CN108069393A - A kind of hydrogenation Copper thin film and preparation method thereof - Google Patents
A kind of hydrogenation Copper thin film and preparation method thereof Download PDFInfo
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- CN108069393A CN108069393A CN201611000760.8A CN201611000760A CN108069393A CN 108069393 A CN108069393 A CN 108069393A CN 201611000760 A CN201611000760 A CN 201611000760A CN 108069393 A CN108069393 A CN 108069393A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/02—Hydrides of transition elements; Addition complexes thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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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
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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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to a kind of hydrogenation Copper thin film and preparation method thereof, the hydrogenation Copper thin film is the hydrogenation Copper thin film formed by the nanocrystalline continuous accumulation of 10~20nm for being formed in substrate surface.Heretofore described hydrogenation Copper thin film can deposit in arbitrary hydrophilic substrate surface, and macro surface is uniform, completely without cracking, microscopic appearance by 10~20 nm it is nanocrystalline it is continuous accumulate, be catalyzed, there is potential application foreground in the fields such as hydrogen storage and optics.
Description
Technical field
The present invention relates to a kind of hydrogenation Copper thin films and preparation method thereof, have in fields such as catalysis, hydrogen storage and optics potential
Application prospect belongs to thin-film material technical field.
Background technology
It is a kind of meta-stable metal hydride with ZnS crystal forms to hydrogenate copper, people is caused widely to study in recent years emerging
Interest.In organic reaction, can have with the hydrosilylation of efficient catalytic acetophenone and ketone in organic synthesis field extensive
Using；Secondly, hydrogenation copper can quick release hydrogen in a heated condition, may serve as efficient hydrogen storage material；And due to hydrogen
Change the special electronic structure of copper, also have potential using value in optics and semiconductor applications.The preparation of hydrogenation copper mainly includes
Chemical reduction method, ultrasonic method and ultraviolet radiation process, and up to now, the hydrogenation copper prepared by document report is powder material
Material, in catalytic applications there are it is very big the drawbacks of：(1) powder is difficult to disperse, and easily reunites, it is difficult to utmostly ensure reaction
The contact area of object and catalyst；(2) hydrogenation copper itself is unstable, and storage and the transport of powder be easy to cause its irreversible point
Solution；(3) after catalytic reaction, powder catalyst is difficult to realize efficiently separate.
The content of the invention
In view of the above-mentioned problems, the present invention's provides a kind of hydrogenation Copper thin film and one kind by the way of filming for the first time
The hydrogenation Copper thin film preparation method that simple economy, safety general can be mass.
On the one hand, the present invention provides a kind of hydrogenation Copper thin films, which is characterized in that the hydrogenation Copper thin film is to be formed in lining
The hydrogenation Copper thin film formed on bottom by the nanocrystalline continuous accumulation of 10~20nm.
Heretofore described hydrogenation Copper thin film can be deposited in arbitrary hydrophilic substrate surface, and macro surface is uniform, and complete nothing is opened
Split, microscopic appearance by 10~20nm it is nanocrystalline it is continuous accumulate, before having potential application in the fields such as catalysis, hydrogen storage and optics
Scape.
It is preferred that the thickness of the hydrogenation Copper thin film is 0.4~156 μm.
It is preferred that the material of the substrate is glass, one kind in ceramics, metal, paper.
It is preferred that it is preferred that the hydrogenation Copper thin film passes through humidifying by the presoma deposition liquid comprising copper source and reducing agent
It learns sedimentation in-situ reducing and is formed in the substrate surface.
On the other hand, the present invention also provides it is a kind of hydrogenate Copper thin film preparation method, including：
Copper source, reducing agent are dissolved in solvent, it is 1~7 to adjust pH, obtains presoma deposition liquid；
By substrate be immersed in presoma deposition liquid in, when deposition reaction 1~10 is small at 0~80 DEG C after, in the table of the substrate
Face obtains that Copper thin film must be hydrogenated.
It is preferred that copper source is at least one of copper chloride, copper sulphate, acetylacetone copper, copper acetate.
It is preferred that the molar concentration in copper source is 0.01~1mol/L in the presoma deposition liquid.
It is preferred that the reducing agent is at least one of sodium borohydride, sodium hypophosphite and hydrazine hydrate.
It is preferred that the reducing agent and the molar concentration rate in copper source are 1:(0.05~1).
It is preferred that the solvent is at least one of ethyl alcohol, methanol, deionized water and acetone.
