CN105689725A - Method for preparing metal palladium or palladium alloy nanowires - Google Patents

Method for preparing metal palladium or palladium alloy nanowires Download PDF

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CN105689725A
CN105689725A CN201610080443.5A CN201610080443A CN105689725A CN 105689725 A CN105689725 A CN 105689725A CN 201610080443 A CN201610080443 A CN 201610080443A CN 105689725 A CN105689725 A CN 105689725A
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palladium
hydrogen
alloy
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metal
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CN105689725B (en
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陈伟
金晶
***
汪伟
杨柯
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Institute of Metal Research of CAS
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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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/023—Hydrogen absorption
    • 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

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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract

The invention discloses a method for preparing metal palladium or palladium alloy nanowires. According to the method, palladium or palladium alloy is used as a raw material; and the raw material is subjected to hydrogen absorption and desorption circulation for multiple times, so that the palladium or palladium alloy material spontaneously grows in the circulation process to form a one-dimensional nanowire structure. The method for preparing the metal palladium or palladium alloy nanowires has the characteristics that operation is easy, large-scale preparation is easy, and products are easy to clean, and the demands for applying the palladium and the palladium alloy to catalysts and gas detection components can be met.

Description

A kind of Metal Palladium or palladium alloy nanowires preparation method
Technical field
The present invention relates to a kind of metal material nanowire preparation method, a kind of preparation method for Metal Palladium or palladium alloy nanowires is provided especially。
Background technology
Metal monodimension nanometer material is widely applied prospect in fields such as optics, electronics, chemical industry, and disclosed monodimension nanometer material preparation method mainly has the methods such as vapor phase growth, solution growth, template and self-assembled growth at present。The present invention is directed to circulate in a large number and inhale metal and the alloy putting hydrogen, it is provided that a kind of simple nanowire preparation method。
Palladium and palldium alloy are excellent catalyst materials, are widely used in petro chemical industry, such as the catalytic reforming of petroleum refining process, hydrogenation reaction, dehydrogenation reaction and purifying vehicle exhaust etc.。The research of catalyst is shown, catalyst carrier selects and catalytic active component is the principal element affecting its catalytic performance in the dispersity of carrier。Therefore palladium and palladium alloy catalysts are prepared into monodimension nanometer material and are expected to become new catalytic material, simultaneously it is reported that, palladium nanometer wire can as the key job medium of hydrogen detector。Therefore prepare palladium and alloy nano-wire has important using value。
The palladium nanometer wire preparation method of open report is mainly template at present。Patent application " preparation method of a kind of palladium nanometer wire oldered array material " (CN100564244C) adopts torpescence metal to be polymerization face, first prepare nano-alumina template with Two-step anodization, it is assemblied in surface of metal titanium, then prepares palladium nanometer wire with DC electrodeposition。Patent application " preparation method of the metal nanometer line that size is controlled " (CN101559492A) uses two-step electrochemical anodizing method to prepare alumina formwork, adopt the gold-plated closure nanohole alumine template of magnetron sputtering subsequently, and metal chloride is instilled template immersion, finally erode alumina formwork with strong base solution and prepare metal nanometer line。Patent application " preparation method of the Metal Palladium nano wire that a kind of size is controlled " (CN103252501A) adopts palladium chloride solution hydrolysis preparation nano palladium oxide particle solution, above-mentioned solution is instilled azelon cultivation and dries up prepared Palladium monoxide nano wire, finally adopt borine dimethyl amine reduction-oxidation palladium to prepare one-dimensional metal palladium nanometer wire。
Summary of the invention
The present invention provides a kind of palladium or palladium alloy nanowires preparation method, the method adopts palladium or palldium alloy for reaction raw material, utilize palladium and the character of alloy reversible hydrogen adsorption and desorption thereof, carry out raw material repeatedly inhaling putting hydrogen circular response, putting in hydrogen cyclic process in suction, palladium and alloy material autonomous growth thereof become monodimension nanometer material (nano wire)。The method adopts raw material simple, is not affected by template and other chemical drugss, can processability is stable in high volume palladium and palladium alloy nanowires。
