CN116253362A - Micrometer motor and preparation method and application thereof - Google Patents
Micrometer motor and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 16
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 15
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000033001 locomotion Effects 0.000 claims description 41
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 12
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 7
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 235000015165 citric acid Nutrition 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 230000029264 phototaxis Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- 239000000174 gluconic acid Substances 0.000 claims description 2
- 235000012208 gluconic acid Nutrition 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
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- 235000011090 malic acid Nutrition 0.000 claims description 2
- 239000012716 precipitator Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
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- 230000007246 mechanism Effects 0.000 abstract description 8
- 238000001962 electrophoresis Methods 0.000 abstract description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 238000003756 stirring Methods 0.000 description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
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- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 230000005684 electric field Effects 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000002105 nanoparticle Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
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- 239000002244 precipitate Substances 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
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- 241000195628 Chlorophyta Species 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
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- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
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- 239000004332 silver Substances 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 241000218378 Magnolia Species 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
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- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000003399 chemotactic effect Effects 0.000 description 1
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- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- AAQNGTNRWPXMPB-UHFFFAOYSA-N dipotassium;dioxido(dioxo)tungsten Chemical compound [K+].[K+].[O-][W]([O-])(=O)=O AAQNGTNRWPXMPB-UHFFFAOYSA-N 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
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- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052730 francium Inorganic materials 0.000 description 1
- KLMCZVJOEAUDNE-UHFFFAOYSA-N francium atom Chemical compound [Fr] KLMCZVJOEAUDNE-UHFFFAOYSA-N 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
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- 229910052744 lithium Inorganic materials 0.000 description 1
- DJZHPOJZOWHJPP-UHFFFAOYSA-N magnesium;dioxido(dioxo)tungsten Chemical compound [Mg+2].[O-][W]([O-])(=O)=O DJZHPOJZOWHJPP-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QNHNSPNFZFBEQR-UHFFFAOYSA-N n'-(3-trihydroxysilylpropyl)ethane-1,2-diamine Chemical compound NCCNCCC[Si](O)(O)O QNHNSPNFZFBEQR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
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- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a micrometer motor, a preparation method and application thereof, and belongs to the technical field of micrometer motors. The micrometer motor comprises tungsten oxide microneedles and silver nano particles, wherein the silver nano particles are unevenly loaded on the surfaces of the tungsten oxide microneedles; the length of the tungsten oxide microneedle is 4-7 mu m, and the width is less than 1 mu m; the particle size of the silver nano particles is 5nm-20nm. The micro motor is driven by a self-electrophoresis mechanism. Said WO 3 The Ag micrometer motor shows the ultraviolet-visible light driving light-shielding cluster behavior, combines the characteristics of instant response and simple controllability, and provides a new research thought for the preparation of the micro-robot.
Description
Technical Field
The invention belongs to the technical field of micrometer motors, and particularly relates to a micrometer motor, a preparation method and application thereof.
Background
In nature, many microorganisms (e.g., green algae, etc.) are able to sense light and take action. They normally exhibit in-situ rotational motion, and when they sense a change in the light signal of the surrounding environment, such as a dim light, they act to access the light source to gain food and energy, i.e., phototactic; in strong light, the light source is far away from the light source, so that the light source is prevented from being damaged, namely, the light source is back-lit, and the movement behavior of light response is shown. Light-driven micro/nanomotors have become an important point of research inspired by nature and have attracted increasing attention in recent years. In order to drive the micro/nanomotor through the input of light, a photo-responsive material must be introduced into the micro/nanomotor in advance so that a chemical or thermal gradient caused by photocatalysis, photo-thermal effects, photo-isomerization, or photo-degradation can be utilized to provide an effective driving force. Such light energy propulsion may even be achieved without external fuel. In addition, the remotely controllable nature makes optically driven micro/nanomotors attractive for a wide range of potential applications, including disease diagnosis, active drug delivery, sensing, environmental remediation, etc., but the electrochemical performance of micro/nanomotors has never been studied.
