CN110098326A - A kind of two dimension Ti3C2- MXene thin-film material and preparation method thereof and the application in resistance-variable storing device - Google Patents
A kind of two dimension Ti3C2- MXene thin-film material and preparation method thereof and the application in resistance-variable storing device Download PDFInfo
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
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- 229910052731 fluorine Inorganic materials 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—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 having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of switching materials, e.g. deposition of layers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
- H10N70/884—Switching materials based on at least one element of group IIIA, IVA or VA, e.g. elemental or compound semiconductors
- H10N70/8845—Carbon or carbides
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Abstract
The present invention relates to a kind of two dimension Ti3C2- MXene thin-film material and preparation method thereof and the application in resistance-variable storing device belong to film preparation and microelectronics function element technical field.The present invention prepares MXene film on conductive substrates surface using one step solwution method of low temperature, and film forming is simple, and more easily large area prepares film.The present invention uses New Two Dimensional material MXene for the first time to substitute traditional resistive material applied to memory area.Resistance-variable storing device of the invention successively includes hard substrates, hearth electrode, change resistance layer, top electrode from bottom to up, in which: the resistive layer material is two dimension Ti3C2- MXene thin-film material, 100~450nm of thickness of the change resistance layer, device obtained are able to maintain original resistance state when power is off, are nonvolatile memory, and be still able to maintain stabilization after device continuous several times circulation, have and follow bad tolerance.
Description
Technical field
The invention belongs to film preparation and microelectronics function element technical fields, and in particular to a kind of two dimension Ti3C2-MXene
Thin-film material and preparation method thereof and the application in resistance-variable storing device.
Background technique
With the arrival of big data era, the requirement that people store data is higher and higher.Based on charge storage principle
Memory, such as flash memory will face size reduction physics limit and technological limit, it is difficult to meet the needs of people, therefore
The new non-volatility memorizer haveing excellent performance of exploitation becomes the research hotspot of semicon industry.
Resistance-variable storing device shows different resistance states under the action of extra electric field using thin-film material to realize number
According to storage.Resistance-variable storing device realizes storage by the reversible transition of material resistance, has a clear superiority compared with conventional flash memory, wraps
Include that device architecture is simple, unit size is small, scaling performance is good, service speed is fast, low in energy consumption and complementary metal oxide
(Complementary Metal Oxide Semiconductor, CMOS) process compatible is easy to three-dimensionally integrated etc., becomes weight
The next-generation memory technology wanted, and be considered as being most suitable for three-dimensionally integrated one of novel memory devices, in different application fields
Present can mass market prospect.
Resistance variation memory structure is simple, and the change resistance layer of core is only made of a kind of material, and resistive dielectric material is that resistive is deposited
The carrier of resistance conversion occurs for reservoir, has most direct influence to the performance of resistance-variable storing device.The material of resistive layer of dielectric material
Expect that type is very more, can probably be divided into several classes: binary oxide, ternary and multivariant oxide, sulfur family solid electrolyte, nitridation
Object and other inorganic material.Binary oxide has that structure is simple, material component is easy to control, preparation process and semiconductor work
The advantages that skill is compatible, a but biggish initial voltage is generally needed to make to form conductive channel in change resistance layer, increase power consumption and
The complexity of peripheral circuit.Ternary and multivariant oxide material preparation process are more complicated, and component ratio is difficult to control and hardly possible
With compatible with current CMOS technology, so the research of the resistance-variable storing device based on multi-element metal oxide is mainly opened in laboratory
Exhibition, this kind of material is in the application prospect of industrial circle and uncertain.Sulfur family solid electrolyte material is as Ag+And Cu2+Ion
Excellent fast ion conducting material, it is very advantageous in terms of the electric resistance changing mechanism of research PMC device, it is still to be ground in laboratory
Study carefully the common dielectric material of electric resistance changing behavior.Other inorganic material it is relatively common have nitride, amorphous carbon and amorphous silicon etc.,
It is same that there is the problems such as the process is more complicated, and preparation cost is higher.It is good in addition to having in order to realize industrialized application requirement
Change resistance performance outside, the economic cost of a variety of materials technology of preparing is also the factor that must be taken into consideration.Therefore seek new having to tie
Structure is simple, material component is easy to control, preparation process is simple, resistive layer material meaning low in cost and having the characteristics that good resistive
Justice is great.
