CN107331771B - A kind of low energy consumption, multi-functional Multilayered Nanowires resistance-variable storing device - Google Patents
A kind of low energy consumption, multi-functional Multilayered Nanowires resistance-variable storing device Download PDFInfo
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- 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
- H10N70/20—Multistable switching devices, e.g. memristors
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H10N70/011—Manufacture or treatment of multistable switching devices
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- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
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Abstract
The present invention provides a kind of low energy consumption, multi-functional Multilayered Nanowires resistive material and its preparation method and application, which includes the conductive layer and insulating layer along the arrangement of nano wire longitudinal periodicity.The present invention increases the defects of insulating layer number by being distributed the magnetic conductive particle of certain amount in its insulating layer initiatively.When material of the invention is used to prepare resistance-variable storing device, these defects facilitate the formation of conductive filament under DC Electric Field, to reduce the operation voltage that electroluminescent resistive effect is answered, make its shift voltage from high-impedance state to low resistance state down to 1.2 ± 0.2V, low resistance state is to the shift voltage of high-impedance state down to -0.56 ± 0.14V, and electric excitation process is not needed before resistive test, effectively reduces energy consumption.Moreover, before and after electroluminescent resistive, the magnetism of the device also has certain modulation.Therefore, which is a kind of multifunction device that should and can carry out Effective Regulation to magnetism with the electroluminescent resistive effect of low energy consumption.
Description
Technical field
The invention belongs to memory technology fields, and in particular to a kind of low energy consumption, multi-functional Multilayered Nanowires resistive are deposited
Reservoir.
Background technique
In recent years, it is received based on the resistance-variable storing device that electroluminescent resistive effect is answered as a kind of novel nonvolatile memory
The extensive concern of academia and industry.Electroluminescent resistive phenomenon is present in many binary oxide thin-film materials, which produces
Raw reason is often related with the formation of conductive filament and disconnection.It is many study found that conductive filament in binary oxide thin-film material
It is randomly formed, it is unstable so as to cause the electroluminescent change resistance performance of thin-film material, seriously affect its application.Moreover, very
Polyoxide, which is required to biggish driving voltage, could generate electroluminescent resistive behavior, so that resistance-variable storing device as made from it is being surveyed
Try and driving voltage must be imposed before to carry out activation operation, this increases energy consumption to a certain extent.Therefore, there is an urgent need to
Exploitation design low energy consumption, high stability new material meet the needs of resistive device practical application.
One-dimensional nano line can receive conductive filament local area control since electronics transmits in the channel by space constraints
In rice noodles, reduce the randomness that conductive filament is formed.Energy when being designed into nanowire array structure applied to electroluminescent resistive device
Enough effectively to solve the problems, such as that electroluminescent change resistance performance is unstable, every nano wire all can be used as a storage unit in addition, thus
Storage density will also be increased substantially.However, the operation voltage of traditional nanowire resistance change memory is all higher, and resistive is surveyed
The electric excitation process that a higher voltage is also needed before examination, it is high not can not still to solve binary oxide thin-film material energy consumption
Foot.For this purpose, technical paper " Using binary resistors to achieve multilevel resistive
switching in multilayer NiO/Pt nanowire arrays(NPG Asia Materials,2014,6:
E85 a kind of preparation method of NiO/Pt Multilayered Nanowires resistance-variable storing device is disclosed in) ", this method uses porous anode
Aluminium obtains Ni/Pt multi-layer nano by the way that W metal and Pt metal are carried out alternating deposit in the template duct as template
Line, then by Ni complete oxidation, NiO/Pt multi-layer nano linear array is obtained, and be made using this nano-wire array as resistive medium
Multilayered Nanowires resistance-variable storing device.Multilayered Nanowires arranged regular in resistance-variable storing device made from above-mentioned technology, and the resistive
The operation voltage of memory is smaller, shift voltage (V of the high-impedance state to low resistance stateSET) down to 3.24V, and low resistance state is to high resistant
Shift voltage (the V of stateRESET) down to -1.20V.Unfortunately, the resistance-variable storing device in above-mentioned technology is surveyed in resistive
Still need the process of an electric excitation before examination, and driving voltage is~15V, this is undoubtedly also increased energy consumption.So
How resistance-variable storing device in test and use required greater energy consumption is effectively reduced, and being that current this field is urgently to be resolved asks
Topic.
Summary of the invention
Technical problem to be solved by the present invention lies in overcome existing Multilayered Nanowires resistance-variable storing device testing and making
The higher problem of used time energy consumption, so provide one kind can be greatly reduced operation voltage, do not need electric excitation process and be able to achieve electricity/
The Multilayered Nanowires resistance-variable storing device of the double store functions of magnetic.
