on it.
Described bottom electrode makes by the following method: on glass substrate, adopt the method growth conductive oxide coating of magnetron sputtering, described conductive oxide coating is the SnO of F-doping
2or In (FTO)
2o
3the SnO of-doping
2(ITO).
Described bottom electrode is the glass substrate that business-like surface is covered with FTO or ITO conductive oxide coating.
Described bismuth-sodium titanate base film is the bismuth-sodium titanate film of oxygen room doping, comprises the bismuth-sodium titanate film of titanium position magnesium doping, the bismuth-sodium titanate film of bismuth position trace bismuth disappearance, and magnesium doping in titanium position adds the bismuth-sodium titanate film of bismuth position trace bismuth disappearance.
Described power on very inert electrode or electrochemical activity electrode.
Described inert electrode is gold or platinum electrode, and described electrochemical activity electrode is titanium, aluminium, copper or silver electrode.
A kind of preparation method of the resistance random access memory based on bismuth-sodium titanate thin film system, it is characterized in that, the method comprises the following steps: adopt the method for magnetron sputtering on insulating glass substrate, grow FTO or ITO conductive oxide coating or directly select business-like surface to be covered with the conducting glass substrate of FTO or ITO conductive oxide coating as the bottom electrode of memory, adopt chemical solution deposition in conductive oxide coating, to prepare bismuth-sodium titanate base film, finally adopt Physical to prepare top electrode on bismuth-sodium titanate base film, by the shape of mask, control the shape of top electrode.
Described chemical solution deposition and the concrete steps of Physical are as follows:
Step 1: the precursor solution of preparing bismuth-sodium titanate base film:
Take EGME and glacial acetic acid as solvent, and acetylacetone,2,4-pentanedione is complexant, three is added in reactor, according to the component proportion of required bismuth-sodium titanate base film, by the solute of respective amount: positive four butyl esters of metatitanic acid, Mg (NO
3)
26H
2o, Bi (NO
3)
35H
2o and NaNO
3add successively respectively in above-mentioned reactor, in stirring at room to each solute, dissolve completely, obtain required precursor solution, finally use EGME to regulate the molar concentration of described precursor solution;
Step 2: adopt the method for spin-coating to prepare bismuth-sodium titanate base film:
Adopt spin coater that described precursor solution is evenly coated in and on bottom electrode, obtains uniform film layer, often obtain after a skim, gained rete is first carried out to preannealing within the scope of 250-350 ℃, then use rta technique, in 600-650 ℃ of temperature range, in oxygen atmosphere, be incubated 5min, repeat said process, the bismuth-sodium titanate base film that deposit thickness is 150nm~200nm;
Step 3: adopt Physical to deposit top electrode on the bismuth-sodium titanate base film of step 2 gained, control the shape of top electrode by mask, obtain the top electrode of this resistance random access memory.
The mol ratio of positive four butyl esters of described acetylacetone,2,4-pentanedione and metatitanic acid is 1: 1, described glacial acetic acid and the volume ratio of EGME 1: (1~10); The volume ratio of acetylacetone,2,4-pentanedione complexant and EGME is 1: (1~10);
It is (0.1~0.5) mol/L that described use EGME regulates the molar concentration of described precursor solution;
The rotating speed of described spin coater is the equal glue 10s of first 1000rpm, the evener glue 30s of 3000rpm.
The thickness of described bismuth-sodium titanate base film is 150nm~200nm.
Bismuth-sodium titanate sill is a kind of novel oxygen ion conductor.We have observed obvious resistor random-access storage effect in the bismuth-sodium titanate film of titanium position magnesium doping in the recent period, and the type of the candidate material of RRAM has been expanded in this discovery.Acceptor doping by titanium position forms flexible chemical bond in addition, be conducive to the diffusion of oxonium ion in bismuth-sodium titanate system, the oxygen conduction of raising system, in addition, by the component proportion of bismuth-sodium titanate system or doping ratio are regulated, can obtain the multiple component with different ionic conductivity, improve the diversity of the high and low resistance state of this resistance random access memory.As the component of bismuth-sodium titanate base film comprises Na
0.5bi
0.49tiO
2.985, Na
0.5bi
0.5ti
0.98mg
0.02o
2.98, Na
0.5bi
0.49ti
0.98mg
0.02o
2.965deng.
