CN107597146A - A kind of three-dimensional material based on copper sulfide lamellar structure, preparation method and applications - Google Patents
A kind of three-dimensional material based on copper sulfide lamellar structure, preparation method and applications Download PDFInfo
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- CN107597146A CN107597146A CN201710779628.XA CN201710779628A CN107597146A CN 107597146 A CN107597146 A CN 107597146A CN 201710779628 A CN201710779628 A CN 201710779628A CN 107597146 A CN107597146 A CN 107597146A
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- copper
- copper sulfide
- lamellar structure
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- dimensional material
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Abstract
The invention discloses a kind of three-dimensional material based on copper sulfide lamellar structure and preparation method thereof.The material includes Nano slices of copper sulphide and grown perpendicular to foam copper skeleton, a diameter of 58 microns of Nano slices of copper sulphide.Characterized in that, using foam copper as substrate framework material, the copper sulfide flake nano structure in its surface vertical-growth.Its preparation method is：Sulphur powder is disperseed in methyl alcohol, to add foam copper in obtained sulphur powder methanol dispersion liquid, be placed in reactor under 60 to 90 degrees Celsius, is incubated 36 hours.Copper sulfide laminated structure provided by the invention has the advantages of preparation technology is simple and catalytic activity is high, therefore has potential application prospect in fields such as photocatalysis, catalyst carrier, electrochemical hydrogen storages.
Description
Technical field
The invention belongs to preparation method of nano material field, more particularly, to a kind of based on copper sulfide lamellar structure
Three-dimensional material, its preparation method and its application.
Background technology
It is well known that the performance of material and application are not only relevant with its chemical composition, the size and shape of material are additionally depended on
Looks structure.Micro Nano material generally with single-size and pattern phase structure can show the physical chemistry better than bulk
Energy.Especially, two-dimensional nanostructure material is highly prone to everybody favor, is due to that this unique nanostructured has significantly
Structure and electronic characteristic.Electric transmission in nano-lamellar structure is limited in some specific plane or particular crystal plane, is in
Reveal the optically and electrically characteristic of uniqueness, and nano-lamellar structure the has spy such as density is low, specific surface area is big, avtive spot is more
Point, therefore there is highly important status in application fields such as photoelectricity, catalysis and energy storage.
With industry and it is economical develop rapidly and the excessive use of natural resources, it is increasingly convex the problem of environmental pollution
It is aobvious, the sustainable development of society is seriously constrained, have impact on the life quality of people.Photocatalysis technology is cheap too using cleaning
Toxic pollutant, using semiconductor as catalyst, can be decomposed into nontoxic material by positive energy, there is provided a kind of preferably energy profit
With with the method curbed environmental pollution.Sulfide has a variety of stoichiometric compositions, and valent state enriches, these advantages make it into
For in photocatalysis and the wide variety of excellent material of sensory field, the value of great development and application.At present, researchers use
Many methods have simultaneously prepared the copper sulfide nano material of many different-shapes, such as：Nanometer rods, nano wire, nanotube, receive
Rice piece, nano flower, hollow ball etc., the material of these unique patterns and structure can often improve the electronics of photo-generated carrier
Hole separation probability, reduce the electron-hole recombination rate of photo-generated carrier, improve photocatalytic activity.However, realize copper sulfide nano
The controllable preparation of rice material still has challenge.Using a kind of effective, easy method, which carrys out large area and prepares high orientation, to be had
The method of the nano structural material of sequence arrangement still needs further to explore, and strengthens the research work of this respect to national economy
Sustainable development and environmental protection are significant.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, object of the present invention is to provide one kind to be based on copper sulfide
The three-dimensional material of lamellar structure and its preparation, the method for proposing directly to participate in solvent thermal reaction using three-dimensional foam copper, its technique
Simply, yield is high.
A further object of the invention, there is provided the three-dimensional material based on copper sulfide lamellar structure drops as the light of organic dyestuff
Solution application.
To achieve the above object, according to one aspect of the present invention, there is provided it is a kind of based on copper sulfide lamellar structure three
Tie up material, the foam copper skeleton surface for being included in three-dimensional has synthesized CuS lamellar structure materials, the lamellar structure material perpendicular to
Foam copper skeleton superficial growth, for its diameter between 5 to 8 microns, thickness is 100 rans.
