CN103466574A - Method for preparing three-dimensional macroporous metal phosphide - Google Patents
Method for preparing three-dimensional macroporous metal phosphide Download PDFInfo
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- CN103466574A CN103466574A CN 201310429974 CN201310429974A CN103466574A CN 103466574 A CN103466574 A CN 103466574A CN 201310429974 CN201310429974 CN 201310429974 CN 201310429974 A CN201310429974 A CN 201310429974A CN 103466574 A CN103466574 A CN 103466574A
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Abstract
The invention relates to a method for preparing a three-dimensional macroporous metal phosphide by heat treatment of foam metal, and belongs to the technical field of preparation processes of inorganic materials. According to the method disclosed by the invention, a mechanical mixture of red phosphorus and the foam metal is taken as a precursor, and the three-dimensional macroporous metal phosphide is prepared by utilizing the reaction of the red phosphorus and metal particles. The method has the advantages of simplicity in operation, good process repeatability, stable product quality, and suitability for large-scale production.
Description
Technical field
The invention belongs to the inorganic material preparation process technical field, relate to the preparation method of inorganic materials, specifically the synthetic method of three-dimensional macropore metal phosphide.Can be applicable to the aspects such as battery material, superconducting material and catalytic material.
Background technology
Three-dimensional macroporous structure has chemistry and the physical properties of optimization because of its hollow feature, thereby has considerable application prospect.Due to less density of material, larger specific surface area and the space that can load, three-dimensional macropore particle can be as the assembled unit of light material and the catalyzer of high surface.Metal phosphide has the physicochemical property that supraconductivity, ferromegnetism, catalytic activity etc. are good and is paid close attention to by scholars, but the control of the phosphide of special construction is synthetic and applied research is huge challenge always.In this invention, we utilize the three-dimensional structure of foamed metal and take it as masterplate, take red phosphorus as the phosphorus source, by roasting simply, provide a kind of metal phosphide synthetic method of pervasive three-dimensional macroporous structure.
Summary of the invention
Meaning of the present invention is to provide a kind of synthetic method of three-dimensional macropore metal phosphide, this method can be controlled by the three-dimensional structure of foamed metal the three-dimensional structure of phosphide, and has simple to operately, and the reaction times is of short duration, good process repeatability, the advantage of constant product quality.
Characteristics of the present invention are can realize preparing different types of three-dimensional macropore metal phosphide by changing the kind of foamed metal.
Three-dimensional macropore metal phosphide synthesis step is as follows:
Get a foamed metal (arbitrary dimension all can); a certain amount of red phosphorus powder is dispersed in to the surface of foamed metal; then said mixture is packed in little porcelain boat; put into tube furnace; pass into rare gas element as shielding gas; then after directly being warmed up to 700-750 ℃, thermal treatment 10-180 minute.Under protection of inert gas, furnace is down to room temperature after completion of the reaction; product soaks the metal of the reaction that defoams and do not have in 5 hours with the hydrochloric acid of 6mol/L 80 ℃ of water-baths; product water is washed till neutrality, 60 ℃ of vacuum-dryings, within 3 hours, obtains corresponding three-dimensional macropore metal phosphide.
Specific embodiments
Embodiment 1
Get the nickel foam of one 5 * 2 square centimeters; 5g red phosphorus powder is dispersed in to the upper surface of nickel foam; then be placed in quartz boat; put into tube furnace, with the flow velocity of 20mL/min, pass into argon gas, then directly be warming up to 700 ℃; at this temperature, reaction is 30 minutes; after drop to room temperature in argon shield, product soaks 5 hours after washings to neutral through the hydrochloric acid of 6mol/L 80 ℃ of water-baths, 60 ℃ of vacuum-dryings, within 3 hours, obtains three-dimensional macropore nickel phosphide.
Embodiment 2
Temperature of reaction in embodiment 1 is become to 750 ℃ by 700 ℃, and other condition is constant, obtains three-dimensional macropore nickel phosphide.
Embodiment 3
Reaction times in embodiment 1 is become to 60min by 30min, and other condition is constant, obtains three-dimensional macropore nickel phosphide.
Embodiment 4
Nickel foam in embodiment 1 is become to foam copper, obtain three-dimensional macropore phosphorized copper.
Embodiment 5
Nickel foam in embodiment 1 is become to foam iron, obtain three-dimensional macropore iron phosphide.