The present invention proposes resistance random access memory of a kind of bismuth-sodium titanate based oxygen ion conductor film based on novel and preparation method thereof, and provided the structure of this resistance random access memory.This resistance random access memory is under the scanning voltage of forward, and its on-off ratio is greater than 10
4, and when the low scanning voltage of+0.3V, the value of its maximum on-off ratio can reach 30159.
The storage principle of above-mentioned bismuth sodium titanate based film resistor random asccess memory is as shown in Figure 3: signal source 200 is for providing positive and negative scanning voltage signal; 201 write probe for signal; 202 and 203 are respectively the upper and lower electrode of resistance random access memory; 204 is bismuth-sodium titanate base film, for recording storage information.
Compared with prior art, the invention has the advantages that:
Adopt novel bismuth-sodium titanate based oxygen ion conductor film as the recording medium of resistance random access memory, it has obvious resistor random-access storage effect, and under the low-voltage of+0.3V, its maximum switch ratio is 30159.Ca-Ti ore type metatitanic acid bismuth sodium sill, as a kind of ferroelectric material, utilizes the characteristic of adjustable its ferroelectric properties of extra electric field to make it aspect FeRAM, also have potential using value, thereby is expected to prepare multi-functional non-volatility memorizer simultaneously.
The described resistance random access memory preparation method based on bismuth-sodium titanate thin film system is simple, cost is low, while especially adopting chemical solution deposition to prepare bismuth-sodium titanate base film, its component proportion is easy to control, simultaneously in conjunction with the oxygen conduction of bismuth-sodium titanate system and the substantial connection between its component, can prepare the different material of a series of oxygen conductions, greatly improve the distribution of the high and low resistance state of this resistance random access memory, thereby can be applied to the resistance states of recording medium to have in the different resistance random access memory parts that require.
Accompanying drawing explanation
Na in Fig. 1: embodiment 1
0.5bi
0.5ti
0.98mg
0.02o
2.98the XRD collection of illustrative plates of film;
Fig. 2: the structural representation of bismuth sodium titanate based film resistor random asccess memory;
Fig. 3: the voltage-to-current curve test schematic diagram of bismuth sodium titanate based film resistor random asccess memory;
In Fig. 4: embodiment 1 based on Na
0.5bi
0.5ti
0.98mg
0.02o
2.98the voltage-to-current graph of relation of the resistance random access memory of film and by the on-off ratio-voltage curve of this resistance random access memory of this current-voltage curve gained.
Embodiment
By specific embodiment, the present invention is described in further detail below, following examples can make professional and technical personnel more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1:
One, selected bismuth-sodium titanate base film consists of Na
0.5bi
0.5ti
0.98mg
0.02o
2.98, the preparation process of corresponding resistance random access memory is:
Step 1: the cleaning of conducting glass substrate, use the ITO electro-conductive glass of directly buying as substrate, select the ito glass substrate of surperficial intact and no marking, its ultrasonic concussion in absolute ethyl alcohol is cleaned to 5min and adhere to one deck liquid film to its surface uniform, remove the spot that substrate surface adheres to, then it is dried on heating plate, standby.
Step 2: use chemical solution deposition growth Na on the clean ito substrate of step 1 gained
0.5bi
0.5ti
0.98mg
0.02o
2.98film, according to the Na shown in Fig. 1
0.5bi
0.5ti
0.98mg
0.02o
2.98the known gained Na of XRD collection of illustrative plates of film
0.5bi
0.5ti
0.98mg
0.02o
2.98film is the perovskite structure of pure phase.
Step 3: by ion sputtering method, adopt mask plate (mask plate is shaped as the rectangle hole of equally distributed 0.5mm * 1mm), at Na
0.5bi
0.5ti
0.98mg
0.02o
2.98on film, preparing thickness is the Au top electrode of 100nm left and right, and electrode size is 0.5mm * 1mm.
