CN112091232A - Rapid preparation of Au-TiO under acidic condition2Method of composite construction - Google Patents

Rapid preparation of Au-TiO under acidic condition2Method of composite construction Download PDF

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CN112091232A
CN112091232A CN202010951606.9A CN202010951606A CN112091232A CN 112091232 A CN112091232 A CN 112091232A CN 202010951606 A CN202010951606 A CN 202010951606A CN 112091232 A CN112091232 A CN 112091232A
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tio
solution
composite structure
stirring
concentration
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鲁颖炜
杨浩
邓小波
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Hefei University of Technology
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    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • 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
    • B22F1/16—Metallic particles coated with a non-metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/08—Drying; Calcining ; After treatment of titanium oxide

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  • Condensed Matter Physics & Semiconductors (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a method for quickly preparing Au-TiO under an acidic condition2Method for the production of a composite structure, in which TiO is first treated by addition of hydrochloric acid2Adjusting the aqueous solution to acidity, then preparing nano gold particles which can stably exist under the acidic condition by using sodium borohydride as a reducing agent and PVP as a protective agent, and finally dissolving the nano gold particlesThe solution is slowly dripped into acidic TiO2In the solution, the Au-TiO is prepared by rapid stirring, centrifugal washing and drying2And (3) a composite structure. The preparation method provided by the invention is simple to operate and high in reaction speed, and the prepared Au-TiO2In the composite structure, the nano-gold particles are in TiO2The surface is uniformly distributed. In addition, the composite structure has broad spectral absorption properties covering the ultraviolet and visible regions.

