CN109530715B - Preparation method of nickel nano powder for ceramic capacitor - Google Patents
Preparation method of nickel nano powder for ceramic capacitor Download PDFInfo
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- CN109530715B CN109530715B CN201811524720.2A CN201811524720A CN109530715B CN 109530715 B CN109530715 B CN 109530715B CN 201811524720 A CN201811524720 A CN 201811524720A CN 109530715 B CN109530715 B CN 109530715B
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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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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a method for preparing nickel nano powder for a ceramic capacitor, which comprises the steps of firstly, preparing a mixed solution of acetic acid and nickel sulfate according to a proportion, uniformly mixing the mixed solution at a certain temperature heated by an oil bath, regulating the pH value by using alkali liquor, drying the prepared mixed solution, grinding the dried mixed solution, pressing the ground mixed solution into a columnar blank body, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank body, quickly placing the columnar blank body in a muffle furnace heated to a certain temperature, and then reducing the obtained powder in a vacuum furnace by using hydrogen to obtain the nickel nano powder. The preparation method of the nickel nano powder for the ceramic capacitor has simple preparation process, can be produced without special equipment, and effectively reduces the production cost; the prepared nickel nano powder has high purity and narrow particle size distribution and can be stored for a long time.
Description
Technical Field
The invention belongs to the technical field of conductive slurry preparation, and particularly relates to a preparation method of nickel nano powder for a ceramic capacitor.
Background
When the material reaches the nanometer level, some properties of the material are mutated, so that the material has more special properties. The grain size, surface state, microstructure and micro-morphology of the nano material have direct influence on the physical and chemical properties and application of the nano material. As the size of the material is reduced to the nanometer level, the material may have singular characteristics such as small-size effect, quantum size effect, macroscopic quantum tunneling effect, etc., and thus the nano material will be one of the main development directions in the future.
In recent years, nickel nano powder is a novel nano material, and the potential application value of the nickel nano powder is attracted by wide attention. Research shows that the nickel nano material has excellent performances in magnetism, catalysis and other performances and has wide application prospects in many aspects. At present, the method for preparing nickel nano powder mainly comprises an electric explosion method, a mechanical ball milling method, a sol-gel method and the like. Although the electric explosion method is a commonly used method for preparing nickel nano powder, the equipment cost investment is large, the collected powder is easy to oxidize, and the particle size distribution of the powder is not uniform; the nickel nano powder prepared by the mechanical ball milling method is mostly flaky, and the nickel slurry used in the ceramic capacitor is mostly spherical and can not meet the requirement. The sol-gel method is a main development trend for preparing nickel nano powder in the future due to simple process and controllable process parameters.
Disclosure of Invention
The invention aims to provide a preparation method of nickel nano powder for a ceramic capacitor, the nickel nano powder prepared by the method has higher purity and narrower particle size distribution, and the cost for producing the nickel nano powder is effectively reduced.
The technical scheme adopted by the invention is that the preparation method of the nickel nano powder for the ceramic capacitor is implemented according to the following steps:
step 1, preparing a mixed solution of acetic acid and nickel sulfate;
step 2, placing the mixed solution prepared in the step 1 in an oil bath, mechanically stirring to uniformly mix the mixed solution, and adjusting the pH value of the mixed solution to 2-4 by using alkali liquor;
step 3, drying the mixed solution prepared in the step 2, grinding the dried mixed solution into powder, and pressing the powder into a columnar green body; the particle size of the ground powder is 1 um-5 um;
step 4, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank, and immediately placing the mixture in a muffle furnace with the preheating temperature of 700-800 ℃ to obtain powder;
and 5, reducing the powder obtained in the step 4 in a vacuum furnace by using hydrogen to obtain the nickel nano powder.
The present invention is also characterized in that,
in the step 1, the molar ratio of nickel sulfate to acetic acid is 1: 1-4, wherein the mass ratio of nickel sulfate to deionized water is 1: 0.2 to 0.5.
In the step 2, the temperature of the oil bath is 60-80 ℃, and the stirring time is 1-4 h.
In the step 2, the alkali liquor is sodium hydroxide solution or potassium hydroxide solution, and the concentration of the sodium hydroxide solution and the concentration of the potassium hydroxide solution are both 0.1-0.5 mol/L.
In the step 3, the drying temperature is 70-90 ℃.
In the step 4, the molar ratio of polytetrafluoroethylene to silicon in the mixed powder is 1-2: 1; the thickness of the mixed powder placed at the upper end and the lower end of the columnar blank body is 1 mm-2 mm.
In the step 5, the reduction temperature is 250-350 ℃, the heat preservation time is 2-5 h, and the hydrogen flow is 100-200 ml/min.