Microorganisms in nature (such as green algae) have the characteristic of "bidirectional" phototropism. It can not only swim in the direction of weak light to gain more energy through photosynthesis, but also can be far away from strong light, thereby avoiding injury or attack by escaping predators. Inspired by green algae, people are constantly striving to develop swimming micro-nano robots which can sense light intensity and can move autonomously depending on the change of the light intensity. So far, the colloid motor can realize self-driving under the light stimulus of different wave bands, and meanwhile, several different propulsion mechanisms are established, for example, the self-driving of the colloid motor can be realized through the generation of bubbles by the decomposition reaction of hydrogen peroxide in the photocatalytic enhancement solution, the movement of the colloid motor can also be driven by utilizing the gradient change of the surface tension of the colloid motor caused by the light doping process, and in addition, the self-electrophoresis mechanism based on the photocatalytic reaction or the self-diffusion electrophoresis mechanism and the self-electrophoresis mechanism caused by the photo-thermal effect are also commonly used for designing and realizing the self-driving of the colloid motor. However, the group swimming micro-nano robot capable of sensing light intensity and autonomously moving depending on the change of the light intensity is required to have the self-sensing and self-adapting capabilities of each component part of the group swimming micro-nano robot on light, and is extremely difficult to realize.
Disclosure of Invention
Therefore, the invention aims to solve the technical problems of slow light response, uncontrollable movement direction, complicated group movement in a movement control mode, limited application in a living body and the like of the micrometer motor in the prior art.
In order to solve the technical problems, the invention provides a micrometer motor and a preparation method and application thereof. The micrometer motor is described in WO 3 The micro-needle is used as a main body, ag nano particles are modified on the surface of the micro-needle by a self-assembly method, and the micro-motor cluster can generate group chemotactic/photophobic behaviors under the drive of ultraviolet light, and the micro-motor cluster is WO 3 The movement direction of the Ag micrometer motor group can be adjusted by the light intensity, and the control mode is simple.
A first object of the present invention is to provide a micro motor including tungsten oxide microneedles and silver nanoparticles unevenly loaded on the surface of the tungsten oxide microneedles; the length of the tungsten oxide microneedle is 4-7 mu m, and the width is less than 1 mu m; the particle size of the silver nano particles is 5nm-20nm.
In one embodiment of the invention, the mass ratio of the tungsten oxide microneedle to the silver nanoparticle is 48-52:1.
a second object of the present invention is to provide a method for manufacturing the micro motor, comprising the steps of,
(1) Dissolving tungstate, a precipitator, organic acid and sulfate in a solvent, and reacting to obtain a tungsten oxide microneedle;
(2) And (3) loading silver nano particles on the surface of the tungsten oxide microneedle in the step (1) to obtain the micrometer motor.
In one embodiment of the invention, in step (1), the concentration of the precipitant is 2.8mol/mL-3.2mol/mL.
In one embodiment of the invention, in step (1), the tungstate is one or more of sodium tungstate, potassium tungstate, magnesium tungstate, rubidium tungstate, cesium tungstate, francium tungstate, and lithium tungstate.
In one embodiment of the present invention, in step (1), the precipitant is one or more of nitric acid, hydrochloric acid, sulfuric acid, and permanganate.
In one embodiment of the present invention, in step (1), the organic acid is one or more of citric acid, malic acid, gluconic acid, formic acid, lactic acid, benzoic acid, acrylic acid, and acetic acid.
In one embodiment of the present invention, in the step (1), the mass ratio of the tungstate, the precipitant, the organic acid and the sulfate is 25 to 28:10-13:22-24:29-31.
In one embodiment of the invention, in step (1), the temperature of the reaction is 170 ℃ to 190 ℃; the reaction time is 22-26 h.
A third object of the present invention is to provide a solar cell prepared from the micro motor.
