CN109440148A - A kind of preparation method and applications of palladium cobalt nanowire - Google Patents

A kind of preparation method and applications of palladium cobalt nanowire Download PDF

Info

Publication number
CN109440148A
CN109440148A CN201811266288.1A CN201811266288A CN109440148A CN 109440148 A CN109440148 A CN 109440148A CN 201811266288 A CN201811266288 A CN 201811266288A CN 109440148 A CN109440148 A CN 109440148A
Authority
CN
China
Prior art keywords
preparation
palladium cobalt
palladium
anodic oxidation
cobalt nanowire
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811266288.1A
Other languages
Chinese (zh)
Inventor
张跃进
曾庆生
李波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhongxiang Bo Qian Mdt Infotech Ltd
Original Assignee
Zhongxiang Bo Qian Mdt Infotech Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhongxiang Bo Qian Mdt Infotech Ltd filed Critical Zhongxiang Bo Qian Mdt Infotech Ltd
Priority to CN201811266288.1A priority Critical patent/CN109440148A/en
Publication of CN109440148A publication Critical patent/CN109440148A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0547Nanofibres or nanotubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/12Anodising more than once, e.g. in different baths
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/16Pretreatment, e.g. desmutting
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/567Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of platinum group metals
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/127Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles

Abstract

The invention discloses a kind of preparation method and applications of palladium cobalt nanowire, include the following steps: to prepare anodic oxidation aluminium formwork first;Configure palladium cobalt electrolyte: by PdCl2、CoSO4·7H2O and H3BO3·7H2O mixing, with salt acid for adjusting pH;By the palladium cobalt bath deposition on anodic oxidation aluminium formwork, the palladium cobalt nanowire has been obtained.By the way that cobalt is added in palladium in the present invention, so that the structurally ordered arrangement of palladium cobalt nanowire of preparation, and then sensitivity, response time and recovery time can be increased when applying in the sensor, and eliminate or reduce the palladium metal stability difference as caused by the conditions such as density of hydrogen, operating temperature defect, obtained high sensitivity, temperature applicable range extensively, integrability, low-power consumption and excellent in stability hydrogen gas sensor.

