CN112317758A - Preparation method of nano nickel - Google Patents
Preparation method of nano nickel Download PDFInfo
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- CN112317758A CN112317758A CN201911044339.0A CN201911044339A CN112317758A CN 112317758 A CN112317758 A CN 112317758A CN 201911044339 A CN201911044339 A CN 201911044339A CN 112317758 A CN112317758 A CN 112317758A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- 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
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
Abstract
The invention discloses a preparation method of nano nickel, which comprises the following steps: s1: carrying out a complexing reaction on metallic nickel and an ammonium bicarbonate solution to generate a nickel-ammonia complex solution; s2: decomposing the nickel-ammonia complex to generate nickel carbonate; s3: and step heating the nickel carbonate obtained in the step S2 in a reducing atmosphere, and carrying out thermal decomposition reduction reaction to generate nano nickel. The nano nickel prepared by the method has a nano-sized strip structure, is easy to disperse, and has a large specific surface area and low resistance.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a preparation method of nano nickel.
Background
Nickel is an important class of metallic material that finds wide application in almost all modern industrial fields. The micro/nano multilevel structure construction technology is combined with the traditional process, and the properties of the assembly are more accurately regulated and controlled by adjusting the components, the sizes, the shapes and the organization modes of the structural units from the molecular level, so that the performances of the metal in the application fields of catalysis, electrodes, chemical protective coatings, soft magnetic materials, low-temperature superplastic materials and the like can be greatly changed. Methods for fabricating metal-based nanostructures have been actively developed recently, and the synthesized nanostructures include nanospheres by chemical reduction, electrochemical template deposition nanorings, and the like.
The nano nickel material prepared by the existing method has the following problems: 1. easy to agglomerate and difficult to disperse uniformly in the solution; 2. the nano nickel material is spherical, and the conductivity needs to be improved; 3. the preparation process is complex, the purity is low, and the waste pollutes the environment.
Disclosure of Invention
The technical problem to be solved by the invention is the problem of the existing nano metallic nickel material.
In order to solve the technical problem, the invention provides a preparation method of nano nickel, which comprises the following steps:
s1: carrying out a complexing reaction on metallic nickel and an ammonium bicarbonate solution to generate a nickel-ammonia complex solution;
s2: decomposing the nickel-ammonia complex to generate nickel carbonate;
s3: and step heating the nickel carbonate obtained in the step S2 in a reducing atmosphere, and carrying out thermal decomposition reduction reaction to generate nano nickel.
The method for heating up the thermal decomposition reduction by adopting a step heating method can comprise the following steps: raising the temperature from the initial reaction temperature to 100-200 ℃, carrying out heat preservation reaction, and raising the temperature to 250-800 ℃ to generate the nano nickel.
As a preferred embodiment, the thermal decomposition and reduction comprises:
first-stage temperature rise: heating to 100-200 ℃ within 3 hours;
and (3) second-stage heat preservation reaction: keeping the temperature at 100-200 ℃ and reacting for more than 8 hours;
and (3) heating in the third stage: the temperature is raised to 250-800 ℃ within 15 hours.
Further preferably, the thermal decomposition reduction reaction in step S3 includes:
first-stage temperature rise: the initial reaction temperature is room temperature, and the temperature is raised to 100-150 ℃ within 0.5-2 hours;
and (3) second-stage heat preservation reaction: reacting for 10-20 hours at the temperature of 100-150 ℃;
and (3) heating in the third stage: heating to 300-600 ℃ within 3-8 hours.
Preferably, the nickel-ammonia complex solution is stirred at the temperature of 80-180 ℃ to decompose into nickel carbonate and ammonia gas in step S2.
Preferably, step S1 includes:
adding metal nickel into ammonium bicarbonate solution, introducing air or oxygen, and performing a complexing reaction to generate nickel-ammonia complex solution; wherein the concentration of nickel ions in the nickel-ammonia complex solution is 40-100 g/L, and NH in the ammonium bicarbonate solution3The concentration is 80-200 g/L, CO2The concentration is 40-200 g/L.
Preferably, after the thermal decomposition reduction reaction in step S3, the method further includes a cooling step of thermally decomposing the reduction product and naturally cooling the product to room temperature.
Preferably, the reducing atmosphere is one of hydrogen or ethanol or a combination thereof.
Preferably, the reducing atmosphere is hydrogen: during the thermal decomposition and reduction reaction of the nickel carbonate, hydrogen is continuously introduced, and the introduction amount of the hydrogen is more than 1 time of the amount of the nickel carbonate. Further preferably, the reducing atmosphere is hydrogen: during the thermal decomposition and reduction reaction of the nickel carbonate, hydrogen is continuously introduced, and the introduction amount of the hydrogen is more than 2 times of the amount of the nickel carbonate.