In one embodiment of the invention, the micro-motors undergo population movement behavior under lighting conditions; when the light intensity is less than 0.05W/cm 2 When the micrometer motor group generates phototactic behavior; when the light intensity is greater than 0.08W/cm 2 When the micrometer motor group is in a light-shielding state.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) The micrometer motor has self-electrophoresis effect, has cluster behavior under the drive of light in ultraviolet light wave band and visible light wave band, and realizes WO (WO) through the load of Ag nano particles 3 Photo-responsiveness of the microneedles. WO which is negatively charged by itself when illuminated 3 The Ag micrometer motor may have photochemical reaction, WO 3 The Ag and Ag are combined together in a self-assembly mode to form a heterojunction, which is favorable for electron transmission and prolongs the time of electron-hole recombination, and the specific reaction is as follows: A. WO (WO) 3 Separation of electrons and holes generated under ultraviolet-visible light excitationSince Ag is a good conductor of electrons, the electrons generated will be from WO 3 The conduction band of (2) moves rapidly through the heterojunction onto Ag; B. due to uneven loading of silver and uneven application of light, inWO 3 The surface of the Ag microneedle generates a photogenerated electric field, and weak light intensity (light intensity is less than 0.05W/cm) 2 ) WO below 3 As the microneedle body, a force moving along the direction of the electric field, i.e. a force moving towards the direction of the light source is generated under the action of the electric field force; in strong light (light intensity of more than 0.08W/cm) 2 ) The lower Ag particles store more electrons, and generate force away from the light source under the action of a spontaneous electric field to drive the micro-needle to move. By dynamically adjusting the power density of the input light, WO 3 The Ag micrometer motor group can show group behavior similar to that of green algae, and show group phototactic behavior in weak light; exhibiting group backlight motion under intense light. The light-driven swimming micro-nano motor has attractive force in various practical fields such as disease treatment, active drug delivery, sensing, environmental remediation and the like, particularly, the material is charged and can move in groups under illumination to be used as a novel green solar cell, and the light-driven swimming micro-nano motor has low price and can be prepared in a large scale.
(2) The micro motor of the present invention is driven by a self-electrophoretic mechanism. Said WO 3 The Ag micrometer motor shows the ultraviolet-visible light driving light-shielding cluster behavior, combines the characteristics of instant response and simple controllability, and provides a new research thought for the preparation of the micro-robot.
(3) The preparation method is simple, does not need complicated preparation process, and is suitable for mass production.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, in which:
FIG. 1 is WO of example 1 of the present invention 3 A preparation flow chart of Ag needle-shaped micrometer motor.
FIG. 2 is WO of example 1 of the present invention 3 SEM, AFM images and particle size distribution plots of the microneedles; wherein a is an SEM image; b-f are high resolution SEM images; g is an AFM image; h is the particle size distribution map.
FIG. 3 is WO of example 1 of the present invention 3 SEM and EDX images of Ag needle micrometer motors; wherein a is an SEM image; b-d is an analysis chart of Ag, O and W elements; e is XRD pairWO 3 And a test pattern of Ag; f is WO 3 /Ag、WO 3 Ag ultraviolet-visible absorbance graph.
FIG. 4 is a diagram of WO of comparative examples 1-2 of the present invention 3 SEM images of the material; wherein a is WO of comparative example 1 3 SEM images of the material; b is WO of comparative example 2 3 SEM image of the material.
FIG. 5 is WO of example 1 of the present invention 3 Group behavior of Ag needle-like micro-motors; wherein a-c are WO 3 Group phototactic behavior video screenshot of Ag needle-shaped micrometer motor; d is WO under strong light 3 Analyzing the motion behavior mechanism of the group of Ag needle-shaped micrometer motors in the direction away from the light source; e is WO in weak light 3 The group of Ag needle-shaped micrometer motors tends to move towards the light source for analysis of the action mechanism; f is WO in weak light 3 Group photochemical reaction production process analysis of Ag needle-like micro-motors.
