CN105591028B - A kind of preparation method using LTCC greens band as the single-layer nano-film memristor of substrate - Google Patents
A kind of preparation method using LTCC greens band as the single-layer nano-film memristor of substrate Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000002356 single layer Substances 0.000 title claims abstract description 39
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- 239000010408 film Substances 0.000 claims description 37
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 229910052697 platinum Inorganic materials 0.000 claims description 30
- 239000010409 thin film Substances 0.000 claims description 27
- 239000010410 layer Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 17
- 229910052709 silver Inorganic materials 0.000 claims description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 11
- 229910052725 zinc Inorganic materials 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 9
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000013077 target material Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
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- 235000013339 cereals Nutrition 0.000 claims 2
- 235000009566 rice Nutrition 0.000 claims 2
- 230000008859 change Effects 0.000 abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 13
- -1 oxonium ion Chemical class 0.000 abstract description 9
- 238000006467 substitution reaction Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
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- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 76
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Inorganic materials [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
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- 230000008021 deposition Effects 0.000 description 6
- 238000004549 pulsed laser deposition Methods 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 230000006870 function Effects 0.000 description 4
- 238000001755 magnetron sputter deposition Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 3
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- 238000011161 development Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
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- 238000003825 pressing Methods 0.000 description 2
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- 239000000377 silicon dioxide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000013528 artificial neural network Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- 210000002569 neuron Anatomy 0.000 description 1
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- 230000007935 neutral effect Effects 0.000 description 1
- 229910021650 platinized titanium dioxide Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 210000000225 synapse Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000011800 void material Substances 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11C—STATIC STORES
- G11C13/00—Digital stores characterised by the use of storage elements not covered by groups G11C11/00, G11C23/00, or G11C25/00
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11C—STATIC STORES
- G11C13/00—Digital stores characterised by the use of storage elements not covered by groups G11C11/00, G11C23/00, or G11C25/00
- G11C13/0002—Digital stores characterised by the use of storage elements not covered by groups G11C11/00, G11C23/00, or G11C25/00 using resistive RAM [RRAM] elements
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- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mathematical Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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Abstract
The invention discloses a kind of preparation method using LTCC greens band as the single-layer nano-film memristor of substrate, with single-layer nano-film memristor, caused hole and ionization oxonium ion under bias are carrier for it, by the change of hole and ionized oxygen ion generation amount, to realize the principle of the change of device resistance, set about from standby simplified technique and in terms of improving resistive film raw material formula two：The advance sintering step of resistive film ceramic material is eliminated, from the lower ceramic raw material of sintering temperature, with reference to using lower calcining heat；And by with X2+Part substitution Ti4+B position substitutions are carried out, are measured with increasing the asymmetry of resistive membrane molecule structure and internal hole；And use the plated film on LTCC green bands to form the series technique means such as " flexibility " bottom electrode, simplify preparation technology, improve production efficiency, and energy consumption and manufacturing cost are reduced, greatly improve the memristor performance of memristor.
Description
Technical field
The present invention relates to a kind of preparation method of single-layer nano-film memristor, more particularly to it is a kind of using LTCC greens band as
The preparation method of the single-layer nano-film memristor of substrate；Belong to micro-nano electronic device and nonlinear circuit application field.
Background technology
Memristor (memory resistor) is that relay resistance, electric capacity and inductance enter the 4th kind of passive circuit member behind mainstream electronic field
Part, it is a passive electric circuit element related to magnetic flux and electric charge.Early in 1971, international nonlinear circuit and cellular neural
Network theory pioneer, integralities of the Leon Chua (Cai Shaotang) based on Circuit theory in logic, has theoretically foretold memristor
Presence.2008, memristor antetype device was experimentally constructed first by HP Lab, it was confirmed that Leon Chua are relevant
The theory of memristor, cause worldwide strong interest.Memristor has novel non-linear electric property, and has concurrently
The features such as density is high, size is small, low in energy consumption, non-volatile, it is considered to be development new nonvolatile storage technologies of future generation
One of ideal scheme.Thus as the study hotspot in the fields such as information, material.In addition, the resistive behavior of memristor and organism
Neural plasticity has the similitude of height, thus in the bionical device of development nerve synapse and neuromorphic computer etc. tool
It is potential.
The structure of existing memristor is that Hewlett-Packard laboratory researchers publish in May, 2008《It is natural》Magazine
On publish thesis it is middle nano level two-layer titanium dioxide semiconductive thin film is clipped in by between two nano wires made of Pt, Sanming City
Control structure.Well-known memristor modeling is actually a nonlinear resistor for having memory function.Pass through control
The change of electric current processed can change its resistance, if high value is defined as " 1 ", low resistance is defined as " 0 ".Then this resistance can
To realize the function of data storage.Generally acknowledged memristor modeling is nano level scarce by pressing from both sides one layer between two Pt nano wires
Oxygen titanium deoxid film and neutral titanium deoxid film are formed, although simple in construction, switching speed compares relatively low.Although
Memristor research in recent years achieves larger progress, but we will also see, for the circuit element basic as one, recall
Resistance device research just starts to walk, and is mainly manifested in the following aspects：
(1) constantly there are new memristor material and memristor system report, but the memristor model of physics realization at present in recent years
It is also seldom and relatively single, it there is no unified Universal Model that memristor behavior is described.
