CN110182839A - A method of using copper aluminum oxide film as precursor preparation cupric oxide nano array - Google Patents
A method of using copper aluminum oxide film as precursor preparation cupric oxide nano array Download PDFInfo
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- CN110182839A CN110182839A CN201910471088.8A CN201910471088A CN110182839A CN 110182839 A CN110182839 A CN 110182839A CN 201910471088 A CN201910471088 A CN 201910471088A CN 110182839 A CN110182839 A CN 110182839A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
A method of using copper aluminum oxide film as precursor preparation cupric oxide nano array, being related to a kind of method for preparing cupric oxide nano array.It is complicated that the present invention is to solve existing cupric oxide nano array preparation process, and the technical problem with target substrate associativity difference.The present invention: one, copper aluminate sull is prepared；Two, it welds；Three, hydro-thermal reaction.Presoma of the copper aluminate sull prepared by the present invention as synthesis CuO nanostructure, convenient for transplanting and operation, and chemical property is stablized in air, easily stored；The present invention prepares copper aluminate sull with heating process using simple impregnate, it is stacked and heated with solder and basis material later, the connection of presoma and matrix can be realized, copper aluminate sull presoma welds together with matrix before hydro-thermal reaction, after hydro-thermal reaction, the CuO nanostructure and matrix generated by forerunner's precursor reactant also has good combination.
Description
Technical field
The present invention relates to a kind of methods for preparing cupric oxide nano array.
Background technique
Copper oxide is a kind of p-type semiconductor material, and nano cupric oxide, can also since scale effect can be used as antibacterial material
For use as fields such as light auxiliary catalysis and electrochemical sensings.The method for preparing nano cupric oxide at present mainly has sol-gal process,
Hydro-thermal method, electrochemical method and use Copper substrate heated oxide etc..The nano cupric oxide prepared using chemical method is usually direct
Or indirectly with Kocide SD (Cu (OH)2) it is presoma or intermediate, and then nanometer CuO is obtained, but prepared by this method
CuO be in it is free powdered, good combination can not be formed with target substrate.It can be straight using the method for heated oxide Cu
It connects and obtains cupric oxide nano structure on Cu matrix, but the CuO that this method obtains is since there are biggish line is swollen with matrix
Swollen difference of coefficients and easily peeled off from matrix, nanometer CuO more stable in conjunction with matrix can only be obtained on very thin copper foil
Structure.
Summary of the invention
It is complicated that the present invention is to solve existing cupric oxide nano array preparation process, and with target substrate associativity difference
Technical problem, and provide a kind of using copper aluminum oxide film as the method for precursor preparation cupric oxide nano array.
Of the invention is by following using copper aluminum oxide film as the method for precursor preparation cupric oxide nano array
What step carried out:
One, it prepares copper aluminate sull: anodised aluminium (AAO) film with nano-pore is subjected to hot place
It manages, 4h~6h is impregnated in the ethanol solution for the dodecyl benzene sulfonic acid for being placed on 0.2mol/L~0.5mol/L after cooling and carries out parent
Water is modified, naturally dry after taking-up, then is placed in the CuCl of 1mol/L~2mol/L210min~30min is impregnated in aqueous solution, is taken
Naturally dry in air after out, is heat-treated again, obtains copper aluminate sull；
Two process of thermal treatment in this step are identical, carry out in Muffle furnace, and heating temperature is 900 DEG C~1000
DEG C, soaking time is 5min~30min；
Two, it welds: basis material is polished with sand paper, be then cleaned by ultrasonic 10min~15min with dehydrated alcohol, it is natural
It dries；Basis material, solder and the copper aluminate sull of step 1 preparation after cleaning is successively folded from top to bottom
It puts together, then heats, be cooled to room temperature, complete the welding of copper aluminate sull and matrix；
Three, hydro-thermal reaction: the product after step 2 is welded is put into high-pressure hydrothermal reaction kettle, and be added 0.2mol/L~
Product after the NaOH aqueous solution of 0.3mol/L welds step 2 is totally submerged, heating rate be 6.5 DEG C/min~7 DEG C/
Under conditions of min from room temperature to 190 DEG C~250 DEG C and 30min~120min is kept the temperature for making copper aluminate oxide
Film, which reacts, generates nano cupric oxide, takes out from reaction kettle after natural cooling, is cleaned with deionized water, obtains copper oxide
Nano-array；The volume of the NaOH aqueous solution of the 0.2mol/L~0.3mol/L is the 45% of high-pressure hydrothermal reaction kettle volume
~55%.
