CN106340586B - A kind of preparation method of carbon/nickel oxide Memister film - Google Patents
A kind of preparation method of carbon/nickel oxide Memister film Download PDFInfo
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- CN106340586B CN106340586B CN201610859007.8A CN201610859007A CN106340586B CN 106340586 B CN106340586 B CN 106340586B CN 201610859007 A CN201610859007 A CN 201610859007A CN 106340586 B CN106340586 B CN 106340586B
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—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 without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of the switching material, e.g. layer deposition
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of the switching material, e.g. layer deposition
- H10N70/026—Formation of the switching material, e.g. layer deposition by physical vapor deposition, e.g. sputtering
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
- H10N70/883—Oxides or nitrides
- H10N70/8833—Binary metal oxides, e.g. TaOx
Abstract
The invention discloses a kind of carbon/nickel oxide Memister film preparation methods, prepare nickel oxide film first；Then prepare carbon film on nickel oxide film, obtain carbon/oxidation nickel composite film, using sputter to carbon/oxidation nickel composite film carry out top electrode preparation to get.The present invention carries out carbon film with nickel oxide film compound, it is compared to other materials with resistive characteristic, carbon/oxidation nickel composite film surface is smooth, preparation cost is low, simple process, is easy to control, the preparation efficiency for preparing laminated film is improved, and its change resistance performance is substantially better than single nickel oxide film.
Description
Technical field
The invention belongs to microelectronic material resistance-variable storing device thin-film material technical fields, and in particular to a kind of carbon/nickel oxide
The preparation method of Memister film.
Background technique
With the raising of people's life requirement, either laptop, mobile hard disk or smart phone and digital phase
Machine etc. is required to the memory haveing excellent performance and guarantees demand of the people to data, to information storage.Meanwhile complexity and the Pang of data
Substantially make requirement of the people to the storage capacity of data, erasable ability and reading speed higher and higher, low cost, low-power consumption and height
The memory of storage density will become the primary trend of future development.Non-volatility memorizer is mainly with " flash memory " memory
(FLASH) based on.FLASH memory since with non-volatile, each restarting equipment can save a large amount of time cost,
Thus it is widely used.But its erasable and writing speed is slow (ms grades or more), and erasing voltage is also relatively high.These are lacked
Point is so that FLASH is difficult to meet the needs of people store information.When especially element height is integrated now, tunnel oxide thickness
Spend more and more thinner, charge tunneling effect makes the bad stability of FLASH memory.At the same time, resistance-type memory is continuous
Ground develops towards low-power consumption, high density, low cost and faster read or write speed, and resistance-type memory of new generation all has respectively
The characteristics of.Therefore, how to reduce erasing voltage while improving its erasable and writing speed is a critical issue.
Summary of the invention
The object of the present invention is to provide a kind of carbon/nickel oxide Memister film preparation methods, solve existing deposit
The problem that reservoir erasable and writing speed is slow and erasing voltage is high.
The technical scheme adopted by the invention is as follows a kind of carbon/nickel oxide Memister film preparation method, is specifically pressed
Implement according to following steps：
Step 1, nickel oxide film is prepared；
Step 2, carbon film is prepared on step 1 gained nickel oxide film, obtains carbon/oxidation nickel composite film；
Step 3, using sputter to step 2 gained carbon/oxidation nickel composite film carry out top electrode preparation to get.
It is of the invention to be further characterized in that,
In step 1, the preparation process of nickel oxide film is：
Step 1.1：Prepare oxidation nickel sol；
Step 1.2：At room temperature, nickel sol will be aoxidized in Pt platinum electrode base using dipping-pulling method obtained by step 1.1
It is lifted on plate, obtains nickel oxide gel film；
Step 1.3：After nickel oxide gel film made from step 1.2 is dried at room temperature for, toasted at 60~80 DEG C
10~15min is then heat-treated 20~30min, to get on Pt platinum electrode substrate after cooling at a temperature of 300~700 DEG C
Nickel oxide film.
In step 1.1, the process for preparation for aoxidizing nickel sol is：By nickel acetate, acetylacetone,2,4-pentanedione, acrylic acid and ethylene glycol monomethyl ether
By 1:1:1:12 dosage mixing.