Currently, being used as the material of change resistance layer can be divided into from scale size, and zero dimensional nanometer materials such as NiO nanoparticle, one
Dimension nano material ZnO nano-wire, two-dimensional thin-film material etc..Atomic scale thickness assigns two-dimensional material high-specific surface area, uniqueness
Electronic structure and physicochemical properties, it is mutually compatible with the microelectronic processing technology of mainstream, be advantageously implemented resistance-variable storing device
Industrial applications, and it is nontoxic, preparation process is simple, at low cost the features such as, cause the extensive concern of people.Wherein, MXene
As a kind of novel two-dimensional material, it is easy preparation, electronic structure is unique, and great research potential becomes research of the invention
Emphasis.
The resistive characteristic of device and material performance itself are closely related, and the performance of material depends greatly on system again
Preparation Method.In numerous resistive dielectric materials, the research of binary oxide is more, and performance is more excellent.Binary oxide is logical
It is often used the preparation of the methods of magnetron sputtering, sol-gel method and plasma oxidation.The shortcomings that magnetron sputtering is to be difficult to prepare
The controllable multicomponent compound film of stoichiometric ratio；Sol-gel method has the drawback that the adhesion property of film and substrate
Poor, the compactness of film is not also high.The shortcomings that plasma oxidation technology is that the requirement for experimental situation is high, experiment system
It is standby at high cost.Therefore based on preparation process is simple, high-efficient, film and substrate associativity are good, is easy to compared with face big under low environment
Under the premise of the advantages that product prepares film, and reduction preparation cost, the present invention is proposed.
Summary of the invention
For the above-mentioned problem of the prior art and defect, the purpose of the present invention is to provide a kind of two dimension Ti3C2-
MXene thin-film material and preparation method thereof and the application in resistance-variable storing device, the present invention use a kind of New Two Dimensional for the first time
Ti3C2- MXene thin-film material substitutes traditional resistive material, and for the first time by Ti3C2- MXene film is led applied to memory
Domain.
In order to realize the above-mentioned one of purpose of the present invention, the present invention adopts the following technical scheme:
A kind of two dimension Ti3C2The preparation method of-MXene thin-film material, includes the following steps:
(1) Ti is prepared3C2- MXene nanometer sheet colloidal solution
According to the ratio by titanium aluminium carbon (Ti3AlC2) powder is added to and is made of hydrochloric acid solution, deionized water and lithium fluoride (LiF)
Mixed solution in, be stirred at room temperature uniformly after obtain mixed reaction solution；Then gained mixed reaction solution is heated to 30~40 DEG C,
Product centrifugation, cleaning to cleaning solution are neutrality, obtained by 18~30h of isothermal reaction under agitation after reaction
Ti3C2- MXene colloidal solution；Again by the Ti3C2- MXene colloidal solution is ultrasonically treated 0.5~2h, obtains the Ti3C2-
MXene nanometer sheet colloidal solution；
(2) Ti is prepared3C2- MXene film
The Ti that step (1) is obtained3C2- MXene nanometer sheet colloidal solution drop coating is in the transparent of pretreated clean dried
Conductive substrates surface after drop coating, is coated with Ti3C2The electrically conducting transparent substrate of-MXene nanometer sheet colloidal solution is transferred to
In heating plate, 2~10min is made annealing treatment under the conditions of 95~105 DEG C, obtains Ti3C2- MXene film.
Further, the mass ratio of above-mentioned technical proposal, step (1) the titanium aluminium carbon and lithium fluoride is 1:(1~1.5).
Further, the amount ratio of above-mentioned technical proposal, step (1) the titanium aluminium carbon and hydrochloric acid is 1 mass parts: (10~
20) parts by volume is using g:mL as benchmark between the mass parts and parts by volume.
Further, above-mentioned technical proposal, the mass percentage concentration of step (1) described hydrochloric acid solution are 30~40%.
Second object of the present invention is to provide two dimension Ti described above3C2The preparation method system of-MXene thin-film material
Standby obtained two-dimentional Ti3C2- MXene thin-film material.
Third object of the present invention is to provide the two-dimentional Ti that method described above is prepared3C2- MXene film material
Expect the application as change resistance layer in resistance-variable storing device.
One kind being based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, the resistive memory from bottom to up according to
Secondary includes hard substrates, hearth electrode, change resistance layer, top electrode, in which: the resistive layer material is made from the above method of the present invention
Two-dimentional Ti3C2- MXene film.
Further, above-mentioned technical proposal, the hearth electrode material are any one of FTO, ITO, ZTO or AZO；Institute
The top electrode material stated is any one of Pt, Au or W.