Description

A kind of preparation method and applications of palladium cobalt nanowire
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of preparation method of palladium cobalt nanowire and its answer With.
Background technique
Hydrogen plays important role in modern industry, and the reasonable employment of hydrogen can be the development of human society Very big power-assisted is provided.However, many unsafe conditions are often faced with during using hydrogen, especially in transport, storage Link, there are all multivariates, small carelessness to be likely to cause hydrogen leak for outdoor diversified environment, endangers huge.Cause This, the hydrogen detectability under unconventional situation is particularly significant.Monodimension nanometer material is because having special construction, in chemistry, object Reason etc. shows outstanding performance, becomes the area research hot spot.
Pd because of metal has good reactivity worth to hydrogen, is largely constantly reported about its correlative study as sensitive material Road.Pd can react in air with hydrogen, form Pd-H system.When contacting the metal surface Pd, H2It can be with Pd atomic surface Electron interaction so that H2Molecule is decomposed into H atom, and depends on Pd.H atom enters Pd metal grate and forms PdHx, At this time according to the difference of H/Pd content, there are two kinds of solid phases of α phase and β phase.When room temperature, as H/Pd < 0.008, it is α phase, works as H/ It is β phase when Pd > 0.067.With increasing for hydrogen atom content, the cell volume of Pd expands, and changes resistivity, causes material Resistance changes.By measuring resistance variation value, the content of Hydrogen in Air can be calculated.
Since the lattice parameter of two-phase has a certain distance, repeatedly two alternate circulations can cause the distortion of material broken It splits, ultimately causes permanent destruction, is i.e. " hydrogen embrittlement " phenomenon, reduce the stability of Pd sensor.In addition, the change of temperature can draw The opposite air-sensitive behavior of Pd metal is played, resistance variations mode is caused to change, becomes resistance reduction from hydrogen resistance increase is absorbed, seriously Influence sensor can temperature range of operation.Pure Pd is mixed usually using some disparate metals atoms, improves the upper of pure Pd material State disadvantage.
For these reasons, the present invention is specifically proposed.
Summary of the invention
In order to solve problem above of the existing technology, the present invention provides a kind of preparation method of palladium cobalt nanowire and It is applied, by the way that cobalt is added in palladium in the present invention, so that the structurally ordered arrangement of palladium cobalt nanowire of preparation, and then in sensor Sensitivity, response time and recovery time can be increased when middle application.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of palladium cobalt nanowire, includes the following steps:
(1) anodic oxidation aluminium formwork is prepared first;
(2) palladium cobalt electrolyte is configured: by PdCl2、CoSO4·7H2O and H3BO3·7H2O mixing, with salt acid for adjusting pH;
(3) the palladium cobalt bath deposition palladium cobalt nanowire has been obtained on anodic oxidation aluminium formwork.
Further, anodic oxidation aluminium formwork is prepared via a method which:
(a) aluminium flake is impregnated in acetone, is rinsed with water, air-dried;
(b) aluminium flake after air-drying makes annealing treatment under argon atmosphere;
(c) aluminium flake then handled with oxalic acid solution oxidizing annealing obtains the aluminium flake of first anode oxidation, is soaked with phosphorus chromic acid Striping is steeped, then carries out second of anodic oxidation with oxalic acid solution;
(d) by SnCl4It is added on the aluminium flake by second of anodic oxidation, is impregnated through water, dry, be then placed in phosphorus It is impregnated in acid solution, metal spraying processing obtains the anodic oxidation aluminium formwork.
Further, 8-12min is impregnated in step (a), it is preferred that impregnate 10min.
Further, annealing temperature is 500-600 DEG C in step (b), time 9-11h, it is preferred that annealing Temperature is 550 DEG C, time 10h.
Further, first time anodic oxidation is identical with the condition of second of anodic oxidation in step (c), oxalic acid solution Concentration is 0.2-0.4mol/L, oxidization time 7-9h.
Further, 25-35min is impregnated in step (d) in water, drying temperature is 60-80 DEG C, dries 10-14h.
Further, the concentration of step (d) phosphoric acid is 4-6%, and 40-60min is impregnated in phosphoric acid.
For the hole of the anodic oxidation aluminium formwork of method preparation of the invention in fine and close, parallelly distribute on, size is close, average hole Gap diameter is about 30nm, has apparent regular hexagon shape, is conducive to a large amount of production hydrogen gas sensor sensitive materials.
Further, PdCl in step (1)2Concentration be 0.008-0.012mol/L, CoSO4·7H2The concentration of O is 0.013-0.017mol/L and H3BO3·7H2The concentration of O is 0.013-0.017mol/L.
Further, pH value is adjusted in step (1) to 2-3.
Application of the palladium cobalt nanowire of preparation method preparation described in a kind of in hydrogen gas sensor.
Palladium cobalt nanowire prepared by the present invention needs to be handled as follows before being prepared into sensor: by what is be prepared Palladium cobalt nanowire, which is dissolved in the sodium hydroxide solution of 4mol/L, removes anodic oxidation aluminium formwork, is repeatedly rinsed using deionized water Sample and drying, finally in ethanol by palladium cobalt nanowire obtained dissolution, ultrasonic vibration, realization is evenly dispersed, obtains palladium cobalt Nano wire/ethanol liquid, it can prepare sensor.
