CN107520462A - A kind of preparation method of tetrahedral CuCl/Au alloys - Google Patents

A kind of preparation method of tetrahedral CuCl/Au alloys Download PDF

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Publication number
CN107520462A
CN107520462A CN201710645373.8A CN201710645373A CN107520462A CN 107520462 A CN107520462 A CN 107520462A CN 201710645373 A CN201710645373 A CN 201710645373A CN 107520462 A CN107520462 A CN 107520462A
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China
Prior art keywords
cucl
alloys
tetrahedral
aqueous solution
preparation
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CN201710645373.8A
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Chinese (zh)
Inventor
张春勇
陆芳
程洁红
赵德建
舒莉
文颖频
秦恒飞
刘维桥
周月
郑纯智
张国华
周全法
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Jiangsu University of Technology
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Jiangsu 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • 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

Abstract

The invention discloses a kind of preparation method of tetrahedral CuCl/Au alloys, comprise the following steps：The Vc aqueous solution is added into forerunner CuCl2In the aqueous solution, reaction, HAuCl is added4The aqueous solution, react, centrifugation, washing is dried to obtain tetrahedral CuCl/Au alloys.The present invention uses Vc reducing agents, without any dispersant, template and organic solvent；Technique is simple, and under normal temperature, normal pressure, short time standing can be completed to react, and gained tetrahedral CuCl/Au alloys pattern, dimensional homogeneity are preferable, reproducible.

