CN110961658A - Preparation method of iron-doped superfine nickel powder - Google Patents
Preparation method of iron-doped superfine nickel powder Download PDFInfo
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- CN110961658A CN110961658A CN201811139447.1A CN201811139447A CN110961658A CN 110961658 A CN110961658 A CN 110961658A CN 201811139447 A CN201811139447 A CN 201811139447A CN 110961658 A CN110961658 A CN 110961658A
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Abstract
The invention discloses a preparation method of iron-doped superfine nickel powder, which comprises the steps of mixing a first precipitator and Fe3O4Adding powder into a reaction kettle, heating the reaction kettle, adding nickel salt, a second precipitator and a surfactant into the reaction kettle, controlling the feeding flow of the nickel salt and the second precipitator to keep the pH value of a reaction system at 7.2-9.2, and obtaining the coated Fe3O4Then wrapping Fe3O4Carrying out high-temperature hydrogen reduction on the basic nickel salt powder to obtain iron-doped superfine nickel powder; thus, the invention is doped in the process of preparing the basic nickel salt precursor and then wraps Fe3O4The basic nickel salt precursor is calcined at high temperature, so that the phenomenon of uneven mixing of iron-nickel composite powder can be effectively avoided, the obtained iron-doped superfine nickel powder has good uniformity, and the performances of conductive shielding, microwave absorption and the like of the nickel powder can be enhanced to be applied to composite materials.
Description
Technical Field
The invention belongs to the technical field of nickel powder preparation, and particularly relates to a preparation method of iron-doped superfine nickel powder.
Background
The superfine nickel powder is a good electric and magnetic heat sensitive material, and has wide application prospect in the aspects of catalysts, magnetic materials, sintering activators, conductive slurry, battery materials, hard alloy binders and the like.
At present, in many alloy aspects, the iron-nickel composite powder is mixed with iron powder for use, the traditional manufacturing method of the iron-nickel composite powder comprises a mechanical mixing method and an atomization method, and the iron-nickel composite powder manufactured by the two methods is not uniformly mixed, so that more defects exist in the alloy easily, and the service life of the alloy is influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of iron-doped superfine nickel powder.
The invention provides a preparation method of iron-doped superfine nickel powder, which is implemented by the following steps:
step 1, adding a first precipitator into a reaction kettle to serve as a base solution, stirring the base solution at a stirring frequency of 25Hz, and adding Fe into the first precipitator3O4Powder is stirred for 30-60 min to the Fe3O4Dispersing powder into a first precipitator, heating the reaction kettle to 60-70 ℃ and keeping the temperature constant, adding nickel salt, a second precipitator and a surfactant into the reaction kettle, controlling the feeding flow of the nickel salt and the second precipitator to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3-5 h to obtain coated Fe3O4The basic nickel salt precursor;
step 2, adopting pure water to coat the Fe obtained in the step 13O4The basic nickel salt precursor is washed and then entersDrying to obtain coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The basic nickel salt powder is crushed by airflow and then is reduced by high-temperature hydrogen to obtain the iron-doped superfine nickel powder.
In the scheme, Fe added in the step 13O4The mass ratio of the powder to the nickel salt is 1: 50-2: 50.
In the above scheme, the nickel salt in step 1 is one of a nickel nitrate solution, a nickel sulfate solution or a nickel chloride solution.
In the scheme, the nickel content of the nickel salt in the step 1 is 2mol/L, and the feeding flow rate of the nickel salt is 200L/H.
In the above scheme, in step 1, the first precipitant and the second precipitant are both one of sodium carbonate, ammonium bicarbonate, ammonium carbonate or sodium hydroxide.
In the scheme, the volume of the first precipitator added in the step 1 is 400-500L, and the concentration of the first precipitator is 0.05 mol/L.
In the scheme, the volume ratio of the second precipitator to the nickel salt added in the step 1 is 1.8: 1-2.5: 1, the concentration of the second precipitator is 2mol/L, and the feeding flow rate of the second precipitator is 400L/H.
