CN107663633B - A kind of preparation method of the silica resistance changing film of doped carbon nanometer pipe - Google Patents
A kind of preparation method of the silica resistance changing film of doped carbon nanometer pipe Download PDFInfo
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- CN107663633B CN107663633B CN201710764056.8A CN201710764056A CN107663633B CN 107663633 B CN107663633 B CN 107663633B CN 201710764056 A CN201710764056 A CN 201710764056A CN 107663633 B CN107663633 B CN 107663633B
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- silica
- nanometer pipe
- carbon nanotube
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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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
- H10N70/801—Constructional details of multistable switching devices
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
Abstract
The invention discloses a kind of preparation methods of the silica resistance changing film of doped carbon nanometer pipe, comprising the following steps: step 1, prepares silica sol and carbon nanotube-dehydrated alcohol mixed solution respectively；Step 2, first the silica sol obtained through step 1 and carbon nanotube-dehydrated alcohol mixed solution are measured respectively according to the volume ratio of 20:0.5-1, then by after measurement silica sol and carbon nanotube-dehydrated alcohol mixed solution mix, and stirred evenly under air-proof condition, obtain carbon nanotube-silica mixed solution；Step 3, choose substrate, and substrate pulling film forming in obtaining carbon nanotube-silica mixed solution through step 3 is made using dip-coating method, prepare carbon nanotube-silica gel film, the carbon nanotube prepared-silica gel film is heat-treated later, finally obtains the silica resistance changing film of doped carbon nanometer pipe.
Description
Technical field
The invention belongs to reservoir technology of thin film material preparation fields, and in particular to a kind of silica of doped carbon nanometer pipe
The preparation method of resistance changing film.
Background technique
What resistance-variable storing device thin-film material was developed earliest is perovskite oxide, such as PCMO, LSMO.It was used as later
It crosses, the oxide of stoicheiometry needed for metal binary oxide is simple, easily prepared with its ingredient, at low cost and CMOS technology
The advantages that compatible and greatly paid close attention to, and obtain the favor of numerous semiconductor manufacturers；Resistance of many based on such material
Transition storage has ambipolar storage characteristics, i.e., by applying opposite polarity voltage, resistance value can be in two states of height
Between carry out reversible transformation.But resistance-variable storing device is in the process of running, there is easily breakdown, fatiguability and proof voltage ability
The disadvantage of difference, causes its change resistance performance poor, develops by larger limitation.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of the silica resistance changing film of doped carbon nanometer pipe, solve resistive
There is easily breakdown, fatiguability and proof voltage ability difference in device.
The technical scheme adopted by the invention is that a kind of preparation method of the silica resistance changing film of doped carbon nanometer pipe,
It is specifically implemented according to the following steps:
It is specifically implemented according to the following steps:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL
Solution；
Step 2, the carbon nanometer for measuring silica sol respectively according to the volume ratio of 20:0.5-1, being prepared through step 1
Pipe solution, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the oxygen of doped carbon nanometer pipe
SiClx solution；
Step 3, substrate is chosen, substrate is placed in the silica solution of the doped carbon nanometer pipe obtained through step 2, and adopt
Layer of gel film is lifted on its surface with dip-coating method；
Step 4, under the protection of inert gas, the gel film lifted out through step 3 is heat-treated, is finally obtained
The silica resistance changing film of doped carbon nanometer pipe.
The features of the present invention also characterized in that:
In the step 3: the material of the substrate is platinum.
In the step 4: the temperature of the heat treatment is 200 DEG C -700 DEG C.
In the step 4: the time of the heat treatment is 20min-30min.
In the step 4: the inert gas is argon gas.
The beneficial effects of the present invention are: preparation method of the invention is easy without complicated preparation process, technological parameter is easy
In control, production cost can be greatly reduced；The silica for the doped carbon nanometer pipe prepared using preparation method of the present invention is hindered
Variation film is as applying when on resistance-variable storing device, which is not easy to puncture in the process of running and fatigue resistance
Good and proof voltage ability has preferable change resistance performance.
Detailed description of the invention
Fig. 1 is the silica resistance changing film for the doped carbon nanometer pipe prepared using preparation method of the present invention in electron microscopic
Scanning figure under mirror；
Fig. 2 be the doped carbon nanometer pipe prepared using preparation method of the present invention silica resistance changing film in air into
The electrical performance testing figure of row heat treatment；
Fig. 3 is the silica resistance changing film using the doped carbon nanometer pipe of the invention prepared by preparation method in argon
The electrical performance testing figure being heat-treated under gas shielded.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The preparation method of the silica resistance changing film of doped carbon nanometer pipe of the present invention, is specifically implemented according to the following steps:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL
Solution；
Step 2, the carbon nanometer for measuring silica sol respectively according to the volume ratio of 20:0.5-1, being prepared through step 1
Pipe solution, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the oxygen of doped carbon nanometer pipe
SiClx solution；
Step 3, substrate is chosen, the material of substrate is platinum, and substrate is placed in the oxygen of the doped carbon nanometer pipe obtained through step 2
In SiClx solution, and layer of gel film is lifted on its surface using dip-coating method；
Step 4, under protection of argon gas, the gel film lifted out through step 3 is carried out with 200 DEG C -700 DEG C of temperature
20min-30min heat treatment, finally obtains the silica resistance changing film of doped carbon nanometer pipe.