The preparation method that the present invention specifically provides a kind of palladium and alloy nano-wire thereof, it is characterised in that: being undertaken Metal Palladium or palldium alloy inhaling the circulation of hydrogen-put hydrogen, with inhaling the carrying out putting hydrogen cyclic process, there is nanowire growth in palladium and alloy thereof, obtain nanowire product。
Palladium provided by the invention and alloy nano-wire preparation method thereof, it is characterized in that: palladium and alloy raw material thereof can directly be applied, or it is coated on carrier material (described carrier material is porous ceramic film material or metal material, and porous material is preferably kieselguhr, molecular sieve or activated carbon) through methods such as palladium salt solution impregnating reduction method, plating, chemical plating, magnetron sputterings。
Palladium provided by the invention and alloy nano-wire preparation method thereof, it is characterized in that: by appropriate heat treatment technique, raw material is prepared into the Granular composite material of palladium or palldium alloy, heat treatment condition is: heat treatment temperature is higher than the recrystallization temperature of palladium or palldium alloy, actual temp ranges for 600-1100 DEG C, heat treatment time scope 0.5h-12h, it is preferable that heat treating regime processes 0.5-1h at being 900-1000 DEG C；Heat treatment can carry out in air atmosphere, inert gas shielding or hydrogen atmosphere。
Palladium provided by the invention and alloy nano-wire preparation method thereof, it is characterised in that: must there is to inhale for more than 100 times hydrogen-put hydrogen circulation with hydrogen in described palladium and alloy raw material thereof, hydrogen can be hydrogen or its isotope deuterium, tritium。
Palladium provided by the invention and alloy nano-wire preparation method thereof, it is characterised in that: the circulation of described suction hydrogen-put hydrogen can be accomplished by:
Constant temperature inhale put hydrogen, namely sample at a constant temperature by improve Hydrogen Vapor Pressure inhale hydrogen, by evacuation dehydrogenation；Concrete grammar can refer to patent " hydrogen bearing alloy performance comprehensive testing device ", the patent No.: ZL200420108336.1；
Thermic is inhaled and is put hydrogen, is placed on appropriate containers by the saturated suction hydrogen of sample and carries out intensification dehydrogenation, cooling suction hydrogen。Concrete grammar and device thereof can refer to patent: " a kind of metal hydride thermal adsorption and desorption hydrogen cycling comprehensive test equipment ", the patent No.: ZL200910011065.5。
Adopt the method for the invention to prepare palladium or palladium alloy nanowires has the features such as simple to operate, prepared by the scale of being prone to, product cleaning, it is possible to meet palladium and alloy thereof the application demand for catalyst, detection of gas parts。
Accompanying drawing explanation
Fig. 1: the one-dimensional palladium nanometer wire product SEM figure of embodiment 1 preparation；
Fig. 2: the palladium of embodiment 2 preparation-diatomaceous earth sample SEM figure；
Fig. 3: embodiment 2 palladium-diatomaceous earth sample SEM figure after heat treatment；
Fig. 4: the one-dimensional palladium nanometer wire product SEM figure of embodiment 2 preparation
Fig. 5: the one-dimensional palladium-silver nanowire product SEM figure of embodiment 3 preparation。
Detailed description of the invention
Describe in detail by the following examples, but the present invention is not limited to following example。
Embodiment 1
Raw material is pure palladium powder (99.99% purity), and it is that hydrogen is put in constant temperature suction that hydrogen mode is put in suction, and detailed process is as follows:
1) weigh palladium powder 1g, sample is loaded sample room；Sample room is placed in thermostatic equipment, and temperature is set to 40 DEG C；Open vacuum pump to sample room evacuation 30 minutes；
2) hydrogen inhaled by sample: closes vacuum pump, sample room passes into high-purity hydrogen (99.999%) until pressure rises to 100kPa, keeps pressure 5 minutes, make the saturated suction hydrogen of palladium powder。
3) sample puts hydrogen: open vacuum pump, to sample room evacuation, makes gas pressure in sample room be down to below 0.1Pa and continue more than 10 minutes, and palladium powder sample puts hydrogen。
4) repeat above 2), 3) after accumulative 2000 times of step, taken out by sample room after sample is put hydrogen, observe palladium nanometer wire by scanning electron microscope (SEM) and generate situation, one-dimensional palladium nanometer wire product is had to occur as it is shown in figure 1, pure palladium powder experiences after hydrogen circulation is put in 2000 constant temperature suctions。