The memristor in kind reported in recent years is applied both for certain class greatly or simulates certain function, as high density is non-volatile
Property memory, Crossbar Latch (intersect dot matrix gate) technology, analog neuron cynapse, and propose.It is used mostly
The switch models and working mechanism similar with HP memristors, and complex manufacturing technology, cost are high, it is special for research memristor
Property, memristor Circuit theory and design of electronic circuits etc. be without general and universality.
(2) not yet realize and commercially produce at present.
Most researchers be difficult to obtain a real memristor element, cause Many researchers research memristor and
During memristor circuit, the hardware experiments in real physical meaning can not be carried out in default of memristor element, be more to rely on
Emulation or analog circuit carry out experimental study.However, memristor simulation model and analog circuit are from actual memristor characteristic
Differ greatly, the hardware carried out with analog circuit realizes more consider and simulation memristor mathematical modeling and have ignored memristor
The intrinsic physical trait of device.
(3) preparation for the memristor in kind reported, require that height, condition are severe in raw material selection and process of preparing
Quarter, condition in general laboratory or R＆D institution are difficult to the preparation for completing related memristor element in kind.
It is in the prior art, more advanced in the physics realization of memristor, Chinese patent application CN103594620A
A kind of single-layer nano-film memristor and preparation method thereof is disclosed, its mode based on physics realization is prepared with composite bed
The memristor of structure type, specific preparation method：Using CaCO3, SrCO3And TiO3Make raw material, sintered at 900-1300 DEG C
15-240min, prepare Ca(1-x)SrxTiO3-δCeramic material, then with Ca(1-x)SrxTiO3-δMake target (wherein, 0<x<1,0<
δ<3), using magnetically controlled sputter method in Pt/TiO2/SiO2Plated film on/Si substrates, the thickness of plated film is 20-900nm, then through 700-
800 DEG C of heat treatment 10-30min；Finally in Ca(1-x)SrxTiO3-δLast layer electrode is plated on nano thin-film.
The essence of its technical scheme, it is exactly generally：First prepare the Ca as target(1-x)SrxTiO3-δ(wherein, 0<
x<1,0<δ<3) ceramic material, after with the Ca(1-x)SrxTiO3-δCeramic material makees target, using magnetically controlled sputter method in Pt/
TiO2/SiO2Plated film on/Si substrates, finally again in Ca(1-x)SrxTiO3-δLast layer electrode is plated on nano thin-film.
The preparation method of above-mentioned technical proposal, its major defect and deficiency are：
1st, prepared memristor memristor poor-performing.
Reason is, its change resistance layer：Ca(1-x)SrxTiO3-δNano thin-film is with Ca(1-x)SrxTiO3-δCeramic material makees target
Material (wherein, 0<x<1,0<δ<3), it is deposited on using magnetically controlled sputter method in lower electrode surface.
The individual layer nanometer film of this structure type, it is that pottery is sintered into the calcining by higher temperature (900-1300 DEG C)
Ceramic material Ca(1-x)SrxTiO3-δFor target, then by magnetron sputtering deposition on bottom electrode base material, its material itself knot
Structure is fine and close, and lattice defect and number of cavities are on the low side.
2nd, preparation technology is complicated, long preparation period, and energy consumption is higher：
Reason is that its preparation technology needs first to calcine at a high temperature of 900-1300 DEG C, prepares Ca(1-x)SrxTiO3-δ
Ceramic material target；After magnetron sputtering shaping, it is also necessary to be heat-treated 10-30min at 700-800 DEG C again.
3rd, obtained memristor material is hard and crisp, not readily transportable easily because collision causes to rupture or damages.
In addition, also there is the problem of process conditions are relatively harsh, and ratio defective product is relatively low and deficiency in it.
The content of the invention
It is an object of the present invention to provide one kind be easy to physics realization, preparation technology is simple, control difficulty is small, steady quality,
Production efficiency is high, the cheap preparation method using LTCC greens band as the single-layer nano-film memristor of substrate of cost, and it is made
There is certain flexible for the memristor gone out, be easy to integrate using LTCC technology, and be suitable to general circuit theoretical research and electricity
Road design, there is general and universality.
