CN107170883B - A kind of flexibility TiO2The preparation method of resistance-variable storing device array - Google Patents
A kind of flexibility TiO2The preparation method of resistance-variable storing device array Download PDFInfo
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- CN107170883B CN107170883B CN201710564097.2A CN201710564097A CN107170883B CN 107170883 B CN107170883 B CN 107170883B CN 201710564097 A CN201710564097 A CN 201710564097A CN 107170883 B CN107170883 B CN 107170883B
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of the switching material, e.g. layer deposition
Abstract
The present invention relates to a kind of flexibility TiO2The preparation method of resistance-variable storing device array, this method is as follows: bis- (levulinic ketone group) ethyoxyl isopropoxy titanate esters, acetylacetone,2,4-pentanedione being dissolved in ethylene glycol monomethyl ether according to the molar ratio of 1:1 and mixed, obtains the precursor solution that titanium ion concentration is 0.5mol/L.By the solution by czochralski method coated in PET/ITO substrate flexible, by 365nm ultraviolet irradiation, ethyl alcohol, which dissolves and washes away, obtains TiO2After gel mould microarray, further ultraviolet irradiation 3-5 hours at 150 DEG C using 254nm and 185nm, are further prepared by Pt electrode, both can get the flexible PET/ITO/TiO with good retention performance and cycle characteristics2Memory array.
Description
Technical field
The present invention relates to information recording device manufacturing technology fields, and in particular to a kind of flexibility TiO2Resistance-variable storing device array
Preparation method.
Background technique
In the current information explosion epoch, information content is skyrocketed through, along with computer technology, internet and various novel
The fast development of popular electronic product such as mobile phone, digital camera, laptop etc., people want the performance of memory
It asks also higher and higher, not only requires it with high density, high speed, low cost, low-power consumption, but also want it with non-volatile
Property.Therefore one of the hot spot that novel non-volatile storage technologies have become current science and technology and industry development is researched and developed.Believed according to storage
The preservability energy of breath, memory can be divided into two major classes: the volatile memory (Volatile that data can lose after power-off
Memory), such as dynamic memory (DRAM) and static memory (SRAM)；It non-volatile is deposited with what data after power-off will not lose
Reservoir (Non-volatile memory), such as flash memory (Flash memory).
Currently, although flash memory Flash technology obtains immense success on the market, the limit by itself Ultrahigh
System, as characteristic size further reduces, the development of the technology is faced with many problems.On the one hand its program voltage cannot be by
Ratio reduces；On the other hand it constantly reduces with device size, the charge holding performance decline of device, makes it in a computer
Using being very limited.In light of this situation, numerous semiconductor company Intel, Samsung and IBM etc. are competitively being researched and developed
Based on the nonvolatile storage technologies of new Ultrahigh, to possess market and technical advantage in the following keen competition.
2000, scientist's Liu et al. people of houston, U.S.A university had found one in huge magnetic resistance sull device
The new physical effect of kind --- electric pulse triggering resistive effect is answered, i.e., under the action of outer Ghana second level width voltage pulse, device
Resistance between low resistance state (" 0 ") and high-impedance state (" l ") reversible transition.Based on this discovery, scientific circles propose one kind
Novel nonvolatile storage concept --- resistive random access memory, abbreviation resistance-variable storing device (RRAM).Subsequent scientific research personnel
This resistance switch effect is had found in many metal oxide materials.As a kind of completely new storage concept, RRAM's is excellent
Gesture is mainly manifested in the following aspects: first is that preparation is simple；Second is that erasable and writing speed is fast, generally less than 100ns is much higher than
Flash storage；Third is that storage density is high；Fourth is that the compatibility of its manufacture craft and traditional CMOS technology is very well, it is easy to
Realize that high-volume, low cost are manufactured.Therefore the research of RRAM is just attracting the concern of more and more scientific research personnel, is considered
It is the most contenders of next-generation nonvolatile memory.
Suitable material is selected, it is crucial factor that suitable method, which prepares flexible device,.TiO2Waiting oxide materials is
Good resistive dielectric material.But if the preparation of this kind of oxide material is prepared using physical deposition techniques, although be easy
Low temperature preparation forms on flexible substrates, but it is subsequent also need etch to form storage unit；If using lower-cost
Wet chemical method preparation, this kind of oxide material need the high-temperature heat treatment by 400 DEG C or more toward contact, destroy organic lining
Bottom.Therefore, either physical deposition or chemical method prepare all also certain predicaments of this kind of flexible device.Invented one kind both
It can be prepared under low temperature, and can be that flexible electronic device is urgently to be solved using the device for forming storage unit by straightforward procedure
Problem.