Further, above-mentioned technical proposal, the hearth electrode with a thickness of 100~300nm, the shape of the hearth electrode
For round or rectangle, diameter or side length are 50nm~2cm, preferably 1~2cm.
Further, above-mentioned technical proposal, the square resistance of the hearth electrode are 10~20 Ω sq-1。
Further, above-mentioned technical proposal, 100~450nm of thickness of the change resistance layer, preferably 200~400nm, institute
The shape of change resistance layer is stated as round or rectangle, diameter or side length are 50nm~2cm.
Further, above-mentioned technical proposal, the top electrode with a thickness of 60~100nm, the shape of the top electrode
For round or rectangle, diameter or side length are 100~900 μm.
Further, above-mentioned technical proposal, the hard substrates are SiO2/Si、Al2O3, quartz, pyroceram or resistance to
Any one of refractory ceramics, preferably pyroceram.
Fourth object of the present invention is to provide described above based on two-dimentional Ti3C2The resistive of-MXene thin-film material
The preparation method of memory, the described method comprises the following steps:
Step 1: cleaning substrate
There is the substrate of hearth electrode material that deionized water, acetone, ethyl alcohol is successively used to be cleaned by ultrasonic in Ultrasound Instrument growth, blows
It is dry；
Step 2: reserved electrode
Insulating cement is pasted at the cleaned hearth electrode material one side edge of step 1；
Step 3: preparing change resistance layer
(a) Ti is prepared3C2- MXene nanometer sheet colloidal solution
According to the ratio by titanium aluminium carbon (Ti3AlC2) powder is added to the mixing being made of hydrochloric acid solution, deionized water and lithium fluoride
In solution, mixed reaction solution is obtained after being stirred at room temperature uniformly；Then gained mixed reaction solution is heated to 30~40 DEG C, stirred
Under the conditions of 18~30h of isothermal reaction, after reaction, by product centrifugation, clean to cleaning solution be neutrality, obtain Ti3C2-MXene
Colloidal solution；Again by the Ti3C2- MXene colloidal solution is ultrasonically treated 0.5~2h, obtains the Ti3C2- MXene nanometers
Piece colloidal solution；
(b) Ti is prepared3C2- MXene film change resistance layer
The Ti that step (a) is obtained3C2- MXene nanometer sheet colloidal solution drop coating is in the bottom of pretreated clean dried electricity
Pole surface after drop coating, is coated with Ti3C2The substrate of-MXene nanometer sheet colloidal solution is transferred in heating plate, 95~
2~20min is made annealing treatment under the conditions of 105 DEG C, obtains Ti3C2- MXene film change resistance layer；
Step 4: preparing top electrode
Top electrode is deposited in resistive layer surface using magnetron sputtered deposition technology.
Compared with prior art, a kind of two dimension Ti of the present invention3C2- MXene thin-film material and preparation method thereof and
Application in resistance-variable storing device has the following beneficial effects:
(1) Ti of the invention3C2- MXene colloidal solution is easy to using ultrasonic mechanical stripping at single layer, relative to current main
For the two-dimensional material graphene of stream, it is easier to modification and processing；
(2) present invention prepares MXene film on conductive substrates surface using one step solwution method of low temperature, and film forming is simple, and more
Easy large area prepares film, and preparation process is stablized.
(3) Ti of the invention3C2- MXene membrane-film preparation process is nontoxic, environmentally friendly.
(4) Ti of the invention3C2- MXene film is not high for preparation environmental requirement, and the failure rate of experiment is lower, will prepare
Material place more than ten days after be tested for the property, material property stablize, in industrial circle large scale preparation in application, can drop
Low preparation cost.
(5) Ti of the invention3C2This New Two Dimensional nano material of-MXene has certain bending strength, makes Ti3C2-
MXene become it is a kind of with development potential with the resistive layer material of researching value.
Detailed description of the invention
Fig. 1 is of the present invention based on two dimension Ti3C2The structural schematic diagram of the resistance-variable storing device of-MXene thin-film material；
Wherein: 1- top electrode；2- change resistance layer；3- has the hard substrates of hearth electrode.