The present invention the first technical scheme used to achieve the above object is, a kind of using LTCC greens band as substrate
The preparation method of single-layer nano-film memristor, it is characterised in that comprise the following steps：
The first step, Ba (Ti are prepared using hydro-thermal method1-yXy)O3-yTarget, comprise the following steps that：
(1), raw material mixes：
By Ba (NO3)2、Ti(OC4H9)4With X (NO3)2, by 1: (1-y): y mixed in molar ratio, wherein, X Mg, Zn,
Ca, 0.0001≤y≤0.03 are standby；
Said mixture is dissolved in 10%-20% dust technology, is placed on magnetic stirring apparatus, is stirred, makes its complete
Fully dissolved；
(2), prepared by powder
NaOH solution is slowly added dropwise into above-mentioned solution until precipitation is complete, filtering is precipitated and is washed with deionized, and is dripped
Add NaOH solution and adjust pH value, and be fitted into reactor, be put into and reach in advance in the thermostatic drying chamber of 150 DEG C of temperature,
Hydro-thermal reaction 24 hours；
After hydro-thermal reaction, reactor is naturally cooled into room temperature, by reactor gained sample with deionized water repeatedly
Cleaning obtains Ba (Ti until removing all soluble-salts after being dried at 60 DEG C1-yXy)O3-yPowder；
(3), it is granulated：
In Ba (Ti1-yXy)O3-yPoly-vinyl alcohol solution is added in powder as binding agent, after uniform mixing, 40 mesh sieves is crossed and enters
Row is granulated；
Wherein：The mass percent concentration of poly-vinyl alcohol solution is 2-5%；The addition of poly-vinyl alcohol solution and above-mentioned baking
The mass ratio of powder after dry is 2-5: 100；
(4), target material moulding：
Compound after granulation is placed on tablet press machine and is pressed into bulk；
Then, gained bulk compound is cut into a diameter of 20-150mm, the highly slice of cylinder for 2-10mm, produces Ba
(Ti1-yXy)O3-yTarget；
Second step, the preparation of bottom electrode：
Take LTCC greens band substrate, using Pt or Au as target, using pulse laser method or magnetically controlled sputter method, by Pt or
Au is deposited on LTCC greens band substrate, forms the bottom electrode that material is Pt or Au；
3rd step, the preparation of individual layer nanometer memristor film：
By obtained Ba (Ti1-yXy)O3-yNano-mixture target, using pulse laser method or magnetically controlled sputter method,
By Ba (Ti1-yXy)O3-yIt is deposited on the surface of bottom electrode；
Then, 10-30 minutes are heat-treated at 700-900 DEG C, it is Ba (Ti to obtain chemical composition1-yXy)O3-yIndividual layer pottery
Porcelain nano thin-film, as individual layer nanometer memristor film；
4th step, the target using material as Au, Ag or Pt, using pulse laser method or magnetically controlled sputter method, by Au,
It is Ba (Ti that Ag or Pt, which is deposited on above-mentioned chemical composition,1-yXy)O3-ySingle-layer ceramic nano thin-film on, be made Top electrode, produce
Finished product；
Or：
By In-Ga electrode solutions, surface print method is used to be plated in above-mentioned chemical composition as Ba (Ti1-yXy)O3-yIndividual layer
On ceramic nano film, Top electrode is made, gets product.
The technical effect directly brought by the technical proposal is that using pulse laser method or magnetically controlled sputter method, directly
By Ba (Ti1-yXy)O3-yIt is deposited on the upper surface of bottom electrode；And the heat treatment process at subsequent 700-900 DEG C, it is complete in the lump
Into Ba (Ti1-yXy)O3-yLTCC sintering, so as on the upper surface of bottom electrode formed there is good resistive
The chemical composition of energy is Ba (Ti1-yXy)O3-ySingle-layer ceramic nano thin-film.
With prior art first by mixed material high-temperature calcination, ceramic material is fired into, again using the ceramic material as target
Magnetron sputtering deposition is carried out in lower electrode surface, is compared with forming the preparation technology of resistive film, the preparation of above-mentioned technical proposal
The most important improvement of technique is：Preceding ceramic material calcine technology step is dispensed.This simplifies the system of memristor
Standby technique, shorten technological process, improve production efficiency, and reducing energy consumption；
Above-mentioned technical proposal is merely not only simply to have dispensed high-temperature calcination to be prefabricated into ceramics compared with prior art
The step of material.What is more important, it is by Ba (Ti in above-mentioned technical proposal of the invention1-yXy)O3-y(X=Mg, Zn, Ca)
Mixture target material deposition has been attached in lower electrode surface, then during the heat treatment 10-30 minutes through low temperature (700-900 DEG C)
Into the thermal sintering of the resistive film of nano ceramics material.This both ensure that the efficiency and quality of film dense sintering, avoid again
Temperature is too low and the too short film of soaking time is not fine and close enough, or temperature is too high and long film and the electrode of causing of soaking time
Damage deformation；
Also, in terms of the chemical composition of resistive film, the memristor ratio with above-mentioned immediate prior art is of the invention
Above-mentioned technical proposal is by using passing through+divalent cation (X2+=Mg2+, Zn2+, Ca2+)+4 valency cation (Ti of part substitution4+)
B position substitutions are carried out, increase Ba (Ti1-yXy)O3-yThe asymmetry of molecular structure, improve Ba (Ti1-yXy)O3-yIn hole
Amount, be advantageous to strengthen Ba (Ti1-yXy)O3-yThe memristor performance of film memristor.
