CN106430227A - Nickel boride powder with network structure and preparation method of nickel boride powder - Google Patents
Nickel boride powder with network structure and preparation method of nickel boride powder Download PDFInfo
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- CN106430227A CN106430227A CN201610815692.4A CN201610815692A CN106430227A CN 106430227 A CN106430227 A CN 106430227A CN 201610815692 A CN201610815692 A CN 201610815692A CN 106430227 A CN106430227 A CN 106430227A
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- powder
- nickel
- cancellated
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- powder body
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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
Abstract
The invention discloses nickel boride powder with a network structure and a preparation method of the nickel boride powder, and belongs to the technical field of inorganic powder preparation. The nickel boride powder is crystalline Ni3B and has the network structure, and the average diameter of network lines is 20 nm. The preparation method comprises the preparation steps as follows: micron-scale metal nickel powder, amorphous boron powder and alkali chloride powder are mixed; the mixed powder is placed in a corundum crucible, heated to 1000 DEG C or higher under argon protection and cooled naturally after thermal insulation for 0.5-2 hours; an obtained product is soaked in hydrochloric acid, filtered, washed with water and ethanol for several times and dried, and the Ni3B powder with the network structure is obtained. The obtained Ni3B powder is crystalline, has the network porous structure, can be used as a catalyst carrier material and is also a potential inorganic function material.
Description
Technical field
The invention belongs to inorganic particle preparing technical field is and in particular to a kind of nickel boridess (Ni3B) the preparation side of powder body
Method, has cancellated Ni particularly to one kind3B raw powder's production technology.
Background technology
Ni-B is high due to mechanical hardness, and corrosion resistance is strong and has good electromagnetism and catalysis characteristicses, in superhard anti-corrosion painting
Layer, electronic functional material and catalytic field have a wide range of applications.At present, Ni-B raw powder's production technology mainly has two kinds：Wet
Chemical method and simple substance direct reaction method.Wet chemistry method typically adopts the nickeliferous presoma of borohydride reduction, and gained Ni-B powder body is
Amorphous state, a size of nanoscale, are a kind of wider base metal hydrogen electrode catalysts of application.Prepared by simple substance direct reaction method
Ni-B powder body be crystalline state, can be implemented by mechanochemical reaction or self-propagating combustion.Ni- prepared by mechanochemical reaction
B diameter of particle is little, but crystallinity is poor, and can introduce some impurity in mechanical milling process.And prepared by self-propagating combustion
Ni-B powder grain size is larger, skewness, and course of reaction is difficult to control to, and the problems such as react incomplete easily.Additionally,
Because Ni-B system contains NiB12, NiB, Ni2B, Ni3B, Ni4B3Etc. multiple crystalline phases, the crystallization Ni-B being synthesized by said method
Powder body mostly is compound phase.
Catalyst is typically all supported on when using with porous or cancellated carrier, and catalyst and carrier need
There is good chemical compatibility.Obviously, crystallization Ni-B is the best carrier of the amorphous Ni-B catalyst chemical compatibility, and makes
More more advantageous in corrosion resistance than other carriers as catalyst carrier with crystallization Ni-B powder body.But, have porous or
Cancellated crystallization Ni-B powder body yet there are no and has been reported that.
Content of the invention
The technical problem to be solved is：One kind is provided to have cancellated crystallization Ni3The preparation side of B powder body
Method.
For achieving the above object, the present invention adopts the following technical scheme that.
The invention provides one kind has cancellated nickel boridess powder body, this powder body is crystalline state Ni3B, has network
Structure, netting twine average diameter is 20nm.