As shown in Figure 1, the silica resistance changing film for the doped carbon nanometer pipe that preparation method is prepared through the invention, by
Particle of uniform size is constituted, and surface is more smooth, and between 15nm-20nm, the height of particle exists the size of particle
Between 1.26nm-1.47nm, surface roughness is in 0.146nm-0.976nm.
During step 4 is heat-treated, with the raising of heat treatment temperature, carbon nanotube can be gradually oxidized to
For carbon dioxide, therefore argon hydrogen protection gas can be used in while being heat-treated protects to carbon nanotube.Atmosphere tube type burning specifically can be used
Freezing of a furnace, the model NBD-T1700 of atmosphere tube type sintering furnace.
After the silica resistance changing film of the substrate doped carbon nanometer pipe that preparation method is prepared through the invention on crossing,
It is put into sputter (the model SBC-12 of sputter, Beijing KYKY Technology Development Co., Ltd.'s production) and carries out electricity
Pole sputtering, electrode obtain resistance-variable storing device after sputtering, which there is the silica of doped carbon nanometer pipe to hinder
Variation film.Using Keithley Current Voltage source table (production of keithley company, model 2400) to this resistance-variable storing device
The carry out Electrical of resistance reverse speed characterisstic, as a result as shown in Figure 3.
It can prepare another resistance-variable storing device by the above method, but the doped carbon nanometer pipe that the resistance-variable storing device has
Silica resistance changing film preparation method is heat-treated to obtain in air through the invention.Using Keithley electric current electricity
Carry out electric property of the potential source table (production of keithley company, model 2400) to the resistance reverse speed characterisstic of the resistance-variable storing device
Analysis, as a result as shown in Figure 2.
By Fig. 2 and Fig. 3 it is found that unipolarity is all presented in the scanning area of the negative voltage of two resistance-variable storing devices, but in Fig. 3
The electric resistance changing effect of resistance-variable storing device is substantially better than the electric resistance changing effect of resistance-variable storing device in Fig. 2；Resistance-variable storing device in Fig. 3
It is initially high-impedance state when adding negative voltage, electric current is almost 0, but since -2V or so, significant change occurs for resistance state, is in
Existing low configuration, proof voltage can reach -4.0V；Resistance-variable storing device then can't see apparent resistance state variation in Fig. 2, and proof voltage can only reach
To -2.0V.
Embodiment 1
The preparation method of the silica resistance changing film of doped carbon nanometer pipe of the present invention, is specifically implemented according to the following steps:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL
Solution；
Step 2, the carbon nanotube for measuring silica sol respectively according to the volume ratio of 20:0.5, being prepared through step 1
Solution, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the oxidation of doped carbon nanometer pipe
Silicon solution；
Step 3, substrate is chosen, substrate is placed in the silica solution of the doped carbon nanometer pipe obtained through step 2, and adopt
Layer of gel film is lifted on its surface with dip-coating method；
Step 4, under protection of argon gas, 20min heat is carried out to the gel film lifted out through step 3 with 200 DEG C of temperature
Processing, finally obtains the silica resistance changing film of doped carbon nanometer pipe.
Embodiment 2
The preparation method of the silica resistance changing film of doped carbon nanometer pipe of the present invention, is specifically implemented according to the following steps:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL
Solution；
Step 2, the carbon nanotube for measuring silica sol respectively according to the volume ratio of 20:0.6, being prepared through step 1
Solution, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the oxidation of doped carbon nanometer pipe
Silicon solution；
Step 3, substrate is chosen, substrate is placed in the silica solution of the doped carbon nanometer pipe obtained through step 2, and adopt
Layer of gel film is lifted on its surface with dip-coating method；
Step 4, under protection of argon gas, 22min heat is carried out to the gel film lifted out through step 3 with 300 DEG C of temperature
Processing, finally obtains the silica resistance changing film of doped carbon nanometer pipe.