The invention also provides the nano nickel prepared by the method, which is in a strip structure, the length of the nano nickel is less than 600nm, and the length-diameter ratio of the nano nickel is 2-50: 1.
The nano nickel prepared by the preparation method provided by the invention is of a strip structure, the length is less than 600nm, and the length-diameter ratio is 2-50: 1; the purity of the product is more than 99.8%, and the specific surface area is 15-35 m2(g) small resistance of 1X 10-5～2.5×10-5Omega cm; and the conductive particles are uniformly dispersed in the solution and can be mutually crosslinked to increase the conductivity of the solution. The preparation method provided by the invention has the advantages that,environmental protection and no waste discharge polluting the environment.
Drawings
FIG. 1 is a first electron micrograph of nano-nickel prepared in example 1 of the present invention;
fig. 2 is an electron microscope image two of the nano nickel prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of nano nickel, wherein nickel carbonate is subjected to thermal decomposition reduction by adopting step temperature rise in a reducing atmosphere, and the preparation method comprises the following steps of:
s1: the method comprises the following steps of (1) carrying out a complex reaction on metallic nickel and an ammonium bicarbonate solution to generate a nickel-ammonia complex solution:
adding metal nickel into ammonium bicarbonate solution, introducing air or oxygen, and performing a complexing reaction to generate nickel-ammonia complex solution; wherein the concentration of nickel ions in the nickel-ammonia complex solution is 40-100 g/L, and NH in the ammonium bicarbonate solution3The concentration is 80-200 g/L, CO2The concentration is 40-200 g/L.
S2: the method for generating nickel carbonate after the nickel-ammonia complex is decomposed comprises the following steps:
and step S2, stirring the nickel-ammonia complex solution at the temperature of 80-180 ℃, and decomposing the nickel-ammonia complex solution into nickel carbonate and ammonia gas.
S3: the nickel carbonate obtained in the step S2 is thermally decomposed and reduced in a reducing atmosphere to generate nano nickel; wherein the thermal decomposition reduction adopts step temperature rise: raising the temperature from the initial reaction temperature to 100-200 ℃, carrying out heat preservation reaction, and raising the temperature to 250-800 ℃ to generate the nano nickel. Under the condition of the step temperature rise, the nickel carbonate prepared by decomposing the nickel-ammonia complex is stably pyrolyzed and reduced, and the nickel carbonate is pyrolyzed and reduced to form strip-shaped nano-sized metallic nickel by the step temperature rise and the reducing airflow.
The reducing atmosphere can be one of hydrogen or ethanol or a combination of the hydrogen and the ethanol. When the reducing atmosphere is hydrogen, the introduction amount of the hydrogen is more than 2 times of the amount of the nickel carbonate substance, the reduction reaction is complete, the purity of the nickel is high, and the formation of strip-shaped nano nickel is facilitated. The flow rate of the reducing gas can be set appropriately in conjunction with the reaction time and the amount of reducing atmosphere required.
The nickel carbonate prepared by decomposing the nickel-ammonia complex is in a nano-sized strip structure, can generate a cross-linked structure in application, has better conductivity than granular nano nickel and better performance.
Example 1
The preparation method of the nano nickel of the embodiment comprises the following steps:
1) 6kg of metallic nickel is added into a complex reaction device, and 110L of ammonium bicarbonate solution (the concentration of ammonia in the ammonium bicarbonate solution is 100g/L and CO is added2The concentration of the nickel is 60g/L), air is introduced, the reaction is completed, and the nickel-ammonia complex aqueous solution is obtained and filtered;
2) adding the filtered nickel-ammonia complex aqueous solution into a decomposition reaction device, reacting completely at the temperature of 100 ℃ to generate nickel carbonate precipitate and ammonia gas, condensing and absorbing the ammonia gas, recycling, dehydrating and drying the nickel carbonate;
3) adding the dehydrated and dried nickel carbonate into a reduction furnace, introducing hydrogen (the hydrogen is continuously introduced in the whole reaction process, and the introduction amount of the hydrogen is 2 times of the amount of the nickel carbonate),
first-stage temperature rise: the initial reaction temperature is room temperature, 1 hour, and the temperature is raised to 120 ℃;
and (3) second-stage heat preservation reaction: keeping the temperature at 120 ℃ for reaction for 12 hours;
and (3) heating in the third stage: after 3 hours, the temperature was raised to 600 ℃.
