CN109607594A - A method of form controllable metal sulfide is prepared using polyacrylamide - Google Patents
A method of form controllable metal sulfide is prepared using polyacrylamide Download PDFInfo
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- CN109607594A CN109607594A CN201811550204.7A CN201811550204A CN109607594A CN 109607594 A CN109607594 A CN 109607594A CN 201811550204 A CN201811550204 A CN 201811550204A CN 109607594 A CN109607594 A CN 109607594A
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Abstract
A method of form controllable metal sulfide being prepared using polyacrylamide, is related to metal sulfide powders preparation and its morphology control technical field.Soluble metallic salt is dissolved in aqueous systems with thiocarbamide first and is mixed, polyacrylamide (PAM) aqueous solution is then added and is uniformly mixed, is reacted by hydrothermal deposition and generates metal sulfide precipitating particle；By adjusting additive amount, control reaction temperature and the time of polyacrylamide (PAM), the metal sulfide product of different shape is obtained.The present invention introduces suitable polyacrylamide (PAM) Polymer Solution in the reaction system, can effectively control the shape and size of CdS powder granule.The CdS powder for obtaining different shape has different visible light absorptions.Meanwhile research also found that this method can be used for preparing the Ag of quadrangle2S, standard cube Co2S3, cotton-shaped In2S3With the powders such as spherical ZnS.
Description
Technical field
The present invention relates to metal sulfide powders preparation and its morphology control technical fields, are specifically related to a kind of using poly-
The method of acrylamide preparation form controllable metal sulfide.
Background technique
As a kind of common metal sulfide, cadmium sulfide is a kind of important semiconductor, its forbidden bandwidth at room temperature
About 2.42eV is living in device for non-linear optical, light emitting diode, laser, solar battery, thin film sensor, photocatalysis
The fields such as property have a wide range of applications.In recent years, the CdS nanometer material of various patterns such as nano particle, nanometer rods, is received
Rice noodles, nanotube etc. are synthesized, and preparation method mainly has chemical precipitation method, electrochemical process, microwave irradiation, hydro-thermal
With solvent-thermal method etc..
Polyacrylamide (PAM) is a kind of water-soluble linear high-molecular compound, is quantified on the main chain of molecule with big
The very big amide group of activity is learned, this just assigns PAM with good surface-active, flocculability etc., makes it in water process, papermaking
It is extensive with the industrial applications such as ore dressing.The present invention is using PAM as form controlling agent, in hydro-thermal method reaction process, utilizes the PAM of chain
Macromolecule assembles to regulate and control CdS nano particle, to obtain variform CdS powder body material.
Summary of the invention
The present invention, which is directed to, has shortcoming in the presence of preparing metal sulfide, provides and a kind of utilizes polyacrylamide
The method for preparing form controllable metal sulfide.
To achieve the goals above, the technical scheme adopted by the invention is as follows: it is a kind of using polyacrylamide prepare form
The method of controllable metal sulfide, including hydrothermal deposition reaction, first dissolve soluble metallic salt and thiocarbamide in aqueous systems
Then mixing is added polyacrylamide (PAM) aqueous solution and is uniformly mixed, reacted by hydrothermal deposition and generate metal sulfide precipitating
Particle；By adjusting additive amount, control reaction temperature and the time of polyacrylamide (PAM), the metal sulphur of different shape is obtained
Compound product.
As the optimal technical scheme of preparation method of the present invention, soluble metallic salt be cadmium nitrate, silver nitrate, cobalt nitrate,
Indium nitrate, zinc nitrate prepare product and respectively correspond cadmium sulfide, silver sulfide, cobalt sulfide, indium sulfide, zinc sulphide.
As the optimal technical scheme of preparation method of the present invention, by the soluble metallic salt and 0.5~1g of 0.05~0.1g
Thiocarbamide mixing is dissolved in 20mL deionized water, then be added 0.01~7mL concentration be 4~6g/L polyacrylamide
(PAM) aqueous solution, which is uniformly mixed, carries out hydrothermal deposition reaction.
As the optimal technical scheme of preparation method of the present invention, the reaction time of hydrothermal deposition reaction is 300min, reaction
Temperature is 180 DEG C.
As the optimal technical scheme of preparation method of the present invention, hydrothermal deposition after reaction, is taken out reactant, is first spent
Ionized water ultrasonic agitation washing 4~5 times, then with ethanol washing 2~3 times, be then centrifuged for, dry and obtain target powder particle.
Compared with prior art, beneficial effects of the present invention are shown:
1), the present invention is with cadmium nitrate (Cd (NO3)2) and thiocarbamide be primary raw material, CdS powder is prepared by hydro-thermal method.?
Suitable polyacrylamide (PAM) Polymer Solution is introduced in the reaction system, can effectively control the shape of CdS powder granule
And size.