In the above scheme, the surfactant in step 1 is one of (L) -tartaric acid, citric acid or oxalic acid.
In the scheme, the volume of the surfactant added in the step 1 is 8-16L.
In the scheme, the reduction temperature of the high-temperature hydrogen reduction in the step 3 is 300-500 ℃, and the reduction time is 2-3 h.
Compared with the prior art, the method is used for doping in the process of preparing the basic nickel salt precursor to obtain the wrapped Fe3O4The basic nickel salt precursor is coated with Fe3O4The basic nickel salt precursor is calcined at high temperature to obtain coated Fe3O4The basic nickel salt powder can be effectively avoidedThe phenomenon of uneven mixing of the iron-nickel composite powder, the obtained iron-doped superfine nickel powder has good uniformity, and the properties of conductive shielding, microwave absorption and the like of the nickel powder can be enhanced to be applied to composite materials.
Drawings
Fig. 1 is a scanning electron microscope image of a method for preparing fe-doped ultrafine nickel powder according to embodiment 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of iron-doped superfine nickel powder, which is implemented by the following steps:
step 1, adding 400L-500L of first precipitator with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the first precipitator3O4Powder, added Fe3O4The mass ratio of the powder to the nickel salt is 1: 50-2: 50, and the mixture is stirred for 30-60 min until the mixture is Fe3O4Dispersing powder into a first precipitator, heating a reaction kettle to 60-70 ℃ and keeping the temperature constant, adding nickel salt with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding a second precipitator with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the second precipitator to the nickel salt is 1.8: 1-2.5: 1, simultaneously adding 8-16L of surfactant to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3-5H to obtain coated Fe3O4The basic nickel salt precursor;
wherein the nickel salt is one of nickel nitrate solution, nickel sulfate solution or nickel chloride solution; the first precipitator and the second precipitator are both one of sodium carbonate, ammonium bicarbonate, ammonium carbonate or sodium hydroxide; the surfactant is one of (L) -tartaric acid, citric acid or oxalic acid;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is placed in a two-in-one washing machine, washed for 4-6 times by pure water at the temperature of 60-80 ℃, placed in a flash evaporation machine after washing, and dried at the temperature of 60-80 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4And crushing the basic nickel salt powder by airflow, then putting the crushed basic nickel salt powder into a reduction furnace, and reducing the crushed basic nickel salt powder for 2 to 3 hours by high-temperature hydrogen at the reduction temperature of 300 to 500 ℃ to obtain the iron-doped superfine nickel powder.
The invention is doped in the process of preparing the basic nickel salt precursor to obtain the wrapped Fe3O4The basic nickel salt precursor is coated with Fe3O4The basic nickel salt precursor is calcined at high temperature to obtain coated Fe3O4The basic nickel salt powder can effectively avoid the phenomenon of uneven mixing of iron-nickel composite powder, the obtained iron-doped superfine nickel powder has good uniformity, and the performances of conductive shielding, microwave absorption and the like of the nickel powder in a composite material can be enhanced; the obtained product can be directly used for alloy mixing by controlling the mass ratio of the iron to the nickel, so that the application range of the iron-nickel powder is enlarged; the Fe is greatly enhanced by adding a small amount of surfactant3O4And the nickel powder precursor, thereby avoiding a large amount of agglomeration, enhancing the applicability of the iron-doped nickel powder in the alloy tool industry, and effectively weakening the limitation of the alloy tool performance caused by uneven mixing in the alloy production process.
Example 1
Embodiment 1 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of sodium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the sodium carbonate3O4Powder, added Fe3O4Powder and nitric acidThe mass ratio of the nickel solution is 1:50, and the nickel solution is stirred for 30min to Fe3O4Dispersing the powder in sodium carbonate, heating a reaction kettle to 60 ℃ and keeping the temperature constant, adding a nickel nitrate solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding sodium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the sodium carbonate to the nickel nitrate solution is 2:1, simultaneously adding 12L of (L) -tartaric acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 4 hours to obtain the coated Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 70 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reducing furnace, and is reduced for 2.8 hours by high-temperature hydrogen at the reducing temperature of 460 ℃, so that the iron-doped superfine nickel powder is obtained.
