CN113579247B - Preparation method of nano nickel powder - Google Patents
Preparation method of nano nickel powder Download PDFInfo
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- CN113579247B CN113579247B CN202110943906.7A CN202110943906A CN113579247B CN 113579247 B CN113579247 B CN 113579247B CN 202110943906 A CN202110943906 A CN 202110943906A CN 113579247 B CN113579247 B CN 113579247B
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of nano nickel powder, which comprises the following steps of S1, putting a precursor into a raw material tank; s2, connecting the raw material tank with the tubular furnace, and vacuumizing the raw material tank and the tubular furnace by using a vacuum pump; s3, continuously introducing pressurized argon into the raw material tank; s4, heating the raw material tank, and introducing carrier gas argon to drive the precursor to uniformly enter a tubular furnace; s5, introducing hydrogen to perform reduction reaction on the hydrogen and the precursor; s6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished; s7, collecting the powder, carrying out ultrasonic cleaning, and drying to obtain the nano nickel powder. The preparation method of the nano nickel powder adopts a chemical vapor deposition method to prepare the nano nickel powder, takes the nickel cyclopentadienyl as a precursor, takes hydrogen as a reducing gas, and obtains the nano nickel powder with uniform particle size distribution, smaller particle size and good oxidation resistance by controlling the reaction pressure, temperature and gas flow. Compared with other methods, the method has the advantages of simple operation and easy control of the particle size of the powder.
Description
Technical Field
The invention belongs to the technical field of nickel powder preparation, and particularly relates to a preparation method of nano nickel powder.
Background
The nano nickel powder refers to nickel powder with the particle size of less than 100nm, has extremely large specific surface area and volume effect, and shows great superiority in catalysts, battery materials, light absorption materials, powder metallurgy, particularly multilayer ceramic capacitors (MLCC). In addition, on the premise of ensuring good conductivity of the Ni electrode, the electron migration rate of nickel atoms is smaller than that of noble metal electrodes, and good process stability can be ensured. There are several factors that restrict the use of nickel electrodes in current research: (1) The nickel electrode slurry and the organic adhesive are easy to oxidize after being co-fired in the air, so that the conductivity of the nickel electrode slurry is reduced; (2) The nickel powder has poor dispersibility and uniformity, and large particles penetrate through a dielectric layer during lamination and pressing and cutting to cause a short circuit problem.
At present, the nickel powder is mainly prepared by a liquid phase reduction method in China, hydrazine hydrate is used as a reducing agent, the hydrazine hydrate is toxic and is not suitable for mass production, the obtained nickel powder often contains moisture and can oxidize a nickel simple substance with strong reducibility, and in order to solve the problem that the nickel powder is easy to oxidize, the nickel powder is generally subjected to coating treatment after being obtained, and the preparation process is complex.
In view of the existing problems, it is desirable to find a method for preparing nickel powder, which simplifies the preparation process, and the obtained nickel powder has small and uniform particle size, good dispersibility, and good oxidation resistance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method which adopts a chemical vapor deposition method to prepare nano nickel powder with small and uniform particle size and good dispersibility.
The technical scheme for solving the technical problems comprises the following steps:
a method for preparing nano nickel powder comprises the following steps:
s1, weighing a precursor, and then putting the precursor into a raw material tank;
s2, connecting the raw material tank with the tubular furnace, and then vacuumizing the raw material tank and the tubular furnace by using a vacuum pump to enable the interior of the raw material tank and the interior of the tubular furnace to be in an initial vacuum environment;
s3, adjusting a vacuum pump valve, and continuously introducing pressurized argon into the raw material tank in the initial vacuum environment to enable the pressure in the raw material tank to be close to the reaction pressure;
s4, heating the raw material tank to heat and volatilize the precursor, and introducing carrier gas argon to drive the precursor to uniformly enter a reaction zone of the tubular furnace;
s5, heating the tube furnace, introducing hydrogen into a reaction zone of the tube furnace, adjusting a vacuum pump, stabilizing the reaction pressure and enabling the hydrogen and the precursor to perform a reduction reaction;
s6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished;
s7, collecting powder after the reduction reaction in the reaction zone is completed, adding the powder into an ethanol solution for ultrasonic cleaning, and then drying the powder to obtain nano nickel powder;
wherein the precursor is nickel chloride, the weight is 0.3-50 g, the particle size range of the nano nickel powder is 40-100 nm, and the initial oxidation temperature is 400-450 ℃.