In step 2, carbon/oxidation nickel composite film preparation process is：
Step 1 gained nickel oxide film is placed on the supporting spring of vacuum evaporation instrument and is fixed, carbon rope is then fixed on carbon
Evaporation source on；Vacuum evaporation instrument power supply is opened, the electric current of vapor deposition instrument is adjusted to 50~60A, is deposited, after carbon fracture of rope,
Stop vapor deposition, to get carbon/oxidation nickel composite film after cooling.
Graphite fibre of the carbon rope by purity 99%, diameter by 2 millimeters is made, and carbon rope length degree is 1 centimetre.
In step 3, it is using the process that sputter carries out top electrode preparation to carbon/oxidation nickel composite film：Open sputtering
Carbon/oxidation nickel composite film sample is put into, fixes mask plate (Mask) by instrument, then opens sputter power supply, is taken out
Gas, when vacuum degree reaches 1*10-3The sputtering of top electrode is carried out after Pa to it.
Sputtering target material is Pt, and purity 99.9%, sputtering time is 5~7min.
The invention has the advantages that carbon film and nickel oxide film progress is compound, other are compared to resistive spy
The material of property, carbon/oxidation nickel composite film surface is smooth, and preparation cost is low, simple process, is easy to control, and improves preparation
The preparation efficiency of laminated film, and its change resistance performance is substantially better than single nickel oxide film.
Detailed description of the invention
Fig. 1 is atomic force (AFM) scanned photograph on 1 gained nickel oxide film surface of the embodiment of the present invention；
Fig. 2 is atomic force (AFM) scanned photograph on 2 gained nickel oxide film surface of the embodiment of the present invention；
Fig. 3 is atomic force (AFM) scanned photograph on 3 nickel oxide film surface of the embodiment of the present invention；
Fig. 4 is nickel oxide film heat treatment cycle curve figure in the method for the present invention；
Fig. 5 is 3 gained carbon of the embodiment of the present invention/nickel oxide Memister thin-film device C-V characteristic (I-V) curve；
Fig. 6 is each element in 3 gained carbon of the embodiment of the present invention/nickel oxide Memister film with the variation of etching depth
Curve graph.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of carbon/nickel oxide Memister film of the present invention, is specifically implemented according to the following steps：
Step 1, nickel oxide film is prepared：
Step 1.1：Prepare oxidation nickel sol：Nickel acetate, acetylacetone,2,4-pentanedione, acrylic acid and ethylene glycol monomethyl ether are pressed 1:1:1:12
Dosage (herein amount ratio be molar ratio) mixing, when preparation prepared (at room temperature) in glove box；
Step 1.2：At room temperature, nickel sol will be aoxidized in Pt platinum electrode base using dipping-pulling method obtained by step 1.1
It is lifted on plate, obtains nickel oxide gel film；
Step 1.3：After nickel oxide gel film made from step 1.2 is dried at room temperature for, toasted at 60~80 DEG C
10~15min, the volatilization that can accelerate liquid phase component promotes intermolecular polymerization reaction, then at a temperature of 300~700 DEG C at heat
20~30min of reason (heat treatment carries out in heat-treatment furnace), is finally cooled to room temperature with heat-treatment furnace, i.e., heat treatment process is one
A heating --- heat preservation --- process of cooling is to get the nickel oxide film on Pt platinum electrode substrate.
Step 2, step 1 gained nickel oxide film is placed on the supporting spring of vacuum evaporation instrument and is fixed, then consolidate carbon rope
It is scheduled on the evaporation source of carbon；Vacuum evaporation instrument power supply is opened, the electric current of vapor deposition instrument is adjusted to 50~60A, is deposited, carbon rope is disconnected
After splitting, stop vapor deposition, to get carbon/oxidation nickel composite film after cooling；Wherein, carbon rope is 2 millimeters by purity 99%, diameter
Graphite fibre is made, and carbon rope length degree is 1 centimetre.
Step 3, top electrode preparation is carried out to step 2 gained carbon/oxidation nickel composite film using sputter：Open sputtering
Carbon/oxidation nickel composite film sample is put into, fixes mask plate (Mask) by instrument, then opens sputter power supply, is taken out
Gas, when vacuum degree reaches 1*10-3It is carried out after Pa the sputtering of top electrode to get.Sputtering target material is Pt, purity 99.9%,
Sputtering time is 5~7min.
