CN110510568B - Silver-molybdenum sulfide dimer colloid motor and preparation method thereof - Google Patents
Silver-molybdenum sulfide dimer colloid motor and preparation method thereof Download PDFInfo
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- B81B3/00—Devices comprising flexible or deformable elements, e.g. comprising elastic tongues or membranes
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Abstract
The invention discloses a silver-molybdenum sulfide dimer colloid motor and a preparation method thereof. The motor is formed by attaching silver nanoparticles on spherical molybdenum sulfide particles; wherein, the particle size of the spherical molybdenum sulfide particle is 130-280nm, the spherical molybdenum sulfide particle is composed of molybdenum sulfide nanosheets, and the particle size of the silver nanoparticle is 20-80 nm; the method comprises the steps of sequentially dispersing ammonium molybdate, thiourea and polyvinylpyrrolidone in deionized water, performing ultrasonic treatment, performing airtight reaction at 220 ℃ under 180 ℃ and then performing centrifugal cleaning on the obtained clear mixed solution, dispersing the obtained spherical molybdenum sulfide particles in the deionized water, stirring the spherical molybdenum sulfide particle dispersion liquid, the deionized water and the tris (hydroxymethyl) aminomethane, quickly injecting a silver nitrate solution into the mixture, continuously stirring, and finally performing solid-liquid separation on the obtained intermediate product to obtain the target product. The method has wide application range and small pushing force, and is very easy to be widely applied to the fields of medicine transportation, environmental purification, ion detection and the like in a commercialized way.
Description
Technical Field
The invention relates to a colloidal motor and a preparation method thereof, in particular to a silver-molybdenum sulfide dimer colloidal motor and a preparation method thereof.
Background
The colloid motor is a device capable of converting chemical, electric, magnetic and other forms of energy into self mechanical motion in a liquid phase, and is expected to complete complex tasks such as drug transportation, environmental purification, ion detection and the like. The motion of the colloid motor mainly depends on the asymmetric distribution of catalytic components (such as Pt, Ag and the like which can catalyze hydrogen peroxide fuel) on the surface of the colloid motor, so that the catalytic fuel generates net resultant force to push the colloid motor to have directional motion. Currently, there are some beneficial attempts and efforts to obtain colloidal motors, such as those titled "Catalytic Nanomotors: Self-Propelled Sphere polymers", Small, 2010, 6 (4): 565-) The article of (1). The nanomotors mentioned therein consist of SiO2Platinum spherical particles are attached to the microspheres to form a dimer; the preparation method uses single-layer SiO2The microspheres are taken as a template, metal Cr used as a transition layer and noble metal Pt used as a catalyst layer are sequentially deposited on the surface of the top of the microspheres, and then the template with the top sequentially coated with the metal Cr and the noble metal Pt is annealed at high temperature to ensure that SiO is formed2And (3) after the precious metal Pt layer on the surface layer of the microsphere is contracted into spherical particles, performing ultrasonic dispersion to obtain a product. This product is though asymmetric Pt to hydrogen peroxide (H)2O2) The catalytic decomposition of (A) produces a net resultant force which makes it useful as a colloidal motor, but has disadvantages in that, first, SiO constituting a dimer2The volume of the microspheres and the platinum spherical particles is larger, wherein, SiO2The diameter of the microsphere is up to 970nm, and the particle size of the platinum spherical particles is up to more than 300nm, so that the application range is narrowed, and the resultant force required by pushing is greatly increased; second, the preparation method removes a single SiO layer2The technology for manufacturing the microsphere template is difficult and complex, annealing at 900 ℃ is needed for 3 hours, and the yield is too small, so that a product with wide application range and small pushing force cannot be obtained.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the silver-molybdenum sulfide dimer colloid motor with wide application range and small pushing resultant force.
The invention also aims to provide a preparation method of the silver-molybdenum sulfide dimer colloid motor.