Description

Rapid preparation of Au-TiO under acidic condition2Method of composite construction
Technical Field
The invention relates to the field of material preparation, in particular to a method for quickly preparing Au-TiO under acidic condition2A method of forming a composite structure.
Background
TiO2Due to the advantages of good physical and chemical stability, high catalytic efficiency, low cost and the like, the catalyst has wide application prospect in the photoelectric, photovoltaic and photochemical fields of solar cells, photocatalysis and the like. However, TiO2The characteristic of the self-wide band gap semiconductor is that the semiconductor can only absorb ultraviolet light in the solar spectrum. Meanwhile, the high electron-hole recombination rate of the material makes the photon-generated carriers difficult to be separated efficiently. These two points limit TiO2Large-scale application in the fields of photocatalysis and photoelectric conversion.
Loading noble metal nano-particles (Au, Ag, etc.) to TiO2Surface, not only can make TiO2The absorption range of (2) is expanded to the visible region, and TiO can be reduced2The electron-hole recombination rate is improved, thereby being beneficial to expanding the application range of the composite material. Currently, noble metal nanoparticle loading deposition onto TiO2The predominant method of surface deposition-precipitation is. The method is characterized in that the preparation solution is adjusted to be alkaline, and the chloroauric acid aqueous solution is selectively prepared from Au (OH)3Is deposited on TiO2And carrying out subsequent heat treatment on the surface to obtain the composite material. However, the method has complicated experimental steps and poor repeatability, and the nano gold is seriously agglomerated in the subsequent heat treatment process, so that the light absorption performance of the composite structure is greatly reduced. In an acid environment, the gold nanoparticles are easy to agglomerate, and the optical performance of the composite structure is reduced. Thus, Au-TiO is prepared under acidic conditions2Methods for composite structures have been rarely reported.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide the following steps: provides a method for rapidly preparing Au-TiO under acidic condition2A method of forming a composite structure.
In order to achieve the above purpose, the invention provides the following technical scheme:
under acidic conditionRapid preparation of Au-TiO2The method for compounding the structure comprises the following specific steps:
(1) weighing TiO2Dispersing the mixture in deionized water, adding hydrochloric acid, and magnetically stirring the mixture uniformly for later use;
(2) weighing chloroauric acid solution, adding deionized water for dilution, then adding polyvinylpyrrolidone, stirring uniformly, quickly injecting sodium borohydride solution, and continuously stirring for 8-15min to obtain nanogold solution for later use;
(3) and (3) measuring the nano gold solution in the step (2), slowly dripping the nano gold solution into the acidic solution prepared in the step (1), quickly stirring for 8-15min, centrifuging and washing the product for 2-4 times, and finally drying at 55-65 ℃.
Preferably, in the step (1), the molar concentration of the hydrochloric acid is 11.97-47.88 mmol/L.
Preferably, in the step (2), the concentration of the chloroauric acid is 10mg/mL, the concentration of the polyvinylpyrrolidone is 0.5-2mg/mL, and the concentration of the sodium borohydride is 0.22-0.56 mg/mL.
Preferably, in the step (3), the volume ratio of the nano gold solution to the acidic solution prepared in the step (1) is 0.111-0.667.
Preferably, in the step (3), the dropping speed of the nano gold solution is 1-2 drops/second.
Preferably, in the step (3), the stirring speed is 1500-.
Compared with the prior art, the invention has the following advantages:
1. the preparation method provided by the invention has the advantages of simple process, simple and convenient operation and high reaction speed.
2. In the invention, Au-TiO is prepared2In the composite structure, the nano-gold particles are in TiO2The surface is uniformly distributed.
3. Au-TiO prepared by the invention2The composite structure has broad spectrum absorption properties covering the ultraviolet and visible regions.
Drawings
FIG. 1 shows Au-TiO compounds prepared in examples 1 to 4 of the present invention2Zeta potential map of the composite structure. It can be seen that the nano gold solution is addedAfter the solution, TiO2The Zeta potential value is reduced, which shows that the Au-TiO can be prepared by the invention2And (3) a composite structure. In addition, TiO is added with the addition of the nano gold solution2The potential value of the catalyst is gradually reduced, which shows that the invention can prepare Au-TiO with different gold loading rates2And (3) a composite structure.
FIG. 2 shows Au-TiO prepared in example 4 of the present invention2X-ray photoelectron spectroscopy. It is obvious that the Au-TiO prepared by the invention2The composite structure contains C, O, Ti and Au elements.
FIG. 3 shows Au-TiO prepared in example 4 of the present invention2TEM photograph of the composite structure. The gold nanoparticles can be seen to be uniformly distributed in the TiO2Surface without obvious agglomeration
FIG. 4 shows Au-TiO compounds prepared in examples 1 to 4 of the present invention2Absorption spectrum of the composite structure. It can be seen that the Au-TiO prepared by the invention2The composite structure has broad spectrum absorption properties covering the ultraviolet and visible regions.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1:
step 1: weigh 0.5g TiO2Dispersing the hydrochloric acid into deionized water, adding a certain amount of hydrochloric acid to enable the molar concentration of the hydrochloric acid to be 23.94mmol/L, and magnetically stirring the hydrochloric acid uniformly for later use;
step 2: 1mL of chloroauric acid solution with a concentration of 10mg/mL was measured and diluted with 7mL of deionized water. Then adding 10mg of polyvinylpyrrolidone (PVP), stirring uniformly, quickly injecting 2mL of sodium borohydride solution to ensure that the concentration of the PVP is 1mg/mL and the concentration of the sodium borohydride is 0.45mg/mL, and continuously stirring for 10min for later use;
