CN106276942B - A kind of flake porous CoB powders and preparation method thereof - Google Patents
A kind of flake porous CoB powders and preparation method thereof Download PDFInfo
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- CN106276942B CN106276942B CN201610814110.0A CN201610814110A CN106276942B CN 106276942 B CN106276942 B CN 106276942B CN 201610814110 A CN201610814110 A CN 201610814110A CN 106276942 B CN106276942 B CN 106276942B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of flake porous CoB powders and preparation method thereof, belong to inorganic particle preparing technical field.The powder is crystalline state CoB, and by average thickness 20nm, the nanometer sheet of 200~300nm of planar dimension forms, and the nanometer sheet is cross-linked to form open porous structure.The specific preparation process of the powder includes：Micro-sized metal cobalt powder, amorphous boron powder and alkali metal chloride powder are mixed；Above-mentioned mixed powder is put into corundum crucible, is heated to 800 DEG C or more under protection of argon gas, keeps the temperature natural cooling after 0.5 2h；Products therefrom is soaked in water, is filtered, cleaning, the flake porous CoB powders of drying to obtain.The obtained CoB powders of the present invention are crystalline state, and with sheet porous structural, can not only be used as catalyst carrier material, but also be a kind of potential inorganic functional material of tool.
Description
Technical field
The invention belongs to inorganic particle preparing technical fields, and in particular to a kind of CoB raw powder's production technologies, more particularly to
A kind of CoB raw powder's production technologies with flake porous pattern.
Background technology
For CoB due to mechanical hardness height, corrosion resistance is strong and with good electromagnetism and catalysis characteristics, is applied in superhard anti-corrosion
Layer, electronic functional material and catalytic field have a wide range of applications.At present, there are mainly two types of CoB raw powder's production technologies：Humidifying
Method and self-propagating combustion.CoB powders prepared by wet chemistry method are amorphous state, and size is generally nanoscale, are usually loaded
It is used as catalyst on porous support.CoB powders prepared by self-propagating combustion are crystalline state, and size is micron order, and anti-
Process is answered to be difficult to control, the powder with special appearance can not be prepared.
The pattern of powder has larger impact to the performance particularly functional performances such as electricity, magnetic, catalysis of material.Therefore, it closes
It is a useful approach for improving CoB powder characteristics into the crystallization CoB powders with special appearance.It is in addition, porous using having
Structure crystallization CoB powders as amorphous CoB carrier than other carriers on chemical compatibility and corrosion resistance have more it is excellent
Gesture.
Invention content
The technical problems to be solved by the invention are：A kind of preparation side of the CoB powders with flake porous pattern is provided
Method.
To achieve the above object, the present invention is achieved by the following technical programs.
The present invention provides a kind of flake porous CoB powders, which is crystalline state CoB, by average thickness 20nm, plane
The nanometer sheet composition of 200~300nm of size, the nanometer sheet are cross-linked to form open porous structure.
Invention also provides above-mentioned sheet porous C oB raw powder's production technologies, specifically comprise the following steps：
(1) micro-sized metal cobalt powder, amorphous boron powder and alkali metal chloride powder are mixed；
The molar ratio of the micro-sized metal cobalt powder and amorphous boron powder is 1：1.2~2；The alkali metal chloride is chlorine
Change one or both of sodium, potassium chloride, quality is 5~15 times of micro-sized metal cobalt powder and amorphous boron powder；
(2) mixed powder that step (1) obtains is put into corundum crucible, it is natural after being heat-treated under argon gas protection
Cooling；
The heat treatment temperature is 800 DEG C or more, and heat treatment time is 0.5~2h；
(3) mixture that step (2) obtains is impregnated into 1~3h into the water, piece is obtained after filtered, cleaning, drying
Shape porous C oB powders.
Preferably, in step (1), mixture of the alkali metal chloride for sodium chloride and potassium chloride, molar ratio
It is 1：1.
The preparation process of the present invention has following features：The present invention is in the solid phase reaction process of metallic cobalt and amorphous boron powder
In introduce alkali metal chloride.Alkali metal chloride has following three effects in the preparation of flake porous CoB powders：
(1) as barrier, inhibit the vigorous reaction between metallic cobalt and amorphous boron powder, make reaction rate controllable；(2) alkali metal chlorine
Compound is melted at 658~801 DEG C, is provided a liquid phase environment for reaction, is accelerated the diffusion of solid matter, make nothing in reaction product
Other crystalline phase impurity (such as Co2B, Co3B, Co4B etc.)；(3) grain growth occurs in liquid phase environment for CoB crystal grain, forms sheet
Porous structure.
The obtained CoB powders of the present invention are crystalline state, and with sheet porous structural, can both be used as catalyst carrier
Material, and be a kind of potential inorganic functional material of tool.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of CoB powders made from the embodiment of the present invention 1.
Fig. 2 is scanning electron microscope (SEM) photo of CoB powders made from the embodiment of the present invention 1.
Specific embodiment
In order to further appreciate that the technology contents of the present invention, the present invention, but this hair are described in detail below in conjunction with drawings and examples
It is bright to be not limited to following embodiments.