Embodiment 1
Step 1：By 1:1:1:12 amount ratio weighs nickel acetate, acetylacetone,2,4-pentanedione, acrylic acid and ethylene glycol monomethyl ether respectively, mixes
After conjunction, oxidation nickel sol is obtained；At room temperature, using dipping-pulling method, oxygen is carried out on Pt platinum electrode substrate using pulling machine
Change the lifting of nickel gel film, will lift after nickel oxide gel film obtained is dried at room temperature, and be toasted at 60 DEG C
10min is then heat-treated 20min at a temperature of 300 DEG C, then takes out cooled to room temperature, that is, obtains in Pt platinum electrode
Nickel oxide film on substrate.
Step 2：The preparation of carbon/oxidation nickel composite film：Step 1 gained nickel oxide film is placed on vacuum evaporation instrument
Fixed on supporting spring, then be 2 millimeters by purity 99%, diameter, the carbon rope of length 1cm is fixed on the evaporation source of carbon；It opens true
Sky vapor deposition instrument power supply adjusts the electric current of vapor deposition instrument to 50A, is deposited, and after carbon fracture of rope, stops vapor deposition, it is cooling after to get
Carbon/oxidation nickel composite film.
Step 3：Sputter is opened, the carbon prepared on Pt platinum electrode/oxidation nickel composite film sample is put into, it is fixed
Good mask plate (Mask), is evacuated, when vacuum degree reaches 1*10-3The sputtering of top electrode can be carried out after Pa to it.Sputtering target material
For Pt, purity 99.9%, sputtering time is 5 minutes.The Pt layer sputtered is carbon/oxidation nickel composite film Memister
Top electrode.One complete carbon/oxidation nickel composite film resistance memory cell just prepares completion.
Nickel oxide film surface obtained by the present embodiment (300 DEG C of heat treatments) is carried out using atomic force microscope (AFM)
Microexamination, Fig. 1 are the flat scanning figure of nickel oxide film, scan area 1*1um2。
Embodiment 2
Step 1：By 1:1:1:12 amount ratio weighs nickel acetate, acetylacetone,2,4-pentanedione, acrylic acid and ethylene glycol monomethyl ether respectively, mixes
After conjunction, oxidation nickel sol is obtained；At room temperature, using dipping-pulling method, oxygen is carried out on Pt platinum electrode substrate using pulling machine
Change the lifting of nickel gel film, will lift after nickel oxide gel film obtained is dried at room temperature, and be toasted at 70 DEG C
13min is then heat-treated 25min at a temperature of 500 DEG C, then takes out natural cooling, that is, obtains on Pt platinum electrode substrate
Nickel oxide film.
Step 2：The preparation of carbon/oxidation nickel composite film：Step 1 gained nickel oxide film is placed on vacuum evaporation instrument
Fixed on supporting spring, then be 2 millimeters by purity 99%, diameter, the carbon rope of length 1cm is fixed on the evaporation source of carbon；It opens true
Sky vapor deposition instrument power supply adjusts the electric current of vapor deposition instrument to 55A, is deposited, and after carbon fracture of rope, stops vapor deposition, it is cooling after to get
Carbon/oxidation nickel composite film.
Step 3：Sputter is opened, the carbon prepared on Pt platinum electrode/oxidation nickel composite film sample is put into, it is fixed
Good mask plate (Mask), is evacuated, when vacuum degree reaches 1*10-3The sputtering of top electrode can be carried out after Pa to it.Sputtering target material
For Pt, purity 99.9%, sputtering time is 6 minutes.The Pt layer sputtered is carbon/oxidation nickel composite film Memister
Top electrode.One complete carbon/oxidation nickel composite film resistance memory cell just prepares completion.