The method takes the nickel cyclopentadienyl as the precursor, has low evaporation temperature compared with other nickel metal organic matters, and is beneficial to the reaction. Taking hydrogen as reducing gas, the following reactions occur in the reaction zone: niCp 2 +H 2 → Ni + nCnHn, niCp in comparison with the decomposition Process of Nickel Dicocene 2 → Ni + nCnHn, the introduction of hydrogen reduces the reaction activation energy, the reaction temperature is reduced from more than 500 ℃ to about 200 ℃, the carbon layer is contained in the outer layer of the nickel powder after the reaction, the oxidation of nickel can be effectively prevented, and the oxidation resistance of the nano nickel powder is improved
The invention has the following beneficial effects:
1. the nano nickel powder is prepared by adopting a chemical vapor deposition method, and the obtained powder has good dispersibility, uniform particle size, good sphericity and good oxidation resistance, and can meet the requirements of MLCC inner electrodes.
2. The obtained powder has high purity, the post-treatment process is simple, and the organic matter can be separated from the nickel powder by cleaning with alcohol.
3. The particle size of the powder is controllable, and the reaction speed and the crystal growth are effectively controlled by changing the parameters of the deposition process.
4. Simple process, low reaction temperature, low requirement on equipment, continuous feeding and easy continuous production.
Drawings
FIG. 1 is an X-ray diffraction pattern of nano nickel powder prepared by the present invention.
FIG. 2 is an SEM image of nano nickel powder prepared by the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1:
the method for preparing nano nickel powder in embodiment 1 of the present invention includes the following steps:
s1, weighing a precursor, and then putting the precursor into a raw material tank; the precursor is nickelocene, and the weight of the precursor is 0.5g in the embodiment.
S2, connecting the raw material tank with the tubular furnace, and then vacuumizing the raw material tank and the tubular furnace by using a vacuum pump to enable the interior of the raw material tank and the interior of the tubular furnace to be in an initial vacuum environment; the pressure of the initial vacuum environment is less than 10Pa.
S3, adjusting a vacuum pump valve, and continuously introducing pressurized argon into the raw material tank in the initial vacuum environment to enable the pressure in the raw material tank to be close to the reaction pressure; in this embodiment, the reaction pressure is 10000Pa, the flow rate of the pressurized argon gas is 100sccm, and the introduction time is 20min.
S4, heating the raw material tank to heat and volatilize the precursor, and introducing carrier gas argon to drive the precursor to uniformly enter a reaction zone of the tube furnace; heating is carried out in an argon gas introducing environment, in the embodiment, the temperature of the heated raw material tank is 120 ℃, and the flow of introducing carrier gas argon gas is 30sccm.
S5, heating the tube furnace, introducing hydrogen into a reaction zone of the tube furnace, adjusting a vacuum pump, stabilizing the reaction pressure and enabling the hydrogen and the precursor to perform a reduction reaction; heating is carried out in an argon-filled environment, the temperature of the tubular furnace after heating in the embodiment is 170 ℃, the flow of the filled hydrogen is 120sccm, and the reaction time of the reduction reaction is 40min.
S6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished; the powder produced after the reaction can be clearly seen by opening the apparatus after the reaction.
S7, collecting powder after the reduction reaction in the reaction zone is completed, adding the powder into an ethanol solution for ultrasonic cleaning, and then drying the powder to obtain nano nickel powder; in this example, the particle size of the obtained nano nickel powder is 58nm, and the initial oxidation temperature is 408 ℃.
Example 2:
the method for preparing nano nickel powder in embodiment 2 of the present invention comprises the following steps:
s1, weighing a precursor, and then putting the precursor into a raw material tank; the precursor is nickelocene, and the weight of the precursor is 5g in the embodiment.
S2, connecting the raw material tank with the tubular furnace, and then vacuumizing the raw material tank and the tubular furnace by using a vacuum pump to enable the interior of the raw material tank and the interior of the tubular furnace to be in an initial vacuum environment; the pressure of the initial vacuum environment is less than 10Pa.