In another aspect, the present invention also provides a kind of applications for hydrogenating Copper thin film in catalysis, hydrogen storage and optics.
The preparation method simple economy of hydrogenation Copper thin film of the present invention, raw material is cheap and easy to get, without professional equipment, has
Industrial production value.
Description of the drawings
Fig. 1 is the digital photograph of 1 differential responses time of the embodiment of the present invention obtained hydrogenation Copper thin film on the glass sheet；
Fig. 2 is the scanning electron of 1 differential responses time of the embodiment of the present invention obtained hydrogenation Copper thin film section on the glass sheet
Microscope (SEM) figure；
X-ray diffraction (XRD) figure of hydrogenation Copper thin film obtained after being the reaction of the embodiment of the present invention 1 3h Fig. 3；
FTIR spectrum (FTIR) figure of hydrogenation Copper thin film obtained after being the reaction of the embodiment of the present invention 1 3h Fig. 4；
The low power (a) and high power (b) SEM of hydrogenation Copper thin film obtained after being the reaction of the embodiment of the present invention 1 3h Fig. 5 are schemed；
Transmission electron microscope (TEM) figure of hydrogenation Copper thin film obtained after being the reaction of the embodiment of the present invention 1 3h Fig. 6；
Nanocrystalline high-resolution transmission electron microscopy in hydrogenation Copper thin film obtained after being the reaction of the embodiment of the present invention 1 3h Fig. 7
Mirror (HRTEM) figure；
Fig. 8 is the digital photograph for the hydrogenation Copper thin film that the embodiment of the present invention 2 is prepared on silicon chip；
Fig. 9 is the digital photograph for the hydrogenation Copper thin film that the embodiment of the present invention 3 is prepared on copper sheet；
Figure 10 is hydrogenation Copper thin film section SEM figures obtained on copper sheet in the embodiment of the present invention 3；
Figure 11 is the digital photograph for the hydrogenation Copper thin film that the embodiment of the present invention 4 is prepared on the scraps of paper.
Specific embodiment
It is further illustrated the present invention below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention is using the non-oxidizable mantoquita such as copper chloride, copper sulphate, acetylacetone copper, copper acetate as copper source, with boron hydrogen
Change sodium, sodium hypophosphite and hydrazine hydrate etc. as reducing agent, using wet-chemical sedimentation in substrate (glass, ceramics, metal, paper
Etc. arbitrary water wetted material) hydrogenation Copper thin film is prepared in surface.Preparing gained hydrogenation Copper thin film includes substrate and in the lining
The hydrogenation Copper thin film formed on bottom by the nanocrystalline continuous accumulation of 10~20nm.The thickness of the hydrogenation Copper thin film can pass through control
Sedimentation time processed is regulated and controled.The hydrogenation Copper thin film thickness can be 0.4~156 μm.Illustrate that the present invention carries to following exemplary
The method of the preparation hydrogenation Copper thin film of confession.
Copper source and reducing agent are dissolved in solvent in proportion, ultrasonic mixing is uniform, and obtaining presoma after adjusting solution ph sinks
Hydrops.Wherein, the solvent can be the common polar solvents such as ethyl alcohol, methanol, deionized water, acetone.The pH value of solution is adopted
With adjustings such as sulfuric acid, acetic acid and citric acids, pH value range can be 1~7.The copper source is mole dense in presoma deposits liquid
Degree can be 0.01~1mol/L.The reducing agent and the molar concentration rate in copper source can be 1:0.05~1:1.
As a preferred embodiment, copper source is selected in copper chloride, copper sulphate, acetylacetone copper and copper acetate at least
It is a kind of.
As a preferred embodiment, the copper source concentration can be 0.1~0.8mol/L.
As a preferred embodiment, the reducing agent selects at least one of sodium borohydride, sodium hypophosphite and hydrazine hydrate.
As a preferred embodiment, the molar ratio in the reducing agent and copper source can be 1:0.05~1:0.8.
As a preferred embodiment, the solvent can be at least one of ethyl alcohol, methanol, deionized water and acetone.
As a preferred embodiment, the solution ph can be 1.5~6.
Under certain reaction temperature (0~80 DEG C), clean substrate material is immersed in presoma deposition liquid, is stood (anti-
Should) substrate is taken out after a certain period of time, it is cleaned with deionized water and ethyl alcohol up to hydrogenation Copper thin film.
As a preferred embodiment, the temperature of the reaction can be 5~60 DEG C.
As a preferred embodiment, when the time of the reaction can be 1~10 small.