Fig. 2 is two-dimentional Ti prepared by the embodiment of the present invention 13C2Scanning electron microscope (SEM) photo of-MXene thin-film material；
(a) is two-dimentional Ti prepared by the embodiment of the present invention 1 in Fig. 33C2The X-ray diffraction (XRD) of-MXene thin-film material is composed
Figure；It (b) is Ti3C2The XRD standard diffraction spectrogram of-MXene；
(a) is the Ti of 1 step of the embodiment of the present invention (3) preparation in Fig. 43C2- MXene colloidal solution on day 1 with place the
15 days mode of appearance photo comparison figures；(b) be 1 step of the embodiment of the present invention (4) preparation two-dimentional Ti3C2- MXene film material
Expect the X-ray diffraction comparison diagram on day 1 with placement the 15th day；
Fig. 5 is the preparation of Application Example 1 of the present invention based on two-dimentional Ti3C2The resistance-variable storing device of-MXene thin-film material
I-V curve test result figure；
Fig. 6 is the preparation of Application Example 1 of the present invention based on two-dimentional Ti3C2The resistance-variable storing device of-MXene thin-film material
Cyclic durability and stability test result figure.
Specific embodiment
Technical solution of the present invention is described in detail below by specific embodiment and attached drawing.Following reality
Applying example is only preferred embodiments of the present invention, is not the restriction that other forms are done to the present invention, any skill for being familiar with this profession
Art personnel are changed to the equivalent embodiment changed on an equal basis possibly also with the technology contents of the disclosure above.It is all without departing from this hair
Bright plan content, any simple modification or equivalent variations made according to the technical essence of the invention to following embodiment, falls
Within the scope of the present invention.
Embodiment 1
A kind of two dimension Ti of the present embodiment3C2The preparation method of-MXene thin-film material, includes the following steps:
Step 1. cleans FTO (tin oxide of fluorine doped) electro-conductive glass substrate
The first step is 14 Ω sq to having with a thickness of 100nm, square resistance-1FTO hearth electrode, side length be 1cm just
Rectangular electro-conductive glass, which is placed in cleanser and the mixed solution of deionized water, is cleaned by ultrasonic 15min, second step, and it is conductive to take out FTO
Glass, which is put into hand cleanser and the mixed liquor of deionized water, is cleaned by ultrasonic 15min, third step, and the taking-up of FTO electro-conductive glass is put into
It is cleaned by ultrasonic 15min, the 4th step in acetone, then FTO electro-conductive glass is put into ethanol solution and is cleaned by ultrasonic 15min.
Step 2.UV handles the surface FTO
By the above-mentioned FTO drying cleaned up, insulating tape is sticked at the edge of piece, reserved electrode is formed, then puts
30min is handled with UV ozone in UV cleaning device.The purpose of UV processing is the wetting capacity in order to improve the surface FTO；
Step 3. prepares Ti3C2- MXene colloidal solution
(1) Ti for taking 300 mesh of 0.5g ground3AlC2It is 37.5% that powder, which is slowly added into 7.5ml mass percentage concentration,
Hydrochloric acid solution, 2.5ml deionized water and 0.5036g LiF mixed solution in, use magnetic stirrer at room temperature,
It is uniformly mixed it.The revolving speed of magnetic stirring apparatus is set as 500rpm/min.
(2) by above-mentioned mixed liquor at 35 DEG C, 500r/min magnetic agitation reaction for 24 hours, then using centrifuge carry out from
Heart cleaning is until pH is neutrality, centrifuge speed 4000r/min, centrifugation time 5min.Last time centrifuged supernatant
Be it is blackish green, indicate Ti3C2The successful synthesis of-MXene.
(3) colloidal solution by above-mentioned synthesis pours into centrifuge tube, places into ultrasonic machine and carries out ultrasonic mechanical stripping 1h.
MXene colloid after ultrasound removing is centrifuged 1h at 3500rpm/min, and the supernatant of collection is MXene nanometer sheet colloid,
Concentration is determined by the amount for the deionized water being added, ultrasonic time, centrifugation time and revolving speed；
Step 4. prepares Ti3C2- MXene film
Ti is prepared using drop-coating3C2- MXene film.100 μ LTi are taken using the liquid-transfering gun of 100~1000ul first3C2-
MXene nanometer sheet colloid drops are coated in step (2) surface FTO, and setting drop coating instrument revolving speed is 1000r/s, acceleration 500r/s2,
The drop coating time is 30s, and then anneal in 100 DEG C of heating plate 5min, obtains the Ti of fine and close 100nm3C2- MXene film.