and step 3: 5mL of the nano-gold solution prepared in the step 2 is measured, slowly and dropwise added into the solution in the step 1 at the speed of 1 drop per second, rapidly stirred for 10min at the stirring speed of 2600r/min, and the product is centrifugally washed for 3 times and finally dried at the temperature of 60 ℃.
Example 2:
step 1: weigh 0.5g TiO2Dispersing in deionized water, adding a certain amount of hydrochloric acid, and making itThe molar concentration is 23.94mmol/L, and the mixture is stirred evenly by magnetic force for standby;
step 2: 1mL of chloroauric acid solution with a concentration of 10mg/mL was measured and diluted with 7mL of deionized water. Then adding 10mg of polyvinylpyrrolidone (PVP), stirring uniformly, quickly injecting 2mL of sodium borohydride solution to ensure that the concentration of the PVP is 1mg/mL and the concentration of the sodium borohydride is 0.45mg/mL, and continuously stirring for 10min for later use;
and step 3: measuring 10mL of the nano-gold solution prepared in the step 2, slowly dripping the nano-gold solution into the solution in the step 1 at the speed of 1 drop per second, rapidly stirring the nano-gold solution for 10min at the stirring speed of 2600r/min, centrifugally washing the product for 3 times, and finally drying the product at the temperature of 60 ℃.
Example 3:
step 1: weigh 0.5g TiO2Dispersing the hydrochloric acid into deionized water, adding a certain amount of hydrochloric acid to enable the molar concentration of the hydrochloric acid to be 23.94mmol/L, and magnetically stirring the hydrochloric acid uniformly for later use;
step 2: 1mL of chloroauric acid solution with a concentration of 10mg/mL was measured and diluted with 7mL of deionized water. Then adding 10mg of polyvinylpyrrolidone (PVP), stirring uniformly, quickly injecting 2mL of sodium borohydride solution to ensure that the concentration of the PVP is 1mg/mL and the concentration of the sodium borohydride is 0.45mg/mL, and continuously stirring for 10min for later use;
and step 3: 15mL of the nano-gold solution prepared in the step 2 is measured, slowly and dropwise added into the solution in the step 1 at the speed of 1 drop per second, rapidly stirred for 10min at the stirring speed of 2600r/min, and the product is centrifugally washed for 3 times and finally dried at 60 ℃.
Example 4:
step 1: weigh 0.5g TiO2Dispersing the hydrochloric acid into deionized water, adding a certain amount of hydrochloric acid to enable the molar concentration of the hydrochloric acid to be 23.94mmol/L, and magnetically stirring the hydrochloric acid uniformly for later use;
step 2: 1mL of chloroauric acid solution with a concentration of 10mg/mL was measured and diluted with 7mL of deionized water. Then adding 10mg of polyvinylpyrrolidone (PVP), stirring uniformly, quickly injecting 2mL of sodium borohydride solution to ensure that the concentration of the PVP is 1mg/mL and the concentration of the sodium borohydride is 0.45mg/mL, and continuously stirring for 10min for later use;
and step 3: measuring 20mL of the nano-gold solution prepared in the step 2, slowly dripping the nano-gold solution into the solution in the step 1 at the speed of 1 drop per second, rapidly stirring the nano-gold solution for 10min at the stirring speed of 2600r/min, centrifugally washing the product for 3 times, and finally drying the product at the temperature of 60 ℃.
Example 5:
step 1: weigh 0.5g TiO2Dispersing the hydrochloric acid into deionized water, adding a certain amount of hydrochloric acid to enable the molar concentration of the hydrochloric acid to be 11.97mmol/L, and magnetically stirring the hydrochloric acid uniformly for later use;
step 2: 1mL of chloroauric acid solution with a concentration of 10mg/mL was measured and diluted with 7mL of deionized water. Then adding 10mg of polyvinylpyrrolidone (PVP), stirring uniformly, quickly injecting 2mL of sodium borohydride solution to ensure that the concentration of the PVP is 1mg/mL and the concentration of the sodium borohydride is 0.45mg/mL, and continuously stirring for 10min for later use;
and step 3: measuring 5mL of the nano-gold solution prepared in the step 2, slowly dripping the nano-gold solution into the solution in the step 1 at the speed of 1 drop per second, rapidly stirring the nano-gold solution for 10min at the stirring speed of 1500r/min, centrifugally washing the product for 3 times, and finally drying the product at the temperature of 60 ℃.
Example 6:
step 1: weigh 0.5g TiO2Dispersing the hydrochloric acid into deionized water, adding a certain amount of hydrochloric acid to enable the molar concentration of the hydrochloric acid to be 35.91mmol/L, and magnetically stirring the hydrochloric acid uniformly for later use;
step 2: 1mL of chloroauric acid solution with a concentration of 10mg/mL was measured and diluted with 7mL of deionized water. Then adding 10mg of polyvinylpyrrolidone (PVP), stirring uniformly, quickly injecting 2mL of sodium borohydride solution to ensure that the concentration of the PVP is 1mg/mL and the concentration of the sodium borohydride is 0.45mg/mL, and continuously stirring for 10min for later use;
and step 3: measuring 5mL of the nano-gold solution prepared in the step 2, slowly dripping the nano-gold solution into the solution in the step 1 at the speed of 2 drops per second, rapidly stirring the nano-gold solution for 10min at the stirring speed of 1500r/min, centrifugally washing the product for 3 times, and finally drying the product at the temperature of 60 ℃.
Example 7:
step 1: weigh 0.5g TiO2Dispersing the hydrochloric acid into deionized water, adding a certain amount of hydrochloric acid to enable the molar concentration of the hydrochloric acid to be 47.88mmol/L, and magnetically stirring the hydrochloric acid uniformly for later use;
step 2: 1mL of chloroauric acid solution with a concentration of 10mg/mL was measured and diluted with 7mL of deionized water. Then adding 10mg of polyvinylpyrrolidone (PVP), stirring uniformly, quickly injecting 2mL of sodium borohydride solution to ensure that the concentration of the PVP is 1mg/mL and the concentration of the sodium borohydride is 0.45mg/mL, and continuously stirring for 10min for later use;
and step 3: 5mL of the nano-gold solution prepared in the step 2 is measured, slowly and dropwise added into the solution in the step 1 at the speed of 1 drop per second, rapidly stirred for 10min at the stirring speed of 2600r/min, and the product is centrifugally washed for 3 times and finally dried at the temperature of 60 ℃.

