CN112974822B - Preparation method of cotton-shaped metal nickel powder - Google Patents
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Abstract
The invention discloses a preparation method of cotton-shaped metallic nickel powder, wherein the metallic nickel powder is produced by adopting a eutectic salt treatment-liquid phase leaching-magnetic separation process, the method adopts the eutectic salt containing LiCl to treat nickel chloride to obtain a eutectic material, the eutectic material is prepared into a thin disc shape to carry out diffusion reaction with lithium at high temperature to obtain reaction clinker, and the reaction clinker is screened out by the liquid phase leaching and magnetic separation processes. The prepared metallic nickel powder has the size of 100nm-10 mu m and is flocculent metallic nickel powder. The method has the advantages of simple preparation process, controllable process, good stability, mass production and suitability for macro preparation.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal nickel metallurgy, and particularly relates to a preparation method of cotton flocculent metal nickel powder.
Background
The nickel is silver metal, is positioned in the fourth stage VIII group, is distributed with peripheral electrons 3d84s2, has active chemical property, is difficult to oxidize in air, and has good magnetism, plasticity and corrosion resistance. With the development of the electronic industry, particularly the wide application of high-nickel anode materials in batteries, nickel powder has become the primary raw material of many electrode materials, particularly the requirement of aerospace power supplies for nickel anode materials, and the square nickel powder with higher surface energy has a wider application prospect.
At present, the preparation method of high-purity nickel powder mainly comprises a reduction method, an electrolysis method, a carbonyl decomposition method and an atomization method. Among them, powders produced by electrolysis and atomization are widely used as raw materials in the metallurgical industry. The electrolysis method has high energy consumption, the particle size distribution is not easy to control, and the carbonyl decomposition method is toxic and not environment-friendly. In patent CN 105728741 a, adding a nickel salt solution and an ammonium oxalate solution into a base solution to react to obtain nickel oxalate, and reducing the nickel oxalate to obtain spherical nickel powder; patent 101837464B dissolves nickel plate in nitric acid, adopts oxalic acid to precipitate, and then uses hydrogen to reduce to prepare nickel powder; 1292866c, nickel powder is prepared by freeze-drying nickel nitrate and sodium carbonate precipitate and then performing hydrogen reduction; patent CN 100450676C adopts a liquid phase method to prepare nano nickel powder by reducing nickel sulfate with sodium borohydride. CN100391663C adopts an electrolytic method preparation method to prepare nano nickel powder; US6596052B2 uses hydrogen to reduce nickel chloride to produce spherical nickel powder.
In the preparation method of the nickel powder, reports of preparing the nickel powder by eutectic salt dispersion treatment and reports of flocculent metal nickel powder are not seen.
Disclosure of Invention
The invention aims to provide a method for preparing fluffy flocculent metal nickel powder with a structure, which provides raw material selection for the design of functional materials.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a preparation method of flocculent metal nickel powder, which adopts a eutectic treatment-high temperature diffusion process-liquid phase leaching-magnetic separation process to produce nickel powder, wherein the size of the prepared metal nickel powder is 100nm-10 mu m, and the prepared metal nickel powder is flocculent metal nickel powder;
the eutectic treatment is to carry out high-temperature eutectic melting on the mixture of layered nickel chloride and molten salt to obtain a nickel-containing halogenated eutectic;
the high-temperature diffusion process is to form a diffusion reaction combination by sequentially preparing reaction materials formed by the nickel-containing halogenated eutectic, molten salt and lithium alloy, and putting the diffusion reaction combination into a high-temperature inert protective atmosphere environment for diffusion reaction; the reaction materials form reaction clinker;
the liquid-phase leaching is to soak the reaction clinker with water or acid solution, stir and disperse to obtain suspension;
the magnetic separation process is to adsorb and extract nickel powder from suspension by virtue of magnetic action and separate the nickel powder (by demagnetization).
As an embodiment, the eutectic treatment is to put a mixture consisting of layered nickel chloride and molten salt into a high-temperature environment, and obtain the nickel-containing halogenated eutectic with uniform components by means of high-temperature corrosion of layered nickel chloride in the reaction material of lithium chloride in the molten salt component. The high temperature is 450-650 ℃, and the heating time is 30min-2 h.
According to one embodiment, the mass ratio of the layered nickel chloride to the molten salt is 70: 30-20: 80. Too high a proportion of nickel chloride results in slow diffusion and high viscosity, while too low a proportion results in low efficiency.