S3, adjusting a vacuum pump valve, and continuously introducing pressurized argon into the raw material tank in the initial vacuum environment to enable the pressure in the raw material tank to be close to the reaction pressure; in this embodiment, the reaction pressure is 10000Pa, the flow rate of the pressurized argon gas is 100sccm, and the introduction time is 20min.
S4, heating the raw material tank to heat and volatilize the precursor, and introducing carrier gas argon to drive the precursor to uniformly enter a reaction zone of the tube furnace; in this embodiment, the temperature of the raw material tank after heating is 130 ℃, and the flow rate of the carrier gas argon introduced is 50sccm.
S5, heating the tube furnace, introducing hydrogen into a reaction zone of the tube furnace, adjusting a vacuum pump, stabilizing the reaction pressure and enabling the hydrogen and the precursor to perform a reduction reaction; heating is carried out in an argon gas introducing environment, the temperature of the tubular furnace after heating in the embodiment is 190 ℃, the flow of introduced hydrogen is 200sccm, and the reaction time of the reduction reaction is 70min.
S6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished; the powder produced after the reaction can be clearly seen by opening the apparatus after the reaction.
S7, collecting powder after reduction reaction in the reaction zone is finished, adding the powder into an ethanol solution for ultrasonic cleaning, and drying the powder to obtain nano nickel powder; in this example, the particle size of the obtained nano nickel powder is 70nm, and the initial oxidation temperature is 419 ℃.
Example 3:
the method for preparing nano nickel powder in embodiment 3 of the present invention includes the following steps:
s1, weighing a precursor, and then putting the precursor into a raw material tank; the precursor is nickelocene, and the weight of the precursor is 0.6g in the embodiment.
S2, connecting the raw material tank with the tubular furnace, and then vacuumizing the raw material tank and the tubular furnace by using a vacuum pump to enable the interior of the raw material tank and the interior of the tubular furnace to be in an initial vacuum environment, wherein the pressure of the initial vacuum environment is lower than 10Pa.
S3, adjusting a vacuum pump valve, and continuously introducing pressurized argon into the raw material tank in the initial vacuum environment to enable the pressure in the raw material tank to be close to the reaction pressure; in this embodiment, the reaction pressure is 10000Pa, the flow rate of the pressurized argon gas is 100sccm, and the flowing time is 20min.
S4, heating the raw material tank to heat and volatilize the precursor, and introducing carrier gas argon to drive the precursor to uniformly enter a reaction zone of the tube furnace; heating is carried out in an argon gas introducing environment, in the embodiment, the temperature of the raw material tank after heating is 140 ℃, and the flow of introducing carrier gas argon gas is 30sccm.
S5, heating the tube furnace, introducing hydrogen into a reaction zone of the tube furnace, adjusting a vacuum pump, stabilizing the reaction pressure and enabling the hydrogen and the precursor to perform a reduction reaction; heating is carried out in an argon gas introducing environment, the temperature of the tubular furnace after heating in the embodiment is 210 ℃, the flow of introduced hydrogen is 200sccm, and the reaction time of the reduction reaction is 40min.
S6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished; the powder produced after the reaction can be clearly seen by opening the apparatus after the reaction.
S7, collecting powder after the reduction reaction in the reaction zone is completed, adding the powder into an ethanol solution for ultrasonic cleaning, and then drying the powder to obtain nano nickel powder; in this example, the particle size of the obtained nano nickel powder is 90nm, and the initial oxidation temperature is 432 ℃.
Comparing examples 1-3, the particle size of the nano nickel powder can be effectively controlled by adjusting the flow rate of the argon gas and the hydrogen gas, and the actual reaction temperature, so that the reaction speed and the growth condition of the crystal can be effectively controlled, and meanwhile, the larger the particle size of the nano nickel powder is, the higher the actual oxidation temperature is, and the actual production parameters can be adjusted according to the actual requirements, so as to obtain the required nano nickel powder.
Example 4:
the method for preparing nano nickel powder of embodiment 4 of the present invention comprises the following steps:
s1, weighing a precursor, and then putting the precursor into a raw material tank; the precursor is nickelocene, and the weight of the precursor is 0.3g in the embodiment.