Claims (6)

1. Rapid preparation of Au-TiO under acidic condition2A method of forming a composite structure, characterized by: the method comprises the following specific steps:
(1) weighing TiO2Dispersing the mixture in deionized water, adding hydrochloric acid, and magnetically stirring the mixture uniformly for later use;
(2) weighing chloroauric acid solution, adding deionized water for dilution, then adding polyvinylpyrrolidone, stirring uniformly, quickly injecting sodium borohydride solution, and continuously stirring for 8-15min to obtain nanogold solution for later use;
(3) and (3) measuring the nano gold solution in the step (2), slowly dripping the nano gold solution into the acidic solution prepared in the step (1), quickly stirring for 8-15min, centrifuging and washing the product for 2-4 times, and finally drying at 55-65 ℃.
2. The method of claim 1 for rapidly preparing Au-TiO under acidic conditions2A method of forming a composite structure, characterized by: in the step (1), the molar concentration of the hydrochloric acid is 11.97-47.88 mmol/L.
3. The method of claim 1 for rapidly preparing Au-TiO under acidic conditions2A method of forming a composite structure, characterized by: step (2)Wherein the concentration of the chloroauric acid solution is 10mg/mL, the concentration of the polyvinylpyrrolidone is 0.5-2mg/mL, and the concentration of the sodium borohydride is 0.22-0.56 mg/mL.
4. The method of claim 1 for rapidly preparing Au-TiO under acidic conditions2A method of forming a composite structure, characterized by: in the step (3), the volume ratio of the nano gold solution to the acidic solution prepared in the step (1) is 0.111-0.667.
5. The method of claim 1 for rapidly preparing Au-TiO under acidic conditions2A method of forming a composite structure, characterized by: in the step (3), the dripping speed of the nano gold solution is 1-2 drops/second.
6. The method of claim 1 for rapidly preparing Au-TiO under acidic conditions2A method of forming a composite structure, characterized by: in the step (3), the stirring speed is 1500-.
CN202010951606.9A 2020-09-11 2020-09-11 Rapid preparation of Au-TiO under acidic condition2Method of composite construction Pending CN112091232A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116004144A (en) * 2023-02-06 2023-04-25 昆明理工大学 Preparation method and application of composite conductive microspheres for anisotropic conductive adhesive

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JPH0616422A (en) * 1992-10-23 1994-01-25 Agency Of Ind Science & Technol Production of superfine gold particle immobilizing titanium oxide, oxidation catalyst, reduction catalyst, combustible gas sensor element and electrodic catalyst
KR20110000091A (en) * 2009-06-26 2011-01-03 강원대학교산학협력단 Gold/tio2 nanoparticle composite for in-vitro diagnostic testing and method for preparation thereof
CN102500287A (en) * 2011-09-28 2012-06-20 重庆大学 Graphene/modified titanium dioxide nano sol composite material and preparation method thereof
CN103601236A (en) * 2013-12-05 2014-02-26 天津工业大学 Preparation method of novel Au/Fe2O3-TiO2 nanotube catalyst
CN105214656A (en) * 2015-11-03 2016-01-06 福州大学 Gold nano cluster-golden nanometer particle-titanium dioxide composite photocatalyst and application
CN106984312A (en) * 2017-04-24 2017-07-28 福州大学 A kind of composite photocatalyst and preparation method thereof
CN107670664A (en) * 2017-10-31 2018-02-09 云南健牛生物科技有限公司 Titanic oxide composite photochemical catalyst system prepares and its application
CN110918095A (en) * 2019-11-12 2020-03-27 华南师范大学 Carbon/titanium dioxide/noble metal composite material, photocatalyst and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0616422A (en) * 1992-10-23 1994-01-25 Agency Of Ind Science & Technol Production of superfine gold particle immobilizing titanium oxide, oxidation catalyst, reduction catalyst, combustible gas sensor element and electrodic catalyst
KR20110000091A (en) * 2009-06-26 2011-01-03 강원대학교산학협력단 Gold/tio2 nanoparticle composite for in-vitro diagnostic testing and method for preparation thereof
CN102500287A (en) * 2011-09-28 2012-06-20 重庆大学 Graphene/modified titanium dioxide nano sol composite material and preparation method thereof
CN103601236A (en) * 2013-12-05 2014-02-26 天津工业大学 Preparation method of novel Au/Fe2O3-TiO2 nanotube catalyst
CN105214656A (en) * 2015-11-03 2016-01-06 福州大学 Gold nano cluster-golden nanometer particle-titanium dioxide composite photocatalyst and application
CN106984312A (en) * 2017-04-24 2017-07-28 福州大学 A kind of composite photocatalyst and preparation method thereof
CN107670664A (en) * 2017-10-31 2018-02-09 云南健牛生物科技有限公司 Titanic oxide composite photochemical catalyst system prepares and its application
CN110918095A (en) * 2019-11-12 2020-03-27 华南师范大学 Carbon/titanium dioxide/noble metal composite material, photocatalyst and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116004144A (en) * 2023-02-06 2023-04-25 昆明理工大学 Preparation method and application of composite conductive microspheres for anisotropic conductive adhesive
CN116004144B (en) * 2023-02-06 2024-09-10 昆明理工大学 Preparation method and application of composite conductive microspheres for anisotropic conductive adhesive

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Application publication date: 20201218