In order to solve the technical problem of the invention, the silver-molybdenum sulfide dimer colloid motor is composed of a spherical dimer, and particularly:
the spherical dimer is silver nanoparticles attached to spherical molybdenum sulfide particles;
the particle size of the spherical molybdenum sulfide particle is 130-280nm, and the spherical molybdenum sulfide particle with the particle size of 130-280nm is composed of molybdenum sulfide nanosheets;
the particle size of the silver nanoparticles is 20-80 nm.
As a further improvement of the silver-molybdenum sulfide dimer colloid motor:
preferably, the silver nanoparticles are single crystal silver nanoparticles.
In order to solve another technical problem of the present invention, another technical solution is that the preparation method of the silver-molybdenum sulfide dimer colloidal motor comprises a hydrothermal synthesis method, and particularly comprises the following main steps:
step 1, firstly, according to the weight ratio of ammonium molybdate, thiourea, polyvinylpyrrolidone and deionized water of 0.17-0.18: 0.37-0.39: 0.12-0.13: 38-42, sequentially dispersing the three materials in deionized water, performing ultrasonic treatment for at least 25min to obtain a clear mixed solution, and performing closed reaction at 220 ℃ for at least 22h to obtain a reaction solution;
step 2, carrying out centrifugal cleaning on the reaction liquid to obtain spherical molybdenum sulfide particles, and then carrying out centrifugal cleaning on the spherical molybdenum sulfide particles and deionized water according to the weight ratio of the spherical molybdenum sulfide particles to the deionized water of 0.1-0.15: 450-550, dispersing the spherical molybdenum sulfide particles in deionized water to obtain a spherical molybdenum sulfide particle dispersion liquid;
step 3, firstly, according to the volume ratio of the spherical molybdenum sulfide particle dispersion liquid, deionized water, 0.1mol/L trihydroxymethyl aminomethane and 25mmol/L silver nitrate solution of 1:20-24:1.8-2.2:0.05-0.15, stirring the three materials at 25-35 ℃ for at least 8min, quickly injecting silver nitrate solution into the mixture, continuously stirring the mixture for at least 0.8h to obtain an intermediate product, and performing solid-liquid separation on the intermediate product to obtain the silver-molybdenum sulfide dimer colloid motor.
As a further improvement of the preparation method of the silver-molybdenum sulfide dimer colloid motor:
preferably, the silver-molybdenum sulfide dimer colloid motor obtained by solid-liquid separation is respectively washed 3 times by using ethanol and water; so as to obtain a purer target product.
Preferably, the power at ultrasound is 100W.
Preferably, the reaction solution is centrifugally washed 3 times with ethanol and water, respectively.
Preferably, the rotation speed of centrifugal separation in the centrifugal cleaning is 8000-10000r/min, and the time is 2-6 min.
Preferably, the solid-liquid separation treatment is centrifugal separation, the rotating speed is 8000-10000r/min, and the time is 2-6 min.
Compared with the prior art, the beneficial effects are that:
firstly, the prepared target product is characterized by using a scanning electron microscope and a transmission electron microscope respectively, and the result is combined with the preparation method to obtain the target product, namely, the spherical molybdenum sulfide particles are attached with silver nano particles; wherein the particle size of the spherical molybdenum sulfide particles is 130-280nm, the spherical molybdenum sulfide particles with the particle size of 130-280nm are composed of molybdenum sulfide nanosheets, and the particle size of the silver nanoparticles is 20-80nm, and the silver nanoparticles are single crystal silver nanoparticles. The target product assembled by the spherical molybdenum sulfide particles and the silver nanoparticles not only provides good nucleation sites for the growth of the silver nanoparticles, and the spherical molybdenum sulfide particles are composed of molybdenum sulfide nanosheets, so that the spherical molybdenum sulfide particles have very high activity, but also can catalyze and decompose fuel hydrogen peroxide solution due to the characteristics of the silver nanoparticles, and also lays a firm foundation for the target product as a colloidal motor due to the asymmetrical distribution of the silver nanoparticles on the surface of the spherical molybdenum sulfide particles, optimized particle diameters of the spherical molybdenum sulfide particles and the silver nanoparticles and the volume ratio of the spherical molybdenum sulfide particles and the silver nanoparticles.