Present invention technical solution used for the above purpose is as follows:
A kind of nanowire resistance change material, it is described exhausted including the conductive layer and insulating layer arranged along nano wire longitudinal periodicity
Edge layer is made of insulating layer ontology and the random magnetic conductive particle being scattered in the insulating layer ontology.
The content of magnetic conductive particle is regulated and controled by changing the temperature and time of oxidation in the insulating layer.
The material of the magnetic conductive particle is one of iron, cobalt, nickel or a variety of.
The material of the insulating layer ontology is one of iron, cobalt, nickel or a variety of oxides.
The thickness of each insulating layer is 20~100nm.
The arrangement period number of the insulating layer is 50~300.
The thickness of each conductive layer is 5~30nm.
A method of preparing nanowire resistance change material above-mentioned, comprising:
Use electrochemical deposition normal direction with two kinds of conductive materials of alternating deposit in the insulation template of through-hole structure with respectively
The precursor of the conductive layer and the insulating layer is formed, to obtain nano-wire array;
Expanding treatment is carried out to the template, incomplete oxidation then is carried out to the nano-wire array in oxygen-containing atmosphere
So that the precursor of the insulating layer is changed into the insulating layer, the nanowire resistance change material is obtained.
By the nano-wire array temperature programming to 300~800 DEG C, 10~20h is kept the temperature under steady temperature, is allowed to incomplete
Oxidation;
Preferably, in described program temperature-rise period, heat preservation operation is carried out at a temperature of each whole hundred;Wherein, at 100 DEG C
When with 200 DEG C, soaking time is 0.5~2h, and at 300 DEG C or more, soaking time is 20~80min.
A kind of Multilayered Nanowires resistance-variable storing device, including hearth electrode, top electrode, and it is located at the hearth electrode and the top
The both ends of resistive dielectric layer between electrode, the resistive dielectric layer are connected with the hearth electrode and the top electrode respectively, institute
Resistive dielectric layer is stated to be made of nanowire resistance change material above-mentioned.
Above-mentioned technical proposal of the invention has the advantage that
1, nanowire resistance change material of the present invention, the magnetism for being distributed certain amount in its insulating layer initiatively are led
Electric particle counts to increase the defects of insulating layer, and when applying extra electric field, these magnetic conductive particles, which can not only serve as, is led
The presoma of the electrical filament and migration for facilitating oxonium ion forms conductive filament, to significantly reduce the operation electricity of resistance-variable storing device
Pressure, makes shift voltage (V of its high-impedance state to low resistance stateSET) down to 1.2 ± 0.2V, low resistance state turns to the shift voltage of high-impedance state
(VRESET) down to -0.56 ± 0.14V, and the step of applying driving voltage to carry out activation operation can be also omitted, it effectively reduces
Energy consumption.
2, nanowire resistance change material of the present invention is controlled in insulating layer by adjusting the temperature and time of oxidation
Conductive particle content maximumlly increases defect number while to ensure insulating layer insulation performance, to be more advantageous to reduction resistance
The energy consumption of transition storage.
3, nanowire resistance change material of the present invention selects the material of conductive particle for magnetic metal iron, cobalt, nickel, this
In material its magnetism while electroluminescent resistive effect is answered, which occurs, for sample can also change, and that is to say nanowire resistance change of the present invention
The resistance states and magnetic state of material can be achieved at the same time resistance-change memory and magnetic storage by regulating and controlling voltage.Cause
This, the present invention can provide important references further to widen the application of random access memory.
4, the preparation method of nanowire resistance change material of the present invention, by control oxidizing condition to nano-wire array into
Thus row incomplete oxidation can obtain nanowire resistance change material.Preparation method of the invention is simple, easily operated, very suitable
In industrial applications and promote.
Detailed description of the invention
Fig. 1 a is the top view of the scanning electron microscope (SEM) photograph of Ni/Pt multi-layer nano linear array in embodiment 1;
Fig. 1 b is the sectional view of the scanning electron microscope (SEM) photograph of Ni/Pt multi-layer nano linear array in embodiment 1;
Fig. 2 is Ni/Pt Multilayered Nanowires and NiO in embodiment 1xThe X ray diffracting spectrum of/Pt Multilayered Nanowires;
Fig. 3 is NiO in embodiment 1xThe current -voltage curve figure of/Pt Multilayered Nanowires resistance-variable storing device;
Fig. 4 is NiO in embodiment 1xThe data retention test effect figure of/Pt Multilayered Nanowires resistance-variable storing device;
Fig. 5 is NiO in embodiment 1x/ Pt Multilayered Nanowires resistance-variable storing device is under low resistance state (LRS) and high-impedance state (HRS)
It is parallel to the hysteresis loop figure in nano wire direction.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
In addition, technical characteristic involved in invention described below different embodiments is as long as they do not conflict with each other
It can be combined with each other.
