CN107663633A - 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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- CN107663633A CN107663633A CN201710764056.8A CN201710764056A CN107663633A CN 107663633 A CN107663633 A CN 107663633A CN 201710764056 A CN201710764056 A CN 201710764056A CN 107663633 A CN107663633 A CN 107663633A
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- silica
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- carbon nanometer
- nanometer pipe
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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 method of the silica resistance changing film of doped carbon nanometer pipe, comprise the following steps:Step 1, silica sol and CNT absolute ethyl alcohol mixed solution are prepared respectively;Step 2, first according to 20:0.5 1 volume ratio measures the silica sol obtained through step 1 and CNT absolute ethyl alcohol mixed solution respectively, then the silica sol after measuring and CNT absolute ethyl alcohol mixed solution are mixed, and stirred under air-proof condition, obtain CNT silica mixed solution;Step 3, choose substrate, and substrate pulling film forming in CNT silica mixed solution is obtained through step 3 is made using dip-coating method, prepare CNT silica gel film, the CNT silica gel film prepared is heat-treated afterwards, finally gives the silica resistance changing film of doped carbon nanometer pipe.
Description
Technical field
The invention belongs to holder technology of thin film material preparation field, and in particular to a kind of silica of doped carbon nanometer pipe
The preparation method of resistance changing film.
Background technology
What resistance-variable storing device thin-film material was developed earliest is perovskite oxide, such as PCMO, LSMO.It was used as afterwards
Cross, metal binary oxide with its composition it is simple, it is easily prepared needed for the oxide of stoicheiometry, cost be low and CMOS technology
The advantages that compatible and greatly paid close attention to, and obtain the favor of numerous semiconductor manufacturers;Many resistances 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 there is easily breakdown, fatiguability and proof voltage ability in resistance-variable storing device during operation
The shortcomings that poor, cause its change resistance performance poor, develop by larger limitation.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the silica resistance changing film of doped carbon nanometer pipe, solves resistive
The problem of easily breakdown, fatiguability and proof voltage ability be present in device.
The technical solution adopted in the present invention is a kind of preparation method of the silica resistance changing film of doped carbon nanometer pipe,
Specifically implement according to following steps:
Specifically implement according to following steps:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT
Solution;
Step 2, according to 20:The carbon nanometer that 0.5-1 volume ratio measures silica sol, is prepared through step 1 respectively
Pipe solution, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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
With dip-coating method layer of gel film is lifted on its surface;
Step 4, under the protection of inert gas, the gel film lifted out through step 3 is heat-treated, finally given
The silica resistance changing film of doped carbon nanometer pipe.
The features of the present invention also resides in:
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 invention are as follows:The preparation method of the present invention is easy without complicated preparation technology simplicity, technological parameter
In control, production cost can be greatly reduced;The silica resistance for the doped carbon nanometer pipe prepared using preparation method of the present invention
Variation film is as applying when on resistance-variable storing device, and the resistance-variable storing device is not easy to puncture in the process of running and fatigue resistance
Good and proof voltage ability, has preferable change resistance performance.
Brief description of the drawings
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 is that the silica resistance changing film for the doped carbon nanometer pipe prepared using preparation method of the present invention is protected in argon gas
The lower electrical performance testing figure being heat-treated;
Fig. 3 is the silica resistance changing film using the doped carbon nanometer pipe prepared by preparation method of the present invention in sky
The electrical performance testing figure being heat-treated in gas.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The preparation method of the silica resistance changing film of doped carbon nanometer pipe of the present invention, specifically implements according to following steps:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT
Solution;
Step 2, according to 20:The carbon nanometer that 0.5-1 volume ratio measures silica sol, is prepared through step 1 respectively
Pipe solution, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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 argon gas protection, the gel film lifted out through step 3 is carried out with 200 DEG C -700 DEG C of temperature
20min-30min is heat-treated, and finally gives 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 being prepared by preparation method of the present invention, by
The particulate of size uniform is formed, and its surface is more smooth, and between 15nm-20nm, the height of particulate exists the size of particulate
Between 1.26nm-1.47nm, surface roughness is in 0.146nm-0.976nm.
During step 4 is heat-treated, with the rise of heat treatment temperature, CNT can be gradually oxidized to
For carbon dioxide, therefore argon hydrogen protection gas can be used to protect CNT when being heat-treated.Can specifically atmosphere tube type be used to burn
Freezing of a furnace, the model NBD-T1700 of atmosphere tube type sintering furnace.