According to one embodiment, the temperature of the high-temperature diffusion process is 450-650 ℃, and the heat preservation time is 1-20 hours. The temperature is a key parameter for achieving the purpose of the invention, below which the nickel-containing halogenated eutectic and the molten salt have high viscosity, slow diffusion and low efficiency, and above which the diffusion reaction combination may have safety problems, such as the molten salt has good fluidity, and the reaction blank and the anode together can have chemical reaction or thermal runaway and the like. The heat preservation time affects the yield, the product generated in too short time is little, the electric energy is wasted in too long time, and the efficiency is low.
As one embodiment, the production steps of the eutectic treatment-high temperature diffusion process-liquid phase leaching-magnetic separation process include:
s1, batching: weighing layered nickel chloride and molten salt according to the proportion of 70: 30-20: 80, and blending;
s2, eutectic melting treatment: heating the material obtained in the step S1 to form a eutectic body, wherein the heating temperature is 450-650 ℃, the heating time is 30min-2h, and placing the eutectic body in a protective atmosphere for cooling, crushing and screening to obtain a reaction material;
s3, press forming: respectively carrying out powder cold pressing on the reaction materials and the molten salt on a hydraulic press to obtain a double-layer composite blank consisting of the reaction materials and the molten salt;
s4, high-temperature diffusion process: one side of the molten salt in the double-layer composite blank is tightly attached, matched and clamped with the lithium alloy, and then quickly sent into a high-temperature furnace protected by inert atmosphere at 450-650 ℃, and cooled after heat preservation for 1-20 hours to obtain reaction clinker;
s5, liquid-phase leaching: adding the reaction clinker into water or an acid solution, and stirring, dissolving and leaching to obtain a suspension;
s6, magnetic separation: performing solid-liquid separation from the suspension by using a magnetic device, and cleaning to obtain aqueous nickel slurry;
s7, drying and grinding: and (3) unloading the water-containing nickel slurry, freeze-drying for 10-24 h at the low temperature of-50 to-10 ℃, and grinding to obtain the flocculent metallic nickel powder.
In one embodiment, in step S1, the blending is performed by physically mixing for 1-15min on a powder mixer at a rotation speed of 200-1500 r/min. The objective is to mix uniformly with additional mechanical activation, since high speed mixing generates heat, making it more uniform and more intimate.
In one embodiment, the molten salt contains 10% to 100% of lithium chloride LiCl, has a melting point of 350 ℃ to 650 ℃, and contains the balance of an alkali metal halide and an alkali metal oxysalt in steps S1 and S3.
As an embodiment, the molten salt is selected from pure LiCl, LiCl-KCl molten salt with a lithium chloride content of 45-65%, LiF-LiCl-LiBr multi-component eutectic salt with a lithium chloride content of 10-30%.
As an embodiment, the molten salt is selected from LiF-LiCl-LiBr (9.6 wt% to 22 wt% to 68.4 wt%), LiCl-LiBr-KBr (12 wt% to 36.5 wt% to 51.5 wt%), LiCl-KCl-RbCl-CsCl, LiCl-LiNO3-KNO3、CaCl2-LiCl-KCl、LiSO4-LiCl-LiBr。
In step S2, the heating temperature for heating to form the eutectic is 450-650 ℃, and the heating time is 30min-2 h. Below this temperature or time, the eutectic may not be available, or the eutectic composition is not uniform, above which temperature electricity is wasted and chlorides may sublimate, causing safety problems. The time is too long, the energy consumption is high, and the efficiency is low.
In step S2, the protective atmosphere is a multi-component mixed gas containing carbon dioxide, nitrogen, argon, and nitrogen or argon as a main phase, which is dried to have a water content of less than 10 ppm.
As an embodiment, in step S3, the pressure of the powder cold pressing is 1 to 25 Mpa; the diameter of the obtained double-layer composite blank is phi 20-120.
In one embodiment, in step S3, the thickness of the molten salt layer in the double-layer composite blank is 0.1-0.5 mm, and the thickness of the reaction material layer is 0.5-5 mm. Too thick a molten salt layer can affect the reaction rate and produce little or no product; too thin (e.g., less than 0.3mm), the double-layer composite blank is difficult to prepare; without the membrane layer, a rapid displacement reaction occurs. Therefore, the thickness of the molten salt layer is more preferably 0.3 to 0.5mm.