Secondly, the preparation method is simple, scientific and efficient. The silver-molybdenum sulfide dimer colloidal motor which is a target product with wide application range and small pushing resultant force is prepared, and the silver-molybdenum sulfide dimer colloidal motor has the characteristics of convenience and rapidness in preparation, energy conservation, low cost, high yield and easiness in industrial mass production; further, the target product is easy to be widely applied to the fields of drug transportation, environmental purification, ion detection and the like in a commercial way.
Drawings
Fig. 1 is one of the results of characterization of spherical molybdenum sulfide particles obtained in the preparation process using a Scanning Electron Microscope (SEM) and a Transmission Electron Microscope (TEM). Fig. 1, panel a, is an SEM image of spherical molybdenum sulfide particles; and b is a TEM image of the spherical molybdenum sulfide particle shown in the a, and the spherical molybdenum sulfide particle is formed by molybdenum sulfide nanosheets.
FIG. 2 is one of the results of the characterization of the objective product obtained by the preparation method using a scanning electron microscope and a transmission electron microscope. In FIG. 1, the a-picture is an SEM image of the target product, and the b-picture is a TEM image of the target product shown in the a-picture.
Detailed Description
The preferred embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
First commercially available or manufactured on its own:
ammonium molybdate;
thiourea;
polyvinylpyrrolidone;
deionized water;
tris (hydroxymethyl) aminomethane;
silver nitrate solution;
ethanol;
and (3) water.
Then:
example 1
Step 1, firstly, according to the weight ratio of ammonium molybdate, thiourea, polyvinylpyrrolidone and deionized water of 0.17: 0.39: 0.12: 42, dispersing the first three in deionized water in sequence, and performing ultrasonic treatment for 25 min; wherein the power during the ultrasonic treatment is 100W, and a clear mixed solution is obtained. And placing the clear mixed solution at 180 ℃ for sealed reaction for 26 hours to obtain reaction liquid.
Step 2, firstly, centrifugally cleaning the reaction solution; wherein, the centrifugal cleaning is respectively performed for 3 times by using ethanol and water, the rotating speed during the centrifugal separation in the centrifugal cleaning is 8000r/min, and the time is 6min, so as to obtain the spherical molybdenum sulfide particles. And then according to the weight ratio of the spherical molybdenum sulfide particles to the deionized water of 0.1: 550, dispersing the spherical molybdenum sulfide particles in deionized water to obtain a spherical molybdenum sulfide particle dispersion liquid.
Step 3, firstly, according to the volume ratio of the spherical molybdenum sulfide particle dispersion liquid, deionized water, 0.1mol/L trihydroxymethyl aminomethane and 25mmol/L silver nitrate solution of 1: 20: 2.2:0.05, stirring the first three at 25 ℃ for 12min, quickly injecting silver nitrate solution into the mixture, and continuously stirring for 0.8h to obtain an intermediate product. Then carrying out solid-liquid separation treatment on the intermediate product; wherein the solid-liquid separation treatment is centrifugal separation, the rotating speed is 8000r/min, the time is 6min, then solid substances obtained by the solid-liquid separation are respectively washed 3 times by using ethanol and water, and the silver-molybdenum sulfide dimer colloid motor similar to that shown in figure 2 is prepared.
Example 2
Step 1, firstly, according to the weight ratio of ammonium molybdate, thiourea, polyvinylpyrrolidone and deionized water of 0.173: 0.385: 0.123: 41, dispersing the three materials in deionized water in sequence, and performing ultrasonic treatment for 28 min; wherein the power during the ultrasonic treatment is 100W, and a clear mixed solution is obtained. And placing the clear mixed solution at 190 ℃ for closed reaction for 25 hours to obtain reaction liquid.