According to another aspect of the present invention, there is provided the preparation method of the three-dimensional material based on copper sulfide lamellar structure,
Comprise the following steps：
（1）Sulphur powder is dispersed in methyl alcohol, sulphur powder methanol dispersion liquid is made so that be dispersed with 0.5 mg in per ml methanol
To 2 mg sulphur powder particles；
（2）By step（1）Obtained sulphur powder methanol dispersion liquid is placed in using polytetrafluoroethylene (PTFE) as in the stainless steel autoclave of liner；
（3）In step（2）Described in reactor in slant setting piece of foam copper so that copper foam and sulphur powder mass ratio are 1：
0.5-1：0.8；
（4）By step（3）Described in reactor be placed in air dry oven, air dry oven temperature setting be 60-90 DEG C, instead
3-6 hours are maintained between seasonable.
Present invention also offers a kind of three-dimensional material based on copper sulfide lamellar structure in terms of methylene blue light urges degraded
Application.
Three-dimensional material product based on copper sulfide lamellar structure prepared by the present invention is cut into 1 × 1 cm sizes, is put into 10
1h is stirred in the methylene blue solution that mL concentration is 10 ppm and in the dark, catalyst surface is reached absorption-desorption attached
Balance.Add 0.1 ml hydrogen peroxide in the solution afterwards, be irradiated using 300 W high-pressure sodium lamps.Used every 3 min purple
The absorption spectrum of outside-visible spectrophotometer measure solution, methylene blue is determined by the characteristic absorption peak at 662 nm
Concentration.
In general, by the contemplated above technical scheme of the present invention compared with prior art, simple solvent is passed through
Hot method, the three-dimensional material of the copper sulfide lamellar structure perpendicular to foam copper substrate grown is obtained, such a structure increases sample
Specific surface area so that sample can contact with more reactants.The course of reaction does not introduce any reducing agent and surface is lived
Property agent, generation sample purity is high, and experimental repeatability is good.It is active provided by the present invention for the catalyst of degradation of methylene blue
High, the advantages that technique is simple.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram of copper foam surface load copper sulfide.
Fig. 2 is the scanning electron microscope diagram of the copper foam surface load copper sulfide of amplification.
Fig. 3 is the X-ray diffractogram of copper foam surface load copper sulfide.
Fig. 4 is the uv absorption spectra of photocatalytic degradation methylene blue.
Embodiment
Embodiment 1
The described three-dimensional material based on copper sulfide lamellar structure, its preparation method comprise the following steps：
（1）Sulphur powder is dispersed in methyl alcohol, sulphur powder methanol dispersion liquid is made so that be dispersed with 2.5 mg in per ml methanol
Sulphur powder particle；
（2）By step（1）Obtained sulphur powder methanol dispersion liquid is placed in using polytetrafluoroethylene (PTFE) as in the stainless steel autoclave of liner；
（3）In step（2）Described in reactor in slant setting piece of foam copper so that copper foam and sulphur powder mass ratio are 1：
0.68；
（4）By step（3）Described in reactor be placed in air dry oven, air dry oven temperature setting be 80 DEG C, reaction
Time is maintained at 6 hours.
Product is imaged by SEM, as shown in figure 1, can determine whether that copper sulfide lamella of the present invention is vertical
In the foam copper skeleton superficial growth of three-dimensional, it is evenly distributed, its diameter is between 5 to 8 microns.Shown by the scanning electron of amplification
Micro mirror is imaged to product, as shown in Fig. 2 can determine whether the three-dimensional material of the present invention based on copper sulfide lamellar structure, wherein piece
Layer vulcanization copper thickness is between 90-110 nanometers.The chemical constituent and crystal structure of product are carried out by X-ray diffraction spectra
Characterize, as shown in figure 3, can determine whether the XRD spectrum of the copper sulfide lamellar structure on foam copper surface with international standard card
(JCPDS, No.06-0464) unanimously, the copper sulfide lamellar structure for determining foam copper surface is the vulcanization copper crystal of hexagonal phase
(P63/mmc).Described its structure of the three-dimensional material based on copper sulfide lamellar structure is consistent with target product.