Embodiment 2
Employing Palladous chloride. is raw material, and kieselguhr (graininess) is carrier, prepares palladium-diatomite composite material by solution impregnating reduction method, puts hydrogen mode by thermic circulation suction and prepares palladium nanometer wire:
1) preparation PdCl2Solution: precise PdCl2It is placed in beaker, drips dilute hydrochloric acid solution after adding distilled water and be stirred continuously, until PdCl2It is completely dissolved, is configured to the solution of palladium mass concentration 0.1g/mL。
2) solution impregnation: by saturated for kieselguhr dipping PdCl2Solution, and in drying baker 60 DEG C air-dry。3) sample reduction: the material after air-dry is placed in tube type vacuum stove, heats in argon gas atmosphere to 550 DEG C, evacuation cooling after Wen Houtong hydrogen (200mL/min) reductase 12 h。Repeating above dipping reduction process until obtaining the palladium-diatomite composite material sample (the present embodiment palladium content is 40%) of required palladium content, sample topography is as shown in Figure 2。
4) palladium-diatomite composite material heat treatment: palladium-diatomite composite material is placed in vacuum drying oven, 900 DEG C of heat treatments 1 hour, lowers the temperature with stove, and gained sample topography is as shown in Figure 3。
5) palladium-diatomite composite material thermic is inhaled and is put hydrogen circulation: the sample after 1g heat treatment loads thermic suction and puts hydrogen recycle unit, to sample evacuation, gas it is flushed with hydrogen to inhaling hydrogen saturated (Hydrogen Vapor Pressure is about 50kPa) under room temperature, later on heating cool cycles, make sample inhale at 50 DEG C/200 DEG C temperature range generation thermics and put hydrogen circulation, continue 1000 times。
Carrying out electron scanning electron microscopic observation by experiencing the sample after hydrogen circulation is put in 1000 thermic suctions, as shown in Figure 4, palladium-diatomite composite material sample generates the one-dimensional palladium nanometer wire of a large amount of diameter 100 ran to result。
Embodiment 3
1) magnetron sputtering prepares palladium-silver sample, prepares one-dimensional palladium-silver nano wire by constant temperature circulating: magnetron sputtering prepares palladium-silver (Pd75Ag25) sample: adopt fine silver (99.99%), pure palladium (99.99%) as target, carry out double; two target magnetic control sputtering using alumina ceramic plate as matrix, prepare Pd by controlling dual-target sputtering parameter75Ag25Alloy film。
2) alloy sample heat treatment: by surface sputtering Pd75Ag25The alumina ceramic plate of alloy film is loaded into vacuum heat treatment furnace, and after evacuation, applying argon gas is protected, and is warming up to 1000 DEG C of insulations, heat treatment 1 hour, lowers the temperature with stove, complete sample heat treatment。
3) hydrogen inhaled by sample: the sample after heat treatment is loaded suction and puts hydrogen storage equipment sample room, sample room is heated constant temperature after 80 DEG C。Open vacuum pump, to sample evacuation 1 hour；Close vacuum pump, sample room is passed into high-purity hydrogen (99.999%) until pressure rises to 100kPa, keep pressure 5 minutes, make the saturated suction hydrogen of palladium-silver。
4) sample puts hydrogen: open vacuum pump, to sample room evacuation, makes gas pressure in sample room be down to below 0.1Pa and continue more than 10 minutes, and palladium-silver sample puts hydrogen。
5) inhale hydrogen more than repeating, put hydrogen step, after accumulative 1000 times, taken out by sample room after sample is put hydrogen, observe palladium-silver nano wire by scanning electron microscope (SEM) and generate situation, as shown in Figure 5, alloy sample experiences after hydrogen circulation is put in 1000 constant temperature suctions has one-dimensional palladium-silver nanowire product to occur。
Embodiment 4
Being raw material by Palladous nitrate. ammonium salt solution and silver nitrate solution, activated carbon is carrier, by material solution alternating impregnating carrier and reduce, after heat treatment prepares Pd90Ag10Sample, puts hydrogen circulation by constant temperature suction and prepares one-dimensional palladium-silver nano wire。
1) preparation Palladous nitrate. ammonium and silver nitrate solution:
Precise palladium sponge is placed in beaker, is placed in by beaker in magnetic force heating and stirring device, instills concentrated nitric acid the stirring that slowly heats up, and stops heating when there being dense Brown gas to produce, and continues stirring and is completely dissolved to palladium, is cooled to room temperature。With ammonia, gained palladium nitrate solution is carried out titration, there is white mist to produce and release heat during initial instillation ammonia, brown precipitate occurs when ammonia is abundant, continue dropping ammonia to obtaining settled solution, now solution ph is about 3～4, and whole titration process to keep being sufficiently stirred for。Finally give the Palladous nitrate. ammonium salt solution of palladium mass concentration 0.1g/mL。