As shown in fig. 1, it can be seen from a scanning electron microscope image of the preparation method of iron-doped ultrafine nickel powder provided in embodiment 1 that iron powder and nickel powder are uniformly mixed and distributed without individual agglomeration.
Example 2
Embodiment 2 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 450L of sodium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the sodium carbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel nitrate solution is 1.5:50, and the mixture is stirred for 45min until the Fe content is reduced3O4Dispersing the powder in sodium carbonate, heating the reaction kettle to 66 ℃ and keeping the temperature constant, and adding a nickel nitrate solution with the nickel content of 2mol/L into the reaction kettle by adopting a metering pump at the feeding flow rate of 200L/H so as toAdding sodium carbonate with the concentration of 2mol/L into a reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the sodium carbonate to the nickel nitrate solution is 2:1, simultaneously adding 12L of (L) -tartaric acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 4H to obtain coated Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 70 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reducing furnace, and is reduced for 2.8 hours by high-temperature hydrogen at the reducing temperature of 460 ℃, so that the iron-doped superfine nickel powder is obtained.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
Example 3
Embodiment 3 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of sodium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the sodium carbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel nitrate solution is 2:50, and the mixture is stirred for 60min until the Fe content is up to3O4Dispersing the powder in sodium carbonate, heating a reaction kettle to 70 ℃ and keeping the temperature constant, adding a nickel nitrate solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding sodium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the sodium carbonate to the nickel nitrate solution is 2:1, simultaneously adding 12L of (L) -tartaric acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 4 hours to obtain the coated Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 70 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reducing furnace, and is reduced for 2.8 hours by high-temperature hydrogen at the reducing temperature of 460 ℃, so that the iron-doped superfine nickel powder is obtained.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
Example 4
Embodiment 4 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of ammonium bicarbonate with the concentration of 0.05mol/L into a reaction kettle to be used as a base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the ammonium bicarbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel sulfate solution is 1:50, and the mixture is stirred for 40min to Fe3O4Dispersing the powder in ammonium bicarbonate, heating a reaction kettle to 68 ℃ and keeping the temperature constant, adding a nickel sulfate solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding ammonium bicarbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the ammonium bicarbonate to the nickel sulfate solution is 1.8:1, simultaneously adding 8L of citric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3 hours to obtain the coated Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 70 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reduction furnace, and is reduced for 3 hours by high-temperature hydrogen at the reduction temperature of 340 ℃, so that the iron-doped superfine nickel powder is obtained.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
Example 5
Embodiment 5 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of ammonium bicarbonate with the concentration of 0.05mol/L into a reaction kettle to be used as a base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the ammonium bicarbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel sulfate solution is 1:50, and the mixture is stirred for 40min to Fe3O4Dispersing the powder in ammonium bicarbonate, heating a reaction kettle to 68 ℃ and keeping the temperature constant, adding a nickel sulfate solution with the nickel content of 2mol/L into the reaction kettle at a feeding flow rate of 200L/H by using a metering pump, adding ammonium bicarbonate with the concentration of 2mol/L into the reaction kettle at a feeding flow rate of 400L/H, wherein the volume ratio of the ammonium bicarbonate to the nickel sulfate solution is 2.3:1, simultaneously adding 12L of citric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 4 hours to obtain the coated Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 70 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reduction furnace, and is reduced for 3 hours by high-temperature hydrogen at the reduction temperature of 340 ℃, so that the iron-doped superfine nickel powder is obtained.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
Example 6