Description

A kind of preparation method of tetrahedral CuCl/Au alloys
Technical field
The invention belongs to technical field of inorganic material, and in particular to be a kind of preparation of tetrahedral CuCl/Au alloys Method.
Background technology
Au based materials receive much concern always in the past few decades.Because it has unique structure, catalysis, electrical property Energy.But Au is noble metal, switch to study Au alloys, the Au and support type Au of specific structure at present, to reduce Au use Amount, improves its performance.At present, the more metal alloys of Au are generally under organic solvent, high temperature, with surfactant or organic polymer Its pattern and size are controlled for template, and preparation condition is harsh, not environmentally.Such as《German applied chemistry》Report with containing Au and Cu solution does presoma and adds lauryl mercaptan in diphenyl ether system, diamond formic acid, 1,2- ten six glycol, cetylamine synthesis The cubical technology of Au-Cu alloy nanos.Chinese patent (CN 104109907B) is reported with CuCl2、HAuCl4For raw material, Portugal Grape sugar is reducing agent, cetylamine (HDA) is that template reacts 30 minutes in 100 DEG C of oil bath and prepares pentalpha Au-Cu Alloy nanocrystals.Chinese patent (CN105689701A) is reported with certain density HAuCl4Added in ethylene glycol solution poly- Dimethyl diallyl ammonium chloride (PDDA) is used as nanoparticle stabilizer and pattern controlling agent, is reacted in 220 DEG C of oil bath pans Prepare golden tetrahedron within two hours.
The content of the invention
To solve the more metal alloys of Au existing for prior art generally under organic solvent, high temperature, with surfactant or Organic polymer is that template controls its pattern and size, preparation condition is harsh, not environmentally the defects of, the present invention provides one kind four The preparation method of face body shape CuCl/Au alloys.
A kind of preparation method of tetrahedral CuCl/Au alloys, comprises the following steps：The Vc aqueous solution is added into forerunner CuCl2In the aqueous solution, reaction, HAuCl is added4The aqueous solution, react, centrifugation, washing is dried to obtain tetrahedral CuCl/Au conjunctions Gold.
Further, the concentration of the Vc aqueous solution is 0.001~1mol/L, CuCl2The concentration of the aqueous solution be 0.001~ 1mol/L, HAuCl4The concentration of the aqueous solution is 0.001~1mol/L.
Further, Vc, CuCl2And HAuCl4Mol ratio be the ﹕ 0.01~10 of 0.01~10 ﹕ 0.01~10.
Further, react and carried out at 0~40 DEG C, carried out under static conditions.
Further, Vc solution is added into forerunner CuCl21~120min of reaction is stood after in the aqueous solution；Add HAuCl4Water 1~120min of reaction is stood after solution.
Further, the tetrahedral CuCl/Au alloys of gained can be impregnated into inorganic acid and/or organic acid and carry out corruption Erosion, obtains porous tetrahedral CuCl/Au alloys.Inorganic acid is phosphoric acid or hydrofluoric acid, and organic acid is acetic acid；Preferably, it is rotten Carried out when erosion under ultrasonic vibration.The specific surface area of porous tetrahedral CuCl/Au alloys is in 14~16m2/ g, hole Rate is 30%~60%, so that analogue enztme has the catalysis of similar oxide enzyme and similar peroxidase concurrently, it is active high, In immunoassay, biological detection and it can face as a kind of new and effective oxide enzyme simulation enzyme and Mimetic enzyme of peroxidase The acquirements such as bed diagnosis are widely applied prospect.
The present invention has positive effect：(1) it is environmental friendly：Using Vc reducing agents, without any dispersant, template and have Solvent.(2) technique is simple, and under normal temperature, normal pressure, short time standing can be completed to react.(3) tetrahedral CuCl/Au alloys Pattern, size uniformly, properly, will not be excessive or too small, and repetitive rate is high.
Brief description of the drawings
Fig. 1 is the SEM spectrum of tetrahedral CuCl/Au alloys prepared by the present invention；
Fig. 2 is the XRD diffracting spectrums of tetrahedral CuCl/Au alloys prepared by the present invention.
Embodiment
Embodiment 1
5mL 0.2mol/L Vc solution is taken to add 2mL 0.1mol/L in 20mL vials with pipettor first CuCl2Solution, after keeping 5min at 20 DEG C, add 2mL 0.01mol/L HAuCl4Solution, reaction 60min is stood at 20 DEG C.Instead Centrifuge is used after should terminating, removes clarified solution, then is washed with deionized water ultrasonic disperse, is centrifuged again afterwards, vacuum Gained black powder is tetrahedral CuCl/Au alloys after drying.
Embodiment 2
15mL 0.1mol/L Vc solution is taken to add 3mL 0.15mol/L in 50mL vials with pipettor first CuCl2Solution, after keeping 10min at 25 DEG C, add 1mL 0.03mol/L HAuCl4Solution, reaction 30min is stood at 25 DEG C. Reaction uses centrifuge after terminating, and removes clarified solution, then is washed with deionized water ultrasonic disperse, centrifuges again afterwards, very Gained black powder is tetrahedral CuCl/Au alloys after sky drying.
Embodiment 3
5mL 0.3mol/L Vc solution is taken to add 3mL 0.15mol/L in 20mL vials with pipettor first CuCl2Solution, after keeping 20min at 0 DEG C, add 2mL 0.03mol/L HAuCl4Solution, reaction 30min is stood at 30 DEG C.Instead Centrifuge is used after should terminating, removes clarified solution, then is washed with deionized water ultrasonic disperse, is centrifuged again afterwards, vacuum Gained black powder is tetrahedral CuCl/Au alloys after drying.Gained alloy is added into the hydrogen fluorine that mass fraction is 38% Acid solution, at room temperature ultrasonic 15min are then centrifuged for removing supernatant, washing, the operation of repeated centrifugation and washing to neutrality, Obtain porous tetrahedral CuCl/Au alloys.
Embodiment 4
20mL 0.25mol/L Vc solution is taken to add 15mL 0.4mol/ in 100mL vials with pipettor first L CuCl2Solution, after keeping 20min at 20 DEG C, add 10mL0.04mol/L HAuCl4Solution, reaction is stood at 30 DEG C 30min.Reaction uses centrifuge after terminating, and removes clarified solution, then washed with deionized water ultrasonic disperse, centrifuges again afterwards point From gained black powder is tetrahedral CuCl/Au alloys after vacuum drying.It is 36% that gained alloy is added into mass fraction Acetic acid solution, ultrasonic 20min at room temperature is then centrifuged for removing supernatant, washing, and the operation of repeated centrifugation and washing is into Property, obtain porous tetrahedral CuCl/Au alloys.
Embodiment 5
20mL 0.001mol/L Vc solution is taken to add 15mL in 100mL vials with pipettor first 0.001mol/L CuCl2Solution, after keeping 1min at 0 DEG C, add 10mL0.01mol/L HAuCl4Solution, stand at 0 DEG C anti- Answer 1min.Reaction uses centrifuge after terminating, and removes clarified solution, then is washed with deionized water ultrasonic disperse, centrifuges again afterwards Separate, gained black powder is tetrahedral CuCl/Au alloys after vacuum drying.
Embodiment 6
20mL 1mol/L Vc solution is taken to add 15mL 1mol/L in 100mL vials with pipettor first CuCl2Solution, after keeping 120min at 40 DEG C, add 10mL 1mol/L HAuCl4Solution, reaction 120min is stood at 40 DEG C. Reaction uses centrifuge after terminating, and removes clarified solution, then is washed with deionized water ultrasonic disperse, centrifuges again afterwards, very Gained black powder is tetrahedral CuCl/Au alloys after sky drying.