4) Cooling to room temperature to prepare the obtained nano nickel.
Through detection, the purity of the nano nickel prepared by the embodiment is 99.9%; as shown in fig. 1 and fig. 2, the nano nickel of the present embodiment has a strip structure, a length of 50nm to 600nm, and an aspect ratio of 2 to 50: 1; ratio of nano nickelSurface area of 35m2(ii) in terms of/g. The resistance is detected by a probing method and is 1 multiplied by 10-5Ω·cm。
Dispersibility test: 0.5kg of nickel powder and 2kg of nickel balls with the diameter of 1mm are put into a container with the diameter of 200mm and ground in an alcohol medium at the speed of 100 revolutions per minute for 1 min. The observation shows that the dispersibility is good and the agglomeration phenomenon is avoided.
Example 2
The preparation method of the nano nickel of the embodiment comprises the following steps:
1) 6kg of metallic nickel is added into a complex reaction device, and 110L of ammonium bicarbonate solution (the concentration of ammonia in the ammonium bicarbonate solution is 100g/L and CO is added2The concentration of the nickel is 60g/L), air is introduced, the reaction is completed, and the nickel-ammonia complex aqueous solution is obtained and filtered;
2) adding the filtered nickel-ammonia complex aqueous solution into a decomposition reaction device, heating to 180 ℃ in a pressure environment, reacting completely to generate nickel carbonate precipitate and ammonia gas, condensing and absorbing the ammonia gas, recycling, dehydrating and drying the nickel carbonate;
3) adding the dehydrated and dried nickel carbonate into a reduction furnace, introducing hydrogen (the hydrogen is continuously introduced in the whole reaction process, and the introduction amount of the hydrogen is 2 times of the amount of the nickel carbonate),
first-stage temperature rise: the initial reaction temperature is room temperature, and the temperature is raised to 100 ℃ within 0.5 hour;
and (3) second-stage heat preservation reaction: keeping the temperature at 100 ℃ for reaction for 20 hours;
and (3) heating in the third stage: the temperature was raised to 300 ℃ over 3 hours.
4) Cooling to room temperature to prepare the obtained nano nickel.
Through detection, the purity of the nano nickel prepared by the method is 99.8%; the nano nickel is in a strip structure, the length is 50 nm-400 nm, and the length-diameter ratio is 2-50: 1; the specific surface area of the nano nickel is 23m2(ii) in terms of/g. The resistance is detected by a probing method and is 1.4 multiplied by 10-5Ω·cm。
Dispersibility test: as in example 1, the dispersibility was good and no agglomeration was observed.
Example 3
The preparation method of the nano nickel of the embodiment comprises the following steps:
1) 6kg of metallic nickel is added into a complex reaction device, and 110L of ammonium bicarbonate solution (the concentration of ammonia in the ammonium bicarbonate solution is 100g/L and CO is added2The concentration of the nickel is 60g/L), air is introduced, the reaction is completed, and the nickel-ammonia complex aqueous solution is obtained and filtered;
2) adding the filtered nickel-ammonia complex aqueous solution into a decomposition reaction device, completely reacting at 120 ℃ in a pressure environment to generate nickel carbonate precipitate and ammonia gas, condensing and absorbing the ammonia gas, recycling, dehydrating and drying the nickel carbonate;
3) adding the dehydrated and dried nickel carbonate into a reduction furnace, introducing hydrogen (the hydrogen is continuously introduced in the whole reaction process, and the introduction amount of the hydrogen is 2 times of the amount of the nickel carbonate),
first-stage temperature rise: the initial reaction temperature is room temperature, and the temperature is raised to 150 ℃ within 2 hours;
and (3) second-stage heat preservation reaction: keeping the temperature at 150 ℃ for reaction for 8 hours;
and (3) heating in the third stage: the temperature was raised to 600 ℃ over 8 hours.
4) Cooling to room temperature to prepare the obtained nano nickel.
Through detection, the purity of the nano nickel prepared by the method is 99.8%; the nano nickel is in a strip structure, the length is 50 nm-400 nm, and the length-diameter ratio is 2-50: 1; the specific surface area of the nano nickel is 25m2(ii) in terms of/g. The resistance is detected by a probing method and is 1.3 multiplied by 10-5Ω·cm。
Dispersibility test: as in example 1, the dispersibility was good and no agglomeration was observed.
