CN107161959A - A kind of preparation method of nickelous selenide micron tube - Google Patents
A kind of preparation method of nickelous selenide micron tube Download PDFInfo
- Publication number
- CN107161959A CN107161959A CN201710288315.4A CN201710288315A CN107161959A CN 107161959 A CN107161959 A CN 107161959A CN 201710288315 A CN201710288315 A CN 201710288315A CN 107161959 A CN107161959 A CN 107161959A
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- Prior art keywords
- nickel
- sulfuric acid
- dissolved
- distilled water
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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
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method of nickelous selenide micron tube, concretely comprise the following steps：Nickel chloride is dissolved in distilled water, ethylenediamine is added and is coordinated with nickel ion；Sodium thiosulfate is dissolved in distilled water and obtains the sodium thiosulfate aqueous solution；Above-mentioned two parts of solution is mixed and produces substantial amounts of seleno sulfuric acid triethylenediamine conjunction nickel precipitation；Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in tube furnace, lead to nitrogen, by diamond heating to 400 ~ 600 DEG C, calcination obtains the nickelous selenide micron tube of black.The preparation method of nickelous selenide micron tube of the present invention is simple, reproducible, and product has good tubular structure.
Description
Technical field
The invention belongs to inorganic material synthesis field, it is related to a kind of preparation method of nickelous selenide micron tube.
Background technology
Transient metal chalcogenide compound receives much attention because of its unique Wuli-Shili-Renli system approach.Ni-based chalcogen compound exists
There is important application in the fields such as catalytic hydrogenation, electrode material, solar cell, laser material, therefore, Ni-based chalcogen compound
Synthesis be also scientific worker research emphasis.
The content of the invention
It is an object of the invention to provide a kind of preparation method of nickelous selenide micron tube.
A kind of preparation method of nickelous selenide micron tube, it is characterised in that concretely comprise the following steps：Nickel chloride is dissolved in distilled water,
Ethylenediamine is added to be coordinated with nickel ion；Sodium thiosulfate is dissolved in distilled water and obtains the sodium thiosulfate aqueous solution；Will
Above-mentioned two parts of solution mixing produces substantial amounts of seleno sulfuric acid triethylenediamine and closes nickel precipitation；Nickel is closed before using seleno sulfuric acid triethylenediamine
Thing is driven, porcelain boat is put it into, is placed in tube furnace, leads to nitrogen, by diamond heating to 400 ~ 600 DEG C, calcination obtains black
Nickelous selenide micron tube.
The mol ratio of the nickel chloride and ethylenediamine is 1/4 ~ 1/8；The mol ratio of the nickel chloride and sodium thiosulfate is
1/1.5~1/3。
The preparation method of nickelous selenide micron tube of the present invention is simple, reproducible, and product has good tubulose knot
Structure.
Brief description of the drawings
Fig. 1 is that predecessor seleno sulfuric acid triethylenediamine closes nickel（Ni(en)3SeSO3）Scanned picture.As can be seen that forerunner
Thing Ni (en)3SeSO3With the prism structure of tubulose six, about 5.2 microns of pipe thickness, about 22.5 microns of nozzle diameter, length of tube is about
100~200 microns.
Fig. 2 is nickelous selenide（NiSe）The scanned picture of micron tube.As can be seen that NiSe micron tubes maintain predecessor Ni
(en)3SeSO3Pattern.
Fig. 3 is the XRD of NiSe micron tubes.As can be seen that NiSe micron tubes are simple hexagonal phase crystal structure.
Embodiment
For a better understanding of the present invention, illustrated by embodiment：
Embodiment 1：
Weigh 0.1mol nickel chlorides to be dissolved in 25mL distilled water, add 0.4mol ethylenediamines and be coordinated with nickel ion.Meanwhile, will
0.15mol sodium thiosulfates are dissolved in other portion 25mL distilled water.Two parts of solution are mixed, that is, produce a large amount of pink
Seleno sulfuric acid triethylenediamine closes nickel needle shape crystal.Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in
In tube furnace, lead to nitrogen, by diamond heating to 400 DEG C, calcination obtains the nickelous selenide micron tube of black.
Embodiment 2：
Weigh 0.1mol nickel chlorides to be dissolved in 25mL distilled water, add 0.6mol ethylenediamines and be coordinated with nickel ion.Meanwhile, will
0.15mol sodium thiosulfates are dissolved in other portion 25mL distilled water.Two parts of solution are mixed, that is, produce a large amount of pink
Seleno sulfuric acid triethylenediamine closes nickel needle shape crystal.Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in
In tube furnace, lead to nitrogen, by diamond heating to 400 DEG C, calcination obtains the nickelous selenide micron tube of black.
Embodiment 3：
Weigh 0.1mol nickel chlorides to be dissolved in 25mL distilled water, add 0.8mol ethylenediamines and be coordinated with nickel ion.Meanwhile, will
0.15mol sodium thiosulfates are dissolved in other portion 25mL distilled water.Two parts of solution are mixed, that is, produce a large amount of pink
Seleno sulfuric acid triethylenediamine closes nickel needle shape crystal.Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in
In tube furnace, lead to nitrogen, by diamond heating to 400 DEG C, calcination obtains the nickelous selenide micron tube of black.