Sensor the preparation method is as follows: palladium cobalt nanowire/ethanol liquid of preparation is added drop-wise in interdigital electrode, divulge information Drying, secondly, interdigital electrode is fixed in sensor base using conductive silver glue.Finally, by welding wire machine pressure welding aluminium wire with Interdigital electrode both ends and pedestal pin are connected, hydrogen gas sensor is obtained.
Compared with prior art, the invention has the benefit that
By the way that cobalt is added in palladium in the present invention, so that the structurally ordered arrangement of palladium cobalt nanowire of preparation, and then sensing Sensitivity, response time and recovery time can be increased when applying in device, and eliminate or reduce by density of hydrogen, operating temperature etc. The defect of palladium metal stability difference caused by condition, has obtained that high sensitivity, temperature applicable range be wide, integrability, low-power consumption With the hydrogen gas sensor of excellent in stability.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with It obtains other drawings based on these drawings.
Fig. 1 is the Electronic Speculum surface sweeping figure of anodic oxidation aluminium formwork of the invention;
Fig. 2 is the Electronic Speculum surface sweeping figure of anodic oxidation aluminium formwork of the invention;
Fig. 3 is the SEM figure of palladium cobalt nanowire of the invention;
Fig. 4 is the XRD diagram of palladium cobalt nanowire of the invention;
Fig. 5 is palladium cobalt sensor sensitivity curve under different hydrogen concentration under room temperature of the invention;
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work Other embodiment belongs to the range that the present invention is protected.
Embodiment 1
The preparation method of the palladium cobalt nanowire of the present embodiment, includes the following steps:
(1) anodic oxidation aluminium formwork is prepared first;
(2) palladium cobalt electrolyte is configured: the PdCl for being 0.008mol/L by concentration2, concentration be 0.013mol/L CoSO4· 7H2The H that O and concentration are 0.013mol/L3BO3·7H2O mixing, with salt acid for adjusting pH to 2;
It (3) is to electrode with graphite plate, at room temperature, adjusting constant voltage is 1.5-2.0V, by the palladium Cobalt bath deposition has obtained the palladium cobalt nanowire in the nanoaperture on anodic oxidation aluminium formwork.
The anodic oxidation aluminium formwork of the present embodiment the preparation method is as follows:
(a) aluminium flake is impregnated into 8min in acetone, is rinsed with deionized water, air-dried;
(b) aluminium flake after air-drying makes annealing treatment under argon atmosphere, and temperature asks 500 DEG C, and constant temperature time is that 9h anneals to go Except inside aluminium flake stress and other defects, improve the crystallinity of aluminium;
(c) then at 5 DEG C, the aluminium flake handled with the oxalic acid solution oxidizing annealing of 0.2mol/L aoxidizes 7h, voltage setting For 50V, the aluminium flake of first anode oxidation is obtained, impregnates striping 2h with phosphorus chromic acid, taking-up washes and dries, and then uses oxalic acid solution It is identical as first time anodic oxidation condition to carry out second of anodic oxidation;
(d) by SnCl4It is added on the aluminium flake by second of anodic oxidation, impregnates 25min through water, be 60 DEG C in temperature Lower drying 10h is then placed in 50 DEG C, impregnates 40min in the phosphoric acid solution that concentration is 4% and carry out through-hole processing, use plasma Body sputter carries out metal spraying processing, obtains the anodic oxidation aluminium formwork.
Embodiment 2
The preparation method of the palladium cobalt nanowire of the present embodiment, includes the following steps:
(1) anodic oxidation aluminium formwork is prepared first;
(2) palladium cobalt electrolyte is configured: the PdCl for being 0.01mol/L by concentration2, concentration be 0.015mol/L CoSO4· 7H2The H that O and concentration are 0.015mol/L3BO3·7H2O mixing, with salt acid for adjusting pH to 2.5;
It (3) is to electrode with graphite plate, at room temperature, adjusting constant voltage is 1.5-2.0V, by the palladium Cobalt bath deposition has obtained the palladium cobalt nanowire in the nanoaperture on anodic oxidation aluminium formwork.
The anodic oxidation aluminium formwork of the present embodiment the preparation method is as follows:
(a) aluminium flake is impregnated into 10min in acetone, is rinsed with deionized water, air-dried;
(b) aluminium flake after air-drying makes annealing treatment under argon atmosphere, and temperature asks 550 DEG C, and constant temperature time is that 10h anneals to go Except inside aluminium flake stress and other defects, improve the crystallinity of aluminium;
(c) then at 5 DEG C, the aluminium flake handled with the oxalic acid solution oxidizing annealing of 0.3mol/L aoxidizes 8h, voltage setting For 50V, the aluminium flake of first anode oxidation is obtained, impregnates striping 2h with phosphorus chromic acid, taking-up washes and dries, and then uses oxalic acid solution It is identical as first time anodic oxidation condition to carry out second of anodic oxidation;
