CN108358208A - A kind of preparation method of the silicide of nanometer calcium - Google Patents

A kind of preparation method of the silicide of nanometer calcium Download PDF

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Publication number
CN108358208A
CN108358208A CN201810396815.4A CN201810396815A CN108358208A CN 108358208 A CN108358208 A CN 108358208A CN 201810396815 A CN201810396815 A CN 201810396815A CN 108358208 A CN108358208 A CN 108358208A
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silicide
calcium
preparation
powder
added
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CN201810396815.4A
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萨百晟
庞旗旗
熊锐
陈建辉
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Fuzhou University
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Fuzhou University
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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
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/06—Metal silicides
    • 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
    • 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
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • 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
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses a kind of preparation methods of the silicide of nanometer calcium, in nitrogen atmosphere, the magnesium chloride of equal proportion are added into the autoclave of stainless steel and sodium chloride and it is made uniformly to mix；Then Si powder, calcium chloride, metallic potassium is added, is uniformly mixed；Autoclave is sealed, heats 8 ~ 10 hours, then cools to room temperature in 600 ~ 700 DEG C in stove；It is washed respectively with hydrochloric acid, dilute alkaline soln, distilled water and absolute ethyl alcohol, to remove impurity；Obtained substance is placed in 50 ~ 60 DEG C of vacuum drying chamber dry 10 ~ 12 hours and obtains powder sample.The silicide of the powdered calcium of the present invention, product purity is higher, and preparation method is easy to operate, product component is easy to control, and the silicide material of obtained calcium, which is expected to apply, can be widely applied to every field.