Embodiment 1
Present embodiments provide a kind of NiOxThe preparation method of/Pt Multilayered Nanowires resistance-variable storing device, includes the following steps:
(1) porous anodic aluminium oxide (PAA) template is prepared using anodizing twice:
Firstly, by high-purity aluminium flake (99.999%) 4 × 10-4Under the vacuum condition of Pa, 500 DEG C of annealing 2h;After annealing
PAA template at 10 DEG C, electrobrightening 3min is carried out in the mixed solution (volume ratio 1:4) of perchloric acid and dehydrated alcohol;
Again using the aluminium flake after polishing as anode, graphite plate as cathode, 0.3mol/L oxalic acid as electrolyte, 5 DEG C, 40V it is constant
Anodic oxidation twice is carried out to aluminium flake under voltage, the time is 5 hours;Then, by volume using saturation copper chloride and hydrochloric acid
The mixed solution of 4:1 is reacted with aluminium base, removes aluminium base;Then through-hole and reaming, time are carried out with the phosphoric acid solution of 5wt% again
For 50min, the PAA template of bilateral is obtained;Finally, the method using magnetron sputtering is led in one layer of Pt of back spatter of PAA template
For electric layer as hearth electrode, operating vacuum degree is 1 × 10-4Pa, power 20W, Ar flow be 40scc, sputtering time 2000s,
Sputter rate is 0.075nm/s, and hearth electrode is with a thickness of 150nm.
(2) Ni/Pt multi-layer nano linear array is prepared:
Silver conductive adhesive is used to be sticked on backing material as work electricity step (1) the PAA template obtained with hearth electrode
Pole deposits Ni/Pt Multilayered Nanowires using the three-electrode system of electrochemical workstation in template duct, and Pt is used as to electrode,
Saturated calomel electrode is reference electrode, and electroplate liquid is 2mol/L NiSO4·6H2O、3mmol/L H2PtCl4、0.5mol/L
H3BO3Mixed solution.Depositing temperature is 22 DEG C, and the potential for depositing Ni is -1.3V, and the potential for depositing Pt is -0.29V, each Pt
Layer with a thickness of 10nm, alternate change deposition potential, deposition cycle is 200, be made with hearth electrode Ni/Pt Multilayered Nanowires
Array.
(3) corrosion and reaming of template in the Ni/Pt multi-layer nano linear array of hearth electrode are had:
Above-mentioned Ni/Pt multi-layer nano linear array is immersed in the phosphoric acid of 30 DEG C of 6.0wt% and the mixing of 1.8wt% chromic acid
Corrode 90min in solution, removes the part that wherein PAA template does not deposit Ni/Pt Multilayered Nanowires;Then 30 DEG C are immersed in
6.0wt% phosphoric acid,diluted in PAA template carry out reaming 15min, make occur one between Ni/Pt Multilayered Nanowires and template hole wall
Fixed gap.
(4) Ni/Pt multi-layer nano linear array is subjected to incomplete oxidation and NiO is madex/ Pt multi-layer nano linear array:
The Ni/Pt multi-layer nano linear array for completing reaming is put into the tube furnace of air atmosphere, temperature programming is carried out, is risen
Warm rate is 5 DEG C/min, keeps the temperature 2h at 100 DEG C, 200 DEG C respectively, keeps the temperature 1.5h at 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C
Steady temperature under aoxidize 10h, obtain NiOx/ Pt multi-layer nano linear array, wherein each NiOxLayer with a thickness of 40nm.
(5) in NiOxTop electrode is arranged in/Pt Multilayered Nanowires array top:
The NiO that step (4) is obtainedxThe multi-layer nano linear array bottom /Pt is viscous on a si substrate, utilizes Ar Ion Beam Etching
For technology to 3min is performed etching at the top of nano wire, the mask plate that then covering diameter is 500 μm at the top of it utilizes magnetron sputtering
Technology deposits Pt top electrode, and top electrode obtains NiO with a thickness of 40nmx/ Pt Multilayered Nanowires array memory.
Respectively to Ni/Pt Multilayered Nanowires obtained above and NiOx/ Pt Multilayered Nanowires have carried out XRD test, survey
Test result is as shown in Fig. 2, NiOxIn/Pt Multilayered Nanowires other than the presence for having NiO, there are also a small amount of Ni simple substance to exist.
To NiO obtained abovex/ Pt Multilayered Nanowires array memory carries out electroluminescent change resistance performance test, and hearth electrode connects
Ground tests its current-voltage (I-V) curve to top electrode making alive, and has carried out stability test, and test result is respectively as schemed
Shown in 3 and Fig. 4, according to Fig. 3 and Fig. 4, NiO made from the present embodimentxThe electroluminescent resistive of/Pt Multilayered Nanowires array memory
It can be as follows:
(1)VSETFor 1.2 ± 0.2V, VRESETFor -0.56 ± 0.14V;
(2) NiO obtained byx/ Pt Multilayered Nanowires array memory does not need electric excitation process, reaches for the first time in voltage
It observed transformation of the high-impedance state (HRS) to low resistance state (LRS) when 1.2V;
(3) on-off ratio is about 1 × 103;
The above results show memory provided by the present embodiment, and the presence of Ni simple substance increases lacking for resistive dielectric layer
Number is fallen into, makes not needing electric excitation process before resistive test, electroluminescent resistance can occur when external voltage reaches 1.2V for the first time
Change effect.