(d) by SnCl4It is added on the aluminium flake by second of anodic oxidation, impregnates 30min through water, be 70 DEG C in temperature Lower drying 12h is then placed in 50 DEG C, impregnates 50min in the phosphoric acid solution that concentration is 5% and carry out through-hole processing, use plasma Body sputter carries out metal spraying processing, obtains the anodic oxidation aluminium formwork.
Anodic oxidation aluminium formwork surface sweeping electron microscope manufactured in the present embodiment is as illustrated in fig. 1 and 2, as shown in Figure 1, anodic oxidation The hole of aluminum alloy pattern plate is in fine and close, parallelly distribute on, and size is close, and average pore diameter is about 30nm, has obvious positive six side Shape shape.It can be seen that, the hole in template keeps orderly repeating substantially, and the depth of each hole can be more than 50 μm, put down in Fig. 2 Equal pore diameter is about 70nm, can satisfy the requirement for preparing hydrogen gas sensor sensitive material.Meanwhile hole is intensive enough, one It is secondary to prepare both available a large amount of nano-materials, conducive to the large-scale production of material.
Palladium cobalt nanowire SEM figure manufactured in the present embodiment is as shown in figure 3, it can be seen from the figure that nanowire diameter is about 70nm, Co are metal-doped among Pd, nano thread ordered arrangement.
XRD analysis is carried out to palladium cobalt nanowire manufactured in the present embodiment, as shown in figure 4, from the figure, it can be seen that with pure Pd It compares, 2 θ values of Pd/Co alloy are smaller, show that the lattice constant of alloy is greater than pure Pd.
Embodiment 3
The preparation method of the palladium cobalt nanowire of the present embodiment, includes the following steps:
(1) anodic oxidation aluminium formwork is prepared first;
(2) palladium cobalt electrolyte is configured: the PdCl for being 0.012mol/L by concentration2, concentration be 0.017mol/L CoSO4· 7H2The H that O and concentration are 0.017mol/L3BO3·7H2O mixing, with salt acid for adjusting pH to 3;
It (3) is to electrode with graphite plate, at room temperature, adjusting constant voltage is 1.5-2.0V, by the palladium Cobalt bath deposition has obtained the palladium cobalt nanowire in the nanoaperture on anodic oxidation aluminium formwork.
The anodic oxidation aluminium formwork of the present embodiment the preparation method is as follows:
(a) aluminium flake is impregnated into 12min in acetone, is rinsed with deionized water, air-dried;
(b) aluminium flake after air-drying makes annealing treatment under argon atmosphere, and temperature asks 600 DEG C, and constant temperature time is that 11h anneals to go Except inside aluminium flake stress and other defects, improve the crystallinity of aluminium;
(c) then at 5 DEG C, the aluminium flake handled with the oxalic acid solution oxidizing annealing of 0.4mol/L aoxidizes 9h, voltage setting For 50V, the aluminium flake of first anode oxidation is obtained, impregnates striping 2h with phosphorus chromic acid, taking-up washes and dries, and then uses oxalic acid solution It is identical as first time anodic oxidation condition to carry out second of anodic oxidation;
(d) by SnCl4It is added on the aluminium flake by second of anodic oxidation, impregnates 35min through water, be 80 DEG C in temperature Lower drying 14h is then placed in 50 DEG C, impregnates 60min in the phosphoric acid solution that concentration is 6% and carry out through-hole processing, use plasma Body sputter carries out metal spraying processing, obtains the anodic oxidation aluminium formwork.
Test example 1
Palladium cobalt nanowire prepared by embodiment 2 is prepared into hydrogen gas sensor, needs to carry out such as before being prepared into sensor Lower processing: the palladium cobalt nanowire being prepared being dissolved in the sodium hydroxide solution of 4mol/L and removes anodic oxidation aluminium formwork, Sample and drying are repeatedly rinsed using deionized water, finally in ethanol by palladium cobalt nanowire obtained dissolution, ultrasonic vibration is real It is existing evenly dispersed, obtain palladium cobalt nanowire/ethanol liquid, it can prepare sensor.
Sensor the preparation method is as follows: palladium cobalt nanowire/ethanol liquid of preparation is added drop-wise in interdigital electrode, divulge information Drying, secondly, interdigital electrode is fixed in sensor base using conductive silver glue.Finally, by welding wire machine pressure welding aluminium wire with Interdigital electrode both ends and pedestal pin are connected, hydrogen gas sensor is obtained.
The detection and analysis of sensitivity are carried out to the hydrogen gas sensor of preparation, as shown in Figure 5, it is specified that transducer sensitivity is electricity Resistive is than reference resistor value (△ R/R0), before measurement sensor performance, it is first passed through enough nitrogen into cavity, makes cavity Inside emptying other impurities gas.And 310K at a temperature of, be passed through the hydrogen of 12sccm, it is more steady to sensor signal Afterwards, hydrogen is closed, waits resistance to restore, repeatedly above-mentioned steps, so that the resistance sizes of material tend in nitrogen environment Steadily, i.e., baseline tends to be steady, and Cong Tuzhong 5 can be seen that under normal temperature condition, as density of hydrogen reduces, transducer sensitivity Also it is constantly reducing, is showing preferable linear.And after inverted sequence is passed through the hydrogen of various concentration, the resistance variations of sensor With approximately reach same level before, sensor sheet reveals preferable repeatability.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.