Above-mentioned gained based on Na
0.5bi
0.5ti
0.98mg
0.02o
2.98the structure of the resistance random access memory of film is as shown in Figure 2: comprise bottom electrode, top electrode 104 that the conductive oxide coating 102 by glass substrate 101 and its upper setting forms, and the bismuth-sodium titanate base film 103 arranging between bottom electrode and top electrode 104, wherein bismuth-sodium titanate base film 103 and top electrode 104 form a memory cell.
Na prepared by the employing chemical solution deposition described in step 2
0.5bi
0.5ti
0.98mg
0.02o
2.98the specific operation process of film is:
1) by positive four butyl esters of metatitanic acid and acetylacetone,2,4-pentanedione, the mol ratio according to 1: 1 adds in the clean beaker that fills a certain amount of EGME, in this beaker, add a clean magneton, and this beaker is placed on magnetic stirring apparatus, under room temperature, be stirred to positive four butyl esters of metatitanic acid and dissolve, in whipping process, to dropwise dripping glacial acetic acid in above-mentioned beaker, to positive four butyl esters of metatitanic acid of partial hydrolysis, dissolve completely and suppress the further hydrolysis of positive four butyl esters of metatitanic acid simultaneously.After positive four butyl esters of metatitanic acid dissolve completely, according to Na
0.5bi
0.5ti
0.98mg
0.02o
2.98mole proportioning, take the Mg (NO of respective amount
3)
26H
2o, Bi (NO
3)
35H
2o and NaNO
3be placed in above-mentioned beaker (need to seal beaker mouth at whipping process and affect precursor liquid quality to prevent airborne dust etc. and fall into solution), in stirring at room to solute wherein, dissolve completely, obtain required Na
0.5bi
0.5ti
0.98mg
0.02o
2.98precursor solution.Finally using EGME to regulate the concentration of above-mentioned precursor solution is 0.3mol/L.
2) adopt the method for spin-coating to prepare Na
0.5bi
0.5ti
0.98mg
0.02o
2.98film, the rotating speed of adjusting spin coater is the equal glue 10s of first 1000rpm, the evener glue 30s of 3000rpm, to be filmed uniformly.Clean conducting glass substrate is placed on the operating desk of spin coater, uses a disposable syringe that is added with the organic filtering head of 0.22 μ m that precursor liquid is dropwise dropped on clean ITO conducting glass substrate, be rotated whirl coating.Often get rid of after one deck, gained rete is carried out within the scope of 250-350 ℃ to preannealing 5min, then use rta technique, in the oxygen atmosphere of 650 ℃, be incubated 5min, repeat said process, the Na that deposit thickness is 150nm
0.5bi
0.5ti
0.98mg
0.02o
2.98film;
Two, based on Na
0.5bi
0.5ti
0.98mg
0.02o
2.98the current-voltage loop testing of the resistance random access memory of film:
As shown in Figure 3, based on Na
0.5bi
0.5ti
0.98mg
0.02o
2.98the test schematic diagram of the current-voltage characteristic curve of the resistance random access memory of film: adopt Keithley2400 to measure the current-voltage characteristic curve of prepared resistance random access memory.In test process, test probe is added in respectively on the upper and lower electrode of top electrode, keeps bottom electrode ground connection simultaneously, applies the voltage of corresponding continuous sweep by test probe on upper and lower electrode.Electric current passes through Na
0.5bi
0.5ti
0.98mg
0.02o
2.98film flows between upper and lower electrode, and the current-voltage characteristic curve of gained as shown in Figure 4.Scan mode according to 0V →+2V → 0V →-2V → 0V (1 → 2 → 3 → 4) is tested, the initial state of system is high-impedance state (HRS), in the scanning process of 0V →+2V (process 1), system still remains HRS, but in process 1, when forward scan voltage is greater than a certain value, the electric current that flows through system increases sharply, and system changes to low resistance state (LRS) gradually.In the scanning process of+2V → 0V (process 2), system remains LRS.In the scanning process of 0V →-2V (process 3), system is HRS, but in process 3, when negative sense scanning voltage is greater than a certain value, the electric current that flows through system increases sharply, and system changes to low resistance state (LRS) gradually.In the scanning process of-2V → 0V (process 4), system is LRS.From the on-off ratio-voltage curve (the embedded figure of Fig. 4) of the current-voltage characteristic curve gained of this device, the maximum of this resistance random access memory its on-off ratio under the scanning voltage of low+0.3V can reach 30159.