FIG. 6 shows the implementation of the invention by adjusting the light intensity for WO at different light intensities 3 Clustered motions of different directions of Ag needle-shaped micrometer motor groups; wherein a-f are WO 3 Ag needle-shaped micrometer motor group phototactic behavior video screenshot; g-i is WO 3 The Ag needle-shaped micrometer motor group is subjected to shading behavior video screenshot; j-k is a motion schematic diagram of phototactic and photophobic cluster behaviors; l-m is WO at moderate light intensity 3 Ag needle micrometer motor population aggregation behavior video shots.
FIG. 7 is a video screenshot of the motion of the invention in a different container; wherein a-c are WO when there is a slope in the container 3 Ag needle micrometer motor group climbing video screenshot; d-f is as in WO 3 After the Ag needle-shaped micrometer motor group climbs up the slope, the group phototactic movement video screenshot can be continuously generated on the platform; g-h is WO when the slope of the ramp increases to 90 DEG 3 Group phototactic behavior video screenshot still occurs for Ag needle-shaped micrometer motor groups; i-k is WO when intense light is applied from the bottom of the container 3 The Ag needle-shaped micrometer motor group can generate a group photophobic behavior video screenshot in the vertical direction.
FIG. 8 is a graph of time versus voltage for clustered motion with different motion directions according to the present invention; wherein a is WO 3 Time-voltage curves accompanying phototactic movement of Ag needle-like micrometer motor populations; b is WO 3 Time-voltage curves accompanying the evasive motion of Ag needle-like micrometer motor populations.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
The invention relates to a reagent:
sodium tungstate dihydrate (Na) 2 WO 4 ·2H 2 O) available from michelia chemical company, inc;
concentrated nitric acid (HNO) 3 ) The concentration of (2) is 65% -68%, and is purchased from national pharmaceutical group chemical reagent company;
citric acid (C) 6 H 8 O 7 ) Purchased from Shanghai Source leaf Biotechnology Co., ltd;
sodium sulfate (Na) 2 SO 4 ) Purchased from Jiangsu-strong chemical Co., ltd;
silver nitrate (AgNO) 3 ) Purchased from sigma aldrich limited;
hydrogen peroxide (H) 2 O 2 ) Purchased from alaa Ding Shiji limited;
ethanol (C) 2 H 5 OH) from sigma aldrich limited;
deionized water was purchased from Shanghai Seiyaka Biotechnology Co., ltd;
sodium hydroxide (NaOH) was purchased from national pharmaceutical chemicals limited.
Example 1
Referring to fig. 1, a micrometer motor and a preparation method thereof specifically include the following steps:
(1)WO 3 preparation of microneedles: preparation of WO by hydrothermal method 3 Microneedle, 1.32g Na 2 WO 4 ·2H 2 O was dissolved in 30mL deionized water and 3mL of HNO was added dropwise with constant stirring 3 After stirring the solution (3M) for 6h, a white precipitate formed, which was then added dropwise6mL of 1M citric acid (C 6 H 8 O 7 ) After obtaining a transparent colloidal solution, 1.5g of Na is added 2 SO 4 Stirring for 30min, adding into a hydrothermal kettle, and keeping the temperature at 180 ℃ for 24h. After the hydrothermal kettle is cooled, centrifugal washing is carried out for 3 times by deionized water and ethanol, the obtained product is dried at 75 ℃ to obtain off-white powder, and the off-white powder is ground by a mortar to obtain WO 3 A microneedle.
(2)WO 3 Preparation of Ag needle-like micrometer motor: WO 0.17g was taken 3 The microneedle was added to the beaker. Subsequently 0.85g of AgNO was added 3 Dissolving in 50mL of deionized water, adding 2mL of the solution into a beaker, and standing for 5min. Stirring on a stirring table for 1 hr, dropwise adding 0.2M NaOH until no precipitate is generated, stirring the brown yellow solution for 5min, and adding sufficient amount of H 2 O 2 The obtained product is centrifugally washed with ethanol and deionized water for 3 times to obtain WO 3 Ag needle-like micrometer motor.