The present embodiment is also to NiO obtained abovexThe HRS and LRS of/Pt Multilayered Nanowires array memory are carried out respectively
Magnetic Test, the hysteresis loop obtained on being parallel to its nano wire direction are as shown in Figure 5, the results showed that:
Before and after electroluminescent resistive, the magnetism of the memory is also changed.Saturation magnetization (Ms) and coercivity under LRS
(Hc) value being both greater than under HRS.
Embodiment 2
FeO provided in this embodimentxThe preparation method of/Au Multilayered Nanowires resistance-variable storing device is similar to Example 1, different
Place is that electrochemical deposition is metallic iron, by the condition of its incomplete oxidation are as follows: programmed rate is 10 DEG C/min,
Respectively in 100 DEG C, 200 DEG C of each heat preservation 0.5h, in 300 DEG C of heat preservation 20h to get to FeOx/ Au Multilayered Nanowires resistance-variable storing device.
FeO made from the present embodimentxIn/Au Multilayered Nanowires resistance-variable storing device, each FeOxThe thickness of insulating layer is
100nm, the thickness of each Au conductive layer are 30nm, FeOxThe arrangement period number of/Au is 50.
Embodiment 3
CoO provided in this embodimentxThe preparation method of/Pt Multilayered Nanowires resistance-variable storing device is similar to Example 1, different
Place is that electrochemical deposition is metallic cobalt, by the condition of its incomplete oxidation are as follows: programmed rate is 10 DEG C/min,
Respectively in 100 DEG C, 200 DEG C of each heat preservation 1h, 1h, 800 DEG C of heat preservations are kept the temperature respectively in 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C
15h to get arrive CoOx/ Pt Multilayered Nanowires resistance-variable storing device.
CoO made from the present embodimentxIn/Pt Multilayered Nanowires resistance-variable storing device, each CoOxThe thickness of insulating layer is
20nm, the thickness of each Pt conductive layer are 5nm, CoOxThe arrangement period number of/Pt is 300.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
Variation is still in the protection scope of this invention.
Claims (7)
1. a kind of nanowire resistance change material, including the conductive layer and insulating layer arranged along nano wire longitudinal periodicity, feature exists
In the insulating layer is made of insulating layer ontology and the random magnetic conductive particle being scattered in the insulating layer ontology;
The preparation method of the nanowire resistance change material includes:
Use electrochemical deposition normal direction with two kinds of conductive materials of alternating deposit in the insulation template of through-hole structure to be respectively formed
The precursor of the conductive layer and the insulating layer, to obtain nano-wire array;
To the template carry out expanding treatment, then in oxygen-containing atmosphere to the nano-wire array carry out incomplete oxidation so that
The precursor of the insulating layer is changed into the insulating layer, obtains the nanowire resistance change material;
By the nano-wire array temperature programming to 300~800 DEG C, 10~20h is kept the temperature under steady temperature, is allowed to endless total oxygen
Change;
In described program temperature-rise period, heat preservation operation is carried out at a temperature of each whole hundred;Wherein, in 100 DEG C and 200 DEG C,
Soaking time is 0.5~2h, and at 300 DEG C or more, soaking time is 20~80min.
2. nanowire resistance change material according to claim 1, which is characterized in that the material of the magnetic conductive particle is
One of iron, cobalt, nickel are a variety of.
3. nanowire resistance change material according to claim 1, which is characterized in that the material of the insulating layer ontology be iron,
One of cobalt, nickel or a variety of oxides.
4. nanowire resistance change material according to claim 1-3, which is characterized in that the thickness of each insulating layer
Degree is 20~100nm.
5. nanowire resistance change material according to claim 1-3, which is characterized in that the arrangement week of the insulating layer
Issue is 50~300.
6. nanowire resistance change material according to claim 1-3, which is characterized in that the material of the conductive layer is
Gold or platinum, the thickness of each conductive layer is 5~30nm.
7. a kind of Multilayered Nanowires resistance-variable storing device, including hearth electrode, top electrode, and it is located at the hearth electrode and top electricity
The both ends of resistive dielectric layer between pole, the resistive dielectric layer are connected with the hearth electrode and the top electrode respectively, special
Sign is: the resistive dielectric layer is made of nanowire resistance change material described in any one of claims 1-6.
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