Step 2, firstly, carrying out centrifugal cleaning on the reaction solution; wherein, the centrifugal cleaning is respectively performed 3 times by using ethanol and water, the rotating speed during centrifugal separation in the centrifugal cleaning is 8500r/min, and the time is 5min, so as to obtain the spherical molybdenum sulfide particles. And then according to the weight ratio of the spherical molybdenum sulfide particles to the deionized water of 0.12: 530, dispersing the spherical molybdenum sulfide particles in deionized water to obtain a spherical molybdenum sulfide particle dispersion.
Step 3, firstly, according to the volume ratio of the spherical molybdenum sulfide particle dispersion liquid, deionized water, 0.1mol/L trihydroxymethyl aminomethane and 25mmol/L silver nitrate solution of 1: 21: 2.1: 0.08, stirring the first three at 28 ℃ for 11min, quickly injecting a silver nitrate solution into the mixture, and continuously stirring the mixture for 0.9h to obtain an intermediate product. Then carrying out solid-liquid separation treatment on the intermediate product; wherein the solid-liquid separation treatment is centrifugal separation with a rotating speed of 8500r/min and a time of 5min, and then solid substances obtained by the solid-liquid separation are respectively washed 3 times by using ethanol and water, so as to prepare the silver-molybdenum sulfide dimer colloid motor similar to that shown in figure 2.
Example 3
Step 1, firstly, according to the weight ratio of ammonium molybdate, thiourea, polyvinylpyrrolidone and deionized water of 0.175: 0.38: 0.125: 40, dispersing the first three in deionized water in sequence, and performing ultrasonic treatment for 30 min; wherein the power during the ultrasonic treatment is 100W, and a clear mixed solution is obtained. And placing the clear mixed solution at 200 ℃ for closed reaction for 24 hours to obtain reaction liquid.
Step 2, firstly, centrifugally cleaning the reaction solution; wherein, the centrifugal cleaning is respectively 3 times of centrifugal cleaning by using ethanol and water, the rotating speed during centrifugal separation in the centrifugal cleaning is 9000r/min, and the time is 4min, so as to obtain the spherical molybdenum sulfide particles. And then according to the weight ratio of the spherical molybdenum sulfide particles to the deionized water of 0.13: 500, dispersing the spherical molybdenum sulfide particles in deionized water to obtain a spherical molybdenum sulfide particle dispersion liquid.
Step 3, firstly, according to the volume ratio of the spherical molybdenum sulfide particle dispersion liquid, deionized water, 0.1mol/L trihydroxymethyl aminomethane and 25mmol/L silver nitrate solution of 1: 22: 2: 0.1, stirring the first three at 30 ℃ for 10min, quickly injecting a silver nitrate solution into the mixture, and continuously stirring the mixture for 1h to obtain an intermediate product. Then carrying out solid-liquid separation treatment on the intermediate product; wherein the solid-liquid separation treatment is centrifugal separation at 9000r/min for 4min, and cleaning the solid obtained by solid-liquid separation with ethanol and water for 3 times to obtain silver-molybdenum sulfide dimer colloid motor shown in FIG. 2.
Example 4
Step 1, firstly, according to the weight ratio of ammonium molybdate, thiourea, polyvinylpyrrolidone and deionized water of 0.178: 0.375: 0.128: 39, dispersing the three materials in deionized water in sequence, and performing ultrasonic treatment for 33 min; wherein the power during the ultrasonic treatment is 100W, and a clear mixed solution is obtained. And placing the clear mixed solution at 210 ℃ for sealed reaction for 23 hours to obtain reaction liquid.