Further, in above-mentioned technical proposal, because substrate is the LTCC green bands that are coated with bottom electrode Pt or Au so that Ba
(Ti1-yXy)O3-yMemristor product has certain flexible, is not only convenient for transport and carries, and is easy to use LTCC technology collection
Into.
Preferably, the thickness of above-mentioned Top electrode is 10nm-50um.
What the optimal technical scheme was directly brought has the technical effect that, on the basis of memristor performance is ensured, in 10nm-
The selection of the thickness of Top electrode is carried out in this wide in range scope of 50um, advantageously reduces technique controlling difficulty, improves yield rate.
Further preferably, the thickness of above-mentioned single-layer ceramic nano thin-film is 10-990nm.
What the optimal technical scheme was directly brought has the technical effect that, ours experience have shown that, single-layer ceramic nano thin-film
Thickness is 10-990nm, on the one hand has more good change resistance performance；On the other hand, it is easy to technology controlling and process.
The present invention second of technical scheme used to achieve the above object is, a kind of using LTCC greens band as substrate
The preparation method of single-layer nano-film memristor, it is characterised in that comprise the following steps：
The first step, Ba (Ti are prepared using hydro-thermal method1-yXy)O3-yTarget, comprise the following steps that：
(1), raw material mixes：
By Ba (NO3)2、Ti(OC4H9)4With X (NO3)2, by 1: (1-y): y mixed in molar ratio, wherein, X Mg, Zn,
Ca, 0.0001≤y≤0.03 are standby；
Said mixture is dissolved in 10%-20% dust technology, is placed on magnetic stirring apparatus, is stirred, makes its complete
Fully dissolved；
(2), prepared by powder
NaOH solution is slowly added dropwise into above-mentioned solution until precipitation is complete, filtering is precipitated and is washed with deionized, and is dripped
Add NaOH solution and adjust pH value, and be fitted into reactor, be put into and reach in advance in the thermostatic drying chamber of 150 DEG C of temperature,
Hydro-thermal reaction 24 hours；
After hydro-thermal reaction, reactor is naturally cooled into room temperature, by reactor gained sample with deionized water repeatedly
Cleaning obtains Ba (Ti until removing all soluble-salts after being dried at 60 DEG C1-yXy)O3-yPowder；
(3), it is granulated：
In Ba (Ti1-yXy)O3-yPoly-vinyl alcohol solution is added in powder as binding agent, after uniform mixing, 40 mesh sieves is crossed and enters
Row is granulated；
Wherein：The mass percent concentration of poly-vinyl alcohol solution is 2-5%；The addition of poly-vinyl alcohol solution and above-mentioned baking
The mass ratio of powder after dry is 2-5: 100；
(4), target material moulding：
Compound after granulation is placed on tablet press machine and is pressed into bulk；
Then, gained bulk compound is cut into a diameter of 20-150mm, the highly slice of cylinder for 2-10mm, produces Ba
(Ti1-yXy)O3-yTarget；
Second step, the preparation of bottom electrode：
Take LTCC greens band substrate, using Pt or Au as target, using pulse laser method or magnetically controlled sputter method, by Pt or
Au is deposited on LTCC greens band substrate, forms the bottom electrode that material is Pt or Au；
3rd step, the preparation of individual layer nanometer memristor film：
By obtained Ba (Ti1-yXy)O3-yNano-mixture target, using pulse laser method or magnetically controlled sputter method,
By Ba (Ti1-yXy)O3-yIt is deposited on the surface of bottom electrode；
4th step, the target using material as Au, Ag or Pt, using heat spraying method, Au, Ag or Pt are deposited on above-mentioned
Chemical composition is Ba (Ti1-yXy)O3-ySingle-layer ceramic nano thin-film on, be made Top electrode；
Finally, 10-30 minutes are heat-treated at 700-900 DEG C, it is Ba (Ti to obtain chemical composition1-yXy)O3-yIndividual layer pottery
On porcelain nano thin-film,
Get product.
The technical effect directly brought by the technical proposal is that it is easy to physics realization, preparation technology is simple, controls difficulty
Small, steady quality, production efficiency are high, cost is cheap.Specific reason no longer repeats with above one by one.