Example 2
A micrometer motor and a preparation method thereof specifically comprise the following steps:
(1)WO 3 preparation of microneedles: preparation of WO by hydrothermal method 3 Microneedle 1.47gK 2 WO 4 Dissolved in 30mL deionized water, 2.5mL of H was added dropwise with constant stirring 2 SO 4 After stirring the solution (3M) for 6h, a white precipitate was formed, then 6mL of 1M formic acid (HCOOH) solution was added dropwise, after obtaining a clear colloidal solution, 1.5g of urea was added, after stirring for 30min, the mixture was added to a hydrothermal kettle and the kettle was thermostated for 24h at 180 ℃. After the hydrothermal kettle is cooled, centrifugal washing is carried out for 3 times by deionized water and ethanol, the obtained product is dried at 75 ℃ to obtain off-white powder, and the off-white powder is ground by a mortar to obtain WO 3 A microneedle.
(2)WO 3 Preparation of Ag needle-like micrometer motor: WO to be obtained 3 The micro needle is dispersed on the substrate, then the substrate is placed in a cavity of a thermal evaporation coating instrument, nano Ag particles are placed in an evaporator, a mask is not added, the temperature is set to be 200 ℃ for 10s, and WO is enabled to be achieved 3 Microneedle surfaceA layer of Ag nano particles is unevenly loaded to obtain WO 3 Ag needle-like micrometer motor.
Example 3
A micrometer motor and a preparation method thereof specifically comprise the following steps:
(1)WO 3 preparation of microneedles: preparation of WO by hydrothermal method 3 Microneedle 1.22g MgWO 4 Dissolved in 30mL deionized water, 3mL HMnO was added dropwise with constant stirring 4 After stirring the solution (3M) for 6 hours, a precipitate was formed, and 6mL of 1M lactic acid (C 3 H 6 O 3 ) After obtaining a transparent colloid solution, adding 1.5g of NaNO 3 Stirring for 30min, adding into a hydrothermal kettle, and keeping the temperature at 180 ℃ for 24h. After the hydrothermal kettle is cooled, centrifugal washing is carried out for 3 times by deionized water and ethanol, the obtained product is dried at 75 ℃ to obtain off-white powder, and the off-white powder is ground by a mortar to obtain WO 3 A microneedle.
(2)WO 3 Preparation of Ag needle-like micrometer motor: WO obtained in step one 3 The micro needle is dispersed on the substrate, the substrate is placed in the cavity of the ion sputtering instrument, the Ag particles are placed in the evaporating dish, the sputtering time is set to be 30s after the cavity is vacuumized, the current is 19 mu A, and WO is obtained after 30s sputtering 3 Ag needle-like micrometer motor.
Comparative example 1
Substantially the same as in example 1, except for WO 3 Is prepared from the following steps:
WO 3 preparation of microneedles: preparation of WO by hydrothermal method 3 Microneedle, 1.32g Na 2 WO 4 ·2H 2 O was dissolved in 30mL deionized water and 0.5mL HNO was added dropwise with constant stirring 3 After stirring the solution (3M) for 6h, no white precipitate was obtained, and then 6mL of 1M citric acid (C 6 H 8 O 7 ) After obtaining a transparent colloidal solution, 1.5g of Na is added 2 SO 4 Stirring for 30min, adding into a hydrothermal kettle, and keeping the temperature at 180 ℃ for 24h. After the hydrothermal kettle is cooled, WO is obtained 3 A material.
Comparative example 2
Substantially the same as in example 1, except for WO 3 Is prepared from the following steps:
WO 3 is prepared from the following steps: preparation of WO by hydrothermal method 3 Microneedle, 1.32g Na 2 WO 4 ·2H 2 O was dissolved in 30mL deionized water and 5mL of HNO was added dropwise with constant stirring 3 The solution (3M) forms a precipitate during stirring, and 6mL of 1M citric acid (C 6 H 8 O 7 ) The solution, which remains opaque after half an hour of stirring, was added 1.5g of Na 2 SO 4 Stirring for 30min, adding into a hydrothermal kettle, and keeping the temperature at 180 ℃ for 24h. After the hydrothermal kettle is cooled, centrifugal washing is carried out for 3 times by deionized water and ethanol, the obtained product is dried at 75 ℃ to obtain white powder, and the white powder is ground by a mortar to obtain WO 3 A material.