Summary of the invention
The present invention provides a kind of flexibility TiO2The preparation method of resistance-variable storing device array, by two step photochemical methods,
Obtain TiO2Flexible resistive device array.
The technical scheme adopted by the invention is as follows:
A kind of flexibility TiO2The preparation method of resistance-variable storing device, using czochralski method by titanium ion precursor solution coated in flexibility
PET/ITO substrate on be formed on its surface TiO2Gel mould, then to PET/ITO/TiO2Successively by being irradiated under high-pressure sodium lamp
Amorphous TiO is obtained with irradiation under low pressure mercury lamp2Membrane array, finally in PET/ITO/TiO2Deposited over arrays Pt electrode, is obtained
There must be the flexible PET/ITO/TiO of good retention performance and cycle characteristics2Memory array.
Specifically includes the following steps:
Step 1), will be bis- (levulinic ketone group) ethyoxyl isopropoxy titanate esters mixed with ethylene glycol monomethyl ether solution, obtain
Ti4+Ion is the solution A of 0.5mol/L；
Step 2) adds acetylacetone,2,4-pentanedione solution into solution A, so that acetylacetone,2,4-pentanedione and Ti4+Molar ratio be 1:1, stirring
After obtain solution B；
Step 3), using the resulting solution B of step 2, using PET/ITO as substrate, using czochralski method, with the speed of 2mm/s
Plated film is lifted, TiO is obtained2Gel mould；
Step 4), the PET/ITO/TiO obtained in step 3)2On, mask plate C is placed, is placed under high-pressure sodium lamp and carries out
Irradiation after irradiation, takes out sample；
Step 5), step 4) is irradiated after sample, be immersed in ethanol solution, impregnate 1 minute after, take out sample
Product obtain TiO with being dried with nitrogen2Gel membrane array；
Step 6), by the resulting TiO2 gel membrane array of step 5), be put in heating plate, be subsequently placed in spoke under low pressure mercury lamp
According to；After irradiation, amorphous TiO is obtained2Membrane array；
Step 7), the amorphous TiO obtained in step 6)2In membrane array, mask plate C is placed again, is then used
Small ion sputter, in PET/ITO/TiO2Deposited over arrays Pt electrode, final to obtain using flexible PET as substrate, ITO is bottom
Electrode, Pt are the TiO of top electrode2Resistance-variable storing device array.
Solution A concentration described in step 1) is controlled in 0.4-0.5mol/l.
The dominant wavelength of high-pressure sodium lamp described in step 4) is 365nm, and irradiation time is 30-60 minutes.
The dominant wavelength of low pressure mercury lamp described in step 5) is 185nm and 254nm, heating temperature 150oC irradiation time
It is 3-5 hours, controlling temperature of heating plate in irradiation process always is 150 DEG C.
According to flexibility TiO made from above-mentioned preparation method2Resistance-variable storing device.
Compared with prior art, the invention has the following advantages that
1. the present invention completes TiO by the ultraviolet lithographic method of wet-chemical, a step2The preparation of gel membrane array, avoids
Conventional wet chemical etching or other high costs of dry etching bring, the disadvantage of technology path complexity；
2. the present invention just obtains amorphous TiO at 150 DEG C of low temperature by deep ultraviolet irradiance method2Film, thus real
The preparation for having showed flexible device avoids high-temperature heat treatment to the destruction problem of flexible substrates；
3. specific presoma and complexing agent through the invention, so that precursor solution has sensitivity to 365nm ultraviolet light
Characteristic, and there is absorption to the deep ultraviolet of 254nm, to realize the step preparation of array, and it is non-to complete low temperature
Crystalline state TiO2Preparation, significantly reduce cost；
Have good memory retention properties and circulation special 4. preparation method obtains flexible resistive device array through the invention
Property, bending 1000 times or more is still able to maintain good resistive behavior.
Detailed description of the invention
Fig. 1 is flexibility PET/ITO/TiO of the invention2The preparation route figure of/Pt resistance-variable storing device；
Fig. 2 is TiO of the present invention2The uv-visible absorption spectroscopy figure of precursor solution；
Fig. 3 is PET/ITO/TiO after being bent 1000 times under the conditions of different curvature (K)2/ Pt flexibility resistance-variable storing device array
Retention performance figure；Wherein, the m of (a) K=0-1；(b) 36.2m-1；(c) 49.1m-1；(d) 79.7m-1；
Fig. 4 is PET/ITO/TiO after being bent 1000 times under the conditions of different curvature (K)2/ Pt flexibility transition storage array
Circulation spy figure；Wherein, the m of (a) K=0-1；(b) 36.2m-1； (c) 49.1m-1；(d) 79.7m-1。
Specific embodiment
The present invention will be described in detail With reference to embodiment.