Precise silver nitrate is positioned in beaker, adds deionized water and is stirred continuously and makes silver nitrate dissolve, and is finally configured to the silver nitrate solution of silver mass concentration 0.02g/mL。
2) Palladous nitrate. ammonium salt solution dipping:
Weigh the activated carbon of certain mass, saturated dipping Palladous nitrate. ammonium salt solution, be placed in drying baker 60 DEG C air-dry。
3) Palladous nitrate. ammonium decomposition-reduction:
The sample of impregnation drying is placed in tube type vacuum stove, through-flow dynamic argon, and heat to 300 DEG C of insulation 2h, Palladous nitrate. ammonium decomposition-reduction is become Metal Palladium-activated carbon。
4) silver nitrate solution dipping:
By the saturated dipping silver nitrate solution of palladium-activated carbon made above, be placed in drying baker 60 DEG C air-dry。
5) silver nitrate decomposition-reduction
Being placed in tube type vacuum stove by sample air-dry for step 4, pass into flowing argon, heat to 450 DEG C of insulation 2h, sample is reduced into palladium-Yin-absorbent charcoal composite material, tail gas need to be passed into sodium hydroxide solution and carry out absorption process by this process。
6) repeat above 2-5 step repeatedly, and control the consumption of two kinds of solution, obtain the composite of predetermined palladium-Yin ratio (atomic ratio Pd:Ag=9:1) and content。
7) composite heat treatment: the palladium-Yin-absorbent charcoal composite material of preparation is inserted vacuum tube furnace, after adopting mechanical pump evacuation, is warming up to 1050 DEG C of insulation 30min, makes the Metal Palladium in sample and sliver diffusion be recrystallised to Pd90Ag10Granule is also uniformly distributed in carried by active carbon body。
8) hydrogen inhaled by sample: the sample after heat treatment is loaded suction and puts hydrogen storage equipment sample room, sample room is heated constant temperature after 150 DEG C。Open vacuum pump, to sample evacuation 1 hour；Close vacuum pump, sample room is passed into high-purity hydrogen (99.999%) until pressure rises to 100kPa, keep pressure 5 minutes, make the saturated suction hydrogen of palladium-silver。
9) sample puts hydrogen: open vacuum pump, to sample room evacuation, makes gas pressure in sample room be down to below 0.1Pa and continue more than 10 minutes, and palladium-silver sample puts hydrogen。
10) inhale hydrogen more than repeating, put hydrogen step, after accumulative 2000 times, taken out by sample room after sample is put hydrogen, Pd90Ag10Alloy sample constant temperature is inhaled after putting hydrogen circulation and is generated one-dimensional palladium-silver nanowire product。
Embodiment 5
Magnetron sputtering prepares palladium-nickel alloy (PdNi5) sample, prepare one-dimensional palladium-nickel alloy nano wire by constant temperature circulating:
1) magnetron sputtering prepares palladium-nickel alloy (PdNi5) sample；
Adopt pure nickel (99.99%), pure palladium (99.99%) as target, carry out double; two target magnetic control sputtering using sieve particle as matrix, prepare PdNi by controlling dual-target sputtering parameter5Alloy film, repeatedly sputters after sieve particle is stirred, and makes particle surface alloy film be evenly distributed。
2), alloy sample heat treatment: by surface sputtering PdNi5The sieve particle of alloy film is loaded into vacuum heat treatment furnace, after evacuation, is flushed with hydrogen gas to 50kPa, is warming up to 900 DEG C of insulations, heat treatment 1 hour, lowers the temperature with stove, complete sample heat treatment after evacuation dehydrogenation。
3), hydrogen inhaled by sample: the sample after heat treatment is loaded suction and puts hydrogen storage equipment sample room, sample room is heated constant temperature after 50 DEG C。Open vacuum pump, to sample evacuation 1 hour；Close vacuum pump, sample room is passed into high-purity hydrogen (99.999%) until pressure rises to 150kPa, keep pressure 5 minutes, make the saturated suction hydrogen of palladium-nickel alloy。
4), sample puts hydrogen: opening vacuum pump, to sample room evacuation, make gas pressure in sample room be down to below 0.1Pa and continue more than 10 minutes, palladium-nickel alloy sample puts hydrogen。
5), repeating to inhale hydrogen above, put hydrogen step, after accumulative 1500 times, taken out by sample room after sample is put hydrogen, molecular sieve surface has one-dimensional palladium nickel nanowire product to occur。
Above-described embodiment only for technology design and the feature of the present invention are described, its object is to allow person skilled in the art will appreciate that present disclosure and to implement according to this, can not limit the scope of the invention with this。All equivalences made according to spirit of the invention change or modify, and all should be encompassed within protection scope of the present invention。