Test example 1
WO to example 1 3 Microneedle and WO 3 The Ag needle-like micrometer motor was characterized and the results are shown in FIGS. 2-3. As can be seen from FIG. 2, WO is prepared 3 The Ag needle-like micrometer motor is about 7 μm in length and the microneedle thickness is about 500nm. The two ends of the microneedle body are symmetrical, in WO 3 The surface of the microneedle was unevenly loaded with Ag nanoparticles, and it was found that the surface of the microneedle was modified with Ag nanoparticles having a particle diameter of 5nm to 20nm by high-power SEM observation of the surface of the microneedle. During the preparation, ag element is derived from the added silver nitrate solution, and larger clusters are generated by the size difference generated in the process of converting silver nitrate into Ag simple substance to be adhered on the surface of the microneedle, and when the clusters are assembled in WO 3 The surface of the microneedle can cause uneven distribution of Ag element on the surface of the microneedle. As can be seen from fig. 3: o and W elements exist in the whole microneedle, and Ag elements are unevenly distributed in WO 3 The surface of the microneedle. And for Ag nanoparticles in WO 3 The modification process of the microneedle surface is explored, and Ag nano particles are modified by combining the Ag nano particles in WO (WO) in a self-assembly mode 3 The surface of the microneedle.
Test example 2
WO for comparative examples 1-2 3 The material was SEM characterized and the results are shown in FIG. 4. As can be seen in FIG. 4aWhen the amount of nitric acid used is too small (the added concentration is 0.5mL of 3M nitric acid), WO is synthesized 3 The structure is biased towards a cuboid. As can be seen from FIG. 4b, when the amount of nitric acid used is excessive (the added concentration is more than 5mL in 3M nitric acid), WO is synthesized 3 The structure is small particle size particles. WO (WO) 3 Structural changes lead to WO 3 After the Ag-loaded comparative example 1-2 micrometer motor is placed in water, the Brownian movement is more severe due to the greatly increased water solubility of the micrometer motor and the reduced size of the micrometer motor, so that the micrometer motor is finally rapidly dispersed in the water, and the application of a solar cell is difficult to realize.
Test example 3
WO to example 1 3 The population behavior of the Ag needle-like micrometer motor was tested and the results are shown in fig. 5. A horizontal long straight glass tube with the length of 12cm, the wall thickness of 0.5mm and the inner diameter of 5mm is filled with a water column with the length of 11cm, and WO is distributed at the bottom of the left side of the water column 3 Ag needle-like micrometer motor, applying ultraviolet-visible light with wavelength of 365nm and 546nm (FIG. 5 a) to right side of water column along horizontal direction, irradiating for 10s, and then making WO at bottom of water column 3 The Ag needle-shaped micrometer motor is obviously aggregated under the stimulation of ultraviolet-visible light, when WO 3 Dynamic adjustment of the input UV-visible Power Density WO when the Ag needle-like micrometer Motor is assembled into a cone shape (10 s-50 s) 3 The Ag needle-like micrometer motor clusters move in the ultraviolet-visible direction (FIG. 5 b), reducing the power density of the instrument by 0.005W/cm per minute 2 Final WO 3 The Ag needle micrometer motor population was moved to the right side of the tube near the light source (FIG. 5 c), at which point the optical power density was 0.1W/cm 2 。WO 3 The group motion of the Ag needle-like micrometer motor is driven by the self-electrophoresis effect, when the power density of the input ultraviolet-visible light is large (more than 0.08W/cm) 2 ) When the Ag particles gather a large amount of electrons, so that the micro needle receives strong electric field force far away from the light source in a spontaneous electric field (figure 5 d), and the micro motor is driven to move in a direction far away from the light source; when the power density of the input ultraviolet-visible light is small (less than 0.05W/cm 2 ) When WO 3 The force of the main body Ag of the microneedle is weak in the direction away from the light source, and the microneedle tends to move along the direction of the electric field, i.e., towardThe light source is moved in direction (fig. 5 e).