Embodiment 6
Nickel foam in embodiment 1 is become to the foam cobalt, obtain three-dimensional macropore phosphatization cobalt.
Embodiment 7
Nickel foam in embodiment 1 is become to foamed molybdenum, obtain three-dimensional macropore phosphatization molybdenum.
Embodiment 8
Nickel foam in embodiment 1 is become to foam tungsten, obtain three-dimensional macropore tungsten phosphide.
Embodiment 9
Nickel foam in embodiment 1 is become to titanium foam, obtain three-dimensional macropore phosphatization titanium.
Claims (2)
1. prepare the method for three-dimensional macropore metal phosphide based on foamed metal and red phosphorus mixture, it is characterized in that comprising the steps:
Get a foamed metal (arbitrary dimension all can); a certain amount of red phosphorus powder is dispersed in to the upper surface of foamed metal; then said mixture is packed in little porcelain boat; put into tube furnace; pass into rare gas element as shielding gas; then after directly being warmed up to 700-750 ℃, thermal treatment 10-180 minute.Under protection of inert gas, furnace is down to room temperature after completion of the reaction; product soaks the metal of the reaction that defoams and do not have in 5 hours with the hydrochloric acid of 6mol/L 80 ℃ of water-baths; product water is washed till neutrality, 60 ℃ of vacuum-dryings, within 3 hours, obtains corresponding three-dimensional macropore metal phosphide.
According to claim 1 prepare the method for three-dimensional macropore metal phosphide based on nickel foam and red phosphorus mixture, it is characterized in that described foamed metal can be nickel foam, foam copper, foam cobalt, foam iron, foamed molybdenum, foam tungsten and titanium foam.
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| CN 201310429974 CN103466574A (en) | 2013-09-17 | 2013-09-17 | Method for preparing three-dimensional macroporous metal phosphide |
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| CN 201310429974 CN103466574A (en) | 2013-09-17 | 2013-09-17 | Method for preparing three-dimensional macroporous metal phosphide |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103887494A (en) * | 2014-03-11 | 2014-06-25 | 三峡大学 | Method for preparing copper phosphide/copper composite material and application of copper phosphide/copper composite material in lithium ion battery |
| CN104630822A (en) * | 2015-01-14 | 2015-05-20 | 太原理工大学 | Foam transition-metal solid (gas) phosphated self-support hydrogen evolution electrode and preparation method thereof |
| CN104810165A (en) * | 2015-04-29 | 2015-07-29 | 华东理工大学 | Nickel phosphide / graphene composite film preparing method |
| CN104868098A (en) * | 2015-05-15 | 2015-08-26 | 三峡大学 | Negative electrode of carbon-composite Cu3P-Cu lithium-ion battery and preparation method of negative electrode |
| CN105688958A (en) * | 2016-01-15 | 2016-06-22 | 复旦大学 | Polyhedron cobalt phosphide/graphite carbon hybrid material and preparing method and application thereof |
| CN105926021A (en) * | 2016-03-24 | 2016-09-07 | 西北师范大学 | Preparation method and application of nickel phosphide nano film |
| CN106486680A (en) * | 2016-11-07 | 2017-03-08 | 济南大学 | A kind of preparation method of phosphatization stainless steel electrolytic water catalysis material |
| CN106498434A (en) * | 2016-11-04 | 2017-03-15 | 重庆工商大学 | The preparation method of the Ni-based porous nickel phosphide hydrogen-precipitating electrode of integration |
| CN106732697A (en) * | 2016-12-07 | 2017-05-31 | 天津工业大学 | Phosphatization rhodium base optic catalytic material and its synthetic method |
| CN106882774A (en) * | 2017-01-20 | 2017-06-23 | 中国科学院合肥物质科学研究院 | A kind of transition metal phosphide nano wire and preparation method and application |
| CN107478699A (en) * | 2017-08-16 | 2017-12-15 | 太原理工大学 | A kind of preparation method and its usage of foam transition metal phosphide carried noble metal |
| CN108796552A (en) * | 2018-06-15 | 2018-11-13 | 北京大学 | A kind of Ni2P loads the preparation method of Ni base catalyst and obtains catalyst and its application |