Nickel oxide film surface obtained by the present embodiment (500 DEG C of heat treatments) is carried out using atomic force microscope (AFM)
Microexamination, Fig. 2 are the flat scanning figure of nickel oxide film, scan area 1*1um2。
Embodiment 3
Step 1：By 1:1:1:12 amount ratio weighs nickel acetate, acetylacetone,2,4-pentanedione, acrylic acid and ethylene glycol monomethyl ether respectively, mixes
After conjunction, oxidation nickel sol is obtained；At room temperature, using dipping-pulling method, oxygen is carried out on Pt platinum electrode substrate using pulling machine
Change the lifting of nickel gel film, will lift after nickel oxide gel film obtained is dried at room temperature, and be toasted at 80 DEG C
15min is then heat-treated 30min at a temperature of 700 DEG C, then takes out cooled to room temperature, that is, obtains in Pt platinum electrode
Nickel oxide film on substrate.
Step 2：The preparation of carbon/oxidation nickel composite film：Step 1 gained nickel oxide film is placed on vacuum evaporation instrument
Fixed on supporting spring, then be 2 millimeters by purity 99%, diameter, the carbon rope of length 1cm is fixed on the evaporation source of carbon；It opens true
Sky vapor deposition instrument power supply adjusts the electric current of vapor deposition instrument to 60A, is deposited, and after carbon fracture of rope, stops vapor deposition, it is cooling after to get
Carbon/oxidation nickel composite film.
Step 3：Sputter is opened, the carbon prepared on Pt platinum electrode/oxidation nickel composite film sample is put into, it is fixed
Good mask plate (Mask), is evacuated, when vacuum degree reaches 1*10-3The sputtering of top electrode can be carried out after Pa to it.Sputtering target material
For Pt, purity 99.9%, sputtering time is 7 minutes.The Pt layer sputtered is carbon/oxidation nickel composite film Memister
Top electrode.One complete carbon/oxidation nickel composite film resistance memory cell just prepares completion.
Nickel oxide film surface obtained by the present embodiment (700 DEG C of heat treatments) is carried out using atomic force microscope (AFM)
Microexamination, Fig. 3 are the flat scanning figure of nickel oxide film, scan area 1*1um2。
The electrology characteristic test of 3 gained carbon of the embodiment of the present invention/oxidation nickel composite film Memister at normal temperature, if
Set the testing research that current protection limit (compliance current) is 10mA；Nickel oxide film is heat-treated in the method for the present invention
Process curve figure is as shown in Figure 4.
Fig. 5 is carbon/oxidation nickel composite film Memister C-V characteristic (I-V) curve, and electric current shown in figure is protected
Shield is limited to 1mA, and the curve in figure is C-V characteristic (I-V) curve after loop test 10 times, shows more stable bipolar
Resistance switch performance.The electric resistance changing effect that Pt/C/NiO/Pt device can be significantly found out from figure is bipolarity, and device
The initial resistance of part is low resistance state, therefore RESET process has occurred in Pt/C/NiO/Pt device.During RESET, voltage is small
When 1.3V, the resistance value of low resistance state is kept approximately constant.When voltage reaches 1.3V, the low-resistance of device with the increase of voltage
The resistance value of state is gradually reduced, and resistance state is changed into high-impedance state by low resistance state, and RESET process occurs for device.
Consulting pertinent literature and obtaining the work function of NiO, C, Pt is respectively 4.8eV, 5eV, 5.6eV, because the work function of C is small
In the work function of Pt, so that the Interfacial Potential Barrier area of C and Pt is very thin, carrier tunnelling probability is greatly enhanced, and has high load
Sub- injection effect is flowed, is similarly also Ohmic contact between NiO/C so being Ohmic contact between C/Pt.The interface of Ohmic contact
Resistance value is smaller, when applying voltage to device, it is only necessary to which the test voltage or electric current of very little can promote Pt/
The inside of NiO/C/Pt resistive memory forms conductive filament.
Deep etching point is carried out to carbon/oxidation nickel composite film Memister using x-ray photoelectron spectroscopy (XPS)
Analysis, obtains Fig. 6.Wherein, curve a is the percentage composition change curve of oxygen element, and b is the percentage composition change curve of carbon, c
For the percentage composition change curve of Ni element.As can be seen from the figure the percentage composition of sample element is with etch period and etching
Depth constantly improves the apparent variation of generation.Since carbon has good adsorptivity, can be adsorbed on the surface of carbon a certain amount of
Oxygen element, with the increase of etching depth, the oxygen element on surface can constantly be worn away, and constituent content constantly declines.Work as quarter
When erosion depth progressivelyes reach the surface layer of carbon film, the content of carbon can constantly be improved with the increase of etching depth, further
Etching, the content of carbon remain unchanged.