The present invention hydrogenates the thickness of Copper thin film as obtained by scanning electron microscope observes section survey.
Hydrogenation Copper thin film of the present invention can be deposited in arbitrary hydrophilic substrate surface, and macro surface is uniform, completely without cracking,
Microscopic appearance is accumulated by 10~20nm is nanocrystalline, has potential application foreground in fields such as catalysis, hydrogen storage and optics.It is described
Preparation method simple economy, raw material is cheap and easy to get, without professional equipment, has industrial production value.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Embodiment 1
0.01mol copper sulphate and 0.2mol sodium hypophosphites are dissolved in 20ml deionized waters at room temperature, after ultrasonic mixing is uniform,
Solution ph is adjusted to obtaining presoma deposition liquid after 5.At 50 DEG C, clean sheet glass substrate material is immersed in presoma
Liquid is deposited, substrate is taken out after standing (reaction) 1h, 3h and 5h respectively, is cleaned with deionized water and ethyl alcohol and be made on the glass sheet
Hydrogenate Copper thin film.
Fig. 1 is the digital photograph of differential responses time obtained hydrogenation Copper thin film on the glass sheet in the embodiment of the present invention
Piece, from left to right respectively sheet glass, stand hydrogenation Copper thin film (the CuH@glass that obtains on the glass sheet after 1h, 3h, 5h respectively
Piece), it can be seen that burgundy, fine and close flawless is presented in hydrogenation Copper thin film surface uniform ground；
Fig. 2 is the scanning electron of 1 differential responses time of the embodiment of the present invention obtained hydrogenation Copper thin film section on the glass sheet
Microscope (SEM) figure, it can be seen that the thickness for standing hydrogenation Copper thin film obtained by (reaction) 1h, 3h and 5h is respectively 0.4 μm, 12 μ
M, 73 μm, film thickness increases with the increase in reaction time；
Fig. 3 is X-ray diffraction (XRD) figure of hydrogenation Copper thin film obtained after reaction 3h in the embodiment of the present invention 1, be can confirm that
The film prepared is pure hydrogenation copper object phase, and free from admixture generates；
Fig. 4 is FTIR spectrum (FTIR) figure of hydrogenation Copper thin film obtained after reaction 3h in the embodiment of the present invention 1, can
To further confirm that significant Cu-H vibrations in film, the presence of the vibration peak of-OH shows that the hydrogenation Copper thin film surface prepared is inhaled
Attached a small amount of hydrone；
Fig. 5 is that the embodiment of the present invention 1 reacts the low power (a) of hydrogenation Copper thin film obtained after 3h and high power (b) SEM schemes, can be with
Find out that hydrogenation Copper thin film microscopic appearance is accumulated by 10~20nm nano particles；
Fig. 6 is transmission electron microscope (TEM) figure of hydrogenation Copper thin film obtained after reaction 3h in the embodiment of the present invention 1,
Further confirm that prepared hydrogenation Copper thin film is accumulated by 10~20nm nano particles；
Fig. 7 is that high-resolution transmitted electron nanocrystalline in hydrogenation Copper thin film obtained after reaction 3h in the embodiment of the present invention 1 is shown
Micro mirror (HRTEM) figure can confirm that nano particle is nanocrystalline for CuH, and a small amount of amorphous substance is contained on surface.
Embodiment 2
0.002mol copper acetates and 0.04mol hydrazine hydrates are dissolved in 20ml ethyl alcohol at room temperature, after ultrasonic mixing is uniform, adjusted
Solution ph is to obtaining presoma deposition liquid after 2.At 20 DEG C, clean silicon chip substrate is immersed in presoma deposition liquid, it is quiet
Substrate is taken out after putting 4h, is cleaned with deionized water and ethyl alcohol and hydrogenation Copper thin film is made i.e. on silicon chip.The present embodiment is on silicon chip
The thickness of gained hydrogenation Copper thin film is 94 μm；
Fig. 8 is the digital photograph of hydrogenation Copper thin film obtained on silicon chip in the embodiment of the present invention 2, it can be seen that hydrogenation copper is thin
Burgundy, fine and close flawless is presented in film surface uniform ground.