After the silica resistance changing film for the doped carbon nanometer pipe that substrate is prepared on crossing by preparation method of the present invention,
It is put into sputter (the model SBC-12 of sputter, Beijing KYKY Technology Development Co., Ltd.'s production) and carries out electricity
Pole sputters, and electrode obtains resistance-variable storing device after sputtering, and the silica that the resistance-variable storing device has doped carbon nanometer pipe hinders
Variation film.Using Keithley Current Voltage source table (keithley companies produce, model 2400) to this resistance-variable storing device
The carry out Electrical of resistance reverse speed characterisstic, as a result as shown in Figure 2.
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 be thermally treated resulting in atmosphere by preparation method of the present invention.Using Keithley electric current electricity
Carry out electric property of the potential source table (keithley companies produce, model 2400) to the resistance reverse speed characterisstic of the resistance-variable storing device
Analysis, as a result as shown in Figure 3.
From Fig. 2 and Fig. 3, unipolarity is all presented in the scanning area of the negative voltage of two resistance-variable storing devices, but in Fig. 1
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. 1
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 obvious resistance state change 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, specifically implements according to following steps:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT
Solution;
Step 2, according to 20:0.5 volume ratio measures silica sol, the CNT being prepared through step 1 respectively
Solution, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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
With dip-coating method layer of gel film is lifted on its surface;
Step 4, under argon gas protection, 20min heat is carried out to the gel film lifted out through step 3 with 200 DEG C of temperature
Processing, finally give 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, specifically implements according to following steps:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT
Solution;
Step 2, according to 20:0.6 volume ratio measures silica sol, the CNT being prepared through step 1 respectively
Solution, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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
With dip-coating method layer of gel film is lifted on its surface;
Step 4, under argon gas protection, 22min heat is carried out to the gel film lifted out through step 3 with 300 DEG C of temperature
Processing, finally give 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, specifically implements according to following steps:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT
Solution;
Step 2, according to 20:0.7 volume ratio measures silica sol, the CNT being prepared through step 1 respectively
Solution, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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
With dip-coating method layer of gel film is lifted on its surface;
Step 4, under argon gas protection, 20min- is carried out to the gel film lifted out through step 3 with 450 DEG C of temperature
30min is heat-treated, and finally gives 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, specifically implements according to following steps:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT
Solution;
Step 2, according to 20:0.8 volume ratio measures silica sol, the CNT being prepared through step 1 respectively
Solution, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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
With dip-coating method layer of gel film is lifted on its surface;
Step 4, under argon gas protection, 28min heat is carried out to the gel film lifted out through step 3 with 600 DEG C of temperature
Processing, finally give 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, specifically implements according to following steps:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT
Solution;
Step 2, according to 20:The CNT that 1 volume ratio measures silica sol respectively, is prepared through step 1 is molten
Liquid, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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
With dip-coating method layer of gel film is lifted on its surface;
Step 4, under argon gas protection, 30min heat is carried out to the gel film lifted out through step 3 with 700 DEG C of temperature
Processing, finally give the silica resistance changing film of doped carbon nanometer pipe.
Claims (5)
1. the preparation method of the silica resistance changing film of a kind of doped carbon nanometer pipe, it is characterised in that specifically according to following steps
Implement:
Step 1, using carbon nanotube powder as solute, absolute ethyl alcohol is solvent, and it is 10 to prepare concentration-5G/ml CNT is molten
Liquid;
Step 2, according to 20:The CNT that 0.5-1 volume ratio measures silica sol respectively, is prepared through step 1 is molten
Liquid, the silica sol after measuring and carbon nano-tube solution are mixed and stirred for uniformly, obtaining to 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 gives doping
The silica resistance changing film of CNT.
2. the preparation method of the silica resistance changing film of doped carbon nanometer pipe according to claim 1, it is characterised 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, it is characterised 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, it is characterised 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, it is characterised in that
In the step 4:The inert gas is argon gas.
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Citations (4)
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US20090078578A1 (en) * | 2007-09-21 | 2009-03-26 | Tsinghua University | Pre-plating solutions for making printed circuit boards and methods for preparing the same |
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 |
US20130295743A1 (en) * | 2010-09-08 | 2013-11-07 | Kabushiki Kaisha Toshiba | Nonvolatile memory device and method for manufacturing same |
CN106809817A (en) * | 2017-01-16 | 2017-06-09 | 东华大学 | A kind of preparation method of porous CNT |
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2017
- 2017-08-30 CN CN201710764056.8A patent/CN107663633B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US20090078578A1 (en) * | 2007-09-21 | 2009-03-26 | Tsinghua University | Pre-plating solutions for making printed circuit boards and methods for preparing the same |
US20130295743A1 (en) * | 2010-09-08 | 2013-11-07 | Kabushiki Kaisha Toshiba | Nonvolatile memory device and method for manufacturing same |
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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