| CN109482208A (en) * | 2018-10-31 | 2019-03-19 | 北京科技大学 | The method that nickel foam in-situ reducing copper ion and subsequent heat treatment prepare catalyst |
| CN115928120A (en) * | 2021-09-27 | 2023-04-07 | 中国科学院福建物质结构研究所 | Composite catalytic material of carbon element doped tungsten phosphide film and preparation method and application thereof |
-
2013
- 2013-09-17 CN CN 201310429974 patent/CN103466574A/en active Pending
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103887494A (en) * | 2014-03-11 | 2014-06-25 | 三峡大学 | Method for preparing copper phosphide/copper composite material and application of copper phosphide/copper composite material in lithium ion battery |
| CN103887494B (en) * | 2014-03-11 | 2015-11-11 | 三峡大学 | A kind of preparation method of copper phosphide/carbon/carbon-copper composite material and the application in lithium ion battery |
| CN104630822A (en) * | 2015-01-14 | 2015-05-20 | 太原理工大学 | Foam transition-metal solid (gas) phosphated self-support hydrogen evolution electrode and preparation method thereof |
| CN104810165A (en) * | 2015-04-29 | 2015-07-29 | 华东理工大学 | Nickel phosphide / graphene composite film preparing method |
| CN104868098A (en) * | 2015-05-15 | 2015-08-26 | 三峡大学 | Negative electrode of carbon-composite Cu3P-Cu lithium-ion battery and preparation method of negative electrode |
| CN104868098B (en) * | 2015-05-15 | 2018-03-27 | 三峡大学 | A kind of carbon composite Cu3P Cu negative electrode of lithium ion battery and preparation method thereof |
| CN105688958A (en) * | 2016-01-15 | 2016-06-22 | 复旦大学 | Polyhedron cobalt phosphide/graphite carbon hybrid material and preparing method and application thereof |
| CN105688958B (en) * | 2016-01-15 | 2019-01-15 | 复旦大学 | Polyhedron shape phosphatization cobalt/graphitic carbon hybrid material and its preparation method and application |
| CN105926021A (en) * | 2016-03-24 | 2016-09-07 | 西北师范大学 | Preparation method and application of nickel phosphide nano film |
| CN105926021B (en) * | 2016-03-24 | 2018-02-27 | 西北师范大学 | A kind of nickel phosphide nano thin-film and its preparation method and application |
| CN106498434A (en) * | 2016-11-04 | 2017-03-15 | 重庆工商大学 | The preparation method of the Ni-based porous nickel phosphide hydrogen-precipitating electrode of integration |
| CN106498434B (en) * | 2016-11-04 | 2018-08-17 | 重庆工商大学 | The preparation method of the Ni-based porous nickel phosphide hydrogen-precipitating electrode of integration |
| CN106486680A (en) * | 2016-11-07 | 2017-03-08 | 济南大学 | A kind of preparation method of phosphatization stainless steel electrolytic water catalysis material |
| CN106732697A (en) * | 2016-12-07 | 2017-05-31 | 天津工业大学 | Phosphatization rhodium base optic catalytic material and its synthetic method |
| CN106882774A (en) * | 2017-01-20 | 2017-06-23 | 中国科学院合肥物质科学研究院 | A kind of transition metal phosphide nano wire and preparation method and application |
| CN107478699A (en) * | 2017-08-16 | 2017-12-15 | 太原理工大学 | A kind of preparation method and its usage of foam transition metal phosphide carried noble metal |
| CN107478699B (en) * | 2017-08-16 | 2019-11-15 | 太原理工大学 | A kind of preparation method and its usage of foam transition metal phosphide carried noble metal |
| CN108796552A (en) * | 2018-06-15 | 2018-11-13 | 北京大学 | A kind of Ni2P loads the preparation method of Ni base catalyst and obtains catalyst and its application |
| CN108796552B (en) * | 2018-06-15 | 2019-11-19 | 北京大学 | A kind of preparation method of Ni2P load Ni base catalyst and obtain catalyst and its application |
| CN109482208A (en) * | 2018-10-31 | 2019-03-19 | 北京科技大学 | The method that nickel foam in-situ reducing copper ion and subsequent heat treatment prepare catalyst |
| CN115928120A (en) * | 2021-09-27 | 2023-04-07 | 中国科学院福建物质结构研究所 | Composite catalytic material of carbon element doped tungsten phosphide film and preparation method and application thereof |
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