As one embodiment, in step S4, the lithium alloy size is smaller than the bi-layer composite billet size, and the diameter thereof is 80% to 95% of the diameter of the bi-layer composite billet. Too large a diameter causes the lithium alloy to soften at high temperature and then to overlap with the reaction blank to react, losing the meaning of preparing flocculent nickel powder by diffusion, and if too small, the efficiency is low and the preparation amount is too small.
As an embodiment, in step S4, the lithium content in the lithium alloy is greater than 30%, and the lithium alloy is mainly lithium silicon alloy, lithium boron alloy, metal-doped lithium boron alloy, or lithium carbon alloy; the doped metal in the metal-doped lithium-boron alloy comprises aluminum, magnesium, indium, tin, lead and bismuth. The lithium content is too low, the free lithium is little, and the reaction rate is slow; since the invention is made by diffusing lithium, the lithium content cannot be too low. Likewise, metallic lithium cannot be used because it is in a liquid phase at high temperature and has too good fluidity, so that it is necessary to use an alloy to restrict the flow of lithium. Preferably, the lithium content in the lithium alloy is 30-85%.
As an embodiment, in step S4, the inert gas is selected from argon gas or argon-hydrogen mixed gas having a hydrogen content of less than 4%.
In one embodiment, in step S5, the reaction clinker is added to water or an acidic solution at a liquid-to-solid ratio of 10:1 to 40: 1.
As an embodiment, in step S6, the magnetic device includes a magnet, an electromagnet, or the like.
In the step S7, the hydrous nickel slurry is subjected to freeze drying for 10-24 hours at a low temperature of-50 to-10 ℃ after being discharged; is a key parameter for achieving the purpose of the invention. Under the condition, the property of nickel can be ensured by freeze drying to remove water. And is generally controlled by a vacuum pump, and the control is mostly 20Pa to 100 Pa. As a specific implementation case, the pre-freezing temperature is 50 ℃ below zero for 2 hours, then the temperature is slowly raised to 25 ℃ below zero, the freeze drying is carried out for 20 hours at 20pa, and finally the water is discharged after the desorption.
Compared with the prior art, the invention has the following beneficial effects:
1) the method adopts the co-melting treatment-high temperature diffusion process-liquid phase leaching-magnetic separation process to prepare the flocculent metal nickel powder, the prepared nickel powder has good chemical stability, high process availability, simple equipment and small investment, and is suitable for batch production;
2) the produced metal nickel powder is of a fluffy cotton-shaped structure, is suitable for the structure and the components of a directional control material, and is expected to be used in the fields of electrocatalysis and electric energy sources in a large scale.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a SEM image of layered nickel chloride;
FIG. 2 is a flow chart of a eutectic treatment-high temperature diffusion process-liquid phase leaching-magnetic separation process;
FIG. 3 is an XRD pattern of the flocculent metallic nickel powder;
FIG. 4 is an SEM image of the flocculent metallic nickel powder;
FIG. 5 is a TEM photograph of flocculent metallic nickel powders.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
The raw material adopted by the invention is the layered nickel chloride, which refers to anhydrous nickel chloride after high-temperature roasting, or sublimed nickel chloride, and is characterized by no crystal water and layered structure.
In the following examples, layered nickel chloride was prepared as follows:
(1) drying commercially available nickel chloride hexahydrate for 12 hours at the temperature of 200-;
(2) placing anhydrous nickel chloride in a high-temperature environment of 800-900 ℃ for 2h to obtain the flocculent sublimed nickel chloride and golden yellow nickel chloride which are layered nickel chloride. As can be seen from the SEM image (fig. 1), the nickel chloride obtained after two high-temperature treatments has a layered structure.
Example 1 Using NiCl2the/LiF-LiCl-LiBr/LiB alloy molten salt system is used for preparing nickel powder with a regular cotton-like structure, as shown in figure 2.
(1) And (4) batching. Weighing layered nickel chloride and molten salt according to a ratio of 60:40, and physically mixing the layered nickel chloride and the molten salt on a powder mixer at a rotating speed of 800r/min for 1-15 min. The molten salt component is LiF-LiCl-LiBr (9.6 wt% -22 wt% -68.4 wt%) halide eutectic salt with 22% LiCl content, and the melting point is about 443 ℃.
(2) And (5) carrying out eutectic treatment. Putting the mixture of layered nickel chloride and LiF-LiCl-LiBr eutectic salt into a quartz crucible, heating the mixture in a well-type furnace to form eutectic, wherein the heating temperature is 550 ℃, the heating time is 1h, placing the eutectic in nitrogen with the water content of less than 10ppm for cooling, and crushing and screening the eutectic by a crusher to obtain a reaction material.