Claims (8)

1. a Metal Palladium or palladium alloy nanowires preparation method, it is characterised in that: being undertaken Metal Palladium or palldium alloy inhaling the circulation of hydrogen-put hydrogen, with inhaling the carrying out putting hydrogen cyclic process, there is nanowire growth in palladium and alloy thereof, obtain nanowire product。
2. Metal Palladium or palladium alloy nanowires preparation method described in claim 1, it is characterized in that: Metal Palladium or palldium alloy raw material are directly applied, or it is coated on carrier material through palladium salt solution impregnating reduction method, plating, chemical plating or magnetron sputtering, and is prepared into the Granular composite material of palladium or palldium alloy by Technology for Heating Processing。
3. Metal Palladium or palladium alloy nanowires preparation method described in claim 2; it is characterized in that; described Technology for Heating Processing is: heat treatment temperature is 600-1100 DEG C, processes time 0.5h-12h, and heat treatment carries out in air atmosphere, inert gas shielding or hydrogen atmosphere。
4. Metal Palladium or palladium alloy nanowires preparation method described in claim 3, it is characterised in that described Technology for Heating Processing is: heat treatment temperature is 900-1000 DEG C, processes time 0.5-1h。
5. according to the arbitrary described Metal Palladium of claims 1 to 3 or palladium alloy nanowires preparation method, it is characterised in that: must there is to inhale for more than 100 times hydrogen-put hydrogen circulation with hydrogen in described palladium and alloy raw material thereof, hydrogen is selected from hydrogen or its isotope deuterium, tritium。
6. Metal Palladium or palladium alloy nanowires preparation method described in claim 5, it is characterised in that: inhale hydrogen-put hydrogen and cycle through in the following manner and realize:
Constant temperature is inhaled and is put hydrogen, and namely hydrogen inhaled at a constant temperature by sample, and by evacuation dehydrogenation；
Or thermic inhales and put hydrogen, it is placed in container by the saturated suction hydrogen of sample to carry out intensification dehydrogenation, hydrogen is inhaled in cooling。
7. Metal Palladium or palladium alloy nanowires preparation method described in claim 2, it is characterised in that: described carrier material is porous material or ceramic material, metal material。
8. Metal Palladium or palladium alloy nanowires preparation method described in claim 7, it is characterised in that: described porous material is kieselguhr, molecular sieve or activated carbon。
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Citations (4)

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US20130084210A1 (en) * 2011-09-30 2013-04-04 The Research Foundation Of State University Of New York Surfactantless metallic nanostructures and method for synthesizing same
CN103252501A (en) * 2013-04-27 2013-08-21 宁波大学 Method for preparing metal palladium nanowires of controllable size

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1883853A (en) * 2006-06-30 2006-12-27 苏州大学 Platinum metal nano-particle size control growth method
CN101318222A (en) * 2007-06-06 2008-12-10 中国科学院金属研究所 Metal alloy nano-stick or nano-wire manufactured with Laves phase hydrogenation method and process thereof
US20130084210A1 (en) * 2011-09-30 2013-04-04 The Research Foundation Of State University Of New York Surfactantless metallic nanostructures and method for synthesizing same
CN103252501A (en) * 2013-04-27 2013-08-21 宁波大学 Method for preparing metal palladium nanowires of controllable size

Non-Patent Citations (1)

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Title
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