Embodiment 6 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of ammonium bicarbonate with the concentration of 0.05mol/L into a reaction kettle to be used as a base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the ammonium bicarbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel sulfate solution is 1:50, and the mixture is stirred for 40min to Fe3O4Dispersing the powder in ammonium bicarbonate, heating a reaction kettle to 68 ℃ and keeping the temperature constant, adding a nickel sulfate solution with the nickel content of 2mol/L into the reaction kettle at a feeding flow rate of 200L/H by using a metering pump, adding ammonium bicarbonate with the concentration of 2mol/L into the reaction kettle at a feeding flow rate of 400L/H, wherein the volume ratio of the ammonium bicarbonate to the nickel sulfate solution is 2.5:1, simultaneously adding 16L of citric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 5 hours to obtain the coated Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 70 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reduction furnace, and is reduced for 3 hours by high-temperature hydrogen at the reduction temperature of 340 ℃, so that the iron-doped superfine nickel powder is obtained.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
Example 7
Embodiment 7 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of ammonium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the ammonium carbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel chloride solution is 2:50, and the mixture is stirred for 60min until the Fe content is up to3O4Dispersing the powder in ammonium carbonate, heating a reaction kettle to 65 ℃ and keeping the temperature constant, adding a nickel chloride solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow rate of 200L/H by using a metering pump, adding ammonium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow rate of 400L/H, wherein the volume ratio of the ammonium carbonate to the nickel chloride solution is 2:1, simultaneously adding 12L of oxalic acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 3.6 hours to obtain the wrapped Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 6 times by pure water at 60 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then put into a reduction furnace, and is reduced for 3 hours by high-temperature hydrogen at the reduction temperature of 300 ℃ to obtain the iron-doped superfine nickel powder.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
Example 8
Embodiment 8 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of ammonium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the ammonium carbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel chloride solution is 2:50, and the mixture is stirred for 60min until the Fe content is up to3O4Dispersing the powder in ammonium carbonate, heating a reaction kettle to 65 ℃ and keeping the temperature constant, adding a nickel chloride solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow rate of 200L/H by using a metering pump, adding ammonium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow rate of 400L/H, wherein the volume ratio of the ammonium carbonate to the nickel chloride solution is 2:1, simultaneously adding 12L of oxalic acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 3.6 hours to obtain the wrapped Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 72 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reduction furnace, and is reduced for 2.2 hours by high-temperature hydrogen at the reduction temperature of 400 ℃, so that the iron-doped superfine nickel powder is obtained.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
Example 9
Embodiment 9 of the present invention provides a method for preparing iron-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of ammonium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding Fe into the ammonium carbonate3O4Powder, added Fe3O4The mass ratio of the powder to the nickel chloride solution is 2:50, and the mixture is stirred for 60min until the Fe content is up to3O4Dispersing the powder in ammonium carbonate, heating the reaction kettle to 65 ℃ and keeping the temperature constant, adding a nickel chloride solution with the nickel content of 2mol/L into the reaction kettle at a feeding flow rate of 200L/H by using a metering pump, adding ammonium carbonate with the concentration of 2mol/L into the reaction kettle at a feeding flow rate of 400L/H, wherein the volume ratio of the ammonium carbonate to the nickel chloride solution is 2:1Simultaneously, adding 12L of oxalic acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 3.6h to obtain the coated Fe3O4The basic nickel salt precursor;
step 2, wrapping the coated Fe obtained in the step 13O4The basic nickel salt precursor is put into a two-in-one washing machine, washed for 4 times by pure water at the temperature of 80 ℃, put into a flash evaporation machine after washing, and dried at the temperature of 80 ℃ to obtain the coated Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The alkali nickel salt powder is crushed by airflow and then is put into a reduction furnace, and is reduced for 2 hours by high-temperature hydrogen at the reduction temperature of 500 ℃ to obtain the iron-doped superfine nickel powder.
