CN106975754B - A kind of preparation method of palladium nanometer wire - Google Patents
A kind of preparation method of palladium nanometer wire Download PDFInfo
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- CN106975754B CN106975754B CN201611265514.5A CN201611265514A CN106975754B CN 106975754 B CN106975754 B CN 106975754B CN 201611265514 A CN201611265514 A CN 201611265514A CN 106975754 B CN106975754 B CN 106975754B
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000005684 electric field Effects 0.000 claims abstract description 26
- 239000011521 glass Substances 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 6
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 14
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 230000009471 action Effects 0.000 claims description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 2
- 230000001808 coupling effect Effects 0.000 claims description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims 2
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000012696 Pd precursors Substances 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 lauryl dimethyl benzyl Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
- B22F1/0547—Nanofibres or nanotubes
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of palladium nanometer wire, first by preparing palladium precursor solution, and surfactant is added, it is enriched with palladium ion in glass substrate template, and reducing agent reduction is added, obtain nanoparticle, precursor solution then is rejoined, apply the electric field of vertical direction and reducing agent is added, make palladium ion directed movement and is grown, effect is lower to be added reducing agent, obtains the palladium nanometer wire of high length-diameter ratio and orientation rule.
Description
Technical field
The present invention relates to a kind of preparation methods of palladium nanometer wire.
Background technique
Metal exists in noble metal due to showing good selective catalysis activity and electric conductivity, the nano material of palladium at present
Catalyst, fuel cell have a good application prospect in many industrial technical fields such as cracking of oil.And closely study hair
Existing, certain good physical characteristics of nanometer Pd material have close relationship with the shape and size of nano material, effectively control
The morphology and size of nanometer Pd material processed is expected to significantly improve the physicochemical characteristics of nanometer Pd material, nanometer Pd material it is one-dimensional
Structure is compared with zero-dimension structural, shows higher draw ratio, less lattice defect, smaller spacing of lattice and very high
The advantages that surface atom number.Additionally due to the anisotropy in structure, one-dimensional palladium nanometer wire will significantly improve electron-transport effect
Rate.It is expensive since metal is in noble metal, how to guarantee that utmostly playing its characteristic is mesh under the premise of same dosage
The hot spot of preceding research, but in the research carried out at present, there is preparation method complex process, synthesis to a certain extent
The not high problem of palladium nanometer wire draw ratio, hamper the application of palladium nanometer wire.
Summary of the invention
In order to solve the above technical problems, being made the present invention provides a kind of preparation method of palladium nanometer wire using glass substrate
For template, the method for electric field driven enrichment obtains large scale palladium nanometer wire.
The complete technical solution of the present invention includes:
A kind of preparation method of palladium nanometer wire, which comprises the steps of:
(1) deionized water is added in PdCl2, prepares the PdCl2 aqueous solution of 0.05mol/L, is added in reaction vessel, reacted
Container side is equipped with glass substrate, and surfactant is then added, and surfactant group becomes lauryl dimethyl benzyl chlorination
Ammonium: C15Trimethylammonium bromide=1:1 mixture, the above are volume ratios, 3h are stood after stirring 5min, then to reaction vessel two
End applies the electric field of 200N/C, and palladium ion is made directed movement and to be enriched to glass baseplate surface under electric field action at room temperature,
The glucose solution of 6mmol/L is added under ultrasonic vibration stirring and field coupling effect, wherein PdCl2, surfactant
Molar ratio with glucose is 1:4.5:60, stands 3h and the Pd nano particle for being enriched in glass baseplate surface is made.
(2) step (1) acquired solution is added in the PdCl2 aqueous solution that concentration is 0.2mol/L again, is then added
The hydrazine hydrate solution of 0.02mol/L, heating temperature apply 400N/C electric field to reaction vessel both ends again, this time to 45-50 DEG C
It is vertical to apply direction and step (1) application direction of electric field of electric field, make palladium ion under electric field action directed movement and along
The direction movement and reducing agent effect lower precipitation growth vertical with step (1) application electric field, obtains having a size of 800-900 nanometers
Palladium nanometer wire.
Pd nano particle obtained by step (1), PdCl2 and hydrazine hydrate added by step (2) molar ratio be 1:50:30.
Surfactant concentration used in step (1) is 0.03mol/L.
The present invention compared with the existing technology the advantages of be: by using glass substrate as template, under electric field action
The enrichment of Pd nano particle is formed, reduction obtains preformed particles, is then enriched with ion again using vertical electric field effect and goes forward side by side
Row reduction, makes nano wire move and grow along direction of an electric field, obtains the palladium nanometer wire of high length-diameter ratio and orientation rule.
Specific embodiment
The present invention will be further described With reference to embodiment.
(1) deionized water is added in PdCl2, prepares 0.05mol/LPdCl2 aqueous solution, is added in reaction vessel, reaction is held
Device side is equipped with glass substrate, and it is lauryl dimethyl benzyl ammonium chloride: C that volume ratio, which is then added,15Trimethylammonium bromide=1:1
Mixture as surfactant, stand 3h after stirring 5min, then reaction vessel both ends applied with the electric field of 200N/C,
Palladium ion is set directed movement and to be enriched to glass baseplate surface under electric field action at room temperature, in ultrasonic vibration stirring and electric field coupling
The lower glucose solution that 6mmol/L is added of cooperation, wherein the molar ratio of PdCl2, surfactant and glucose is 1:
4.5:60 stands 3h and the Pd nano particle for being enriched in glass baseplate surface is made.