Preferably, the thickness of above-mentioned Top electrode is 10nm-50um.
What the optimal technical scheme was directly brought has the technical effect that, on the basis of memristor performance is ensured, in 10nm-
The selection of the thickness of Top electrode is carried out in this wide in range scope of 50um, advantageously reduces technique controlling difficulty, improves yield rate.
Further preferably, the thickness of above-mentioned single-layer ceramic nano thin-film is 10-990nm.
What the optimal technical scheme was directly brought has the technical effect that, ours experience have shown that, single-layer ceramic nano thin-film
Thickness is 10-990nm, on the one hand has more good change resistance performance；On the other hand, it is easy to technology controlling and process.
It should be noted that the single-layer nano-film memristor prepared by the present invention, its memristor resistive principle are, with
Hole and ionization oxonium ion are carrier caused by bias is lower, under electric field action, are produced by the hole and ionization oxonium ion
The change of amount, to realize the change of device resistance.
It is not difficult to find out, its working mechanism and mathematical modeling possess general and universality.
To more fully understand the technical characterstic of the present invention, carried out specifically from principle with reference to memristor correlation theory
It is bright.
The present invention based on Ba (Ti1-yXy)O3-yThe memristor of (X=Mg, Zn, Ca) nano thin-film, its memristor mechanism sum
Learning model is specially：The memristor is by the individual layer Ba (Ti between being sandwiched in two electrodes1-yXy)O3-yNano thin-film is formed.
Due to+divalent cation (X2+=Mg2+, Zn2+, Ca2+)+4 valency cation (Ti of part substitution4+), increase Ba
(Ti1-yXy)O3-yThe asymmetry of molecular structure, improve Ba (Ti1-yXy)O3-yIn hole amount.When a voltage or electric current add
When on to the device, because film thickness is nanoscale, the voltage of very little will produce huge electric field, Ba (Ti1-yXy)O3-y
O can occur with the oxygen in air under bias with the surface of air contact2+4e-→2O2-Reaction, and make to produce in film
Hole.
Meanwhile function influence is biased against inside film O occurs2-→e-+O-, hole and ionization oxonium ion (O-) as master
Carrier displacement under electric field action is wanted, with hole and ionization oxonium ion (O-) change of yield can cause two electrodes
Between resistance variations, correspond to film therewith and minimum (R be presentedmin) or maximum (Rmax) two kinds of different resistance, this is Ba
(Ti1-yXy)O3-yShow the mechanism of memristor characteristic.Current O (t) represents a certain moment Ba (Ti1-yXy)O3-yProduce under bias
Raw hole amount, M represent caused maximum void amount under bias effect, and v represents to produce the speed in hole under bias effect.Due to
Hole and ionization oxonium ion (O-) yield it is relevant with the size of current by it and its duration (i.e. charge accumulated)：I.e.：Therefore, film resistor is its function by electric charge：Work as Rmin<<RmaxWhen,
Because bias (electric current) to interrupt in rear film without driving electric field, and each ion, electronics, hole etc. are moved at normal temperatures
It is inactive, hole and ionization oxonium ion (O in film-) amount can not retract the state before biasing (electric current passes through), therefore have
Memory effect and keep bias (electric current) interrupt when resistance.
In summary, the present invention is relative to prior art, technically the improvement of the core in terms of thought and technical principle
Point is two aspects：
First, eliminate the ceramic material as resistive film component fires step in advance；Second, resistive film ceramic material
Study a point improvement (+divalent cation (X for aspect2+=Mg2+, Zn2+, Ca2+)+4 valency cation (Ti of part substitution4+) carry out B positions
Substitution, increases Ba (Ti1-yXy)O3-yThe asymmetry of molecular structure, improve Ba (Ti1-yXy)O3-yIn hole amount, favorably
In enhancing Ba (Ti1-yXy)O3-yThe memristor performance of film memristor).
Also, improved based on above-mentioned both sides so that for the resistive film of ceramic material in structure, there occurs beneficial good
Property change (being added significantly to number of cavities), cause significantly improving and improving for final memristor memristor performance.
It should be further stated that：In above two technical scheme, basis each selects upper electrode material or plating respectively
The difference of electrode method is different to the order of used nano thin-film heat treatment.Its object is to：
Ensure Ba (Ti1-yXy)O3-yNano thin-film has high fitness and associativity with Top electrode, to avoid Top electrode
Damage or combination between electrode and film are bad.
Be not difficult to find out, the present invention relative to prior art, have preparation technology is simple, control difficulty is small, steady quality, life
Produce that efficiency high, cost are cheap, the beneficial effects such as the memristor performance of obtained memristor product is more preferable.