Embodiment 3
The preparation method of the silica resistance changing film of doped carbon nanometer pipe of the present invention, is specifically implemented according to the following steps:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL
Solution；
Step 2, the carbon nanotube for measuring silica sol respectively according to the volume ratio of 20:0.7, being prepared through step 1
Solution, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the oxidation of doped carbon nanometer pipe
Silicon solution；
Step 3, substrate is chosen, substrate is placed in the silica solution of the doped carbon nanometer pipe obtained through step 2, and adopt
Layer of gel film is lifted on its surface with dip-coating method；
Step 4, under protection of argon gas, 20min- is carried out to the gel film lifted out through step 3 with 450 DEG C of temperature
30min heat treatment, finally obtains the silica resistance changing film of doped carbon nanometer pipe.
Embodiment 4
The preparation method of the silica resistance changing film of doped carbon nanometer pipe of the present invention, is specifically implemented according to the following steps:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL
Solution；
Step 2, the carbon nanotube for measuring silica sol respectively according to the volume ratio of 20:0.8, being prepared through step 1
Solution, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the oxidation of doped carbon nanometer pipe
Silicon solution；
Step 3, substrate is chosen, substrate is placed in the silica solution of the doped carbon nanometer pipe obtained through step 2, and adopt
Layer of gel film is lifted on its surface with dip-coating method；
Step 4, under protection of argon gas, 28min heat is carried out to the gel film lifted out through step 3 with 600 DEG C of temperature
Processing, finally obtains the silica resistance changing film of doped carbon nanometer pipe.
Embodiment 5
The preparation method of the silica resistance changing film of doped carbon nanometer pipe of the present invention, is specifically implemented according to the following steps:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL
Solution；
Step 2, measure silica sol respectively according to the volume ratio of 20:1, the carbon nanotube that is prepared through step 1 it is molten
Liquid, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the silica of doped carbon nanometer pipe
Solution；
Step 3, substrate is chosen, substrate is placed in the silica solution of the doped carbon nanometer pipe obtained through step 2, and adopt
Layer of gel film is lifted on its surface with dip-coating method；
Step 4, under protection of argon gas, 30min heat is carried out to the gel film lifted out through step 3 with 700 DEG C of temperature
Processing, finally obtains the silica resistance changing film of doped carbon nanometer pipe.
Claims (5)
1. a kind of preparation method of the silica resistance changing film of doped carbon nanometer pipe, which is characterized in that specifically according to the following steps
Implement:
Step 1, using carbon nanotube powder as solute, dehydrated alcohol is solvent, and preparation concentration is 10-5The carbon nanotube of g/mL is molten
Liquid；
Step 2, measure silica sol respectively according to the volume ratio of 20:0.5-1, the carbon nanotube that is prepared through step 1 it is molten
Liquid, by after measurement silica sol and carbon nano-tube solution be mixed and stirred for uniformly obtaining the silica of doped carbon nanometer pipe
Solution；
Step 3, substrate is chosen, substrate is placed in the silica solution of the doped carbon nanometer pipe obtained through step 2, and using leaching
Stain czochralski method lifts layer of gel film on its surface；
Step 4, under the protection of inert gas, the gel film lifted out through step 3 is heat-treated, finally obtains doping
The silica resistance changing film of carbon nanotube.
2. the preparation method of the silica resistance changing film of doped carbon nanometer pipe according to claim 1, which is characterized in that
In the step 3: the material of the substrate is platinum.
3. the preparation method of the silica resistance changing film of doped carbon nanometer pipe according to claim 1, which is characterized in that
In the step 4: the temperature of the heat treatment is 200 DEG C -700 DEG C.
4. the preparation method of the silica resistance changing film of doped carbon nanometer pipe according to claim 3, which is characterized in that
In the step 4: the time of the heat treatment is 20min-30min.
5. the preparation method of the silica resistance changing film of doped carbon nanometer pipe according to claim 1, which is characterized in that
In the step 4: the inert gas is argon gas.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102157684A (en) * | 2010-12-17 | 2011-08-17 | 天津理工大学 | Resistive random access memory (RRAM) using carbon nano tube (CNT) as solid state electrolyte |
| CN106809817A (en) * | 2017-01-16 | 2017-06-09 | 东华大学 | A kind of preparation method of porous CNT |
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| CN101394712B (en) * | 2007-09-21 | 2010-08-25 | 清华大学 | Hole blackening solution and preparation thereof |
| JP2012059862A (en) * | 2010-09-08 | 2012-03-22 | Toshiba Corp | Non-volatile memory device and method of manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102157684A (en) * | 2010-12-17 | 2011-08-17 | 天津理工大学 | Resistive random access memory (RRAM) using carbon nano tube (CNT) as solid state electrolyte |
| CN106809817A (en) * | 2017-01-16 | 2017-06-09 | 东华大学 | A kind of preparation method of porous CNT |
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