(3) And (5) pressing and forming. And (3) respectively carrying out powder cold pressing on the reaction materials and LiF-LiCl-LiBr fused salt on a hydraulic press under the pressure of 10Mpa to obtain a phi 60 double-layer composite blank consisting of the reaction materials and the fused salt, wherein the thickness of the fused salt layer in the composite blank is 0.5mm, and the thickness of the reaction material layer is 3 mm.
(4) And (4) performing a high-temperature diffusion process. One side of the molten salt in the composite blank is closely matched with the lithium alloy, and the lithium alloy is lithium boron alloy with the lithium content of 55 percent, the diameter phi 55 is about 90 percent of the diameter of the composite blank. And (3) after the materials are matched and clamped, quickly sending the materials into a high-temperature furnace protected by inert gas argon at 550 ℃, preserving heat for 5 hours, and cooling to obtain reaction clinker.
(5) Liquid phase leaching. Adding water into the reaction clinker according to the liquid-solid ratio of 10:1, and stirring, dissolving and leaching to obtain suspension.
(6) And (5) magnetic separation. And (3) carrying out solid-liquid separation from the suspension by adopting a U-shaped magnet, and repeatedly cleaning the magnet absorbed matter for three times to obtain the water-containing nickel slurry.
(7) Drying and grinding. The aqueous slurry is discharged and then is analyzed and discharged at the temperature of between 50 ℃ below zero and 10 ℃ below zero (between 50 ℃ below zero and 10 ℃ below zero), specifically, in the embodiment, the pre-freezing temperature is firstly between 50 ℃ below zero and 50 ℃ below zero for 2 hours, then the temperature is slowly increased to 25 ℃ below zero, 20pa is used for freeze drying for 18 hours, and finally the analyzed and discharged water is subjected to freeze drying for 20 hours, and the flocculent metallic nickel powder is obtained after grinding. FIGS. 3 to 5 are XRD, SEM and TEM images of metallic nickel powder for preparing fluffy cotton wool structure, respectively; as can be seen from fig. 3, XRD analysis shows that the obtained product has only the characteristic peak of metallic nickel powder, and does not contain other miscellaneous peaks, indicating that the product has only metallic nickel powder. As can be seen from fig. 4, the morphology of the product is cotton-wool-shaped, and as can be seen from the high-power transmission analysis in fig. 5, the obtained product is a nickel (111) crystal face, the lattice spacing is 0.20nm, and the product is further proved to be nickel metal.
Example 2 use of NiCl2Preparing nickel powder with a regular cotton-shaped structure by using a LiCl-LiBr-KBr/LiSi alloy molten salt system.
(1) And (4) batching. Weighing layered nickel chloride and molten salt according to a ratio of 50:50, and physically mixing for 4min on a powder mixer at a rotating speed of 700 r/min. The molten salt component is LiCl-LiBr-KBr (12. wt% -36.5 wt% -51.5 wt%) halide eutectic salt with 12% LiCl content, and the melting point is about 310 ℃.
(2) And (5) carrying out eutectic treatment. Putting a mixture of layered nickel chloride and LiCl-LiBr-KBr molten salt into a quartz crucible, heating the mixture in a well type furnace to form a eutectic body, wherein the heating temperature is 450 ℃, the heating time is 1h, placing the eutectic body in argon with the water content of less than 10ppm for cooling, and crushing and screening the eutectic body by a crusher to obtain a reaction material.
(3) And (5) pressing and forming. And respectively carrying out powder cold pressing on the reaction materials and LiCl-LiBr-KBr fused salt on a hydraulic press under the pressure of 7Mpa to obtain a double-layer composite blank with the diameter of phi 45 and consisting of the reaction materials and the fused salt, wherein the thickness of the fused salt layer in the composite blank is 0.45mm, and the thickness of the reaction material layer is 2 mm.
(4) And (4) performing a high-temperature diffusion process. One side of the molten salt in the composite blank is closely matched with the lithium alloy, the lithium alloy is a lithium silicon alloy with the lithium content of 45%, and the lithium silicon alloy is pressed into a circular sheet with the diameter phi 42 by adopting powder. And after the materials are matched and clamped, the materials are quickly sent into a high-temperature furnace with the protection of inert gas argon at 450 ℃, and after heat preservation is carried out for 5 hours, the materials are cooled to obtain reaction clinker.