The Ti that the present embodiment is prepared3C2- MXene film is scanned Electronic Speculum (SEM) test respectively and X-ray is spread out
It penetrates (XRD), test result difference is as shown in Figure 2 and Figure 3, is schemed by SEM it can be seen that the Ti prepared3C2- MXene film extremely causes
It is close smooth.By comparing with the standard XRD pattern of MXene in document, the XRD diffracting spectrum of this patent Fig. 3 (a) is in 7 ° and 28 °
Diffraction maximum and document in standard diffraction peak (such as Fig. 3 (shown in b)) it is corresponding, it was confirmed that the thin-film material of preparation is exactly
Ti3C2-MXene.Fig. 4 (b) is two-dimentional Ti3C2The 1st day of-MXene thin-film material and the X-ray diffraction comparison for placing the 15th day
Figure confirms that the performance of material is stablized by comparing, therefore can place for a long time.
Embodiment 2
A kind of two dimension Ti of the present embodiment3C2The preparation method of-MXene thin-film material, includes the following steps:
Step 1. cleans ITO electro-conductive glass substrate
The first step is 15 Ω sq to having with a thickness of 200nm, square resistance-1ITO hearth electrode, side length be 1.5cm
Square conductive glass, which is placed in cleanser and the mixed solution of deionized water, is cleaned by ultrasonic 15min, second step, takes out ITO and leads
Electric glass, which is put into hand cleanser and the mixed liquor of deionized water, is cleaned by ultrasonic 15min, third step, and the taking-up of ITO electro-conductive glass is put
Enter and is cleaned by ultrasonic 15min in acetone, the 4th step, then ITO electro-conductive glass is put into ethanol solution and is cleaned by ultrasonic 15min.
Step 2.UV handles the surface ITO
By the above-mentioned ITO drying cleaned up, insulating tape is sticked at the edge of piece, reserved electrode is formed, then puts
30min is handled with UV ozone in UV cleaning device.The purpose of UV processing is the wetting capacity in order to improve the surface ITO.
Step 3. prepares Ti3C2- MXene colloidal solution
(1) Ti for taking 300 mesh of 1.0g ground3AlC2Powder is slowly added into the salt that 15ml mass percentage concentration is 36%
In the mixed solution of acid solution, 5ml deionized water and 1.2g LiF, magnetic stirrer is used at room temperature, makes it sufficiently
It mixes.The revolving speed of magnetic stirring apparatus is set as 500rpm/min.
(2) by above-mentioned mixed liquor at 30 DEG C, 500r/min magnetic agitation react 30h, then using centrifuge carry out from
Heart cleaning is until pH is neutrality, centrifuge speed 4000r/min, centrifugation time 5min.Last time centrifuged supernatant
Be it is blackish green, indicate Ti3C2The successful synthesis of-MXene.
(3) colloidal solution by above-mentioned synthesis pours into centrifuge tube, places into ultrasonic machine and carries out ultrasonic mechanical stripping
1.5h.MXene colloid after ultrasound removing is centrifuged 1h at 3500rpm/min, and the supernatant of collection is MXene nanometer sheet glue
Body, concentration are determined by the amount for the deionized water being added, ultrasonic time, centrifugation time and revolving speed；
Step 4. prepares Ti3C2- MXene film
Ti is prepared using drop-coating3C2- MXene film.100 μ LMXene are taken using the liquid-transfering gun of 100~1000ul first
Nanometer sheet colloid drops are coated in the ITO hearth electrode surface of step (2) acquisition, and setting drop coating instrument revolving speed is 1000r/s, and acceleration is
500r/s2, the drop coating time is 60s, and then anneal in 100 DEG C of heating plate 10min, is obtained fine and close with a thickness of 200nm's
Ti3C2- MXene film.
Embodiment 3
A kind of two dimension Ti of the present embodiment3C2The preparation method of-MXene thin-film material, includes the following steps:
Step 1. cleans AZO electro-conductive glass substrate
The first step is 20 Ω sq to having with a thickness of 300nm, square resistance-1AZO hearth electrode, side length be 2cm just
Rectangular electro-conductive glass, which is placed in cleanser and the mixed solution of deionized water, is cleaned by ultrasonic 15min, second step, and it is conductive to take out AZO
Glass, which is put into hand cleanser and the mixed liquor of deionized water, is cleaned by ultrasonic 15min, third step, and the taking-up of AZO electro-conductive glass is put into
It is cleaned by ultrasonic 15min, the 4th step in acetone, then AZO electro-conductive glass is put into ethanol solution and is cleaned by ultrasonic 15min.