The present invention is based on the preparations of carbon/oxidation nickel composite film, are compared to other materials with resistive characteristic, binary
Metal oxide and amorphous carbon material have the characteristics that structure is simple, material component is easy to control, and its resistive characteristic wants excellent
There is good compatibility in single nickel oxide film, while with traditional CMOS technology.
The present invention is used carries out the preparation of carbon/oxidation nickel composite film and further to carbon/oxidation on Pt platinum electrode
The electric property of nickel composite film is studied.
Sol-gel method is respectively adopted using the method for the present invention and vacuum vapour deposition combines, the oxidation nickel sol of configuration
Stablize and use preparation method nickel oxide film obtained on Pt platinum electrode, then makes on the surface of nickel oxide film
Carbon film is prepared with vacuum vapour deposition, the excellent carbon of change resistance performance/oxidation nickel composite film can be obtained.Carbon/nickel oxide THIN COMPOSITE
The surface of film is smooth, and preparation cost is low, simple process, is easy to control, and improves the preparation efficiency for preparing laminated film, and its
Change resistance performance is substantially better than single nickel oxide film.
Claims (7)
1. a kind of carbon/nickel oxide Memister film preparation method, which is characterized in that be specifically implemented according to the following steps：
Step 1, nickel oxide film is prepared；
Step 2, carbon film is prepared on step 1 gained nickel oxide film, obtains carbon/oxidation nickel composite film；
Step 3, using sputter to step 2 gained carbon/oxidation nickel composite film carry out top electrode preparation to get.
2. a kind of carbon according to claim 1/nickel oxide Memister film preparation method, which is characterized in that step
In rapid 1, the preparation process of nickel oxide film is：
Step 1.1：Prepare oxidation nickel sol；
Step 1.2：At room temperature, nickel sol will be aoxidized on Pt platinum electrode substrate using dipping-pulling method obtained by step 1.1
Lifting, obtains nickel oxide gel film；
Step 1.3：After nickel oxide gel film made from step 1.2 is dried at room temperature for, at 60~80 DEG C toast 10~
15min is then heat-treated 20~30min, to get the oxygen on Pt platinum electrode substrate after cooling at a temperature of 300~700 DEG C
Change nickel film.
3. a kind of carbon according to claim 2/nickel oxide Memister film preparation method, which is characterized in that step
In rapid 1.1, the process for preparation for aoxidizing nickel sol is：Nickel acetate, acetylacetone,2,4-pentanedione, acrylic acid and ethylene glycol monomethyl ether are pressed 1:1:1:12
Molar ratio mixing.
4. a kind of carbon according to claim 1/nickel oxide Memister film preparation method, which is characterized in that step
In rapid 2, carbon/oxidation nickel composite film preparation process is：
Step 1 gained nickel oxide film is placed on the supporting spring of vacuum evaporation instrument and is fixed, then carbon rope is fixed on to the steaming of carbon
On rising；Vacuum evaporation instrument power supply is opened, the electric current of vapor deposition instrument is adjusted to 50~60A, is deposited, after carbon fracture of rope, is stopped
Vapor deposition, to get carbon/oxidation nickel composite film after cooling.
5. a kind of carbon according to claim 4/nickel oxide Memister film preparation method, which is characterized in that carbon
The graphite fibre by purity 99%, diameter by 2 millimeters of restricting is made, and carbon rope length degree is 1 centimetre.
6. a kind of carbon according to claim 1/nickel oxide Memister film preparation method, which is characterized in that step
In rapid 3, it is using the process that sputter carries out top electrode preparation to carbon/oxidation nickel composite film：Sputter is opened, by carbon/oxygen
Change nickel composite film sample to be put into, fix mask plate, then opens sputter power supply, be evacuated, when vacuum degree reaches 1*
10-3The sputtering of top electrode is carried out after Pa to it.
7. a kind of carbon according to claim 6/nickel oxide Memister film preparation method, which is characterized in that splash
Material of shooting at the target is Pt, and purity 99.9%, sputtering time is 5~7min.
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