S2, connecting the raw material tank with the tubular furnace, and then vacuumizing the raw material tank and the tubular furnace by using a vacuum pump to enable the interior of the raw material tank and the interior of the tubular furnace to be in an initial vacuum environment; the pressure of the initial vacuum environment is less than 10Pa.
S3, adjusting a vacuum pump valve, and continuously introducing pressurized argon into the raw material tank in the initial vacuum environment to enable the pressure in the raw material tank to be close to the reaction pressure; in this embodiment, the reaction pressure is 500Pa, the flow rate of the pressurized argon gas is 100sccm, and the introduction time is 10min.
S4, heating the raw material tank to heat and volatilize the precursor, and introducing carrier gas argon to drive the precursor to uniformly enter a reaction zone of the tubular furnace; heating is carried out in an argon gas introducing environment, in the embodiment, the temperature of the heated raw material tank is 100 ℃, and the flow of introducing carrier gas argon gas is 20sccm.
S5, heating the tube furnace, introducing hydrogen into a reaction zone of the tube furnace, adjusting a vacuum pump, stabilizing the reaction pressure and enabling the hydrogen and the precursor to perform a reduction reaction; heating is carried out in an argon-filled environment, the temperature of the tubular furnace after heating in the embodiment is 140 ℃, the flow of the filled hydrogen is 30sccm, and the reaction time of the reduction reaction is 40min.
S6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished; the powder produced after the reaction can be clearly seen by opening the apparatus after the reaction.
S7, collecting powder after the reduction reaction in the reaction zone is completed, adding the powder into an ethanol solution for ultrasonic cleaning, and then drying the powder to obtain nano nickel powder; in this example, the particle size of the obtained nano nickel powder is 62nm, and the initial oxidation temperature is 413 ℃.
Example 5:
the method for preparing nano nickel powder of embodiment 5 of the present invention comprises the following steps:
s1, weighing a precursor, and then putting the precursor into a raw material tank; the precursor is nickelocene, and the weight of the precursor is 50g.
S2, connecting the raw material tank with the tubular furnace, and then vacuumizing the raw material tank and the tubular furnace by using a vacuum pump to enable the interior of the raw material tank and the interior of the tubular furnace to be in an initial vacuum environment; the pressure of the initial vacuum environment is less than 10Pa.
S3, adjusting a vacuum pump valve, and continuously introducing pressurized argon into the raw material tank in the initial vacuum environment to enable the pressure in the raw material tank to be close to the reaction pressure; in this embodiment, the reaction pressure is 50000Pa, the flow rate of the pressurized argon introduced is 500sccm, and the introduction time is 50min.
S4, heating the raw material tank to heat and volatilize the precursor, and introducing carrier gas argon to drive the precursor to uniformly enter a reaction zone of the tube furnace; heating is carried out in an argon gas introducing environment, in the embodiment, the temperature of the heated raw material tank is 220 ℃, and the flow of introducing carrier argon gas is 2000sccm.
S5, heating the tube furnace, introducing hydrogen into a reaction zone of the tube furnace, adjusting a vacuum pump, stabilizing the reaction pressure and enabling the hydrogen and the precursor to perform a reduction reaction; heating is carried out in an argon gas introducing environment, the temperature of the tubular furnace after heating in the embodiment is 550 ℃, the flow of introduced hydrogen is 5000sccm, and the reaction time of the reduction reaction is 200min.
S6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished; the powder produced after the reaction can be clearly seen by opening the apparatus after the reaction.
S7, collecting powder after reduction reaction in the reaction zone is finished, adding the powder into an ethanol solution for ultrasonic cleaning, and drying the powder to obtain nano nickel powder; in this example, the particle size of the obtained nano nickel powder is 105nm, and the initial oxidation temperature is 436 ℃.