Embodiment 4：
Weigh 0.1mol nickel chlorides to be dissolved in 25mL distilled water, add 0.4mol ethylenediamines and be coordinated with nickel ion.Meanwhile, will
0.2mol sodium thiosulfates are dissolved in other portion 25mL distilled water.Two parts of solution are mixed, that is, produce a large amount of pink
Seleno sulfuric acid triethylenediamine closes nickel needle shape crystal.Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in
In tube furnace, lead to nitrogen, by diamond heating to 400 DEG C, calcination obtains the nickelous selenide micron tube of black.
Embodiment 5：
Weigh 0.1mol nickel chlorides to be dissolved in 25mL distilled water, add 0.4mol ethylenediamines and be coordinated with nickel ion.Meanwhile, will
0.3mol sodium thiosulfates are dissolved in other portion 25mL distilled water.Two parts of solution are mixed, that is, produce a large amount of pink
Seleno sulfuric acid triethylenediamine closes nickel needle shape crystal.Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in
In tube furnace, lead to nitrogen, by diamond heating to 400 DEG C, calcination obtains the nickelous selenide micron tube of black.
Embodiment 6：
Weigh 0.1mol nickel chlorides to be dissolved in 25mL distilled water, add 0.4mol ethylenediamines and be coordinated with nickel ion.Meanwhile, will
0.15mol sodium thiosulfates are dissolved in other portion 25mL distilled water.Two parts of solution are mixed, that is, produce a large amount of pink
Seleno sulfuric acid triethylenediamine closes nickel needle shape crystal.Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in
In tube furnace, lead to nitrogen, by diamond heating to 500 DEG C, calcination obtains the nickelous selenide micron tube of black.
Embodiment 7：
Weigh 0.1mol nickel chlorides to be dissolved in 25mL distilled water, add 0.4mol ethylenediamines and be coordinated with nickel ion.Meanwhile, will
0.15mol sodium thiosulfates are dissolved in other portion 25mL distilled water.Two parts of solution are mixed, that is, produce a large amount of pink
Seleno sulfuric acid triethylenediamine closes nickel needle shape crystal.Nickel is closed as predecessor using seleno sulfuric acid triethylenediamine, porcelain boat is put it into, is placed in
In tube furnace, lead to nitrogen, by diamond heating to 600 DEG C, calcination obtains the nickelous selenide micron tube of black.
Claims (2)
1. a kind of preparation method of nickelous selenide micron tube, it is characterised in that concretely comprise the following steps：Nickel chloride is dissolved in distilled water, plus
Enter ethylenediamine to be coordinated with nickel ion；Sodium thiosulfate is dissolved in distilled water and obtains the sodium thiosulfate aqueous solution；Will be upper
State two parts of solution mixing and produce substantial amounts of seleno sulfuric acid triethylenediamine conjunction nickel precipitation；Nickel is closed as forerunner using seleno sulfuric acid triethylenediamine
Thing, puts it into porcelain boat, is placed in tube furnace, leads to nitrogen, by diamond heating to 400 ~ 600 DEG C, calcination obtains the selenium of black
Change nickel micron tube.
2. preparation method as claimed in claim 1, it is characterised in that the mol ratio of the nickel chloride and ethylenediamine is 1/4 ~ 1/
8；The mol ratio of the nickel chloride and sodium thiosulfate is 1/1.5 ~ 1/3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710288315.4A CN107161959A (en) | 2017-04-27 | 2017-04-27 | A kind of preparation method of nickelous selenide micron tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710288315.4A CN107161959A (en) | 2017-04-27 | 2017-04-27 | A kind of preparation method of nickelous selenide micron tube |
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| Publication Number | Publication Date |
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| CN107161959A true CN107161959A (en) | 2017-09-15 |
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ID=59812645
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710288315.4A Pending CN107161959A (en) | 2017-04-27 | 2017-04-27 | A kind of preparation method of nickelous selenide micron tube |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107818873A (en) * | 2017-10-10 | 2018-03-20 | 安阳师范学院 | Cellular nickelous selenide nano-chip arrays electrode material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049917A (en) * | 2007-03-29 | 2007-10-10 | 上海交通大学 | Method for preparing Nano nickelous diselenide in hexagon |
| CN102583273A (en) * | 2012-02-13 | 2012-07-18 | 安徽大学 | Method for preparing nano nickel selenide with octahedral structure |
| CN103043630A (en) * | 2013-01-11 | 2013-04-17 | 长沙理工大学 | Preparation method of spherical nickel diselenide powder |
| CN103466563A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution |
-
2017
- 2017-04-27 CN CN201710288315.4A patent/CN107161959A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049917A (en) * | 2007-03-29 | 2007-10-10 | 上海交通大学 | Method for preparing Nano nickelous diselenide in hexagon |
| CN102583273A (en) * | 2012-02-13 | 2012-07-18 | 安徽大学 | Method for preparing nano nickel selenide with octahedral structure |
| CN103043630A (en) * | 2013-01-11 | 2013-04-17 | 长沙理工大学 | Preparation method of spherical nickel diselenide powder |
| CN103466563A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution |
Non-Patent Citations (1)
| Title |
|---|
| ZHONGBIN ZHUANG ET AL.: "Controlled Hydrothermal Synthesis and Structural Characterization of a Nickel Selenide Series", 《CHEMISTRY A EUROPEAN JOURNAL》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107818873A (en) * | 2017-10-10 | 2018-03-20 | 安阳师范学院 | Cellular nickelous selenide nano-chip arrays electrode material and preparation method thereof |
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Application publication date: 20170915 |