Example 4
The preparation method of the nano nickel of the embodiment comprises the following steps:
1) 6kg of metallic nickel is added into a complex reaction device, and 60L of ammonium bicarbonate solution (the concentration of ammonia in the ammonium bicarbonate solution is 180g/L and CO is added2The concentration of the nickel is 200g/L), air is introduced, the reaction is completed, and the nickel-ammonia complex aqueous solution is obtained and filtered;
2) adding the filtered nickel-ammonia complex aqueous solution into a decomposition reaction device, reacting completely at the temperature of 80 ℃ to generate nickel carbonate precipitate and ammonia gas, condensing and absorbing the ammonia gas, recycling, dehydrating and drying the nickel carbonate;
3) adding the dehydrated and dried nickel carbonate into a reduction furnace, introducing hydrogen (the hydrogen is continuously introduced in the whole reaction process, and the introduction amount of the hydrogen is 2 times of the amount of the nickel carbonate),
first-stage temperature rise: the initial reaction temperature is room temperature, and the temperature is raised to 200 ℃ within 3 hours;
and (3) second-stage heat preservation reaction: keeping the temperature at 200 ℃ for reaction for 8 hours;
and (3) heating in the third stage: the temperature was raised to 250 ℃ over 2 hours.
4) Cooling to room temperature to prepare the obtained nano nickel.
Through detection, the purity of the nano nickel prepared by the method is 99.9%; the nano nickel is in a strip structure, the length is 50 nm-400 nm, and the length-diameter ratio is 2-50: 1; the specific surface area of the nano nickel is 25m2(ii) in terms of/g. The resistance is detected by a probing method and is 1.8 multiplied by 10-5Ω·cm。
Dispersibility test: as in example 1, the dispersibility was good and no agglomeration was observed.
Example 5
The preparation method of the nano nickel of the embodiment comprises the following steps:
1) 6kg of metallic nickel is added into a complex reaction device, and 110L of ammonium bicarbonate solution (the concentration of ammonia in the ammonium bicarbonate solution is 100g/L and CO is added2The concentration of the nickel is 60g/L), air is introduced, the reaction is completed, and the nickel-ammonia complex aqueous solution is obtained and filtered;
2) adding the filtered nickel-ammonia complex aqueous solution into a decomposition reaction device, reacting completely at the temperature of 100 ℃ to generate nickel carbonate precipitate and ammonia gas, condensing and absorbing the ammonia gas, recycling, dehydrating and drying the nickel carbonate;
3) adding the dehydrated and dried nickel carbonate into a reduction furnace, introducing hydrogen (the hydrogen is continuously introduced in the whole reaction process, and the introduction amount of the hydrogen is 2 times of the amount of the nickel carbonate),
first-stage temperature rise: the initial reaction temperature is room temperature, and the temperature is raised to 120 ℃ within 1 hour;
and (3) second-stage heat preservation reaction: keeping the temperature at 120 ℃ for reaction for 10 hours;
and (3) heating in the third stage: after 15 hours, the temperature was raised to 800 ℃.
4) Cooling to room temperature to prepare the obtained nano nickel.
Through detection, the purity of the nano nickel prepared by the embodiment is 99.9%; as shown in FIG. 1, the nano nickel of the present embodiment has a strip structure, a length of 50nm to 400nm, and an aspect ratio of 2 to 50: 1; the specific surface area of the nano nickel is 28m2(ii) in terms of/g. The resistance is detected by a probing method and is 1 multiplied by 10-5Ω·cm。
Dispersibility test: as in example 1, the dispersibility was good and no agglomeration was observed.
Comparative example 1
The preparation method of the nano nickel of the embodiment comprises the following steps:
1) drying 12kg of commercial nickel carbonate;
3) adding the dried nickel carbonate into a reduction furnace, introducing hydrogen,
first-stage temperature rise: the initial reaction temperature is room temperature, and the temperature is raised to 120 ℃ within 1 hour;
and (3) second-stage heat preservation reaction: keeping the temperature at 120 ℃ for reaction for 12 hours;
and (3) heating in the third stage: after 6 hours, the temperature was raised to 600 ℃.
4) Cooling to room temperature to prepare the obtained nano nickel.
Through detection, the purity of the nano nickel prepared by the method is 99.7 percent; the nano nickel is granular, and the particle size is 400-500 nm; the specific surface area of the nano nickel is 15m2(ii) in terms of/g. The resistance is detected by a probing method and is 1 multiplied by 10-4Ω·cm。
Dispersibility test: as in example 1, agglomeration was observed.