Claims (10)

1. a kind of preparation method of palladium cobalt nanowire, which comprises the steps of:
(1) anodic oxidation aluminium formwork is prepared first;
(2) palladium cobalt electrolyte is configured: by PdCl2、CoSO4·7H2O and H3BO3·7H2O mixing, with salt acid for adjusting pH;
(3) the palladium cobalt bath deposition palladium cobalt nanowire has been obtained on anodic oxidation aluminium formwork.
2. the preparation method of palladium cobalt nanowire according to claim 1, which is characterized in that anodic oxidation aluminium formwork is by such as Lower section method is prepared:
(a) aluminium flake is impregnated in acetone, is rinsed with water, air-dried;
(b) aluminium flake after air-drying makes annealing treatment under argon atmosphere;
(c) aluminium flake then handled with oxalic acid solution oxidizing annealing obtains the aluminium flake of first anode oxidation, is gone with the immersion of phosphorus chromic acid Then film carries out second of anodic oxidation with oxalic acid solution;
(d) by SnCl4It is added on the aluminium flake by second of anodic oxidation, is impregnated through water, dry, it is molten to be then placed in phosphoric acid It is impregnated in liquid, metal spraying processing obtains the anodic oxidation aluminium formwork.
3. the preparation method of palladium cobalt nanowire according to claim 2, which is characterized in that impregnate 8- in step (a) 12min, it is preferred that impregnate 10min.
4. the preparation method of palladium cobalt nanowire according to claim 2, which is characterized in that annealing temperature in step (b) Degree is 500-600 DEG C, time 9-11h, it is preferred that annealing temperature is 550 DEG C, time 10h.
5. the preparation method of palladium cobalt nanowire according to claim 2, which is characterized in that first time anode in step (c) Oxidation is identical with the condition of second of anodic oxidation, and the concentration of oxalic acid solution is 0.2-0.4mol/L, oxidization time 7-9h.
6. the preparation method of palladium cobalt nanowire according to claim 2, which is characterized in that impregnated in water in step (d) 25-35min, drying temperature are 60-80 DEG C, dry 10-14h.
7. the preparation method of palladium cobalt nanowire according to claim 2, which is characterized in that the concentration of step (d) phosphoric acid is 4-6% impregnates 40-60min in phosphoric acid.
8. the preparation method of palladium cobalt nanowire according to claim 1, which is characterized in that PdCl in step (1)2Concentration For 0.008-0.012mol/L, CoSO4·7H2The concentration of O is 0.013-0.017mol/L and H3BO3·7H2The concentration of O is 0.013-0.017mol/L。
9. the preparation method of palladium cobalt nanowire according to claim 1, which is characterized in that adjust in step (1) pH value to 2-3。
10. a kind of palladium cobalt nanowire of preparation method preparation described in any one of claim 1-9 is in hydrogen gas sensor Using.
CN201811266288.1A 2018-10-29 2018-10-29 A kind of preparation method and applications of palladium cobalt nanowire Pending CN109440148A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811266288.1A CN109440148A (en) 2018-10-29 2018-10-29 A kind of preparation method and applications of palladium cobalt nanowire

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811266288.1A CN109440148A (en) 2018-10-29 2018-10-29 A kind of preparation method and applications of palladium cobalt nanowire

Publications (1)

Publication Number Publication Date
CN109440148A true CN109440148A (en) 2019-03-08

Family

ID=65549127

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811266288.1A Pending CN109440148A (en) 2018-10-29 2018-10-29 A kind of preparation method and applications of palladium cobalt nanowire

Country Status (1)

Country Link
CN (1) CN109440148A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05137979A (en) * 1991-11-25 1993-06-01 Mitsubishi Kakoki Kaisha Ltd Production of hydrogen separating membrane
KR20050108646A (en) * 2004-05-12 2005-11-17 한국과학기술연구원 High density nanwire hydrogen gas sensor and its fabrication method
CN1911782A (en) * 2006-07-21 2007-02-14 东莞理工学院 Preparation method of palladium nanometer wire oldered array material
US20090013824A1 (en) * 2007-07-09 2009-01-15 Bong Soo Kim Binary alloy single-crystalline metal nanostructures and fabrication method thereof
CN102495045A (en) * 2011-11-07 2012-06-13 华中科技大学 Hydrogen sensitive material for optical fiber hydrogen sensor and preparation method of hydrogen sensitive material
CN106770598A (en) * 2016-12-08 2017-05-31 东莞理工学院 Pd nano wire modified electrodes and its production and use