Description

A kind of preparation method of the silicide of nanometer calcium
Technical field
The invention belongs to the silicide preparation fields of calcium, and in particular to a kind of preparation method of the silicide of nanometer calcium.
Background technology
In recent decades, intermetallic compound is since it is with peculiar performance and in metallurgical technology, chemical engineering, boat The potential utilization of its aviation field so that intermetallic compound is widely studied.In these intermetallic compounds, Ca-Si gold Compound is also a kind of mostly important intermetallic compound between category because its be widely used in thermoelectricity, photoelectric material and For designing novel electronic equipment.The calcium silicon of the current preparation that succeeded has Ca2Si、Ca5Si3、CaSi、Ca3Si4、 CaSi2Deng.Ca in this kind of material2Si、Ca3Si4、CaSi2These three calcium silicons are semi-conducting materials, wherein Ca2Si with Mg2Si shows huge potential applying value similar to them in thermoelectric material field, and Ca3Si4、CaSi2Both semiconductors It is widely used in photoelectronic device.And Ca5Si3Metalline is shown with the silicide of CaSi both calcium, reports this recently The silicide of two kinds of calcium is a kind of hydrogen storage material well, is the candidate of follow-on hydrogen storage material.However most importantly Ca elements and the element silicon rich content and environmentally safe in the earth, therefore the silicide of calcium is a kind of fine environmentally friendly material Material.
It, can be along with Ca in preparation process because of the presence of a variety of phases of Ca-Si bianry alloys5Si3The silicide life of equal calcium At.The silicide of calcium is prepared by chemical reaction by the ratio of stringent control reactant by the present invention.It is prepared by the present invention Method is simple, and cost of material is low, it is more likely that industrialization, and the silicide grain for the calcium being prepared can more carefully reach nanometer Rank.
Invention content
The purpose of the present invention is providing a kind of preparation method of the silicide of nanometer calcium.The silication of the powdered calcium of the present invention Object, product purity is higher, and preparation method is easy to operate, product component is easy to control, and the silicide material of obtained calcium has Prestige is widely used in every field.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of the silicide of nanometer calcium, specifically includes following steps：
(1) in nitrogen atmosphere, into stainless steel autoclave be added equal quality ratio magnesium chloride and sodium chloride and make its uniformly Mixing；
(2) continue that 0.005 ~ 0.04 mol Si powder is added into stainless steel autoclave, be uniformly mixed；
(3) calcium chloride of 0.01 ~ 0.03 mol is added in above-mentioned uniformly mixed powder；
(4) metallic potassium of 0.8 ~ 1.6 g is put into the uniform mixed-powder obtained in step (3)；
(5) stainless steel autoclave is sealed, heats 8 ~ 10 hours, then cools to room temperature in 600 ~ 700 DEG C in stove；
(6) it is washed respectively with hydrochloric acid, dilute alkaline soln, distilled water and absolute ethyl alcohol, to remove impurity；
(7) substance obtained in step (6) is placed in 50 ~ 60 DEG C of vacuum drying chamber dry 10 ~ 12 hours and obtains powder Last sample.
The dosage of magnesium chloride and sodium chloride is 10g in step (1).
The metallic potassium used in step (4) is graininess, and particle is answered as small as possible, and the diameter range of particle is 0.05 ~0.1 cm。
Dilute alkaline soln used in step (6) is the sodium hydroxide solution of a concentration of 0.1M.
The chemical formula of the silicide of nanometer calcium obtained is Ca2Si, CaSi or CaSi2。
The beneficial effects of the present invention are：The present invention is with simple for process, operation is easy, at low cost and product component is easily-controllable The advantages such as system, the silicide of powdered calcium of the invention, product purity is higher, and preparation method is easy to operate, product component Easy to control, the silicide material of obtained calcium, which is expected to apply, can be widely applied to every field.
The effect of magnesium chloride and sodium chloride is that inorganic solvent, the hot method of inorganic solvent have the characteristics that a series of the most：It provides Media environment, the solvent of liquid there is mass-and heat-transfer in outstanding solvability, chemical reaction process to pass energy speed other substances Rate it is fast it is efficient, reaction temperature is low, product purity is high, granularity is small and be evenly distributed, solvent it is easy to clean.The work of metallic potassium is used as Can fully be reacted to be contacted with reactant uniformly for reducing agent.
Description of the drawings
Fig. 1 is Ca2The XRD diagram of Si；
Fig. 2 is Ca2The SEM of Si schemes；
Fig. 3 is the XRD diagram of CaSi；
The SEM that Fig. 4 is CaSi schemes;
Fig. 5 is CaSi2XRD diagram；
Fig. 6 is CaSi2SEM figure.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
（1）In nitrogen atmosphere, 10g magnesium chlorides and 10g sodium chloride powders are added into stainless steel autoclave, it is made to be uniformly mixed Be uniformly mixed powder.
（2）To step（1）The Si powder of 0.005mol is added in the homogeneously mixed product of middle gained, it is made uniformly to mix.
（3）To step（2）In the calcium chloride of 0.01mol is added in obtained uniform mixed-powder.
（4）To step（3）In the metal k particle of 0.8g is added in obtained uniform mixed-powder, autoclave is sealed, It heats 8 hours, then cools to room temperature in 700 DEG C in stove.
（5）It is washed respectively with 0.1M hydrochloric acid, 0.1M sodium hydroxide solutions, distilled water and absolute ethyl alcohol, to remove impurity.
（6）By step（5）In obtained substance be placed in 50 DEG C of vacuum drying chamber dry 10 hours and obtain powder sample.
The XRD of the powder arrived in this example is as shown in Figure 1, the chemical formula of the silicide of calcium obtained is Ca2Si, grain size are big Small about 50nm ~ 300nm.
Embodiment 2
（1）In nitrogen atmosphere, 10g magnesium chlorides and 10g sodium chloride are added into stainless steel autoclave, so that it is uniformly mixed and obtains Uniform mixed-powder.
（2）To step（1）The Si powder of 0.01mol is added in the uniform mixed-powder of middle gained, stirs evenly.
（3）To step（2）In the calcium chloride solution of 0.01mol be added in obtained homogeneous mixture solotion and stir evenly.
（4）To step（3）In the metallic potassium of 0.8g is added in obtained homogeneous mixture solotion, autoclave is sealed, in stove Interior 650 DEG C are heated 9 hours, are then cooled to room temperature.
（5）It is washed respectively with 0.1M hydrochloric acid, 0.1M sodium hydroxide solutions, distilled water and absolute ethyl alcohol, to remove impurity.
（6）By step（5）In obtained substance be placed in 60 DEG C of vacuum drying chamber dry 12 hours and obtain powder sample.
For the XRD of the powder arrived in this example as shown in figure 3, the chemical formula of the silicide of calcium obtained is CaSi, grain size is big Small about 50nm ~ 200nm.
Embodiment 3
（1）In nitrogen atmosphere, 10g magnesium chlorides and 10g sodium chloride powders are added into stainless steel autoclave, it is made to be uniformly mixed Be uniformly mixed powder.
（2）To step（1）The Si powder of 0.02mol is added in the uniform mixed-powder of middle gained, stirs evenly.
（3）To step（2）In the calcium chloride solution of 0.01mol be added in obtained uniform mixed-powder and stir evenly.
（4）To step（3）In the metallic potassium of 0.8g is added in obtained homogeneous mixture solotion, autoclave is sealed, in stove Interior 600 DEG C are heated 10 hours, are then cooled to room temperature.
（5）It is washed respectively with 0.1M hydrochloric acid, 0.1M sodium hydroxide solutions, distilled water and absolute ethyl alcohol, to remove impurity.
（6）By step（5）In obtained substance be placed in 60 DEG C of vacuum drying chamber dry 12 hours and obtain powder sample
The XRD of the powder arrived in this example is as shown in figure 5, the chemical formula of the silicide of calcium obtained is CaSi2, particle size is about For 50nm ~ 300nm.
Embodiment 4
（1）In nitrogen atmosphere, 10g magnesium chlorides and 10g sodium chloride powders are added into the autoclave of stainless steel, keeps its mixing equal The even powder that is uniformly mixed.
（2）To step（1）The Si powder of 0.02mol is added in the homogeneously mixed product of middle gained, it is made uniformly to mix.
（3）To step（2）In the calcium chloride of 0.01mol is added in obtained uniform mixed-powder.
（4）To step（3）In the metallic potassium of 1.6g is added in obtained uniform mixed-powder, autoclave is sealed, in stove Interior 550 DEG C are heated 10 hours, are then cooled to room temperature.
（5）It is washed respectively with 0.1M hydrochloric acid, 0.1M sodium hydroxide solutions, distilled water and absolute ethyl alcohol, to remove impurity.
（6）By step（5）In obtained substance be placed in 60 DEG C of vacuum drying chamber dry 10 hours and obtain powder sample.
Embodiment 5
（1）In nitrogen atmosphere, 10g magnesium chlorides and 10g sodium chloride powders are added into the autoclave of stainless steel, keeps its mixing equal The even powder that is uniformly mixed.
（2）To step（1）The Si powder of 0.04mol is added in the homogeneously mixed product of middle gained, it is made uniformly to mix.
（3）To step（2）In the calcium chloride of 0.02mol is added in obtained uniform mixed-powder.
（4）To step（3）In the metallic potassium of 1.6g is added in obtained uniform mixed-powder, autoclave is sealed, in stove Interior 600 DEG C are heated 10 hours, are then cooled to room temperature.
（5）It is washed respectively with 0.1M hydrochloric acid, 0.1M sodium hydroxide solutions, distilled water and absolute ethyl alcohol, to remove impurity.
（6）By step（5）In obtained substance be placed in 60 DEG C of vacuum drying chamber dry 10 hours and obtain powder sample.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification should all belong to the covering scope of the present invention.