Embodiment 2
The three-dimensional material based on copper sulfide lamellar structure described in Application Example 1, as photochemical catalyst, catalytic degradation methylene
Indigo plant, so as to evaluate the catalytic activity of the described three-dimensional material based on copper sulfide lamellar structure.At ambient temperature, selection is ultraviolet
Light (300 W high-pressure sodium lamps, wavelength are 365 nm).Experimentation is as follows:
Three-dimensional material product based on copper sulfide lamellar structure prepared by the present invention is cut into 1 × 1 cm sizes, is put into 10 mL
1h is stirred in the methylene blue solution that concentration is 10 ppm and in the dark, catalyst surface is reached absorption-desorption attached flat
Weighing apparatus.Add 0.1 ml hydrogen peroxide in the solution afterwards, be irradiated using 300 W high-pressure sodium lamps.Treat that light-catalyzed reaction starts,
Absorption spectrum every 3 min using ultraviolet-visible spectrophotometer measure solution, passes through the characteristic absorption peak at 662 nm
To determine the concentration of methylene blue.The catalytic efficiency of photochemical catalyst is inhaled with ultraviolet-uisible spectrophotometer monitoring methylene blue solution
The change of luminosity is evaluated, and its result is as shown in figure 4, show that catalytic reaction drops aqueous solution of methylene blue in 18 minutes completely
Solution.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (8)
1. a kind of three-dimensional material based on copper sulfide lamellar structure, it is characterised in that synthesized on the foam copper skeleton surface of three-dimensional
Copper sulfide lamellar structure material.
2. the three-dimensional material as claimed in claim 1 based on copper sulfide lamellar structure, it is characterised in that copper sulfide lamella is vertical
In the foam copper skeleton superficial growth of three-dimensional.
3. the three-dimensional material as claimed in claim 1 based on copper sulfide lamellar structure, it is characterised in that the copper sulfide lamella
Diameter between 5 to 8 microns, thickness is 100 rans.
4. the preparation method of the three-dimensional material based on copper sulfide lamellar structure as described in claims 1 to 3 any one, it is special
Sign is, comprises the following steps：
（1）Methanol is added in polytetrafluoroethylene (PTFE) is the stainless steel autoclave of liner, by sulphur powder ultrasonic disperse in methanol, is made
Sulphur powder dispersion liquid A；
（2）Clean foam copper sheet is obliquely placed in the solution A, heating response, after terminating, naturally cools to room temperature, will
Product is respectively with deionized water and washes of absolute alcohol 3 times, and then 50 DEG C are dried in vacuo 4 hours.
5. the preparation method according to claim 4, it is characterised in that step obtains solution A described in (1) so that every
0.5 mg is dispersed with ml methanol to 2 mg sulphur powders.
6. the preparation method according to claim 4, it is characterised in that foam copper mass and sulphur powder described in step (2)
Mass ratio is 1：0.5-1：0.8.
7. preparation method according to claim 4, it is characterised in that the heating response described in step (2), temperature 60-
90 DEG C, hour in reaction time 3-6.
8. light of the copper sulfide sheetlike material as organic dyestuff methylene blue as described in claims 1 to 3 any one
Catalytic degradation application.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110180555A (en) * | 2019-04-02 | 2019-08-30 | 中原工学院 | A kind of preparation method and applications with three-layer laminated structure C uS catalyst |
| CN111974415A (en) * | 2020-08-31 | 2020-11-24 | 北京化工大学 | Copper sulfide/brass mesh electrode material with nanosheet array structure and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133534A (en) * | 2011-03-11 | 2011-07-27 | 许昌学院 | Preparation method and application of CuS catalyst with three-dimensional framework structure |
| CN103219491A (en) * | 2013-03-29 | 2013-07-24 | 湘潭大学 | Copper sulfide anode and preparation method thereof |
-
2017
- 2017-09-01 CN CN201710779628.XA patent/CN107597146A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133534A (en) * | 2011-03-11 | 2011-07-27 | 许昌学院 | Preparation method and application of CuS catalyst with three-dimensional framework structure |
| CN103219491A (en) * | 2013-03-29 | 2013-07-24 | 湘潭大学 | Copper sulfide anode and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ZHEN LI ET AL.: "Three-dimensional CuS hierarchical architectures as recyclable catalysts for dye decolorization", 《CRYSTENGCOMM》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110180555A (en) * | 2019-04-02 | 2019-08-30 | 中原工学院 | A kind of preparation method and applications with three-layer laminated structure C uS catalyst |
| CN111974415A (en) * | 2020-08-31 | 2020-11-24 | 北京化工大学 | Copper sulfide/brass mesh electrode material with nanosheet array structure and preparation method and application thereof |
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Application publication date: 20180119 |