Brief description of the drawings
Fig. 1 is the single-layer nano-film memristor structural representation under one embodiment of the present invention；
Fig. 2 is the mathematical modeling of single-layer nano-film memristor M (q) of the present invention.
Embodiment
Below in conjunction with the accompanying drawings, the present invention is briefly described.
Fig. 1 is the single-layer nano-film memristor structural representation using LTCC greens band as substrate of the present invention.
As shown in figure 1, single-layer nano-film memristor of the present invention using LTCC greens band as substrate include two electrodes (on
Electrode and bottom electrode), and the Ba (Ti being placed between two electrodes1-yXy)O3-yNano thin-film structure, Top electrode Au, Ag, In-
Ga or Pt, bottom electrode is Pt or Au, using LTCC greens band as substrate.
Fig. 2 is mathematical modeling of the present invention using LTCC greens band as the single-layer nano-film memristor M (q) of substrate.
From figure 2 it can be seen that single-layer nano-film memristor of the present invention using LTCC greens band as substrate, its memristor machine
Reason is with hole and ionization oxonium ion (O-) change of yield can cause resistance variations between two electrodes, film is corresponded to therewith
Minimum (R is presentedmin) or maximum (Rmax) two kinds of different resistance, i.e. Ba (Ti1-yXy)O3-yMemristor Mechanism of characters.
With reference to embodiment, the present invention is described in further detail.
Explanation：
1st, embodiment 1-9, it is that Ba (Ti are prepared using hydro-thermal method1-yXy)O3-yTarget；Preparing raw material and formula composition
For mol ratio Ba (NO3)2∶(1-y)Ti(OC4H9)4∶y X(NO3)2(X=Mg, Zn, Ca), wherein, 0<y<1；
Ba (Ti are prepared using hydro-thermal method1-yXy)O3-yTarget, comprise the steps：
1st step：By Ba (NO3)2、Ti(OC4H9)4With X (NO3)2, by 1: (1-y): y mixed in molar ratio, wherein, X is
Mg, Zn, Ca, 0<y<1, it is standby；
2nd step：Said mixture is dissolved in 10%-20% dust technology, is placed on magnetic stirring apparatus, is stirred,
It is completely dissolved it；
3rd step：NaOH solution is slowly added dropwise into above-mentioned solution until precipitation is complete, filtering is precipitated and is washed with deionized water
Wash, NaOH solution is added dropwise and adjusts pH value, and be fitted into reactor, be put into the freeze-day with constant temperature for reaching 150 DEG C of temperature in advance
In case, hydro-thermal reaction 24 hours；
4th step：After hydro-thermal reaction, reactor is naturally cooled into room temperature, by the sample deionization of gained in reactor
Water is cleaned until removing all soluble-salts repeatedly, and Ba (Ti are obtained after being dried at 60 DEG C1-yXy)O3-yPowder；
5th step：It is granulated, it is 2-5% poly-vinyl alcohol solution as binding agent, the addition of binding agent to use mass fraction
For the 2-5% of mixture quality fraction to be granulated, cross 40 mesh sieves and be granulated；
6th step：Compacting, the compound being granulated after sieving is suppressed using tablet press machine, and be cut to a diameter of 20-
150mm, the highly slice of cylinder for 2-10mm.
2nd, embodiment 10~12 is using the Ba (Ti with embodiment 11-yXy)O3-yTarget identical composition of raw materials；
Also, the respectively target using material as Au, Ag or Pt, will using pulse laser method or magnetically controlled sputter method
Au, Ag or Pt are deposited on Ba (Ti1-yXy)O3-yOn nano thin-film.
Using the preparation method of identical single-layer nano-film memristor, using pulsed laser deposition PLD or magnetron sputtering
Method is comprised the following steps using Au, Ag, Pt plating Top electrode, the preparation method：
1st step, with Ba (Ti1-yXy)O3-y(X=Mg, Zn, Ca) makees target, is splashed using pulsed laser deposition PLD or magnetic control
Shooting method plated film on the LTCC green bands for be coated with advance bottom electrode Pt or Au, change resistance layer is formed, the thickness of plated film is 10-
990nm, then through 700-900 DEG C of heat treatment 10-30 minute；
2nd step, the target using material as Au, Ag or Pt, using pulse laser method or magnetically controlled sputter method, in Ba
(Ti1-yXy)O3-yLast layer Top electrode is plated on nano thin-film.
3rd, embodiment 13 is using the Ba (Ti with embodiment 11-yXy)O3-yTarget identical composition of raw materials；Also, it is to use
Printing process uses In-Ga electrode solutions plating last layer Top electrode.