Claims (8)

1. a kind of preparation method of tetrahedral CuCl/Au alloys, it is characterised in that comprise the following steps：The Vc aqueous solution is added Enter forerunner CuCl2In the aqueous solution, reaction, HAuCl is added4The aqueous solution, react, centrifugation, washing is dried to obtain tetrahedral CuCl/Au alloys.
2. the preparation method of tetrahedral CuCl/Au alloys as claimed in claim 1, it is characterised in that the Vc aqueous solution it is dense Spend for 0.001~1mol/L, CuCl2The concentration of the aqueous solution is 0.001~1mol/L, HAuCl4The concentration of the aqueous solution be 0.001~ 1mol/L。
3. the preparation method of tetrahedral CuCl/Au alloys as claimed in claim 1, it is characterised in that Vc, CuCl2With HAuCl4Mol ratio be the ﹕ 0.01~10 of 0.01~10 ﹕ 0.01~10.
4. the preparation method of tetrahedral CuCl/Au alloys as claimed in claim 1, it is characterised in that reaction is at 0~40 DEG C Lower progress.
5. the preparation method of the tetrahedral CuCl/Au alloys as described in claim 1 or 4, it is characterised in that reaction is being stood Under the conditions of carry out.
6. the preparation method of tetrahedral CuCl/Au alloys as claimed in claim 1, it is characterised in that add Vc solution Forerunner CuCl21~120min of reaction is stood after in the aqueous solution.
7. the preparation method of the tetrahedral CuCl/Au alloys as described in claim 1 or 6, it is characterised in that add HAuCl4 1~120min of reaction is stood after the aqueous solution.
8. the preparation method of the tetrahedral CuCl/Au alloys as described in claim any one of 1-4, it is characterised in that by institute The tetrahedral CuCl/Au alloys obtained, which are impregnated into inorganic acid and/or organic acid, to be corroded, and obtains porous tetrahedral CuCl/Au alloys.
CN201710645373.8A 2017-08-01 2017-08-01 A kind of preparation method of tetrahedral CuCl/Au alloys Withdrawn CN107520462A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1861299A (en) * 2005-05-13 2006-11-15 中国科学院理化技术研究所 Method for preparing hollow ball shaped copper particles
CN103387258A (en) * 2013-08-07 2013-11-13 武汉理工大学 Cuprous oxide nano hollow spheres as well as synthetic method and application method thereof
CN105478794A (en) * 2015-12-11 2016-04-13 中国科学院深圳先进技术研究院 Platinum-copper alloy nano particle and preparation method thereof
CN105945298A (en) * 2016-04-25 2016-09-21 陕西师范大学 Preparation method for hollow palladium nanospheres

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1861299A (en) * 2005-05-13 2006-11-15 中国科学院理化技术研究所 Method for preparing hollow ball shaped copper particles
CN103387258A (en) * 2013-08-07 2013-11-13 武汉理工大学 Cuprous oxide nano hollow spheres as well as synthetic method and application method thereof
CN105478794A (en) * 2015-12-11 2016-04-13 中国科学院深圳先进技术研究院 Platinum-copper alloy nano particle and preparation method thereof
CN105945298A (en) * 2016-04-25 2016-09-21 陕西师范大学 Preparation method for hollow palladium nanospheres

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
EUN DUCK PARK ET AL.: "Characterization of Pd/C and Cu Catalysts for the Oxidation of Methane to a Methanol Derivative", 《JOURNAL OF CATALYSIS》 *
GRUSHEVSKAYA,SN ET AL.: "Kinetics of the initial step of anodic formation of CuCl on copper and copper-gold alloys with low gold contents", 《PROTECTION OF METALS》 *
吴伟主编: "《材料的晶体结构》", 31 January 2015, 中国铁道出版社 *
龚睿等: "绿色化学方法合成CuCl微晶", 《云南大学学报( 自然科学版)》 *

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Application publication date: 20171229