Design principle of the invention:
The AAO template selected in the present invention is transparent membrane, and chemical component is aluminum oxide (Al2O3), at normal temperature
For amorphous state, can be converted into after 900 DEG C~1000 DEG C of heating with η-Al in air2O3Based on activated alumina, and
And η-Al can be remained after dropping to room temperature2O3This crystal form.Al2O3With a variety of crystal forms, wherein η-Al2O3Belong to aluminium oxide function
One kind of energy ceramics, lattice types are spinel structure, and Ag base solder can be used and be attached, and chemistry with higher
Activity can react with many oxide and generate composite oxides, stable in the air can store.
AAO film heating is allowed to be converted into η-Al first by the present invention2O3, it is immersed in CuCl2Cover its surface in aqueous solution
Cover CuCl2, CuCl2Can become CuO first when heating in air, so with η-Al2O3Reaction generates Copper-Aluminum compound spinelle oxygen
Compound is welded on basis material with solder, as the presoma for generating CuO nanostructure finally by hydro-thermal later
Reaction makes copper aluminate sull decompose the CuO for generating nanostructure, obtains CuO nanometers good with matrix connectivity
Array.
The invention has the following advantages:
1, presoma of the copper aluminate sull prepared by the present invention as synthesis CuO nanostructure, convenient for moving
It plants and operates, and chemical property is stablized in air, it is easily stored；
2, operation of the present invention is simple and effective, and it is thin to prepare copper aluminate oxide using simple immersion and heating process
It is successively stacked and is heated with solder and basis material later, the connection of presoma and matrix can be realized by film；
3, the present invention is before hydro-thermal reaction, and copper aluminate sull presoma welds together with matrix, hydro-thermal
After reaction, the CuO nanostructure and matrix generated by forerunner's precursor reactant also has good combination.
The present invention proposes a kind of using copper aluminum oxide film as the method for precursor preparation cupric oxide nano array, behaviour
Make simple and effective, while a kind of method for connecting cupric oxide nano array with target substrate is proposed, before there is application well
Scape.
Detailed description of the invention
Fig. 1 is XRD diagram；
Fig. 2 is the SEM figure of three obtained cupric oxide nano arrays the step of testing one；
Fig. 3 is the SEM figure of three obtained products the step of testing three.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of using copper aluminum oxide film as precursor preparation copper oxide
The method of nano-array specifically carries out according to the following steps:
One, it prepares copper aluminate sull: the anodic aluminum oxide film with nano-pore is heat-treated, it is cold
But it is placed on immersion 4h~6h in the ethanol solution of the dodecyl benzene sulfonic acid of 0.2mol/L~0.5mol/L afterwards and carries out hydrophilic change
Property, naturally dry after taking-up, then it is placed in the CuCl of 1mol/L~2mol/L210min~30min is impregnated in aqueous solution, after taking-up
Naturally dry in air is heat-treated again, obtains copper aluminate sull；
Two process of thermal treatment in this step are identical, carry out in Muffle furnace, and heating temperature is 900 DEG C~1000
DEG C, soaking time is 5min~30min；
Two, it welds: basis material is polished with sand paper, be then cleaned by ultrasonic 10min~15min with dehydrated alcohol, it is natural
It dries；Basis material, solder and the copper aluminate sull of step 1 preparation after cleaning is successively folded from top to bottom
It puts together, then heats, be cooled to room temperature, complete the welding of copper aluminate sull and matrix；
Three, hydro-thermal reaction: the product after step 2 is welded is put into high-pressure hydrothermal reaction kettle, and be added 0.2mol/L~
Product after the NaOH aqueous solution of 0.3mol/L welds step 2 is totally submerged, heating rate be 6.5 DEG C/min~7 DEG C/
Under conditions of min from room temperature to 190 DEG C~250 DEG C and 30min~120min is kept the temperature for making copper aluminate oxide
Film, which reacts, generates nano cupric oxide, takes out from reaction kettle after natural cooling, is cleaned with deionized water, obtains copper oxide
Nano-array；The volume of the NaOH aqueous solution of the 0.2mol/L~0.3mol/L is the 45% of high-pressure hydrothermal reaction kettle volume
~55%.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: CuCl described in step 12
The concentration of aqueous solution is 1.5mol/L.Other are same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: described in step 2
Basis material is the ceramic material of high-temperature stable, specially Al2O3, BSCF, BCFN or BCFZ.Other and specific embodiment one
Or two is identical.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 2
The basis material stated is the metal material that fusing point is high and chemical property is stable, specially Pt, Crofer22APU, AISI310S or
AISI314.Other are identical as one of specific embodiment one to three.