4th, embodiment 14~16 is Ba (Ti1-yXy)O3-yThe Top electrode processing of (X=Mg, Zn, Ca) nano thin-film, is used
Embodiment 1Ba (Ti1-yXy)O3-yTarget identical composition of raw materials, using the preparation side of identical single-layer nano-film memristor
Method, comprised the following steps using other deposition methods using Au, Ag, Pt plating Top electrode, the preparation method：
1st step, with Ba (Ti1-yXy)O3-yMake target, plated using pulsed laser deposition PLD or magnetically controlled sputter method in advance
There is plated film on bottom electrode Pt or Au LTCC green bands, form change resistance layer, the thickness of plated film is 10-990nm；
2nd step, in Ba (Ti1-yXy)O3-yLast layer Top electrode is plated on nano thin-film, then through 700-900 DEG C of heat treatment 10-
30 minutes.
The preparation method of above-mentioned nano-film memristor, its thickness of electrode are 10nm-50um, and the upper electrode material is
Au, Ag, In-Ga or Pt.
5th, embodiment 10-16 is respectively adopted Au, Ag, In-Ga or Pt and makees upper electrode material, the technique in specific preparation process
Parameter is as shown in table 1 below.
Embodiment 1
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=100:99:1
(mol ratio).
Embodiment 2
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=100:98:2
(mol ratio).
Embodiment 3
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=100:97:3
(mol ratio).Embodiment 4
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=1000:999:
1 (mol ratio).
Embodiment 5
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=1000:998:
2 (mol ratios).
Embodiment 6
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=1000:997:
3 (mol ratios).
Embodiment 7
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=10000:
9999:1 (mol ratio).
Embodiment 8
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=10000:
9998:2 (mol ratios).
Embodiment 9
Prepare Ba (Ti1-yXy)O3-yThe composition of raw materials of target is：Ba(NO3)2：Ti(OC4H9)4：X(NO3)2=10000:
9997:3 (mol ratios).
The embodiment 10-16 of table 1 technological parameter
| Embodiment is numbered | Upper electrode material | Top electrode depositional mode | Heat treatment temperature (DEG C) |
| Embodiment 10 | Au | Pulse laser method or magnetically controlled sputter method | 800 |
| Embodiment 11 | Ag | Pulse laser method or magnetically controlled sputter method | 750 |
| Embodiment 12 | Pt | Pulse laser method or magnetically controlled sputter method | 900 |
| Embodiment 13 | In-Ga | Printing | 850 |
| Embodiment 14 | Au | Heat deposition | 700 |
| Embodiment 15 | Ag | Heat deposition | 700 |
| Embodiment 16 | Pt | Heat deposition | 800 |
The detection and inspection of product：
The final obtained memristors of above-described embodiment 1-16 are subjected to I-V characteristic test, the results showed that:
" 8 " font is presented in the I-V characteristic curve of such memristor；
And by changing pressurization size and pressing time, its I-V characteristic can show non-easy specific to memristor
The property lost (that is, Memorability).
Claims (6)
- A kind of 1. preparation method using LTCC greens band as the single-layer nano-film memristor of substrate, it is characterised in that including with Lower step：The first step, Ba (Ti are prepared using hydro-thermal method1-yXy)O3-yTarget, comprise the following steps that：(1), raw material mixes：By Ba (NO3)2、Ti(OC4H9)4With X (NO3)2, by 1: (1-y): y mixed in molar ratio, wherein, X Mg, Zn, Ca, 0.0001≤y≤0.03, it is standby；Said mixture is dissolved in 10%-20% dust technology, is placed on magnetic stirring apparatus, is stirred, makes it completely molten Solution；(2), prepared by powderNaOH solution is slowly added dropwise into above-mentioned solution until precipitation is complete, filtering is precipitated and is washed with deionized, and is added dropwise NaOH solution simultaneously adjusts pH value, and is fitted into reactor, is put into and reaches in advance in the thermostatic drying chamber of 150 DEG C of temperature, water Thermal response 24 hours；After hydro-thermal reaction, reactor is naturally cooled into room temperature, the sample of gained in reactor is cleaned repeatedly with deionized water Until removing all soluble-salts, Ba (Ti are obtained after being dried at 60 DEG C1-yXy)O3-yPowder；(3), it is granulated：In Ba (Ti1-yXy)O3-yPoly-vinyl alcohol solution is added in powder as binding agent, after uniform mixing, 40 mesh sieves is crossed and is made Grain；Wherein：The mass percent concentration of poly-vinyl alcohol solution is 2-5%；After the addition of poly-vinyl alcohol solution and above-mentioned drying The mass ratio of powder be 2-5 ︰ 100；(4), target material moulding：Compound after granulation is placed on tablet press machine and is pressed into bulk；Then, gained bulk compound is cut into a diameter of 20-150mm, the highly slice of cylinder for 2-10mm, produces Ba (Ti1-yXy)O3-yTarget；Second step, the preparation of bottom electrode：LTCC greens band substrate is taken, using Pt or Au as target, using pulse laser method or magnetically controlled sputter method, Pt or Au are sunk Product forms the bottom electrode that material is Pt or Au on LTCC greens band substrate；3rd step, the preparation of individual layer nanometer memristor film：By obtained Ba (Ti1-yXy)O3-yNano-mixture target, using pulse laser method or magnetically controlled sputter method, by Ba (Ti1-yXy)O3-yIt is deposited on the surface of bottom electrode；Then, 10-30 minutes are heat-treated at 700-900 DEG C, it is Ba (Ti to obtain chemical composition1-yXy)O3-ySingle-layer ceramic receive Rice film, as individual layer nanometer memristor film；4th step, the target using material as Au, Ag or Pt, using pulse laser method or magnetically controlled sputter method, by Au, Ag or Pt It is Ba (Ti to be deposited on above-mentioned chemical composition1-yXy)O3-ySingle-layer ceramic nano thin-film on, be made Top electrode, get product；Or：By In-Ga electrode solutions, surface print method is used to be plated in above-mentioned chemical composition as Ba (Ti1-yXy)O3-ySingle-layer ceramic On nano thin-film, Top electrode is made, gets product.