Test example 4
Exploration WO based on test example 3 3 The motion characteristics of the Ag needle-like micrometer motor are shown in FIG. 6. WO under stable UV-visible light irradiation 3 The distribution state of the Ag needle-shaped micrometer motor group is adjusted to be conical (within 1 min) from being horizontally paved at the bottom of a water column, and the power of the instrument is manually reduced to be 0.05W/cm 2 Initially decreasing by 0.005W/cm per minute 2 After dynamically adjusting the power density of the input UV-visible light, WO 3 Ag needle-like micrometer motor group moves towards ultraviolet-visible light direction (figure 6a-6e, time interval is 2 min), and WO is realized by continuously adjusting input ultraviolet-visible light power density 3 The Ag needle-like micrometer motor population eventually aggregates in the uv-visible direction of the cluster motion (after 9min, fig. 6 f). When the position of ultraviolet-visible light is adjusted to the left side of the tube, the input direction is from left to right irradiation, thus realizing WO 3 The Ag needle-shaped micrometer motor group moves towards the left side of the tube with unchanged movement characteristics, namely the original path returns (fig. 6g-6i, time interval is 1 min). The motion diagram is shown in the figure, and the motion diagram is shown in weak light (the optical power density is lower than 0.05W/cm) 2 ) WO below 3 Ag needle-like micrometer motor group phototactic movement (FIG. 6 j) in strong light (optical power density higher than 0.08W/cm) 2 ) WO below 3 Ag needle micrometer motor population backlight motion (fig. 6 k). When the optical power density is 0.05W/cm 2 And 0.08W/cm 2 The particles agglomerate under the action of the electric field and no trend movement occurs (figures 6l-6 m).
Test example 5
Exploration of WO of example 1 3 Applicability of the Ag needle-like micrometer motor population in different situations and potential applications, 100mg of WO 3 Ag needle-like micrometer motor dispersed in 1.5mL water with optical power density of 0.1W/m 2 The results are shown in fig. 7 under uv-vis drive: when WO 3 Ag needle-like micrometer motor in container with slope, and ultraviolet-visible light excited electric field force is large enough to overcome WO 3 The Ag needle-shaped micrometer motor part gravity and resistance encountered by climbing realize clustered movement upwards along the slope; when the gradient continues to increase to 90 DEGWO 3 The Ag needle-shaped micrometer motor completely overcomes the self gravity and the resistance encountered by climbing under the action of the electric field force excited by ultraviolet-visible light to realize the clustered movement along the vertical slope; WO when uv-vis light is applied from the bottom of the container 3 The Ag needle-shaped micrometer motor realizes that WO is continuously conveyed to the upper surface of the solution from the bottom of the container under the action of the electric field force excited by ultraviolet-visible light 3 Movement of Ag needle-like micrometer motor. In other words, the movement of the particles is independent of the structure of the container, WO when the container is changed from a parent tube to a cube 3 The Ag needle-like micrometer motor group also shows climbing (FIGS. 7a-7 c), ascending stairs (FIGS. 7d-7 f), and adherence climbing (FIGS. 7g-7 h). WO (WO) 3 The Ag needle-shaped micro-motor realizes breakthrough of the group behaviors of the micro-nano motor, and brings great promotion to the practical application of the micro-nano motor in the fields of disease diagnosis, active drug delivery (fig. 7i-7 k), sensing, environmental repair and the like, especially the application in the field of green solar cells.