Embodiment 1
By micro-sized metal cobalt powder and amorphous boron powder (molar ratio 1:2) sodium chloride/potassium chloride with 10 times of quality (is rubbed
You are than being 1：1) powder is put into corundum crucible after mixing, is heated to 1000 DEG C under protection of argon gas, keeps the temperature nature after 1h
Then product is soaked in water 1h by cooling, filtering is cleaned repeatedly, the flake porous CoB powder of drying to obtain with water and ethyl alcohol respectively
Body.
Fig. 1 is the XRD spectrum of CoB powders prepared by the present embodiment, it can be seen that the powder prepared by the present embodiment is knot
The CoB of crystalline state.Fig. 2 be CoB powders prepared by the present embodiment SEM photograph, it can be seen that the powder by many thickness about
The nanometer sheet composition of 20nm, planar dimension about 200-300nm, these nanometer sheets are cross-linked to form open porous structure.
Embodiment 2
By micro-sized metal cobalt powder and amorphous boron powder (molar ratio 1:1.5) the sodium chloride powder with 5 times of quality mixes
It is put into corundum crucible after uniformly, is heated to 1000 DEG C under protection of argon gas, natural cooling after 1h is kept the temperature, then by product water
1h is impregnated, filtering is cleaned repeatedly, the flake porous CoB powders of drying to obtain with water and ethyl alcohol respectively.
Embodiment 3
By micro-sized metal cobalt powder and amorphous boron powder (molar ratio 1:1.2) the sodium chloride powder with 5 times of quality mixes
It is put into corundum crucible after uniformly, is heated to 1100 DEG C under protection of argon gas, natural cooling after 1h is kept the temperature, then by product water
2h is impregnated, filtering is cleaned repeatedly, the flake porous CoB powders of drying to obtain with water and ethyl alcohol respectively.
Embodiment 4
By micro-sized metal cobalt powder and amorphous boron powder (molar ratio 1:1.8) the potassium chloride powder with 10 times of quality mixes
It is put into corundum crucible after uniformly, is heated to 800 DEG C under protection of argon gas, natural cooling after 2h is kept the temperature, then by product water
3h is impregnated, filtering is cleaned repeatedly, the flake porous CoB powders of drying to obtain with water and ethyl alcohol respectively.
Claims (2)
1. a kind of flake porous CoB powders, which is characterized in that the powder is crystalline state CoB, by average thickness 20nm, plane meter
The nanometer sheet composition of very little 200~300nm, the nanometer sheet are cross-linked to form open porous structure；
The raw powder's production technology specifically comprises the following steps：
(1) micro-sized metal cobalt powder, amorphous boron powder and alkali metal chloride powder are mixed；
The molar ratio of the micro-sized metal cobalt powder and amorphous boron powder is 1：1.2~2；The alkali metal chloride is chlorination
One or both of sodium, potassium chloride, quality are 5~15 times of micro-sized metal cobalt powder and amorphous boron powder；
(2) mixed powder that step (1) obtains is put into corundum crucible, it is naturally cold after being heat-treated under argon gas protection
But；
The heat treatment temperature is 800 DEG C or more, and heat treatment time is 0.5~2h；
(3) mixture that step (2) obtains is impregnated into 1~3h into the water, it is more to obtain sheet after filtered, cleaning, drying
Hole CoB powders.
2. a kind of flake porous CoB powders as described in claim 1, which is characterized in that in step (1), the alkali metal
Mixture of the chloride for sodium chloride and potassium chloride, molar ratio 1：1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610814110.0A CN106276942B (en) | 2016-09-09 | 2016-09-09 | A kind of flake porous CoB powders and preparation method thereof |
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| CN201610814110.0A CN106276942B (en) | 2016-09-09 | 2016-09-09 | A kind of flake porous CoB powders and preparation method thereof |
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| CN106276942B true CN106276942B (en) | 2018-06-29 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1188098A1 (en) * | 1983-08-31 | 1985-10-30 | Ставропольский политехнический институт | Method of producing iron borides |
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2016
- 2016-09-09 CN CN201610814110.0A patent/CN106276942B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1188098A1 (en) * | 1983-08-31 | 1985-10-30 | Ставропольский политехнический институт | Method of producing iron borides |
Non-Patent Citations (4)
| Title |
|---|
| Facile preparation and goode lectrochemical hydrogen storage properties of chain-like and rod-like Co-B nanomaterials;Qinghong Wang et al;;《Electrochimica Acta》;20100708;第55卷;第7199–7203页 * |
| Mechanochemical synthesis and high-capacity performances of transition-metal borides as aqueous anode materials;WANG YaDong et al;;《Chin Sci Bull》;20120331;第57卷(第32期);第4225-4228页 * |
| Solid-state reaction induced by milling of a mixture of cobalt and boron powders;A. CORRIAS et al;;《JOURNAL OF MATERIALS SCIENCE》;19911231;第26卷;第5081-5084页 * |
| Towards easy reversible dehydrogenation of LiBH4 by catalyzing hierarchic nanostructured CoB;Weitong Cai et al;;《Nano Energy》;20140909;第10卷;第235–244页 * |
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