- 2. the preparation method according to claim 1 using LTCC greens band as the single-layer nano-film memristor of substrate, its It is characterised by, the thickness of the Top electrode is 10nm-50um.
- 3. the preparation method according to claim 1 or 2 using LTCC greens band as the single-layer nano-film memristor of substrate, Characterized in that, the thickness of the single-layer ceramic nano thin-film is 10-990nm.
- A kind of 4. preparation method using LTCC greens band as the single-layer nano-film memristor of substrate, it is characterised in that including with Lower step：The first step, Ba (Ti are prepared using hydro-thermal method1-yXy)O3-yTarget, comprise the following steps that：(1), raw material mixes：By Ba (NO3)2、Ti(OC4H9)4With X (NO3)2, by 1: (1-y): y mixed in molar ratio, wherein, X Mg, Zn, Ca, 0.0001≤y≤0.03, it is standby；Said mixture is dissolved in 10%-20% dust technology, is placed on magnetic stirring apparatus, is stirred, makes it completely molten Solution；(2), prepared by powderNaOH solution is slowly added dropwise into above-mentioned solution until precipitation is complete, filtering is precipitated and is washed with deionized, and is added dropwise NaOH solution simultaneously adjusts pH value, and is fitted into reactor, is put into and reaches in advance in the thermostatic drying chamber of 150 DEG C of temperature, water Thermal response 24 hours；After hydro-thermal reaction, reactor is naturally cooled into room temperature, the sample of gained in reactor is cleaned repeatedly with deionized water Until removing all soluble-salts, Ba (Ti are obtained after being dried at 60 DEG C1-yXy)O3-yPowder；(3), it is granulated：In Ba (Ti1-yXy)O3-yPoly-vinyl alcohol solution is added in powder as binding agent, after uniform mixing, 40 mesh sieves is crossed and is made Grain；Wherein：The mass percent concentration of poly-vinyl alcohol solution is 2-5%；After the addition of poly-vinyl alcohol solution and above-mentioned drying The mass ratio of powder be 2-5 ︰ 100；(4), target material moulding：Compound after granulation is placed on tablet press machine and is pressed into bulk；Then, gained bulk compound is cut into a diameter of 20-150mm, the highly slice of cylinder for 2-10mm, produces Ba (Ti1-yXy)O3-yTarget；Second step, the preparation of bottom electrode：LTCC greens band substrate is taken, using Pt or Au as target, using pulse laser method or magnetically controlled sputter method, Pt or Au are sunk Product forms the bottom electrode that material is Pt or Au on LTCC greens band substrate；3rd step, the preparation of individual layer nanometer memristor film：By obtained Ba (Ti1-yXy)O3-yNano-mixture target, using pulse laser method or magnetically controlled sputter method, by Ba (Ti1-yXy)O3-yIt is deposited on the surface of bottom electrode；4th step, the target using material as Au, Ag or Pt, using heat spraying method, Au, Ag or Pt are deposited on to above-mentioned chemistry Composition is Ba (Ti1-yXy)O3-ySingle-layer ceramic nano thin-film on, be made Top electrode；Finally, 10-30 minutes are heat-treated at 700-900 DEG C, it is Ba (Ti to obtain chemical composition1-yXy)O3-ySingle-layer ceramic receive On rice film, get product.
- 5. the preparation method according to claim 4 using LTCC greens band as the single-layer nano-film memristor of substrate, its It is characterised by, the thickness of the Top electrode is 10nm-50um.
- 6. the preparation method using LTCC greens band as the single-layer nano-film memristor of substrate according to claim 4 or 5, Characterized in that, the thickness of the single-layer ceramic nano thin-film is 10-990nm.
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