Embodiment 3
0.016mol copper chlorides and 0.03mol sodium hypophosphites are dissolved in 20ml deionized waters at room temperature, ultrasonic mixing is uniform
Afterwards, solution ph is adjusted to obtaining presoma deposition liquid after 6.At 5 DEG C, clean copper sheet substrate is immersed in presoma deposition
Liquid takes out substrate after standing 10h, is cleaned with deionized water and ethyl alcohol and hydrogenation Copper thin film is made i.e. on copper sheet；
Fig. 9 is the digital photograph of hydrogenation Copper thin film obtained on copper sheet in the embodiment of the present invention 3, it can be seen that hydrogenation copper is thin
Burgundy, fine and close flawless is presented in film surface uniform ground；
Figure 10 is hydrogenation Copper thin film section SEM figures obtained on copper sheet in the embodiment of the present invention 3, it can be seen that gained hydrogenates
The thickness of Copper thin film is 156 μm.
Embodiment 4
0.006mol acetylacetone coppers and 0.024mol sodium borohydrides are dissolved in 20ml methanol at room temperature, ultrasonic mixing is uniform
Afterwards, solution ph is adjusted to obtaining presoma deposition liquid after 3.At 25 DEG C, clean scraps of paper substrate is immersed in presoma and is sunk
Hydrops takes out substrate after standing 4h, is cleaned with deionized water and ethyl alcohol and hydrogenation Copper thin film is made i.e. on the scraps of paper.The present embodiment exists
The thickness of gained hydrogenation Copper thin film is 85 μm on the scraps of paper；
Figure 11 is the digital photograph of hydrogenation Copper thin film obtained on the scraps of paper in the embodiment of the present invention 4, it can be seen that hydrogenation copper
Burgundy, fine and close flawless is presented in film surface uniform ground.
In summary as it can be seen that hydrogenation Copper thin film provided by the invention can be deposited in arbitrary hydrophilic substrate surface, macro surface
Uniformly, completely without cracking, microscopic appearance continuous is accumulated by 10~20nm is nanocrystalline.
Wet-chemical sedimentation simple economy provided by the invention, raw material is cheap and easy to get, without professional equipment, has higher
Versatility.The hydrogenation Copper thin film has potential application foreground in fields such as catalysis, hydrogen storage and optics.
It is it is necessary to described herein finally：Above example is served only for making technical scheme further detailed
Ground explanation, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art's the above according to the present invention
Some the nonessential modifications and adaptations made all belong to the scope of protection of the present invention.
Claims (11)
1. a kind of hydrogenation Copper thin film, which is characterized in that it is described hydrogenation Copper thin film be formed in substrate surface by 10~20nm's
The hydrogenation Copper thin film that nanocrystalline continuous accumulation forms.
2. hydrogenation Copper thin film according to claim 1, which is characterized in that the thickness of the hydrogenation Copper thin film is 0.4~156
μm。
3. hydrogenation Copper thin film according to claim 1 or 2, which is characterized in that the material of the substrate for glass, ceramics,
One kind in metal, paper.
4. hydrogenation Copper thin film according to any one of claim 1-3, which is characterized in that it is described hydrogenation Copper thin film by comprising
The presoma of copper source and reducing agent deposition liquid is formed in the substrate surface by wet-chemical sedimentation in-situ reducing.
5. a kind of preparation method that Copper thin film is hydrogenated as any one of claim 1-4, which is characterized in that including：
Copper source, reducing agent are dissolved in solvent, it is 1~7 to adjust pH, obtains presoma deposition liquid；
By substrate be immersed in presoma deposition liquid in, when deposition reaction 1~10 is small at 0~80 DEG C after, in the table of the substrate
Face obtains that Copper thin film must be hydrogenated.
6. preparation method according to claim 5, which is characterized in that copper source is copper chloride, copper sulphate, acetylacetone,2,4-pentanedione
At least one of copper, copper acetate.
7. preparation method according to claim 5 or 6, which is characterized in that mole in copper source in the presoma deposition liquid
Concentration is 0.01~1 mol/L.
8. according to the preparation method any one of claim 5-7, which is characterized in that the reducing agent for sodium borohydride,
At least one of sodium hypophosphite and hydrazine hydrate.
9. according to the preparation method any one of claim 5-8, which is characterized in that the reducing agent and mole in copper source
Than for 1:（0.05~1）.
10. according to the preparation method any one of claim 5-9, which is characterized in that the solvent for ethyl alcohol, methanol,
At least one of deionized water and acetone.
11. a kind of application of the hydrogenation Copper thin film in catalysis, hydrogen storage and optics as any one of claim 1-4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111710873A (en) * | 2020-06-23 | 2020-09-25 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111710873A (en) * | 2020-06-23 | 2020-09-25 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
| CN111710873B (en) * | 2020-06-23 | 2021-09-17 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
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