Test example 6
As a result of further examining the phenomenon of test example 4, as shown in FIG. 8, when one platinum wire electrode was inserted into each of both sides of the tube, 0.05W/m was applied to the right side of the tube 2 WO in the tube 3 The Ag needle-like micrometer motor will gather in the tube and then be moved in the direction of the light source in clusters by manually reducing the power of the instrument to from 0.05W/cm 2 Initially decreasing by 0.005W/cm per minute 2 Dynamically adjusting the power density of the input ultraviolet-visible light to realize WO 3 The final movement of the Ag needle-like micrometer motor population to the light source is detected in WO by the open circuit voltage mode of the electrochemical workstation 3 The potential change is accompanied in the moving process of the Ag needle-shaped micrometer motor group, and the WO is used for the inside of the circular tube 3 The Ag needle-like micro motor movement produced a potential difference of about 70mV (fig. 8 a); applying 0.08W/m on the right side of the tube 2 WO in the tube 3 The Ag needle-like micrometer motor will gather in the tube and then be moved in the direction of the light source in clusters by manually setting the power of the instrument from 0.08W/cm 2 The increase of 0.01W/cm per minute was started 2 Dynamically adjusting input UV-variableImplementation of the power density of visible light WO 3 The Ag needle-like micrometer motor population moves to the electrode surface far from the light source at 90s, which can be detected in WO by the open circuit voltage mode of the electrochemical workstation 3 The potential change is accompanied in the moving process of the Ag needle-shaped micrometer motor group, and the WO is used for the inside of the circular tube 3 The Ag needle-like micro motor movement produced a potential difference of about 100mV (fig. 8 b). According to the theory of sedimentation potential (sedimentation potential means that when colloidal particles suspended in an electrolyte solution undergo sedimentation (movement from top to bottom) by external forces (gravity, centrifugal force, etc.), the particles have a tendency to separate from their electric double layer diffusion portions, thus generating an electric field in the direction of movement. The reason for the difference in the potential difference between the two movements is the phototactic cluster movement WO during the test 3 Less than the total number of the light-shading cluster motions WO of the Ag needle-shaped micrometer motors 3 Ag needle-like micrometer motor total number.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. The micro-motor is characterized by comprising tungsten oxide microneedles and silver nanoparticles, wherein the silver nanoparticles are unevenly loaded on the surfaces of the tungsten oxide microneedles; the length of the tungsten oxide microneedle is 4-7 mu m, and the width is less than 1 mu m; the particle size of the silver nano particles is 5nm-20nm.
2. The micro motor of claim 1, wherein the mass ratio of the tungsten oxide microneedles to the silver nanoparticles is 48-52:1.
3. a method for producing a micrometer motor according to claim 1 or 2, comprising the steps of,
(1) Dissolving tungstate, a precipitator, organic acid and sulfate in a solvent, and reacting to obtain a tungsten oxide microneedle;
(2) And (3) loading silver nano particles on the surface of the tungsten oxide microneedle in the step (1) to obtain the micrometer motor.
4. A method of producing a micrometer motor according to claim 3, wherein in step (1), the concentration of the precipitant is 2.8mol/mL to 3.2mol/mL.
5. A method of manufacturing a micrometer motor according to claim 3, wherein in step (1), the precipitant is one or more of nitric acid, hydrochloric acid, sulfuric acid, and permanganate.
6. The method of claim 3, wherein in the step (1), the organic acid is one or more of citric acid, malic acid, gluconic acid, formic acid, lactic acid, benzoic acid, acrylic acid, and acetic acid.
7. A method of producing a micrometer motor according to claim 3, wherein in step (1), the mass ratio of tungstate, precipitant, organic acid and sulfate is 25 to 28:10-13:22-24:29-31.
8. A method of producing a micrometer motor according to claim 3, wherein in step (1), the temperature of the reaction is 170 ℃ to 190 ℃; the reaction time is 22-26 h.
9. A solar cell, characterized in that it is produced from the micrometer motor according to claim 1 or 2.
10. The method according to claim 9The solar cell is characterized in that the micrometer motor generates group movement behavior under the illumination condition; when the light intensity is less than 0.05W/cm 2 When the micrometer motor group generates phototactic behavior; when the light intensity is greater than 0.08W/cm 2 When the micrometer motor group is in a light-shielding state.
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