Claims (5)

1. a kind of preparation method of the silicide of nanometer calcium, it is characterised in that：Specifically include following steps：
(1) in nitrogen atmosphere, into stainless steel autoclave be added equal quality ratio magnesium chloride and sodium chloride and make its uniformly Mixing；
(2) continue that 0.005 ~ 0.04 mol Si powder is added into stainless steel autoclave, be uniformly mixed；
(3) calcium chloride of 0.01 ~ 0.03 mol is added in above-mentioned uniformly mixed powder；
(4) metallic potassium of 0.8 ~ 1.6 g is put into the uniform mixed-powder obtained in step (3)；
(5) stainless steel autoclave is sealed, heats 8 ~ 10 hours, then cools to room temperature in 600 ~ 700 DEG C in stove；
(6) it is washed respectively with hydrochloric acid, dilute alkaline soln, distilled water and absolute ethyl alcohol, to remove impurity；
(7) substance obtained in step (6) is placed in 50 ~ 60 DEG C of vacuum drying chamber dry 10 ~ 12 hours and obtains powder Last sample.
2. preparation method according to claim 1, it is characterised in that：The dosage of magnesium chloride and sodium chloride in step (1) It is 10g.
3. preparation method according to claim 1, it is characterised in that：The metallic potassium used in step (4) is graininess, The diameter range of particle is in 0.05 ~ 0.1 cm.
4. preparation method according to claim 1, it is characterised in that：Dilute alkaline soln used in step (6) is a concentration of The sodium hydroxide solution of 0.1M.
5. according to any preparation methods of claim 1-4, it is characterised in that：The chemistry of the silicide of nanometer calcium obtained Formula is Ca2Si, CaSi or CaSi2。
CN201810396815.4A 2018-04-28 2018-04-28 A kind of preparation method of the silicide of nanometer calcium Pending CN108358208A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244814A (en) * 2007-02-13 2008-08-20 深圳市比克电池有限公司 Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material
CN101619403A (en) * 2009-07-23 2010-01-06 上海交通大学 Method for removing silicon out of aluminium alloy
CN106116587A (en) * 2016-06-22 2016-11-16 福州大学 A kind of Emission in Cubic Ca2si thermoelectric material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244814A (en) * 2007-02-13 2008-08-20 深圳市比克电池有限公司 Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material
CN101619403A (en) * 2009-07-23 2010-01-06 上海交通大学 Method for removing silicon out of aluminium alloy
CN106116587A (en) * 2016-06-22 2016-11-16 福州大学 A kind of Emission in Cubic Ca2si thermoelectric material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马剑华 等: "金属硅化物纳米材料的化学合成", 《无机化学学报》 *

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