2), the CdS powder for the different shape that the present invention obtains has different visible light absorptions.Meanwhile research is also
It was found that this method can be used for preparing the Ag of quadrangle2S, standard cube Co2S3, cotton-shaped In2S3With the powders such as spherical ZnS.
3), the method for the present invention has easy to operate, and the product form and performance of acquisition are controllable, can be applied to other vulcanizations
The controllable preparation of powder.
Detailed description of the invention
Fig. 1 is influence of the PAM usage amount to CdS powder morphology is prepared in embodiment 1；
Fig. 2 is the XRD spectra of different shape CdS powder in embodiment 1；
Fig. 3 is the UV-Vis absorption properties of different shape CdS powder in embodiment 1；
Fig. 4 is the form of the other several sulfide powders prepared in embodiment 2.
Specific embodiment
Form controllable metal sulfide is prepared using polyacrylamide to of the invention with attached drawing with reference to embodiments
Method, which is made, to be discussed further.Flied emission scanning electron is respectively adopted in structure, the form performance of the method for the present invention products therefrom
Microscope (FE-SEM, SU8010) and chemical composition are characterized and are analyzed using X-ray powder diffraction (XRD, D3500).
Embodiment 1
Morphology influence of the PAM usage amount to CdS powder granule
1) the cadmium nitrate Cd (NO of 0.4g, is weighed with electronic balance3)2It is dissolved in the deionized water of 120mL with the thiocarbamide of 4g
It is uniformly mixed, and 6 parts of equal part, beaker is successively marked as 1,2,3,4,5,6.The polyacrylamide (PAM) for weighing 1g again is molten
Solution (solution concentration is 5g/L) into the deionized water of 200mL, is allowed to dissolution and is uniformly dispersed.
2), PAM is not added in No. 1 beaker, is sequentially added into 1mL, 2mL, 3mL, 5mL, 7mL into 2,3,4,5,6 beakers
PAM.And be stirred continuously, when solution after mixing, pour into the reaction kettle of 20mL and put baking oven into, setting reaction temperature be 180
DEG C, reaction time 300min.
3) reactant, after reaction, is taken out, and first with deionized water ultrasonic agitation washing 4~5 times, then washed with ethyl alcohol
It washs 2~3 times, obtains precipitating powder particle solution, powder granule is obtained by centrifugation, finally drying obtains target powder particle.
Macroscopically see, the color of 6 samples: No. 1 sample is red, and No. 2 and No. 3 samples are equal light red, No. 4 and No. 5 samples it is equal
To be light yellow, No. 6 samples are yellow.It is seen on microcosmic, by field emission scanning electron microscope observation, (1-6 sample respectively corresponds figure
1a~f), by Fig. 1 a it is found that the shape of the product of acquisition is mostly random when not adding PAM Polymer Solution in reaction system
Bulky grain is made of several primary and secondary particles, and particle is all larger；When adding a certain amount of PAM in the reaction system
After solution, the shape of product will gradually change: when PAM solution additive amount is less, the product of acquisition is by second particle group
At size is about 300nm~500nm, and the primary particle size in second particle is larger that (about 50nm~200nm is shown in figure
Shown in 1b, Fig. 1 c and Fig. 1 d)；When PAM solution is added to 5mL in reaction system, the product of acquisition is also by second particle group
At size is about 200nm, and shape is torispherical, and constituting its primary particle is about 20nm (see shown in Fig. 1 e).Work as reaction
When PAM solution additive amount is excessive in system, see that Fig. 1 f, product remain second particle composition, size becomes smaller, but its shape is not
It is smaller to form its particle size for rule.
Above-mentioned Electronic Speculum observation result is comprehensively compared it may be concluded that when not adding PAM, the product of acquisition is by primary and secondary
Particle mixing composition；As PAM amount gradually increases in reaction system, product is made of second particle, size will gradually
Reduce, and a CdS particle for constituting second particle is also gradually reduced；When PAM additional amount is excessive, though the size of product is
Second particle, but its size becomes irregularly again, meanwhile, excessive PAM addition will bring difficulty to the washing of subsequent products.
Therefore, it is 2~5mL that this optimum experimental, which goes out optimal PAM solution usage,.
Fig. 2 is the XRD spectra for the CdS powder product that the present embodiment obtains 3 kinds of different shapes, big of random CdS in figure
It is product prepared by 0mL, 2mL, 5mL that grain, CdS nano particle, CdS nanoparticle aggregate ball, which respectively correspond PAM solution additive amount,.
It is found that the different shape product that experiment obtains is high-purity CdS object phase after being compared with CdS standard x RD spectrogram.It further illustrates
, in the reaction system, the use of PAM does not change the structure of CdS.Based on the above results and analysis, CdS in reaction system
Available two reaction equations once of formation indicate:
Fig. 3 is the uv-visible absorption spectroscopy for the CdS powder product that the present embodiment obtains 3 kinds of different shapes, and comparison can
To obtain, the band ABSORPTION EDGE of CdS nano particle is about 565nm, and the band ABSORPTION EDGE of random CdS bulky grain is about 650nm, CdS
The band ABSORPTION EDGE of nanoparticle aggregate ball is about 600nm.As can be seen that the form of CdS has a significant impact to visible absorption.