The beneficial effect of the invention is that,
the nickel nano powder prepared by the method has high purity and narrow particle size distribution, can be stored for a long time, has simple preparation flow, can be produced without special equipment, and effectively reduces the production cost.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of nickel nano powder for a ceramic capacitor, which is implemented according to the following steps:
step 1, preparing a mixed solution of acetic acid and nickel sulfate;
wherein the molar ratio of nickel sulfate to acetic acid is 1: 1-4, wherein the mass ratio of nickel sulfate to deionized water is 1: 0.2 to 0.5;
step 2, placing the mixed solution prepared in the step 1 in an oil bath, mechanically stirring to uniformly mix the mixed solution, and adjusting the pH value of the mixed solution to 2-4 by using alkali liquor;
wherein the temperature of the oil bath is 60-80 ℃, and the stirring time is 1-4 h;
the alkali liquor is sodium hydroxide solution or potassium hydroxide solution, and the concentration of the sodium hydroxide solution and the concentration of the potassium hydroxide solution are both 0.1-0.5 mol/L;
step 3, drying the mixed solution prepared in the step 2 at 70-90 ℃, grinding into powder, and pressing into a columnar green body;
the particle size of the ground powder is 1 um-5 um;
step 4, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank, and immediately placing the mixture in a muffle furnace with the preheating temperature of 700-800 ℃ to obtain powder;
wherein the molar ratio of polytetrafluoroethylene to silicon in the mixed powder is 1-2: 1;
the thickness of the mixed powder placed at the upper end and the lower end of the columnar blank body is 1 mm-2 mm;
step 5, reducing the powder obtained in the step 4 in a vacuum furnace by using hydrogen to obtain nickel nano powder;
wherein the reduction temperature is 250-350 ℃, the heat preservation time is 2-5 h, and the hydrogen flow is 100-200 ml/min.
The invention relates to a method for preparing nickel nano powder for a ceramic capacitor, which comprises the steps of preparing a mixed solution of acetic acid and nickel sulfate according to a proportion, uniformly mixing the mixed solution at a certain temperature heated by an oil bath, adjusting the pH value by using sodium hydroxide or potassium hydroxide, drying the prepared mixed solution, grinding the dried mixed solution, pressing the ground mixed solution into a columnar blank body, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank body, rapidly placing the columnar blank body in a muffle furnace heated to a certain temperature, and reducing the obtained powder in a vacuum furnace by using hydrogen to obtain the nickel nano powder.
Example 1
According to the molar ratio of nickel sulfate to acetic acid of 1: 1, and mixing nickel sulfate and deionized water according to a mass ratio of 1: adding deionized water in an amount of 0.2 to prepare a mixed solution;
step 2, uniformly mixing the mixed solution prepared in the step 1 in an oil bath at 60 ℃ by adopting a mechanical stirring mode, wherein the stirring time is 1h, and adjusting the pH value of the mixed solution to 2 by using sodium hydroxide;
the concentration of the sodium hydroxide solution is 0.1 mol/L;
step 3, drying the mixed solution prepared in the step 2 at 70 ℃, grinding into powder, and pressing into a columnar green body;
the particle size of the ground powder is 1 um;
and 4, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank, wherein the molar ratio of the polytetrafluoroethylene to the silicon in the mixed powder is 1: 1, placing the mixed powder at two ends with the thickness of 1mm in a muffle furnace with the preheating temperature of 700 ℃ to obtain powder;
and 5, reducing the powder obtained in the step 4 in a vacuum furnace by using hydrogen, wherein the reduction temperature is 250 ℃, the heat preservation time is 2 hours, and the hydrogen flow is 100ml/min, so that the nickel nano powder can be obtained.
Example 2
Step 1, mixing nickel sulfate and acetic acid according to a molar ratio of 1: 4, and mixing nickel sulfate and deionized water according to a mass ratio of 1: adding deionized water in an amount of 0.5 to prepare a mixed solution;
step 2, uniformly mixing the mixed solution prepared in the step 1 in an oil bath at 80 ℃ by adopting a mechanical stirring mode, wherein the stirring time is 4h, and adjusting the pH value of the mixed solution to 4 by using sodium hydroxide;
the concentration of the sodium hydroxide solution is 0.3 mol/L;
step 3, drying the mixed solution prepared in the step 2 at 90 ℃, grinding, and pressing into a columnar green body;
the particle size of the ground powder is 2 um;
and 4, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank body, wherein the molar ratio of the mixed powder to the polytetrafluoroethylene to the silicon is 2: 1, placing the mixed powder at two ends with the thickness of 2mm in a muffle furnace with the preheating temperature of 800 ℃ to obtain powder;
and 5, reducing the powder obtained in the step 4 in a vacuum furnace by using hydrogen, wherein the reduction temperature is 350 ℃, the heat preservation time is 5 hours, and the hydrogen flow is 200ml/min, so that the nickel nano powder can be obtained.