Specific embodiment 5: present embodiment is unlike specific embodiment three and four: using single in step 2
Matter Ag is as solder, and heating described in step 2, the technique being cooled to room temperature are as follows: with 10 DEG C/min~15 in Muffle furnace
DEG C/heating rate of min to 970 DEG C~1000 DEG C and keeps the temperature 15min~45min from room temperature, it is then 5 in rate of temperature fall
DEG C/min~10 DEG C/min under conditions of be cooled to room temperature, connect matrix and copper aluminate sull.Other with it is specific
Embodiment three and four is identical.
Specific embodiment 6: the present embodiment is different from the first embodiment in that: matrix described in step 2
Material is in air easily by the material of high-temperature oxydation, specially Ti, Nb, Ni or carbon material.Other and specific embodiment one
It is identical.
Specific embodiment 7: present embodiment is unlike specific embodiment six: using AgCuTi in step 2
As solder, and heating described in step 2, the technique being cooled to room temperature are as follows: in a vacuum furnace, under conditions of vacuum with
The heating rate of 10 DEG C/min~15 DEG C/min to 780 DEG C~850 DEG C and keeps the temperature 15min under conditions of vacuum from room temperature
Then~45min is cooled to room temperature under conditions of vacuum and rate of temperature fall are 5 DEG C/min~10 DEG C/min, connects matrix
With copper aluminate sull.Other are identical as specific embodiment six.
Specific embodiment 8: present embodiment is unlike specific embodiment one to seven: described in step 1
Anodic aluminum oxide film with nano-pore is duplex structure, and with a thickness of 30 μm~60 μm, aperture is 40nm~100nm.Other
It is identical as specific embodiment one to seven.
Specific embodiment 9: the present embodiment is different from the first embodiment in that: Pt paillon is used in step 2
Sand paper polishing, is then cleaned by ultrasonic 10min~15min, naturally dry with dehydrated alcohol；Ag solder piece, step 1 are prepared into copper
Totally four samples are successively stacked together from top to bottom for aluminate sull, Ag solder piece and Pt paillon, are placed in Muffle
It is heated in furnace, to 970 DEG C and keeps the temperature 30min from room temperature under conditions of heating rate is 10 DEG C/min, be cooled to room temperature,
Weld together copper aluminate sull with Pt paillon.Other are same as the specific embodiment one.
The present invention is verified with following tests:
Test one: this test is a kind of using copper aluminum oxide film as the side of precursor preparation cupric oxide nano array
Method specifically carries out according to the following steps:
One, it prepares copper aluminate sull: the anodic aluminum oxide film with nano-pore is heat-treated, it is cold
But it is placed on afterwards in the ethanol solution of the dodecyl benzene sulfonic acid of 0.2mol/L and impregnates 4h progress hydrophilic modifying, dry in the air naturally after taking-up
It is dry, then it is placed in the CuCl of 1.5mol/L215min is impregnated in aqueous solution, naturally dry in air after taking-up carries out hot place again
Reason obtains copper aluminate sull；
Two process of thermal treatment in this step are identical, carry out in Muffle furnace, and heating temperature is 970 DEG C, heat preservation
Time is 30min；The anodic aluminum oxide film with nano-pore is duplex structure, with a thickness of 50 μm, aperture 60nm
~80nm；
Two, it welds: basis material Pt foil is polished with sand paper, be then cleaned by ultrasonic 10min~15min with dehydrated alcohol,
Naturally dry；From top to bottom successively by Pt foil, Ag solder and the copper aluminate sull of step 1 preparation after cleaning
It is stacked together, 30min to 970 DEG C and is kept the temperature from room temperature with the heating rate of 15 DEG C/min in Muffle furnace, is then existed
Rate of temperature fall is cooled to room temperature under conditions of being 10 DEG C/min, completes welding matrix and copper aluminate sull；
Three, hydro-thermal reaction: the product after step 2 is welded is put into high-pressure hydrothermal reaction kettle, and is added 0.2mol/L's
Product after NaOH aqueous solution welds step 2 is totally submerged, from room temperature liter under conditions of heating rate is 6.5 DEG C/min
Temperature is to 250 DEG C and keeps the temperature 60min and generates nano cupric oxide for making copper aluminate sull react, natural cooling
It takes out from reaction kettle, is cleaned with deionized water afterwards, obtain cupric oxide nano array；The NaOH aqueous solution of the 0.2mol/L
Volume be high-pressure hydrothermal reaction kettle volume 50%.