Compared with the prior art, the iron-doped superfine nickel powder obtained by the preparation process has the advantages that the iron powder and the nickel powder are uniformly mixed and distributed, and the independent agglomeration behavior is avoided.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (10)
1. The preparation method of the iron-doped superfine nickel powder is characterized by comprising the following steps:
step 1, adding a first precipitator into a reaction kettle to serve as a base solution, stirring the base solution at a stirring frequency of 25Hz, and adding Fe into the first precipitator3O4Powder is stirred for 30-60 min to the Fe3O4Dispersing powder into a first precipitator, heating the reaction kettle to 60-70 ℃ and keeping the temperature constant, adding nickel salt, a second precipitator and a surfactant into the reaction kettle, controlling the feeding flow of the nickel salt and the second precipitator to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3-5 h to obtain coated Fe3O4The basic nickel salt precursor;
step 2, adopting pure water to coat the Fe obtained in the step 13O4Washing the basic nickel salt precursor, and drying after washing to obtain the wrapped Fe3O4The basic nickel salt powder of (4);
step 3, wrapping the wrapped Fe obtained in the step 23O4The basic nickel salt powder is crushed by airflow and then is reduced by high-temperature hydrogen to obtain the iron-doped superfine nickel powder.
2. The method of claim 1, wherein Fe added in step 1 is added3O4The mass ratio of the powder to the nickel salt is 1: 50-2: 50.
3. The method of claim 2, wherein the nickel salt in step 1 is one of a nickel nitrate solution, a nickel sulfate solution, or a nickel chloride solution.
4. The method of claim 3, wherein the nickel content of the nickel salt in step 1 is 2mol/L, and the feeding flow rate of the nickel salt is 200L/H.
5. The method of claim 4, wherein the first precipitant and the second precipitant are selected from sodium carbonate, ammonium bicarbonate, ammonium carbonate and sodium hydroxide in step 1.
6. The method of claim 5, wherein the volume of the first precipitant added in step 1 is 400-500L, and the concentration of the first precipitant is 0.05 mol/L.
7. The method for preparing Fe-doped extra-fine nickel powder according to claim 6, wherein the volume ratio of the second precipitator to the nickel salt added in step 1 is 1.8: 1-2.5: 1, the concentration of the second precipitator is 2mol/L, and the feeding flow rate of the second precipitator is 400L/H.
8. The method of claim 7, wherein the surfactant in step 1 is one of (L) -tartaric acid, citric acid, and oxalic acid.
9. The method of claim 8, wherein the volume of the surfactant added in step 1 is 8-16L.
10. The method for preparing Fe-doped extra-fine nickel powder according to any one of claims 1 to 9, wherein the reduction temperature of the high-temperature hydrogen reduction in step 3 is 300 to 500 ℃ and the reduction time is 2 to 3 hours.
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| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
| CN107088660A (en) * | 2017-07-03 | 2017-08-25 | 张成亮 | A kind of preparation method of ultra-fine cobalt nickel powder |
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| CN1034689A (en) * | 1987-12-09 | 1989-08-16 | 中国科学院化工冶金研究所 | The preparation method of submicron metal |
| CN1593819A (en) * | 2004-06-29 | 2005-03-16 | 北京科技大学 | Preparation method of nanometer sized superfine ferro nickel alloy powder |
| CN1830606A (en) * | 2006-04-14 | 2006-09-13 | 北京科技大学 | Method of preparing ultrafine alloy powder by coprecipitation coreduction |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN101332515A (en) * | 2008-08-05 | 2008-12-31 | 中南大学 | Preparation method of fibrous iron-nickel alloy powder |
| CN101837464A (en) * | 2009-08-28 | 2010-09-22 | 上海九鼎粉体材料有限公司 | Metal nickel powder and preparation method thereof |
| CN101797650A (en) * | 2010-04-22 | 2010-08-11 | 昆明贵金属研究所 | Method for producing surface-activated superfine nickel powder |
| WO2012113217A1 (en) * | 2011-02-23 | 2012-08-30 | 荆门市格林美新材料有限公司 | Nickel powder having high fsss particle size, and preparation method therefor |
| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
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