Invention also provides above-mentioned have cancellated nickel boridess raw powder's production technology, specifically include following step
Suddenly：
(1) micro-sized metal nikel powder, amorphous boron powder and alkali metal chloride powder body are mixed；
The mol ratio of described micro-sized metal nikel powder and amorphous boron powder is 3～5：1；Described alkali metal chloride is chlorination
One of sodium, potassium chloride or two kinds, its quality is 5～15 times of micro-sized metal nikel powder and amorphous boron powder quality；
(2) mixed powder obtaining step (1) is put in corundum crucible, natural after heat treatment under argon gas protection
Cooling；
Described heat treatment temperature is more than 1000 DEG C, and heat treatment time is 0.5～2h；
(3) step (2) products therefrom is put into immersion 2-8h in the hydrochloric acid of 1.0～4.0mol/L, filter, cleaning, it is dried
Obtain that there is cancellated nickel boridess powder body.
Preferably, described alkali metal chloride is the mixture of sodium chloride and potassium chloride, and its mol ratio is 1：1.
The preparation process of the present invention has following features：The present invention is in the solid state reaction process of metallic nickel and amorphous boron powder
In introduce alkali metal chloride.Alkali metal chloride is in Ni3There is in the preparation of B powder body three below effect：(1) as resistance
Every agent, suppress the vigorous reaction between metallic nickel and amorphous boron powder, make reaction rate controlled；(2) alkali metal chloride is 658
～801 DEG C of meltings, provide a liquid phase environment for reaction, accelerate the diffusion of solid matter, make no other crystallizations in product
Phase impurity (such as NiB, Ni2B, Ni4B3Deng)；(3)Ni3There is grain growth in B crystal grain in liquid phase environment, form network structure.
Ni obtained by the present invention3B powder body is crystalline state, and has reticulated porous structures, both can carry as catalyst
Body material, is a kind of potential inorganic functional material of tool again.
Brief description
Fig. 1 is the Ni that the embodiment of the present invention 1 is obtained3X-ray diffraction (XRD) collection of illustrative plates of B powder body.
Fig. 2 is the Ni that the embodiment of the present invention 1 is obtained3Scanning electron microscope (SEM) photo of B powder body.
Specific embodiment
In order to further appreciate that the technology contents of the present invention, below in conjunction with drawings and Examples in detail the present invention is described in detail, but this
Bright it is not limited to following embodiments.
Embodiment 1
By micro-sized metal nikel powder and amorphous boron powder, (mol ratio is 3:1) (rub with the sodium chloride/potassium chloride of 10 times of quality
That ratio is 1：1) put in corundum crucible after powder body mix homogeneously, under argon protection, be heated to 1000 DEG C, natural after insulation 1h
Then product is put into immersion 2h in the hydrochloric acid of 1.0mol/L, is filtered by cooling, uses water and ethanol purge respectively repeatedly, drying is
Obtain that there is cancellated Ni3B powder body.
Fig. 1 is Ni prepared by the present embodiment3The XRD spectrum of B powder body is it can be seen that the powder body prepared by the present embodiment is
Crystallization Ni3B, no other impurities phases.Fig. 2 is Ni prepared by the present embodiment3The SEM photograph of B powder body is it can be seen that this powder body has
Network structure, sealike colour is about 20nm.
Embodiment 2
By micro-sized metal nikel powder and amorphous boron powder, (mol ratio is 4:1) mix all with the sodium chloride powder body of 5 times of quality
Put into after even in corundum crucible, under argon protection, be heated to 1100 DEG C, natural cooling after insulation 1h, then product is put into
Soak 4h in the hydrochloric acid of 2.0mol/L, filter, use water and ethanol purge respectively repeatedly, drying to obtain has cancellated
Ni3B powder body.
Embodiment 3
By micro-sized metal nikel powder and amorphous boron powder, (mol ratio is 4.5:1) mix with the sodium chloride powder body of 5 times of quality
Put in corundum crucible after uniformly, under argon protection, be heated to 1100 DEG C, natural cooling after insulation 1h, then product is put into
Soak 5h in the hydrochloric acid of 3.0mol/L, filter, use water and ethanol purge respectively repeatedly, drying to obtain has cancellated
Ni3B powder body.