Embodiment 2:
In the present embodiment, the preparation method of related bismuth sodium titanate based resistance random access memory is identical with embodiment 1, and difference is only that selected bottom electrode is FTO conducting glass substrate, and the annealing temperature of film is 600 ℃.By XRD, the bismuth-sodium titanate base film of gained in the present embodiment has been carried out to structural characterization.Film shows as the perovskite structure of pure phase, but its crystallinity is lower than gained film on ITO conducting glass substrate.
Embodiment 3
In the present embodiment, the preparation method of related bismuth sodium titanate based resistance random access memory is identical with embodiment 1, and difference is only that the bottom electrode using in the present embodiment is ITO or the FTO conductive oxide coating of being prepared on glass substrate by magnetron sputtering method.Mainly comprise the following steps:
(1) adopt the method for the magnetron sputtering bottom electrode of ITO conductive oxide coating as this resistance random access memory of growing on insulating glass substrate;
(2) adopt method as described in example 1 above to prepare the Na that thickness is 150nm in the ITO of gained conductive oxide coating
0.5bi
0.5ti
0.98mg
0.02o
2.98film.
Embodiment 4:
In the present embodiment, the preparation method of related bismuth sodium titanate based resistance random access memory is identical with embodiment 1, and difference is only that the component proportion of selected bismuth-sodium titanate base film is: Na
0.5bi
0.49tiO
2.985.
Embodiment 5:
In the present embodiment, the preparation method of related bismuth sodium titanate based resistance random access memory is identical with embodiment 1, and difference is only that the component of selected bismuth-sodium titanate base film is: Na
0.5bi
0.49ti
0.98mg
0.02o
2.965.
Embodiment 6
In the present embodiment, the preparation method of related bismuth sodium titanate based resistance random access memory is identical with embodiment 1, and difference is only the preparation Na using in the present embodiment
0.5bi
0.5ti
0.98mg
0.02o
2.98the concentration of the precursor solution of film is 0.1mol/L.
Embodiment 7
In the present embodiment, the preparation method of related bismuth sodium titanate based resistance random access memory is identical with embodiment 1, and difference is only the preparation Na using in the present embodiment
0.5bi
0.5ti
0.98mg
0.02o
2.98the concentration of the precursor solution of film is 0.5mol/L.The mol ratio of positive four butyl esters of described glacial acetic acid and metatitanic acid is 1: 1, and the mol ratio of positive four butyl esters of described acetylacetone,2,4-pentanedione and metatitanic acid is 1: 1, described glacial acetic acid and the volume ratio of EGME 1: 1; The volume ratio of acetylacetone,2,4-pentanedione complexant and EGME is 1: 1.
Embodiment 8
In the present embodiment, the preparation method of related bismuth sodium titanate based resistance random access memory is identical with embodiment 1, and difference is only Na prepared in the present embodiment
0.5bi
0.5ti
0.98mg
0.02o
2.98the thickness of film is 200nm.The mol ratio of positive four butyl esters of described glacial acetic acid and metatitanic acid is 1: 1, and the mol ratio of positive four butyl esters of described acetylacetone,2,4-pentanedione and metatitanic acid is 1: 1, described glacial acetic acid and the volume ratio of EGME 1: 10; The volume ratio of acetylacetone,2,4-pentanedione complexant and EGME is 1: 10.
Although by reference to the accompanying drawings specific embodiments of the invention are described above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing from the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of various ways, within these all belong to protection scope of the present invention.