Step 2.UV handles the surface AZO
By the above-mentioned AZO drying cleaned up, insulating tape is sticked at the edge of piece, reserved electrode is formed, then puts
30min is handled with UV ozone in UV cleaning device.The purpose of UV processing is the wetting capacity in order to improve the surface AZO；
Step 3. prepares Ti3C2- MXene colloidal solution
(1) Ti for taking 300 mesh of 1.0g ground3AlC2It is 37.5% that powder, which is slowly added into 20ml mass percentage concentration,
In the mixed solution of hydrochloric acid solution, 7.5ml deionized water and 1.15g LiF, magnetic stirrer is used at room temperature, makes it
It mixes well.The revolving speed of magnetic stirring apparatus is set as 500rpm/min.
(2) by above-mentioned mixed liquor at 40 DEG C, 500r/min magnetic agitation react 18h, then using centrifuge carry out from
Heart cleaning is until pH is neutrality, centrifuge speed 4000r/min, centrifugation time 5min.Last time centrifuged supernatant
Be it is blackish green, indicate Ti3C2The successful synthesis of-MXene.
(3) colloidal solution by above-mentioned synthesis pours into centrifuge tube, places into ultrasonic machine and carries out ultrasonic mechanical stripping
1.5h.MXene colloid after ultrasound removing is centrifuged 1h at 3500rpm/min, and the supernatant of collection is Ti3C2- MXene receives
Rice piece colloid, concentration is determined by the amount for the deionized water being added, ultrasonic time, centrifugation time and revolving speed；
Step 4. prepares Ti3C2- MXene film
MXene film is prepared using drop-coating.100 μ LTi are taken using the liquid-transfering gun of 100~1000ul first3C2-MXene
Nanometer sheet colloid drops are coated in step (2) AZO hearth electrode surface, and setting drop coating instrument revolving speed is 1000r/s, acceleration 500r/s2,
The drop coating time is 120s, and then anneal in 100 DEG C of heating plate 20min, obtains the fine and close Ti with a thickness of 400nm3C2-
MXene film.
Application Example 1
One kind of this application embodiment is based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, the resistance-change memory
Device successively includes glass substrate, hearth electrode, change resistance layer, top electrode from bottom to up；
Wherein: the hearth electrode material is FTO, and the resistive layer material is two dimension Ti3C2- MXene film, the top electricity
Pole material is W；
The hearth electrode with a thickness of 100nm, square resistance is 14 Ω sq-1；The change resistance layer with a thickness of 100nm,
The top electrode is with a thickness of 100nm；
The hearth electrode shape is square, side length 1cm；The change resistance layer shape is square, side length 1cm；Institute
Top electrode shape is stated as circle, diameter is 100 μm.
It is described above based on two-dimentional Ti3C2The resistance-variable storing device of-MXene thin-film material is specifically to use magnetron sputtering skill
The Ti that art is prepared in 1 step 4 of embodiment3C2- MXene film surface prepares top electrode and obtains.The specific method is as follows: using mask plate
It is covered on Ti3C2- MXene film surface is placed in magnetron sputtering apparatus, opens D. C magnetic control sputter power source, controls vacuum chamber
Interior system pressure is 4Torr, temperature 300K, under conditions of power is 100W, in Ti3C2- MXene film surface deposits W
Top electrode, sedimentation time 450s after deposition, close D. C magnetic control sputter power source, are cooled to room temperature, obtain based on two
Tie up Ti3C2The resistance-variable storing device of-MXene thin-film material.
This application embodiment resistance-variable storing device obtained above is tested using Agilent B1500A Semiconductor Parameter Analyzer
Performance.Firstly, removing the insulating tape of resistance-variable storing device, expose hearth electrode, and place it in probe station, is visited with two
Needle contacts the hearth electrode and top electrode of device respectively.Application -7V~7V dc sweeps voltage on top electrode, hearth electrode ground connection,
I-V curve is measured, as a result as shown in Figure 5.I-V curve reveals apparent bipolarity resistance transformation characteristic.One scanning voltage
Recycle includes four parts: first from 0 scanning to+7V, then from+7V scanning to 0, then reverse scan is scanned from 0 to -7V, then
From -7V scanning to 0, that is, a scan period is completed, every partial scan step number is identical, is 101.It is electric in test process in order to prevent
It flows through greatly and device breakdown, a limitation electric current, size 1mA is set in forward scan.When voltage is from 0 scanning to+7V
When, electric current gradually increases, and resistance is transformed into low resistance state by high-impedance state, this process is known as SET process, from Fig. 5 it is observed that
SET process is a progressive formation, and device has self-rectifying ability；When voltage is from 0 scanning to -7V, device can be tieed up
Low resistance state is held, when negative voltage reaches certain value, resistance is transformed into high-impedance state by low resistance state, this process is known as RESET mistake
Journey.Device is able to maintain original resistance state when power is off, illustrates that the memory is non-volatile.Meanwhile using Agilent
B1500A Semiconductor Parameter Analyzer tests the bad tolerance of following of device, i.e. continuous 700 circulations of scanning voltage, device exists
High low resistance state is still stablized under the current limliting of 5mA, keeps good resistive window, illustrates that the circulation tolerance of device and stability are good
It is good, as shown in Figure 6.