Embodiment 4
By micro-sized metal nikel powder and amorphous boron powder, (mol ratio is 5:1) mix all with the potassium chloride powder body of 10 times of quality
Put into after even in corundum crucible, under argon protection, be heated to 1000 DEG C, natural cooling after insulation 1h, then product is put into
Soak 8h in the hydrochloric acid of 4.0mol/L, filter, use water and ethanol purge respectively repeatedly, drying to obtain has cancellated
Ni3B powder body.
Claims (3)
1. one kind has cancellated nickel boridess powder body it is characterised in that this powder body is crystalline state Ni3B, has network structure,
Netting twine average diameter is 20nm.
2. one kind as claimed in claim 1 has cancellated nickel boridess raw powder's production technology it is characterised in that including
Following steps：
(1) micro-sized metal nikel powder, amorphous boron powder and alkali metal chloride powder body are mixed；
The mol ratio of described micro-sized metal nikel powder and amorphous boron powder is 3～5：1；Described alkali metal chloride be sodium chloride,
One of potassium chloride or two kinds, its quality is 5～15 times of micro-sized metal nikel powder and amorphous boron powder quality；
(2) mixed powder obtaining step (1) is put in corundum crucible, naturally cold after heat treatment under argon gas protection
But；
Described heat treatment temperature is more than 1000 DEG C, and heat treatment time is 0.5～2h；
(3) step (2) products therefrom is put into immersion 2～8h in the hydrochloric acid of 1.0～4.0mol/L, after filtering, clean, being dried
Obtain that there is cancellated nickel boridess powder body.
3. one kind as claimed in claim 2 has cancellated nickel boridess raw powder's production technology it is characterised in that described
Alkali metal chloride is the mixture of sodium chloride and potassium chloride, and its mol ratio is 1：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610815692.4A CN106430227B (en) | 2016-09-09 | 2016-09-09 | A kind of nickel borides powder and preparation method thereof with reticular structure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610815692.4A CN106430227B (en) | 2016-09-09 | 2016-09-09 | A kind of nickel borides powder and preparation method thereof with reticular structure |
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| CN106430227A true CN106430227A (en) | 2017-02-22 |
| CN106430227B CN106430227B (en) | 2018-08-24 |
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| CN201610815692.4A Active CN106430227B (en) | 2016-09-09 | 2016-09-09 | A kind of nickel borides powder and preparation method thereof with reticular structure |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114524438A (en) * | 2022-03-03 | 2022-05-24 | 吉林大学 | High-temperature high-pressure preparation method of nickel-boron compound single-phase block material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1188098A1 (en) * | 1983-08-31 | 1985-10-30 | Ставропольский политехнический институт | Method of producing iron borides |
| US5587140A (en) * | 1994-05-18 | 1996-12-24 | Sumitomo Chemical Company, Limited | Process for producing powders of transition metal boride |
| EP2423164A1 (en) * | 2010-08-25 | 2012-02-29 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | General synthesis of metal borides in liquid salt melts |
-
2016
- 2016-09-09 CN CN201610815692.4A patent/CN106430227B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1188098A1 (en) * | 1983-08-31 | 1985-10-30 | Ставропольский политехнический институт | Method of producing iron borides |
| US5587140A (en) * | 1994-05-18 | 1996-12-24 | Sumitomo Chemical Company, Limited | Process for producing powders of transition metal boride |
| EP2423164A1 (en) * | 2010-08-25 | 2012-02-29 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | General synthesis of metal borides in liquid salt melts |
Non-Patent Citations (1)
| Title |
|---|
| ZACHARY L. SCHAEFER ET AL;: "Direct Solution Synthesis, Reaction Pathway Studies, and Structural Characterization of Crystalline Ni3B Nanoparticles", 《J.PHYS.CHEM.C》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114524438A (en) * | 2022-03-03 | 2022-05-24 | 吉林大学 | High-temperature high-pressure preparation method of nickel-boron compound single-phase block material |
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| CN106430227B (en) | 2018-08-24 |
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