(2) step (1) acquired solution is added in the PdCl2 aqueous solution that concentration is 0.2mol/L again, is then added
The hydrazine hydrate solution of 0.02mol/L, heating temperature apply 400N/C electric field to reaction vessel both ends again, this time to 45-50 DEG C
It is vertical to apply direction and step (1) application direction of electric field of electric field, make palladium ion under electric field action directed movement and along
The direction movement and reducing agent effect lower precipitation growth vertical with step (1) application electric field, obtains having a size of 800-900 nanometers
Palladium nanometer wire, wherein Pd nano particle obtained by step (1), PdCl2 and hydrazine hydrate added by step (2) molar ratio be 1:
50:30。
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification to the above embodiments, change and equivalent structural changes, still fall within skill of the present invention
In the protection scope of art scheme.
Claims (3)
1. a kind of preparation method of palladium nanometer wire, which comprises the steps of:
(1) deionized water is added in PdCl2, prepares the PdCl2 aqueous solution of 0.05mol/L, is added in reaction vessel, reaction vessel
Side is equipped with glass substrate, surfactant is then added, surfactant group is as lauryl dimethyl benzyl ammonium chloride: ten
Five alkyl trimethyl ammonium bromides=1:1 mixture, the above are volume ratios, 3h are stood after stirring 5min, then to reaction vessel
Both ends apply the electric field of 200N/C, and palladium ion is made directed movement and to be enriched to glass substrate table under electric field action at room temperature
The glucose solution of 6mmol/L is added, wherein PdCl2, surface-active in face under ultrasonic vibration stirring and field coupling effect
The molar ratio of agent and glucose is 1:4.5:60, stands 3h and the Pd nano particle for being enriched in glass baseplate surface is made；
(2) step (1) acquired solution is added in the PdCl2 aqueous solution that concentration is 0.2mol/L, the water of 0.02mol/L is then added
Close hydrazine solution, heating temperature to 45-50 DEG C, to reaction vessel both ends apply 400N/C electric field, this time apply electric field direction and
Step (1) apply electric field direction it is vertical, make palladium ion under electric field action directed movement and along with step (1) apply electric field
Vertical direction movement and reducing agent effect is lower to be precipitated growth, obtains the palladium nanometer wire that length is 800-900 nanometers.
2. the method according to claim 1, wherein wherein, Pd nano particle obtained by step (1), step (2)
The molar ratio of added PdCl2 and hydrazine hydrate is 1:50:30.
3. the method according to claim 1, wherein surfactant concentration used in step (1) is 0.03mol/
L。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611265514.5A CN106975754B (en) | 2016-12-30 | 2016-12-30 | A kind of preparation method of palladium nanometer wire |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611265514.5A CN106975754B (en) | 2016-12-30 | 2016-12-30 | A kind of preparation method of palladium nanometer wire |
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| CN106975754A CN106975754A (en) | 2017-07-25 |
| CN106975754B true CN106975754B (en) | 2019-08-30 |
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| CN111069625B (en) * | 2020-01-06 | 2021-10-01 | 昆明理工大学 | Preparation method of flaky platinum nanoparticles |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3275787A (en) * | 1963-12-30 | 1966-09-27 | Gen Electric | Process and apparatus for producing particles by electron melting and ultrasonic agitation |
| CN1911782A (en) * | 2006-07-21 | 2007-02-14 | 东莞理工学院 | Preparation method of palladium nanometer wire oldered array material |
| CN101310899A (en) * | 2008-03-18 | 2008-11-26 | 江苏工业学院 | Method for preparing silver nano-wire in large batch |
| CN101935017A (en) * | 2010-07-29 | 2011-01-05 | 中国科学院生态环境研究中心 | Method for synthesizing noble metal superfine nanowire water phase and establishing noble metal nanopore membrane by self-precipitation thereof |
| CN103252501A (en) * | 2013-04-27 | 2013-08-21 | 宁波大学 | Method for preparing metal palladium nanowires of controllable size |
| CN104018189A (en) * | 2014-06-05 | 2014-09-03 | 东北大学 | Preparation method for novel nano-silver wire |
-
2016
- 2016-12-30 CN CN201611265514.5A patent/CN106975754B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3275787A (en) * | 1963-12-30 | 1966-09-27 | Gen Electric | Process and apparatus for producing particles by electron melting and ultrasonic agitation |
| CN1911782A (en) * | 2006-07-21 | 2007-02-14 | 东莞理工学院 | Preparation method of palladium nanometer wire oldered array material |
| CN101310899A (en) * | 2008-03-18 | 2008-11-26 | 江苏工业学院 | Method for preparing silver nano-wire in large batch |
| CN101935017A (en) * | 2010-07-29 | 2011-01-05 | 中国科学院生态环境研究中心 | Method for synthesizing noble metal superfine nanowire water phase and establishing noble metal nanopore membrane by self-precipitation thereof |
| CN103252501A (en) * | 2013-04-27 | 2013-08-21 | 宁波大学 | Method for preparing metal palladium nanowires of controllable size |
| CN104018189A (en) * | 2014-06-05 | 2014-09-03 | 东北大学 | Preparation method for novel nano-silver wire |
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| CN106975754A (en) | 2017-07-25 |
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