Comparative example 2
The preparation method of the nano nickel of the embodiment comprises the following steps:
1) 6kg of metallic nickel is added into a complex reaction device, and 110L of ammonium bicarbonate solution (the concentration of ammonia in the ammonium bicarbonate solution is 100g/L and CO is added2The concentration of the nickel is 60g/L), air is introduced, the reaction is complete, and the nickel-ammonia complex is obtainedFiltering the aqueous solution;
2) adding the filtered nickel-ammonia complex aqueous solution into a decomposition reaction device, reacting completely at the temperature of 100 ℃ to generate nickel carbonate precipitate and ammonia gas, condensing and absorbing the ammonia gas, recycling, dehydrating and drying the nickel carbonate;
3) adding the dehydrated and dried nickel carbonate into a reduction furnace, introducing hydrogen, heating to 600 ℃ within 8 hours at the initial reaction temperature, and reacting for 10 hours with heat preservation;
4) cooling to room temperature to prepare the obtained nano nickel.
Through detection, the purity of the nano nickel prepared by the method is 99.8%; the nano nickel in the embodiment has a mixed structure of a strip structure and a granular structure, and has an agglomeration phenomenon, wherein the length of the strip structure is 50-400 nm, the length-diameter ratio is 2-50: 1, and the grain diameter of the granular structure is about 100 nm; specific surface area of 10m2In terms of/g, the melting point is 401 ℃. The resistance is detected by a probing method and is 4 multiplied by 10-5Ω·cm。
Dispersibility test: in the same manner as in example 1, partial agglomeration was observed.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above description is only an example of the present invention, and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. The preparation method of the nano nickel is characterized by comprising the following steps:
s1: carrying out a complexing reaction on metallic nickel and an ammonium bicarbonate solution to generate a nickel-ammonia complex solution;
s2: decomposing the nickel-ammonia complex to generate nickel carbonate;
s3: and step heating the nickel carbonate obtained in the step S2 in a reducing atmosphere, and carrying out thermal decomposition reduction reaction to generate nano nickel.
2. The method of claim 1, wherein the step temperature rise of the thermal decomposition reduction reaction in step S3 includes: raising the temperature from the initial reaction temperature to 100-200 ℃, carrying out heat preservation reaction, and raising the temperature to 250-800 ℃ to generate the nano nickel.
3. The method of claim 1, wherein the step temperature rise of the thermal decomposition reduction reaction in step S3 includes:
first-stage temperature rise: heating to 100-200 ℃ within 3 hours;
and (3) second-stage heat preservation reaction: keeping the temperature at 100-200 ℃ and reacting for more than 8 hours;
and (3) heating in the third stage: the temperature is raised to 250-800 ℃ within 15 hours.
4. The method of claim 1, wherein the step temperature rise of the thermal decomposition reduction reaction in step S3 includes:
first-stage temperature rise: the initial reaction temperature is room temperature, and the temperature is raised to 100-150 ℃ within 0.5-2 hours;
and (3) second-stage heat preservation reaction: reacting for 10-20 hours at the temperature of 100-150 ℃;
and (3) heating in the third stage: heating to 300-600 ℃ within 3-8 hours.
5. The method for preparing nano nickel according to claim 1, wherein the nickel ammonia complex solution is decomposed into nickel carbonate and ammonia gas by stirring at a temperature of 80-180 ℃ in step S2.
6. The method for preparing nickel carbonate according to claim 1, wherein step S1 includes:
adding metal nickel into ammonium bicarbonate solution, introducing air or oxygen, and performing a complexing reaction to generate nickel-ammonia complex solution; wherein the concentration of nickel ions in the nickel-ammonia complex solution is 40-100 g/L, and NH in the ammonium bicarbonate solution3The concentration is 80-200 g/L, CO2The concentration is 40-200 g/L.
7. The method for preparing nano nickel according to claim 1, wherein after the thermal decomposition reduction reaction in step S3, a cooling step is further included, and the thermal decomposition reduction reaction product is naturally cooled to room temperature to obtain nano nickel.
8. The method for preparing nano nickel according to claim 1, wherein the reducing atmosphere is one of hydrogen or ethanol or a combination thereof.
9. The method for preparing nano nickel according to claim 7, wherein the reducing atmosphere is hydrogen: during the thermal decomposition and reduction reaction of the nickel carbonate, hydrogen is continuously introduced, and the introduction amount of the hydrogen is more than 1 time of the amount of the nickel carbonate.
10. The nano nickel prepared by the preparation method of any one of claims 1 to 9.
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| CN113003618A (en) * | 2021-03-01 | 2021-06-22 | 杭州申柯新材料有限公司 | Production line for producing high-purity nickel protoxide by direct oxidation method of metallic nickel and production process thereof |
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| WO2021022801A1 (en) | 2021-02-11 |
| CN112317758B (en) | 2023-05-19 |
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