(5) Liquid phase leaching. Adding water into the reaction clinker according to the liquid-solid ratio of 10:1, and stirring, dissolving and leaching to obtain suspension.
(6) And (5) magnetic separation. And (3) carrying out solid-liquid separation from the suspension by adopting a U-shaped magnet, and repeatedly cleaning the magnet absorbed matter for three times to obtain the water-containing nickel slurry.
(7) Drying and grinding. And (3) unloading the aqueous slurry, freeze-drying for 20h at the low temperature of-50 to-10 ℃, and grinding to obtain the flocculent metallic nickel powder.
Example 3 use of NiCl2Preparing nickel powder with a regular cotton-shaped structure by using a LiCl-LiBr-KBr/metal doped LiB alloy molten salt system.
(1) And (4) batching. Weighing layered nickel chloride and molten salt according to a ratio of 75:25, and physically mixing for 6min on a powder mixer at a rotating speed of 600 r/min. The molten salt component is LiF-LiCl-LiBr (9.6 wt% -22 wt% -68.4 wt%) halide eutectic salt with 22% LiCl content, and the melting point is about 443 ℃.
(2) And (5) carrying out eutectic treatment. Putting a mixture of layered nickel chloride and LiF-LiCl-LiBr molten salt into a quartz crucible, heating the mixture in a well-type furnace to form a eutectic body, wherein the heating temperature is 500 ℃, the heating time is 1h, placing the eutectic body in argon with the water content of less than 10ppm for cooling, and crushing and screening the eutectic body by a crusher to obtain a reaction material.
(3) And (5) pressing and forming. And respectively carrying out powder cold pressing on the reaction materials and LiCl-LiBr-KBr fused salt on a hydraulic press under the pressure of 14Mpa to obtain a phi 70 double-layer composite blank consisting of the reaction materials and the fused salt, wherein the thickness of the fused salt layer in the composite blank is 0.55mm, and the thickness of the reaction material layer is 3.5 mm.
(4) And (4) performing a high-temperature diffusion process. One side of the molten salt in the composite blank is closely matched with a lithium alloy, wherein the lithium alloy adopts a lithium boron alloy with the lithium content of 55 percent, the aluminum content of 1 percent and the magnesium content of 4 percent, and a round piece with the diameter phi 65 of the lithium boron alloy. And after the materials are matched and clamped, the materials are quickly sent into a high-temperature furnace protected by inert gas argon at 480 ℃, and after heat preservation is carried out for 5 hours, the materials are cooled to obtain reaction clinker.
(5) Liquid phase leaching. Adding water into the reaction clinker according to the liquid-solid ratio of 12:1, and stirring, dissolving and leaching to obtain suspension.
(6) And (5) magnetic separation. And (3) carrying out solid-liquid separation from the suspension by adopting a U-shaped magnet, and repeatedly cleaning the magnet absorbed matter for three times to obtain the water-containing nickel slurry.
(7) Drying and grinding. And (3) unloading the aqueous slurry, freeze-drying for 20h at the low temperature of-50 to-10 ℃, and grinding to obtain the flocculent metallic nickel powder.
In conclusion, the metallic nickel powder with a flocculent structure can be obtained by adopting the method of the invention. Moreover, the flocculent metal nickel powder has a fluffy structure, a large specific surface area and high powder pressing performance. However, the flocculent metallic nickel powder has a special morphology, plays an important role in material chemistry, electrode materials and catalytic material design, can effectively regulate and control the morphology of the material, and ensures the stability of the material structure.
The preparation of the flocculent metal nickel powder can be realized by adjusting the process parameters according to the content of the invention, and the appearance basically consistent with the appearance of the invention is shown by tests. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. A method for preparing flocculent metallic nickel powder is characterized in that the nickel powder is produced by adopting a eutectic treatment-high temperature diffusion process-liquid phase leaching-magnetic separation process, the size of the prepared metallic nickel powder is 100nm-10 mu m, and the metallic nickel powder is flocculent;
the eutectic treatment is to carry out high-temperature eutectic melting on the mixture of layered nickel chloride and molten salt to obtain a nickel-containing halogenated eutectic;
the high-temperature diffusion process is to form a diffusion reaction combination by pairing reaction materials formed by the nickel-containing halogenated eutectic, molten salt and lithium alloy in sequence, and put the diffusion reaction combination into a high-temperature inert protective atmosphere environment for diffusion reaction; the reaction materials form reaction clinker;
the liquid-phase leaching is to soak the reaction clinker with water or acid solution, stir and disperse to obtain suspension;
the magnetic separation process is to adsorb, extract and separate nickel powder from suspension by means of magnetic action.