Fig. 1 is XRD diagram, and A is the anodic aluminum oxide film tested in one with nano-pore, and B is to have nanometer in test one
The anodic aluminum oxide film in hole is 970 DEG C in heating temperature, and soaking time is the sample after 30min, as can be seen from the figure non-
The anodic aluminum oxide film of crystalline state can be converted into the η-Al of crystalline state after 970 DEG C of heating in air2O3.Curve D is test
The copper aluminate sull that one the step of one obtains.
Test two: by CuCl2It in air, is 500 DEG C in heating temperature, the sample after soaking time is 30min carries out
XRD test, curve C as shown in figure 1, it can be seen that be CuO.
Fig. 2 is the SEM figure of three obtained cupric oxide nano arrays the step of testing one, it can be seen that this test preparation
In the form of sheets, the length in the direction z is larger for CuO nano-array, and links together with matrix.
Test three: this test is unlike test one: Pt paillon being polished with sand paper in step 2, then with anhydrous second
Alcohol is cleaned by ultrasonic 10min~15min, naturally dry；Ag solder piece, step 1 are prepared into copper aluminate sull, Ag
Totally four samples are successively stacked together from top to bottom for solder piece and Pt paillon, are placed in Muffle furnace and heat, are in heating rate
To 970 DEG C and 30min is kept the temperature from room temperature under conditions of 10 DEG C/min, is cooled to room temperature, keeps copper aluminate oxide thin
Film welds together with Pt paillon.It is other identical as test one.
Fig. 3 is the SEM figure of three obtained products the step of testing three, and region 1 is Ag, and region 2 is CuO, can see entirety
Structure is in sandwich-like, and CuO nano-array links together upper and lower two-part Ag.
Claims (9)
1. a kind of using copper aluminum oxide film as the method for precursor preparation cupric oxide nano array, it is characterised in that utilize
Copper aluminum oxide film carries out according to the following steps as the method for precursor preparation cupric oxide nano array:
One, it prepares copper aluminate sull: the anodic aluminum oxide film with nano-pore is heat-treated, after cooling
It is placed in the ethanol solution of the dodecyl benzene sulfonic acid of 0.2mol/L~0.5mol/L and impregnates 4h~6h progress hydrophilic modifying, take
Naturally dry after out, then it is placed in the CuCl of 1mol/L~2mol/L210min~30min is impregnated in aqueous solution, in air after taking-up
Middle naturally dry, is heat-treated again, obtains copper aluminate sull；
Two process of thermal treatment in this step are identical, carry out in Muffle furnace, and heating temperature is 900 DEG C~1000 DEG C,
Soaking time is 5min~30min；
Two, it welds: basis material is polished with sand paper, be then cleaned by ultrasonic 10min~15min, naturally dry with dehydrated alcohol；
Basis material, solder and the copper aluminate sull of step 1 preparation after cleaning is successively overlayed one from top to bottom
It rises, then heats, be cooled to room temperature, complete the welding of copper aluminate sull and matrix；
Three, hydro-thermal reaction: the product after step 2 is welded is put into high-pressure hydrothermal reaction kettle, and be added 0.2mol/L~
Product after the NaOH aqueous solution of 0.3mol/L welds step 2 is totally submerged, heating rate be 6.5 DEG C/min~7 DEG C/
Under conditions of min from room temperature to 190 DEG C~250 DEG C and 30min~120min is kept the temperature for making copper aluminate oxide
Film, which reacts, generates nano cupric oxide, takes out from reaction kettle after natural cooling, is cleaned with deionized water, obtains copper oxide
Nano-array；The volume of the NaOH aqueous solution of the 0.2mol/L~0.3mol/L is the 45% of high-pressure hydrothermal reaction kettle volume
~55%.
2. according to claim 1 a kind of using copper aluminum oxide film as precursor preparation cupric oxide nano array
Method, it is characterised in that CuCl described in step 12The concentration of aqueous solution is 1.5mol/L.