Application Example 2
One kind of this application embodiment is based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, the resistance-change memory
Device successively includes glass substrate, hearth electrode, change resistance layer, top electrode from bottom to up；
Wherein: the hearth electrode material is ITO, and the resistive layer material is two dimension Ti3C2- MXene thin-film material, it is described
Top electrode material is Au；
The hearth electrode with a thickness of 200nm, square resistance is 15 Ω sq-1；The change resistance layer with a thickness of 200nm,
The top electrode is with a thickness of 80nm；
The hearth electrode shape is square, side length 1.5cm；The change resistance layer shape is square, and side length is
1.5cm；The top electrode shape is circle, and diameter is 500 μm.
It is described above based on two-dimentional Ti3C2The resistance-variable storing device of-MXene thin-film material is specifically to use magnetron sputtering skill
The Ti that art is prepared in 2 step 4 of embodiment3C2- MXene film surface prepares top electrode and obtains.The specific method is as follows: using mask plate
It is covered on Ti3C2- MXene film surface is placed in magnetron sputtering apparatus, opens D. C magnetic control sputter power source, controls vacuum chamber
Interior system pressure is 4Torr, temperature 300K, under conditions of power is 100W, in Ti3C2- MXene film surface deposition
Au top electrode, sedimentation time 360s after deposition, close D. C magnetic control sputter power source, are cooled to room temperature, obtain and be based on
Two-dimentional Ti3C2The resistance-variable storing device of-MXene thin-film material.
Application Example 3
One kind of this application embodiment is based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, the resistance-change memory
Device successively includes glass substrate, hearth electrode, change resistance layer, top electrode from bottom to up；
Wherein: the hearth electrode material is AZO, and the resistive layer material is two dimension Ti3C2- MXene thin-film material, it is described
Top electrode material is Pt；
The hearth electrode with a thickness of 300nm, square resistance is 20 Ω sq-1；The change resistance layer with a thickness of 400nm,
The top electrode is with a thickness of 60nm；
The hearth electrode shape is square, side length 2cm；The change resistance layer shape is square, side length 2cm；Institute
Top electrode shape is stated as circle, diameter is 900 μm.
It is described above based on two-dimentional Ti3C2The resistance-variable storing device of-MXene thin-film material is specifically to use magnetron sputtering skill
The Ti that art is prepared in 3 step 4 of embodiment3C2- MXene film surface prepares top electrode and obtains.The specific method is as follows: using mask plate
It is covered on Ti3C2- MXene film surface is placed in magnetron sputtering apparatus, opens D. C magnetic control sputter power source, controls vacuum chamber
Interior system pressure is 4Torr, temperature 300K, under conditions of power is 100W, in Ti3C2- MXene film surface deposition
Pt top electrode, sedimentation time 270s after deposition, close D. C magnetic control sputter power source, are cooled to room temperature, obtain and be based on
Two-dimentional Ti3C2The resistance-variable storing device of-MXene thin-film material.
The performance of resistance-variable storing device made from Application Example 2~3 is tested, test result is shown, application implementation
The performance of device made from example 2~3 and the performance for the resistance-variable storing device that Application Example 1 obtains are essentially identical, have good
Change resistance performance and tolerance.