Step 2, firstly, carrying out centrifugal cleaning on the reaction solution; wherein, the centrifugal cleaning is respectively 3 times of centrifugal cleaning by using ethanol and water, the rotating speed during centrifugal separation in the centrifugal cleaning is 9500r/min, and the time is 3min, so that the spherical molybdenum sulfide particles are obtained. And then according to the weight ratio of the spherical molybdenum sulfide particles to the deionized water of 0.14: 480, dispersing the spherical molybdenum sulfide particles in deionized water to obtain a spherical molybdenum sulfide particle dispersion liquid.
Step 3, firstly, according to the volume ratio of the spherical molybdenum sulfide particle dispersion liquid, deionized water, 0.1mol/L trihydroxymethyl aminomethane and 25mmol/L silver nitrate solution of 1: 23: 1.9: 0.13, stirring the first three at 33 ℃ for 9min, quickly injecting a silver nitrate solution into the mixture, and continuously stirring the mixture for 1.1h to obtain an intermediate product. Then carrying out solid-liquid separation treatment on the intermediate product; wherein the solid-liquid separation treatment is centrifugal separation with the rotation speed of 9500r/min and the time of 3min, and then solid substances obtained by the solid-liquid separation are respectively washed 3 times by using ethanol and water, so as to prepare the silver-molybdenum sulfide dimer colloid motor similar to that shown in figure 2.
Example 5
Step 1, firstly, according to the weight ratio of ammonium molybdate, thiourea, polyvinylpyrrolidone and deionized water of 0.18: 0.37: 0.13: 38, dispersing the first three components in deionized water in sequence, and performing ultrasonic treatment for 35 min; wherein the power during the ultrasonic treatment is 100W, and a clear mixed solution is obtained. And placing the clear mixed solution at 220 ℃ for closed reaction for 22 hours to obtain reaction liquid.
Step 2, firstly, carrying out centrifugal cleaning on the reaction solution; wherein, the centrifugal cleaning is respectively performed 3 times by using ethanol and water, the rotating speed during centrifugal separation in the centrifugal cleaning is 10000r/min, and the time is 2min, so as to obtain the spherical molybdenum sulfide particles. And then according to the weight ratio of the spherical molybdenum sulfide particles to the deionized water of 0.15: 450, dispersing the spherical molybdenum sulfide particles in deionized water to obtain the spherical molybdenum sulfide particle dispersion liquid.
Step 3, firstly, according to the volume ratio of the spherical molybdenum sulfide particle dispersion liquid, deionized water, 0.1mol/L trihydroxymethyl aminomethane and 25mmol/L silver nitrate solution of 1: 24: 1.8: 0.15, stirring the first three at 35 ℃ for 8min, quickly injecting silver nitrate solution into the mixture, and continuously stirring the mixture for 1.2h to obtain an intermediate product. Then carrying out solid-liquid separation treatment on the intermediate product; wherein the solid-liquid separation is centrifugal separation with rotation speed of 10000r/min and time of 2min, and then solid obtained by solid-liquid separation is respectively washed for 3 times by using ethanol and water to prepare the silver-molybdenum sulfide dimer colloid motor similar to that shown in figure 2.