2. The method for preparing flocculent metallic nickel powder according to claim 1, wherein the eutectic process-high temperature diffusion process-liquid phase leaching-magnetic separation process production steps comprise:
s1, batching: weighing layered nickel chloride and molten salt according to the proportion of 70: 30-20: 80, and blending;
s2, eutectic melting treatment: heating the material obtained in the step S1 to form a eutectic body, wherein the heating temperature is 450-650 ℃, the heating time is 30min-2h, and placing the eutectic body in a protective atmosphere for cooling, crushing and screening to obtain a reaction material;
s3, press forming: carrying out powder cold pressing on the reaction materials and the molten salt on a hydraulic press to obtain a double-layer composite blank consisting of the reaction materials and the molten salt;
s4, high-temperature diffusion process: one side of the molten salt in the double-layer composite blank is tightly attached, matched and clamped with the lithium alloy, and then quickly sent into a high-temperature furnace protected by inert atmosphere at 450-650 ℃, and cooled after heat preservation for 1-20 hours to obtain reaction clinker;
s5, liquid-phase leaching: adding the reaction clinker into water or an acid solution, and stirring, dissolving and leaching to obtain a suspension;
s6, magnetic separation: performing solid-liquid separation from the suspension by using a magnetic device, and cleaning to obtain aqueous nickel slurry;
s7, drying and grinding: and (3) unloading the water-containing nickel slurry, freeze-drying for 10-24 h at the low temperature of-50 to-10 ℃, and grinding to obtain the flocculent metallic nickel powder.
3. The method for preparing nickel powder of flocculent metal according to claim 2, wherein in step S1 and step S3, the molten salt contains 10% to 100% of lithium chloride LiCl, has a melting point of 350 ℃ to 650 ℃, and the balance is mainly alkali metal halide and alkali metal oxysalt.
4. The method for preparing flocculent metallic nickel powder according to claim 3, wherein said molten salt is selected from pure LiCl, LiCl-KCl molten salt having a lithium chloride content of 45-65%, LiF-LiCl-LiBr multi-component eutectic salt having a lithium chloride content of 10-30%.
5. The method for preparing flocculent metallic nickel powder according to claim 3, wherein said molten salt is selected from the group consisting of LiF-LiCl-LiBr, LiCl-LiBr-KBr, LiCl-KCl-RbCl-CsCl, LiCl-LiNO3-KNO3、CaCl2-LiCl-KCl、LiSO4-LiCl-LiBr。
6. The method for producing flocculent metallic nickel powder according to claim 2, wherein in step S2, the protective atmosphere is a multi-component mixed gas having carbon dioxide, nitrogen, argon and nitrogen or argon as a main phase, which is dried and has a water content of less than 10 ppm.
7. The method for preparing flocculent metallic nickel powder according to claim 2, wherein in step S3, the thickness of the molten salt layer in the double-layered composite billet is 0.1 to 0.5mm, and the thickness of the reaction material layer is 0.5 to 5mm.
8. The method for preparing flocculent metallic nickel powder according to claim 2, wherein in step S4, the size of the lithium alloy is smaller than the size of the double-layered composite billet and is 80% to 95% of the size of the double-layered composite billet.
9. The method for preparing flocculent metallic nickel powder according to claim 2, wherein in step S4, the lithium content in the lithium alloy is greater than 30%, and the lithium alloy is mainly lithium silicon alloy, lithium boron alloy, metal-doped lithium boron alloy, or lithium carbon alloy; the doped metal in the metal-doped lithium-boron alloy comprises aluminum, magnesium, indium, tin, lead and bismuth.
10. The method for producing flocculent metallic nickel powder according to claim 2, wherein in step S4, the inert gas used in the inert atmosphere is selected from argon gas or argon-hydrogen mixed gas having a hydrogen content of less than 4%.
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| CN104625081B (en) * | 2015-01-26 | 2017-02-01 | 北京科技大学 | Method for preparing aluminum alloy powder through salt melting method |
| CN108011091B (en) * | 2017-12-05 | 2020-08-14 | 桂林电器科学研究院有限公司 | Method for preparing ferrosilicon powder by coating magnesium-silicon-iron particles with indium-bismuth alloy and ferrosilicon powder |
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