A kind of flexibility TiO2The preparation method of resistance-variable storing device, using czochralski method by titanium ion precursor solution coated in flexibility
PET/ITO substrate on be formed on its surface TiO2Gel mould, then to PET/ITO/TiO2Successively by being irradiated under high-pressure sodium lamp
Amorphous TiO is obtained with irradiation under low pressure mercury lamp2Membrane array, finally in PET/ITO/TiO2Deposited over arrays Pt electrode, is obtained
There must be the flexible PET/ITO/TiO of good retention performance and cycle characteristics2Memory array.
Specifically includes the following steps:
Step 1), will be bis- (levulinic ketone group) ethyoxyl isopropoxy titanate esters mixed with ethylene glycol monomethyl ether solution, obtain
Ti4+Ion is the solution A of 0.5mol/L；
Step 2) adds acetylacetone,2,4-pentanedione solution into solution A, so that acetylacetone,2,4-pentanedione and Ti4+Molar ratio be 1:1, stirring
After obtain solution B；
Step 3), using the resulting solution B of step 2, using PET/ITO as substrate, using czochralski method, with the speed of 2mm/s
Plated film is lifted, TiO is obtained2Gel mould；
Step 4), the PET/ITO/TiO obtained in step 3)2On, mask plate C is placed, is placed under high-pressure sodium lamp and carries out
Irradiation after irradiation, takes out sample；
Step 5), step 4) is irradiated after sample, be immersed in ethanol solution, impregnate 1 minute after, take out sample
Product obtain TiO with being dried with nitrogen2Gel membrane array；
Step 6), by the resulting TiO2 gel membrane array of step 5), be put in heating plate, be subsequently placed in spoke under low pressure mercury lamp
According to；After irradiation, amorphous TiO is obtained2Membrane array；
Step 7), the amorphous TiO obtained in step 6)2In membrane array, mask plate C is placed again, is then used
Small ion sputter, in PET/ITO/TiO2Deposited over arrays Pt electrode, final to obtain using flexible PET as substrate, ITO is bottom
Electrode, Pt are the TiO of top electrode2Resistance-variable storing device array.
Solution A concentration described in step 1) is controlled in 0.4-0.5mol/l.
The dominant wavelength of high-pressure sodium lamp described in step 4) is 365nm, and irradiation time is 30-60 minutes.
The dominant wavelength of low pressure mercury lamp described in step 5) is 185nm and 254nm, heating temperature 150oC irradiation time
It is 3-5 hours, controlling temperature of heating plate in irradiation process always is 150 DEG C.
According to flexibility TiO made from above-mentioned preparation method2Resistance-variable storing device.
The preparation route of above-mentioned preparation process is as shown in Figure 1, wherein (a) lifts plated film；(b) under mask plate obstruction conditions
365nm ultraviolet irradiation；(c) ethyl alcohol dissolves and washes away；(d) TiO is obtained2Gel membrane array；(e) the dark purple external irradiation of 185+254nm；(f)Pt
Electrode preparation；(h) PET/ITO/TiO flexible is obtained2/ Pt resistance-variable storing device array.
The present invention is further detailed below by several embodiments:
Embodiment 1:
Will be bis- (levulinic ketone group) ethyoxyl isopropoxy titanate esters, mixed with ethylene glycol monomethyl ether solution, obtain Ti4+Ion
For the solution of 0.5mol/L；Acetylacetone,2,4-pentanedione solution is added, so that acetylacetone,2,4-pentanedione and Ti4+Molar ratio be 1:1, obtained after stirring clear
Clear solution；Using the solution, by czochralski method, using PET/ITO as substrate, plated film is lifted with the speed of 2mm/s, obtains TiO2It is solidifying
Glue film；In the PET/ITO/TiO of acquisition2Upper placement mask plate is placed under the high-pressure sodium lamp that dominant wavelength is 365nm and is irradiated
30 minutes, after irradiation, by PET/ITO/TiO2It is immersed in ethanol solution, after impregnating 1 minute, takes out, use nitrogen
Drying obtains TiO2Gel membrane array；Then it is put in 150 DEG C of heating plates, is placed in the low pressure that wavelength is 185nm and 254nm
Under mercury lamp, irradiation 3 hours is carried out.Always it is 150 DEG C that temperature of heating plate is controlled in irradiation process.After irradiation, amorphous is obtained
The TiO of state2Membrane array；In amorphous TiO2In membrane array, identical mask plate is placed, then uses small ion
Sputter, in PET/ITO/TiO2Deposited over arrays Pt electrode, final to obtain using flexible PET as substrate, ITO is hearth electrode, Pt
For top electrode, structure is " PET/ITO/TiO2The flexible resistance-variable storing device array of/Pt ".The height resistance ratio of the device can be with
Reach 1000 or more, alternating bending 1000 times or more without significant change.