Embodiment 2
PAM adds the influence grown to other sulfide grains
Based on the experimental method of embodiment 1, when other experiment conditions all keep identical, respectively with silver nitrate, cobalt nitrate,
Indium nitrate and zinc nitrate replace cadmium nitrate, are observed by field emission scanning electron microscope product is prepared, as shown in figure 4, can
To find out the Ag that quadrangle has successfully been obtained respectively2S (Fig. 4 a), standard cube Co2S3(Fig. 4 b), cotton-shaped (interweaved by several nanometer sheets
Into) In2S3The ZnS (Fig. 4 d) of (Fig. 4 c) and spherical shape, it follows that PAM also functions to regulation to the growthform of these sulfide
Effect.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (5)
1. a kind of method using polyacrylamide preparation form controllable metal sulfide, including hydrothermal deposition reaction, feature
It is, soluble metallic salt is dissolved in aqueous systems with thiocarbamide mix first, polyacrylamide (PAM) aqueous solution is then added
It is uniformly mixed, is reacted by hydrothermal deposition and generate metal sulfide precipitating particle；By the addition for adjusting polyacrylamide (PAM)
Amount, control reaction temperature and time, obtain the metal sulfide product of different shape.
2. preparation method as described in claim 1, which is characterized in that soluble metallic salt is cadmium nitrate, silver nitrate, nitric acid
Cobalt, indium nitrate, zinc nitrate prepare product and respectively correspond cadmium sulfide, silver sulfide, cobalt sulfide, indium sulfide, zinc sulphide.
3. preparation method as claimed in claim 2, which is characterized in that by the soluble metallic salt of 0.05~0.1g and 0.5~
The thiocarbamide of 1g dissolves mixing in 20mL deionized water, and the polyacrylamide that 0.01~7mL concentration is 4~6g/L is then added
(PAM) aqueous solution, which is uniformly mixed, carries out hydrothermal deposition reaction.
4. preparation method as claimed in claim 2, which is characterized in that the reaction time of hydrothermal deposition reaction is 300min, instead
Answering temperature is 180 DEG C.
5. preparation method as claimed in claim 1 or 2, which is characterized in that hydrothermal deposition after reaction, takes out reactant,
First with deionized water ultrasonic agitation washing 4~5 times, then with ethanol washing 2~3 times, it is then centrifuged for, dries and obtain target powder
Grain.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849786A (en) * | 2012-09-27 | 2013-01-02 | 电子科技大学 | Method for preparing cluster indium sulfide material |
| CN103011439A (en) * | 2011-09-20 | 2013-04-03 | 无锡尚德太阳能电力有限公司 | Cadmium-containing wastewater treatment method |
| CN103073073A (en) * | 2013-01-30 | 2013-05-01 | 吉林大学 | Synthetic method of transition metal sulfide |
| CN103553121A (en) * | 2013-10-18 | 2014-02-05 | 华东师范大学 | Preparation method of nano metal sulfide material |
| CN107117644A (en) * | 2017-06-16 | 2017-09-01 | 常州大学 | The preparation method of cadmium sulfide nano wires in miniemulsion colloid |
| CN108658128A (en) * | 2018-08-02 | 2018-10-16 | 合肥中航纳米技术发展有限公司 | A kind of MoS with hierarchical structure2The preparation method of micro-nano ball |
-
2018
- 2018-12-18 CN CN201811550204.7A patent/CN109607594A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011439A (en) * | 2011-09-20 | 2013-04-03 | 无锡尚德太阳能电力有限公司 | Cadmium-containing wastewater treatment method |
| CN102849786A (en) * | 2012-09-27 | 2013-01-02 | 电子科技大学 | Method for preparing cluster indium sulfide material |
| CN103073073A (en) * | 2013-01-30 | 2013-05-01 | 吉林大学 | Synthetic method of transition metal sulfide |
| CN103553121A (en) * | 2013-10-18 | 2014-02-05 | 华东师范大学 | Preparation method of nano metal sulfide material |
| CN107117644A (en) * | 2017-06-16 | 2017-09-01 | 常州大学 | The preparation method of cadmium sulfide nano wires in miniemulsion colloid |
| CN108658128A (en) * | 2018-08-02 | 2018-10-16 | 合肥中航纳米技术发展有限公司 | A kind of MoS with hierarchical structure2The preparation method of micro-nano ball |
Non-Patent Citations (1)
| Title |
|---|
| BISWAJIT MONDAL • SHYAMAL KUMAR SAHA: "Surfactant-assisted hydrothermal synthesis of CdS nanotips:optical and magnetic properties", 《J NANOPART RES》 * |
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