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05137979A (en) * 1991-11-25 1993-06-01 Mitsubishi Kakoki Kaisha Ltd Production of hydrogen separating membrane
KR20050108646A (en) * 2004-05-12 2005-11-17 한국과학기술연구원 High density nanwire hydrogen gas sensor and its fabrication method
CN1911782A (en) * 2006-07-21 2007-02-14 东莞理工学院 Preparation method of palladium nanometer wire oldered array material
US20090013824A1 (en) * 2007-07-09 2009-01-15 Bong Soo Kim Binary alloy single-crystalline metal nanostructures and fabrication method thereof
CN102495045A (en) * 2011-11-07 2012-06-13 华中科技大学 Hydrogen sensitive material for optical fiber hydrogen sensor and preparation method of hydrogen sensitive material
CN106770598A (en) * 2016-12-08 2017-05-31 东莞理工学院 Pd nano wire modified electrodes and its production and use

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
B. CHADWICK等: "A hydrogen sensor based on the optical generation of surface plasmons in a palladium alloy", 《SENSORS AND ACTUATORS B》 *
PO-CHUN CHANG等: "Hydrogenation-induced reversible spin reorientation transition in Co50Pd50 alloy thin films", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
VENKATA RAMANA MUDINEPALLI等: "Hydrogenation effect on uniaxial magnetic anisotropy of a CoxPd1-x alloy microstructure", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
W. JUSZCZYK等: "The Structure and Activity of Silica-Supported Palladium-Cobalt Alloys", 《JOURNAL OF CATALYSIS》 *
WEN-CHIN LIN等: "Hydrogen absorption-induced reversible change in magnetic properties of Co-Pd alloy films", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
刘漫红等: "《纳米材料及其制备技术》", 31 August 2014, 冶金工业出版社 *
周淑娟等: "泡沫镍负载Pd-Co作为H2O2电还原反应阴极研究", 《内蒙古民族大学学报》 *

Similar Documents

Publication Publication Date Title
Casillas et al. Pitting corrosion of titanium
Zhang et al. Supported Noble Metals on Hydrogen‐Treated TiO2 Nanotube Arrays as Highly Ordered Electrodes for Fuel Cells
Olu et al. Insights into the potential dependence of the borohydride electrooxidation reaction mechanism on platinum nanoparticles supported on ordered carbon nanomaterials
Lasia Modeling of impedance of porous electrodes
CN113325053B (en) Cadmium ion electrochemical sensor working electrode and preparation method, detection method and application thereof
CN104911667B (en) A kind of preparation method of the novel MULTILAYER COMPOSITE noble metal nano hole array SERS substrates with honeycomb array structure
Alvarez et al. Formation of Cu/Pd bimetallic crystals by electrochemical deposition
Nugraha et al. Block‐Copolymer‐Assisted Electrochemical Synthesis of Mesoporous Gold Electrodes: Towards a Non‐Enzymatic Glucose Sensor
Rahman et al. Electrochemical dopamine sensors based on graphene
Xiang et al. Gold nanoparticles/electrochemically expanded graphite composite: A bifunctional platform toward glucose sensing and SERS applications
US7820587B2 (en) Porous anodic aluminum oxide membranes for nanofabrication
Ren et al. Grain boundaries dependent hydrogen sensitivity in MAO-TiO2 thin films sensors
Shcherbakov et al. Impedance of an Aluminum Electrode with a Nanoporous Oxide
CN109440148A (en) A kind of preparation method and applications of palladium cobalt nanowire
Benea et al. Electrochemically obtained Al2O3 nanoporous layers with increased anticorrosive properties of aluminum alloy
Albani et al. Comparative study of the passivity and the breakdown of passivity of polycrystalline iron in different alkaline solutions
Fan et al. Scanning tunneling microscopic studies of platinum electrode surfaces
Guo et al. Good sensitivity and high stability of humidity sensor using micro-arc oxidation alumina film
GB2614811A (en) Aluminum-based porous alumina film humidity-sensitive sensor and manufacturing method thereof
US20080112881A1 (en) Systems and methods for hydrogen loading and generation of thermal response
Krivenko et al. Electrochemical modification of electrodes based on highly oriented carbon nanowalls
Yang et al. A new method for the preparation of highly dispersed metal/carbon catalyst—Pd/C catalyst and its properties
Miao et al. Graphene/nano-ZnO hybrid materials modify Ni-foam for high-performance electrochemical glucose sensors
Chen et al. A novel capacitive low-humidity sensor based on a double-sided structure
Zhao et al. Determination of heavy metals in water using an FTO electrode modified with CeO 2/rGO nanoribbons prepared by an electrochemical method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190308