Referring to fig. 2, in solution made from embodiment 1, titanium ion is complexed with acetylacetone,2,4-pentanedione.There is a suction in 360nm
Peak is received, this shows that acetylacetone,2,4-pentanedione is complexed with titanium ion, forms network-like complex compound；The generation of this complex compound, because
To be main peak in 360nm, therefore there is sensitivity characteristic to the ultraviolet light that 365nm is dominant wavelength, after 365nm ultraviolet irradiation,
This complex compound can be made to decompose, polymerization reaction can occur for the titanium organic matter after decomposition, to form titanium oxide amorphous
State gel mould.Because in advance in film upper cover mask plate, by illumination partly because foring titanium oxide amorphous state gel
Film cannot be dissolved and washed away by ethyl alcohol, and not be still organic titanium gel mould by ultraviolet light irradiation part, then can be dissolved and washed away by ethyl alcohol
Fall, so as to form TiO shown in Fig. 1 (d)2Gel membrane array.
It can further be seen that TiO from Fig. 22Gel mould also has absorption to 254nm, therefore in subsequent 185nm+254nm
In irradiation process, the ultraviolet light of 254nm is further absorbed, and is reacted with 185nm and generates ozone, so that TiO2Gel mould battle array
The elements such as the C in column, H are volatilized, obtain truly without C, amorphous titanium oxide battle array of the impurity elements such as H
Column, as shown in Fig. 1 (e).Fig. 3 and Fig. 4 is respectively with regard to the flexible PET/ITO/TiO under differently curved curvature2/ Pt device is protected
Hold the test of characteristic and cycle characteristics, the results showed that, after continuous bend 1000 times, device still has good resistive characteristic,
The ratio of high-impedance state and low resistance state maintains always 1000 or more, has good memory effect.
Embodiment 2:
Will be bis- (levulinic ketone group) ethyoxyl isopropoxy titanate esters, mixed with ethylene glycol monomethyl ether solution, obtain Ti4+Ion
For the solution of 0.5mol/L；Acetylacetone,2,4-pentanedione solution is added, so that acetylacetone,2,4-pentanedione and Ti4+Molar ratio be 1:1, obtained after stirring clear
Clear solution；Using the solution, by czochralski method, using PET/ITO as substrate, plated film is lifted with the speed of 2mm/s, obtains TiO2It is solidifying
Glue film；In the PET/ITO/TiO of acquisition2Upper placement mask plate is placed under the high-pressure sodium lamp that dominant wavelength is 365nm and is irradiated
60 minutes, after irradiation, by PET/ITO/TiO2It is immersed in ethanol solution, after impregnating 1 minute, takes out, use nitrogen
Drying obtains TiO2Gel membrane array；Then it is put in 150 DEG C of heating plates, is placed in the low pressure that wavelength is 185nm and 254nm
Under mercury lamp, irradiation 5 hours is carried out.Always it is 150 DEG C that temperature of heating plate is controlled in irradiation process.After irradiation, amorphous is obtained
The TiO of state2Membrane array；In amorphous TiO2In membrane array, identical mask plate is placed, then uses small ion
Sputter, in PET/ITO/TiO2Deposited over arrays Pt electrode, final to obtain using flexible PET as substrate, ITO is hearth electrode, Pt
For top electrode, structure is " PET/ITO/TiO2The flexible resistance-variable storing device array of/Pt ".The height resistance ratio of the device can be with
Reach 1000 or more, alternating bending 1400 times or more without significant change.