Claims (10)
1. the resistance random access memory based on bismuth-sodium titanate thin film system, it is characterized in that, comprise bottom electrode, top electrode (104), and the bismuth-sodium titanate base film (103) arranging between bottom electrode and top electrode (104), wherein bismuth-sodium titanate base film (103) and top electrode (104) form a memory cell.
2. a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 1, is characterized in that, described bottom electrode is comprised of the conductive oxide coating (102) of glass substrate (101) and setting on it.
3. a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 1 and 2, it is characterized in that, described bottom electrode makes by the following method: on glass substrate, adopt the method growth conductive oxide coating of magnetron sputtering, described conductive oxide coating is the SnO of F-doping
2or In (FTO)
2o
3the SnO of-doping
2(ITO).
4. a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 1 and 2, is characterized in that, described bottom electrode is the glass substrate that business-like surface is covered with FTO or ITO conductive oxide coating.
5. a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 1, it is characterized in that, described bismuth-sodium titanate base film (103) is the bismuth-sodium titanate film of oxygen room doping, the bismuth-sodium titanate film that comprises the magnesium doping of titanium position, the bismuth-sodium titanate film of bismuth position trace bismuth disappearance, and magnesium doping in titanium position adds the bismuth-sodium titanate film of bismuth position trace bismuth disappearance.
6. a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 1, is characterized in that, described top electrode (104) is inert electrode or electrochemical activity electrode.
7. a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 6, is characterized in that, described inert electrode is gold or platinum electrode, and described electrochemical activity electrode is titanium, aluminium, copper or silver electrode.
8. the preparation method of the resistance random access memory based on bismuth-sodium titanate thin film system as claimed in claim 1, it is characterized in that, the method comprises the following steps: adopt the method for magnetron sputtering on insulating glass substrate, grow FTO or ITO conductive oxide coating or directly select business-like surface to be covered with the electric glass substrate of FTO or ITO conductive oxide coating as the bottom electrode of memory, adopt chemical solution deposition in conductive oxide coating, to prepare bismuth-sodium titanate base film, finally adopt Physical to prepare top electrode on bismuth-sodium titanate base film, by the shape of mask, control the shape of top electrode.
9. the preparation method of a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 8, is characterized in that, described chemical solution deposition and the concrete steps of Physical are as follows:
Step 1: the precursor solution of preparing bismuth-sodium titanate base film:
Take EGME and glacial acetic acid as solvent, and acetylacetone,2,4-pentanedione is complexant, three is added in reactor, according to the component proportion of required bismuth-sodium titanate base film, by the solute of respective amount: positive four butyl esters of metatitanic acid, Mg (NO
3)
26H
2o, Bi (NO
3)
35H
2o and NaNO
3add successively respectively in above-mentioned reactor, in stirring at room to each solute, dissolve completely, obtain required precursor solution, finally use EGME to regulate the molar concentration of described precursor solution;
Step 2: adopt the method for spin-coating to prepare bismuth-sodium titanate base film:
Adopt spin coater that described precursor solution is evenly coated in and on bottom electrode, obtains uniform film layer, often obtain after a skim, gained rete is first carried out to preannealing within the scope of 250-350 ℃, then use rta technique, in 600-650 ℃ of temperature range, in oxygen atmosphere, be incubated 5min, repeat said process, the bismuth-sodium titanate base film that deposit thickness is 150nm~200nm;
Step 3: adopt Physical to deposit top electrode on the bismuth-sodium titanate base film of step 2 gained, control the shape of top electrode by mask, obtain the top electrode of this resistance random access memory.
10. the preparation method of a kind of resistance random access memory based on bismuth-sodium titanate thin film system according to claim 9, is characterized in that, the mol ratio of described acetylacetone,2,4-pentanedione complexant and positive four butyl esters of metatitanic acid is 1: 1; Described glacial acetic acid and the volume ratio of EGME are 1: (1~10); Described acetylacetone,2,4-pentanedione and the volume ratio of EGME are 1: (1~10).
It is (0.1~0.5) mol/L that described use EGME regulates the molar concentration of described precursor solution;
The rotating speed of described spin coater is the equal glue 10s of first 1000rpm, the evener glue 30s of 3000rpm.
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