Claims (10)
1. a kind of two dimension Ti3C2The preparation method of-MXene thin-film material, characterized by the following steps:
(1) Ti is prepared3C2- MXene nanometer sheet colloidal solution
Titanium aluminium carbon dust is added in the mixed solution being made of hydrochloric acid solution, deionized water and lithium fluoride according to the ratio, room temperature
Mixed reaction solution is obtained after mixing evenly；Then gained mixed reaction solution is heated to 30~40 DEG C, under agitation constant temperature
18~30h is reacted, after reaction, is neutrality by product centrifugation, cleaning to cleaning solution, obtains Ti3C2- MXene colloidal solution；
Again by the Ti3C2- MXene colloidal solution is ultrasonically treated 0.5~2h, obtains the Ti3C2- MXene nanometer sheet colloid is molten
Liquid；
(2) Ti is prepared3C2- MXene film
The Ti that step (1) is obtained3C2Electrically conducting transparent of-MXene nanometer sheet colloidal solution the drop coating in pretreated clean dried
Substrate surface after drop coating, is coated with Ti3C2The electrically conducting transparent substrate of-MXene nanometer sheet colloidal solution is transferred to heating
On plate, 2~10min is made annealing treatment under the conditions of 95~105 DEG C, obtains Ti3C2- MXene film.
2. two dimension Ti according to claim 13C2The preparation method of-MXene thin-film material, it is characterised in that: step (1)
The mass ratio of the titanium aluminium carbon and lithium fluoride is 1:1~1.5.
3. two dimension Ti according to claim 13C2The preparation method of-MXene thin-film material, it is characterised in that: step (1)
The amount ratio of the titanium aluminium carbon and hydrochloric acid is 1 mass parts: (10~20) parts by volume is with g between the mass parts and parts by volume:
ML is as benchmark.
4. any one of claims 1 to 3 two dimension Ti3C2The two dimension that the preparation method of-MXene thin-film material is prepared
Ti3C2- MXene thin-film material.
5. the two-dimentional Ti that any one of claims 1 to 3 the method is prepared3C2- MXene thin-film material is that change resistance layer is hindering
Application in transition storage.
6. one kind is based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, it is characterised in that: the resistive memory
It from bottom to up successively include hard substrates, hearth electrode, change resistance layer, top electrode, in which: the resistive layer material is claim 1
The two-dimentional Ti that any one of~3 the methods are prepared3C2- MXene film.
7. according to claim 6 be based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, it is characterised in that: institute
The hearth electrode material stated is any one of FTO, ITO, ZTO or AZO；The top electrode material is any in Pt, Au or W
Kind.
8. according to claim 6 be based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, it is characterised in that: institute
The hearth electrode stated with a thickness of 100~300nm, 100~450nm of thickness of the change resistance layer, the top electrode with a thickness of
60~100nm.
9. according to claim 6 be based on two dimension Ti3C2The resistance-variable storing device of-MXene thin-film material, it is characterised in that: institute
The shape of hearth electrode is stated as round or rectangle, diameter or side length are 50nm~2cm；The shape of the change resistance layer is round or square
Shape, diameter or side length are 50nm~2cm；The shape of the top electrode is round or rectangle, and diameter or side length are 100~900 μ
m。
10. being based on two dimension Ti described in any one of claim 6~93C2The preparation side of the resistance-variable storing device of-MXene thin-film material
Method, it is characterised in that: the described method comprises the following steps:
Step 1: cleaning substrate
There is the substrate of hearth electrode material that deionized water, acetone, ethyl alcohol is successively used to be cleaned by ultrasonic in Ultrasound Instrument growth, dries up；
Step 2: reserved electrode
Insulating cement is pasted at the cleaned hearth electrode material one side edge of step 1；
Step 3: preparing change resistance layer
(a) Ti is prepared3C2- MXene nanometer sheet colloidal solution
Titanium aluminium carbon dust is added in the mixed solution being made of hydrochloric acid solution, deionized water and lithium fluoride according to the ratio, room temperature
Mixed reaction solution is obtained after mixing evenly；Then gained mixed reaction solution is heated to 30~40 DEG C, under agitation constant temperature
18~30h is reacted, after reaction, is neutrality by product centrifugation, cleaning to cleaning solution, obtains Ti3C2- MXene colloidal solution；
Again by the Ti3C2- MXene colloidal solution is ultrasonically treated 0.5~2h, obtains the Ti3C2- MXene nanometer sheet colloid is molten
Liquid；
(b) Ti is prepared3C2- MXene film change resistance layer
The Ti that step (a) is obtained3C2The hearth electrode table of-MXene nanometer sheet colloidal solution drop coating in pretreated clean dried
Face after drop coating, is coated with Ti3C2The substrate of-MXene nanometer sheet colloidal solution is transferred in heating plate, 95~105
2~20min is made annealing treatment under the conditions of DEG C, obtains Ti3C2- MXene film change resistance layer；
Step 4: preparing top electrode
Top electrode is deposited in resistive layer surface using magnetron sputtered deposition technology.
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Application publication date: 20190806 |