Embodiment 3:
Will be bis- (levulinic ketone group) ethyoxyl isopropoxy titanate esters, mixed with ethylene glycol monomethyl ether solution, obtain Ti4+Ion
For the solution of 0.4mol/L；Acetylacetone,2,4-pentanedione solution is added, so that acetylacetone,2,4-pentanedione and Ti4+Molar ratio be 1:1, obtained after stirring clear
Clear solution；Using the solution, by czochralski method, using PET/ITO as substrate, plated film is lifted with the speed of 2mm/s, obtains TiO2It is solidifying
Glue film；In the PET/ITO/TiO of acquisition2Upper placement mask plate is placed under the high-pressure sodium lamp that dominant wavelength is 365nm and is irradiated
60 minutes, after irradiation, by PET/ITO/TiO2It is immersed in ethanol solution, after impregnating 1 minute, takes out, use nitrogen
Drying obtains TiO2Gel membrane array；Then it is put in 150 DEG C of heating plates, is placed in the low pressure that wavelength is 185nm and 254nm
Under mercury lamp, irradiation 4 hours is carried out.Always it is 150 DEG C that temperature of heating plate is controlled in irradiation process.After irradiation, amorphous is obtained
The TiO of state2Membrane array；In amorphous TiO2In membrane array, identical mask plate is placed, then uses small ion
Sputter, in PET/ITO/TiO2Deposited over arrays Pt electrode, final to obtain using flexible PET as substrate, ITO is hearth electrode, Pt
For top electrode, structure is " PET/ITO/TiO2The flexible resistance-variable storing device array of/Pt ".The height resistance ratio of the device can be with
Reach 800 or more, alternating bending 2000 times or more without significant change.
The contents of the present invention are not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And to any equivalent transformation that technical solution of the present invention is taken, all are covered by the claims of the invention.
Claims (6)
1. a kind of flexibility TiO2The preparation method of resistance-variable storing device, which is characterized in that applied titanium ion precursor solution using czochralski method
It applies and is formed on its surface TiO in PET/ITO substrate flexible2Gel mould, then to PET/ITO/TiO2Successively pass through high-pressure mercury
The amorphous TiO of acquisition is irradiated under irradiation and low pressure mercury lamp under lamp2Membrane array, finally in PET/ITO/TiO2Deposited over arrays
Pt electrode obtains the flexible PET/ITO/TiO with good retention performance and cycle characteristics2Memory array.
2. flexibility TiO according to claim 12The preparation method of resistance-variable storing device, which is characterized in that specifically include following
Step:
Step 1), will be bis- (levulinic ketone group) ethyoxyl isopropoxy titanate esters mixed with ethylene glycol monomethyl ether solution, obtain Ti4+From
Son is the solution A of 0.5mol/L；
Step 2) adds acetylacetone,2,4-pentanedione solution into solution A, so that acetylacetone,2,4-pentanedione and Ti4+Molar ratio be 1:1, obtained after stirring
Obtain solution B；
Step 3), using the resulting solution B of step 2, using PET/ITO as substrate, using czochralski method, lifted with the speed of 2mm/s
Plated film obtains TiO2Gel mould；
Step 4), the PET/ITO/TiO obtained in step 3)2On, mask plate C is placed, is placed under high-pressure sodium lamp and is irradiated,
After irradiation, sample is taken out；
Step 5), step 4) is irradiated after sample, be immersed in ethanol solution, impregnate 1 minute after, take out sample, use
It is dried with nitrogen, obtains TiO2Gel membrane array；
Step 6), by the resulting TiO2 gel membrane array of step 5), be put in heating plate, be subsequently placed under low pressure mercury lamp and irradiate；
After irradiation, amorphous TiO is obtained2Membrane array；
7), the amorphous TiO obtained in step 6)2In membrane array, mask plate C is placed again, is then splashed using small ion
Instrument is penetrated, in PET/ITO/TiO2Deposited over arrays Pt electrode, final to obtain using flexible PET as substrate, ITO is hearth electrode, and Pt is
The TiO of top electrode2Resistance-variable storing device array.
3. a kind of flexibility TiO according to claim 22The preparation method of resistance-variable storing device array, which is characterized in that step
1) the solution A concentration described in is controlled in 0.4-0.5mol/l.
4. flexibility TiO according to claim 2 or 32The preparation method of resistance-variable storing device array, which is characterized in that step 4)
Described in high-pressure sodium lamp dominant wavelength be 365nm, irradiation time be 30-60 minutes.
5. flexibility TiO according to claim 42The preparation method of resistance-variable storing device array, which is characterized in that in step 5)
The dominant wavelength of the low pressure mercury lamp is 185nm and 254nm, heating temperature 150oC irradiation time is 3-5 hours, irradiated
Always it is 150 DEG C that temperature of heating plate is controlled in journey.
6. according to flexibility TiO made from preparation method described in above-mentioned any one claim2Resistance-variable storing device.
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| CN110707211B (en) * | 2019-09-29 | 2023-02-17 | 西安理工大学 | Preparation method of cerium oxide memristor film |
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