Comparative example 1:
ni (CH 3 COO) was added at a concentration of 0.1mol/L 2 ·4H 2 Preparation of Ni (OH) by direct chemical precipitation method by using O and 0.1mol/L KOH as raw materials 2 A precursor; dispersing a precursor in ethanol, and preparing nano potassium sulfate salt by an anti-solvent precipitation method (adding 4% of PAA), so that the prepared nano potassium sulfate salt wraps precursor particles, and the precursor particles are dispersed and isolated from one another, thereby forming a nano salt + precursor mixture (wherein the molar ratio of the salt to the precursor is 1; washing the mixture with ethanol for 2 times, removing water, drying at 80 deg.C in oven, adding organic polymer PAA, pre-baking at 700 deg.C, and further H 2 Reducing for 4h at 550 ℃ in the atmosphere to obtain nickel powder, wherein the particle size of the nickel powder is 290nm.
As compared with the nickel powders obtained in comparative example 1, it is apparent that the average particle size of the nano nickel powders obtained in examples 1-5 is less than 200nm, the average particle size of the nickel powder obtained in comparative example 1 is 290nm, and the nickel powders prepared in examples 1-5 have good oxidation resistance, the initial oxidation temperature is above 400 ℃, the comparative example is only 300 ℃, and the specific parameters are as shown in the following table.
| Average particle diameter | Initial oxidation temperature | |
| Example 1 | 58nm | 408℃ |
| Example 2 | 70nm | 419℃ |
| Example 3 | 90nm | 432℃ |
| Example 4 | 62nm | 413℃ |
| Example 5 | 103nm | 436℃ |
| Comparative example 1 | 290nm | 300℃ |
Compared with other methods, the preparation method provided by the invention is simple to operate, the sample can be obtained at a lower temperature, the obtained sample has uniform particle size and good dispersibility, and the nickel cyclopentadienyl is selected as a precursor, so that a carbon layer can be formed in decomposition and wraps the surface of the nickel powder, the oxidation of the nickel powder is effectively prevented, and the requirements of the MLCC electrode are met.
The foregoing is a further detailed description of the invention in connection with specific preferred embodiments and it is not intended to limit the invention to the specific embodiments described. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (6)
1. A method for preparing nano nickel powder is characterized by comprising the following steps:
s1, weighing a precursor, and then putting the precursor into a raw material tank;
s2, connecting the raw material tank with the tubular furnace, and then vacuumizing the raw material tank and the tubular furnace by using a vacuum pump to enable the interior of the raw material tank and the interior of the tubular furnace to be in an initial vacuum environment;
s3, adjusting a vacuum pump valve, and continuously introducing pressurized argon into the raw material tank in the initial vacuum environment to enable the pressure in the raw material tank to be close to the reaction pressure;
s4, heating the raw material tank to heat and volatilize the precursor, and introducing carrier gas argon to drive the precursor to uniformly enter a reaction zone of the tube furnace;
s5, heating the tube furnace, introducing hydrogen into a reaction zone of the tube furnace, adjusting a vacuum pump, stabilizing the reaction pressure and enabling the hydrogen and the precursor to perform a reduction reaction;
s6, cooling the raw material tank and the tubular furnace to room temperature after the reaction is finished;
s7, collecting powder after the reduction reaction in the reaction zone is completed, adding the powder into an ethanol solution for ultrasonic cleaning, and then drying the powder to obtain nano nickel powder;
wherein the precursor is nickelocene, the weight of the precursor is 0.3-50 g, the particle size range of the nano nickel powder is 40-100 nm, and the initial oxidation temperature is 400-450 ℃.
2. The method for producing nano nickel powder according to claim 1, characterized in that: the pressure of the initial vacuum environment is lower than 10Pa, and the reaction pressure is 500-50000 Pa.
3. The method for producing nano nickel powder according to claim 2, wherein: in the step S3, the flow of the pressurized argon is 100-500 sccm, and the introduction time is 10-50 min.
4. The method for producing nano nickel powder according to claim 2, wherein: and in the step S4, the flow of the carrier gas argon is introduced into the reactor and is 20-2000 sccm.
5. The method for producing nano nickel powder according to claim 4, characterized in that: in the step S5, the flow of the introduced hydrogen is 30-50000 sccm, and the reaction time of the reduction reaction is 40-200 min.
6. The method for producing nano nickel powder according to any one of claims 1 to 5, characterized in that: the temperature of the raw material tank after being heated is 100-220 ℃, and the temperature of the tubular furnace after being heated is 140-550 ℃.
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