It is apparent that those skilled in the art can make various modifications and variations to the silver-molybdenum sulfide dimer colloid motor of the present invention and the method of preparing the same without departing from the spirit and scope of the present invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (6)
1. A preparation method of a silver-molybdenum sulfide dimer colloid motor, which consists of a spherical dimer, is characterized in that:
the spherical dimer is silver nanoparticles attached to spherical molybdenum sulfide particles;
the particle size of the spherical molybdenum sulfide particle is 130-280nm, and the spherical molybdenum sulfide particle with the particle size of 130-280nm is composed of molybdenum sulfide nanosheets;
the particle size of the silver nanoparticles is 20-80nm, and the silver nanoparticles are single crystal silver nanoparticles;
the preparation method comprises the following steps:
step 1, firstly, sequentially dispersing ammonium molybdate, thiourea, polyvinylpyrrolidone and deionized water in a weight ratio of 0.17-0.18: 0.37-0.39: 0.12-0.13: 38-42 in the deionized water, then carrying out ultrasonic treatment for at least 25min to obtain a clear mixed solution, and then placing the clear mixed solution at a temperature of 180 ℃ for a closed reaction for at least 22h to obtain a reaction solution;
step 2, carrying out centrifugal cleaning on the reaction liquid to obtain spherical molybdenum sulfide particles, and dispersing the spherical molybdenum sulfide particles in deionized water according to the weight ratio of the spherical molybdenum sulfide particles to the deionized water of 0.1-0.15: 450-550 to obtain a spherical molybdenum sulfide particle dispersion liquid;
and 3, firstly stirring the spherical molybdenum sulfide particle dispersion liquid, the deionized water, the 0.1mol/L trihydroxymethyl aminomethane and the 25mmol/L silver nitrate solution at a volume ratio of 1:20-24:1.8-2.2:0.05-0.15 at 25-35 ℃ for at least 8min, then quickly injecting the silver nitrate solution into the mixture and continuously stirring for at least 0.8h to obtain an intermediate product, and then carrying out solid-liquid separation treatment on the intermediate product to obtain the silver-molybdenum sulfide dimer colloidal motor.
2. The method of manufacturing a silver-molybdenum sulfide dimer colloid motor according to claim 1, wherein the silver-molybdenum sulfide dimer colloid motor obtained by solid-liquid separation is washed 3 times with ethanol and water, respectively.
3. The method of manufacturing a silver-molybdenum sulfide dimer colloid motor according to claim 1, wherein the power at the time of the ultrasonic treatment is 100W.
4. The method of manufacturing a silver-molybdenum sulfide dimer colloid motor according to claim 1, wherein the centrifugal washing of the reaction solution is performed 3 times by using ethanol and water, respectively.
5. The method for preparing a silver-molybdenum sulfide dimer colloid motor as claimed in claim 4, wherein the rotation speed of centrifugal separation in the centrifugal cleaning is 8000-10000r/min, and the time is 2-6 min.
6. The method for preparing a silver-molybdenum sulfide dimer colloid motor as claimed in claim 1, wherein the solid-liquid separation is centrifugal separation, and the rotation speed is 8000-10000r/min, and the time is 2-6 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5414194A (en) * | 1991-08-27 | 1995-05-09 | The Regents Of The University Of Colorado | Method of production of novel molybdenum-sulfide dimers and reactions of the same |
| CN105664976A (en) * | 2016-01-13 | 2016-06-15 | 三峡大学 | Supported two-dimensional layered molybdenum sulfide composite material and preparation method and application thereof |
| CN106964370A (en) * | 2017-03-21 | 2017-07-21 | 山东科技大学 | One kind oxidation silver nano-grain/ultrasonic near infrared light catalyst of molybdenum sulfide nanometer sheet heterojunction structure and preparation method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6878676B1 (en) * | 2001-05-08 | 2005-04-12 | Crompton Corporation | Nanosized particles of molybdenum sulfide and derivatives, method for its preparation and uses thereof as lubricant additive |
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|---|---|---|---|---|
| US5414194A (en) * | 1991-08-27 | 1995-05-09 | The Regents Of The University Of Colorado | Method of production of novel molybdenum-sulfide dimers and reactions of the same |
| CN105664976A (en) * | 2016-01-13 | 2016-06-15 | 三峡大学 | Supported two-dimensional layered molybdenum sulfide composite material and preparation method and application thereof |
| CN106964370A (en) * | 2017-03-21 | 2017-07-21 | 山东科技大学 | One kind oxidation silver nano-grain/ultrasonic near infrared light catalyst of molybdenum sulfide nanometer sheet heterojunction structure and preparation method |
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| "The adsorption and diffusion behavior of noble metal adatoms (Pd, Pt, Cu, Ag and Au) on a MoS2 monolayer: a first-principles study";Ping Wu等;《PHYSICAL CHEMISTRY CHEMICAL PHYSICS》;20170821;第19卷(第31期);第20713-20722页 * |
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