3. according to claim 1 a kind of using copper aluminum oxide film as precursor preparation cupric oxide nano array
Method, it is characterised in that basis material described in step 2 is the ceramic material of high-temperature stable, specially Al2O3、BSCF、
BCFN or BCFZ.
4. according to claim 1 a kind of using copper aluminum oxide film as precursor preparation cupric oxide nano array
Method, it is characterised in that basis material described in step 2 is the metal material that fusing point is high and chemical property is stable, specially
Pt, Crofer22 APU, AISI310S or AISI314.
5. according to claim 3 or 4 a kind of using copper aluminum oxide film as precursor preparation cupric oxide nano battle array
The method of column, it is characterised in that using simple substance Ag as solder in step 2, and heating described in step 2, it is cooled to room temperature
Technique are as follows: in Muffle furnace with 10 DEG C/min~15 DEG C/min heating rate from room temperature to 970 DEG C~1000 DEG C simultaneously
15min~45min is kept the temperature, is then cooled to room temperature under conditions of rate of temperature fall is 5 DEG C/min~10 DEG C/min, matrix is connected
With copper aluminate sull.
6. according to claim 1 a kind of using copper aluminum oxide film as precursor preparation cupric oxide nano array
Method, it is characterised in that basis material described in step 2 be in air easily by the material of high-temperature oxydation, specially Ti,
Nb, Ni or carbon material.
7. according to claim 6 a kind of using copper aluminum oxide film as precursor preparation cupric oxide nano array
Method, it is characterised in that using AgCuTi as solder in step 2, and heating described in step 2, the work being cooled to room temperature
Skill are as follows: in a vacuum furnace, with 10 DEG C/min~15 DEG C/min heating rate from room temperature to 780 DEG C under conditions of vacuum
~850 DEG C and heat preservation 15min~45min under conditions of vacuum, be then 5 DEG C/min~10 in vacuum and rate of temperature fall
DEG C/min under conditions of be cooled to room temperature, connect matrix and copper aluminate sull.
8. according to claim 1 a kind of using copper aluminum oxide film as precursor preparation cupric oxide nano array
Method, it is characterised in that the anodic aluminum oxide film described in step 1 with nano-pore is duplex structure, with a thickness of 30 μm
~60 μm, aperture is 40nm~100nm.
9. a kind of using copper aluminum oxide film as the method for precursor preparation cupric oxide nano array, it is characterised in that utilize
Copper aluminum oxide film carries out according to the following steps as the method for precursor preparation cupric oxide nano array:
One, it prepares copper aluminate sull: the anodic aluminum oxide film with nano-pore is heat-treated, after cooling
It is placed in the ethanol solution of the dodecyl benzene sulfonic acid of 0.2mol/L~0.5mol/L and impregnates 4h~6h progress hydrophilic modifying, take
Naturally dry after out, then it is placed in the CuCl of 1mol/L~2mol/L210min~30min is impregnated in aqueous solution, in air after taking-up
Middle naturally dry, is heat-treated again, obtains copper aluminate sull；
Two process of thermal treatment in this step are identical, carry out in Muffle furnace, and heating temperature is 900 DEG C~1000 DEG C,
Soaking time is 5min~30min；
Two, it welds: Pt paillon is polished with sand paper, be then cleaned by ultrasonic 10min~15min, naturally dry with dehydrated alcohol；It will
Ag solder piece, step 1 prepare copper aluminate sull, Ag solder piece and Pt paillon totally four samples from top to bottom according to
It is secondary to be stacked together, it is placed in Muffle furnace and heats, under conditions of heating rate is 10 DEG C/min simultaneously from room temperature to 970 DEG C
30min is kept the temperature, is cooled to room temperature, the welding of copper aluminate sull and Pt paillon is completed；
Three, hydro-thermal reaction: the product after step 2 is welded is put into high-pressure hydrothermal reaction kettle, and be added 0.2mol/L~
Product after the NaOH aqueous solution of 0.3mol/L welds step 2 is totally submerged, heating rate be 6.5 DEG C/min~7 DEG C/
Under conditions of min from room temperature to 190 DEG C~250 DEG C and 30min~120min is kept the temperature for making copper aluminate oxide
Film, which reacts, generates nano cupric oxide, takes out from reaction kettle after natural cooling, is cleaned with deionized water, obtains copper oxide
Nano-array；The volume of the NaOH aqueous solution of the 0.2mol/L~0.3mol/L is the 45% of high-pressure hydrothermal reaction kettle volume
~55%.
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