Example 3
Step 1, mixing nickel sulfate and acetic acid according to a molar ratio of 1: 4, and mixing nickel sulfate and deionized water according to a mass ratio of 1: adding deionized water in an amount of 0.5 to prepare a mixed solution;
step 2, uniformly mixing the mixed solution prepared in the step 1 in an oil bath at 80 ℃ by adopting a mechanical stirring mode, wherein the stirring time is 3 hours, and adjusting the pH value of the mixed solution to 3 by using a sodium hydroxide solution;
the concentration of the sodium hydroxide solution is 0.5 mol/L;
step 3, drying the mixed solution prepared in the step 2 at 90 ℃, grinding, and pressing into a columnar green body;
the particle size of the ground powder is 4 um;
and 4, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank body, wherein the molar ratio of the mixed powder to the polytetrafluoroethylene to the silicon is 2: 1, placing the mixed powder at two ends with the thickness of 1.5mm in a muffle furnace with the preheating temperature of 750 ℃ to obtain powder;
and 5, reducing the powder obtained in the step 4 in a vacuum furnace by using hydrogen, wherein the reduction temperature is 300 ℃, the heat preservation time is 4 hours, and the hydrogen flow is 150ml/min, so that the nickel nano powder can be obtained.
Example 4
Step 1, mixing nickel sulfate and acetic acid according to a molar ratio of 1: 2, and mixing nickel sulfate and deionized water according to a mass ratio of 1: adding deionized water in an amount of 0.4 to prepare a mixed solution;
step 2, uniformly mixing the mixed solution prepared in the step 1 in an oil bath at 70 ℃ by adopting a mechanical stirring mode, wherein the stirring time is 4h, and adjusting the pH value of the mixed solution to 3 by using a potassium hydroxide solution;
the concentration of the potassium hydroxide solution is 0.1 mol/L;
step 3, drying the mixed solution prepared in the step 2 at 80 ℃, grinding, and pressing into a columnar green body;
the particle size of the ground powder is 5 um;
and 4, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank body, wherein the molar ratio of the mixed powder to the polytetrafluoroethylene to the silicon is 2: 1, placing the mixed powder at two ends with the thickness of 2mm in a muffle furnace with the preheating temperature of 800 ℃ to obtain powder;
and 5, reducing the powder obtained in the step 4 in a vacuum furnace by using hydrogen, wherein the reduction temperature is 350 ℃, the heat preservation time is 2 hours, and the hydrogen flow is 200ml/min, so that the nickel nano powder can be obtained.
The particle size distribution of the nickel nanopowders prepared in examples 1-4 was as shown in table 1 by passing them through a laser particle size analyzer, and it can be seen from table 1 that the nickel nanopowders prepared by the method of the present invention have a narrow particle size distribution and a high purity, and can be stored for a long period of time.
TABLE 1 particle size distribution of nickel nanopowders prepared in examples 1-4
The preparation method of the nickel nano powder for the ceramic capacitor has simple preparation process, can be produced without special equipment, and effectively reduces the production cost; the nano nickel slurry prepared from the nickel nano powder prepared by the method can be used for inner electrodes of multilayer ceramic capacitors, and has no lead and cadmium components and no pollution.
Claims (4)
1. A preparation method of nickel nano powder for ceramic capacitors is characterized by comprising the following steps:
step 1, preparing a mixed solution of acetic acid and nickel sulfate; the molar ratio of nickel sulfate to acetic acid is 1: 1-4, wherein the mass ratio of nickel sulfate to deionized water is 1: 0.2 to 0.5;
step 2, placing the mixed solution prepared in the step 1 in an oil bath, mechanically stirring to uniformly mix the mixed solution, and adjusting the pH value of the mixed solution to 2-4 by using alkali liquor; the alkali liquor is sodium hydroxide solution or potassium hydroxide solution, and the concentration of the sodium hydroxide solution and the concentration of the potassium hydroxide solution are both 0.1-0.5 mol/L;
step 3, drying the mixed solution prepared in the step 2, grinding the dried mixed solution into powder, and pressing the powder into a columnar green body; the particle size of the ground powder is 1 um-5 um;
step 4, placing mixed powder of polytetrafluoroethylene and silicon at the upper end and the lower end of the columnar blank, and immediately placing the mixture in a muffle furnace with the preheating temperature of 700-800 ℃ to obtain powder;
the molar ratio of polytetrafluoroethylene to silicon in the mixed powder is 1-2: 1; the thickness of the mixed powder placed at the upper end and the lower end of the columnar blank body is 1 mm-2 mm;
and 5, reducing the powder obtained in the step 4 in a vacuum furnace by using hydrogen to obtain the nickel nano powder.
2. The method for preparing nickel nanopowder for ceramic capacitors as claimed in claim 1, wherein in step 2, the temperature of the oil bath is 60-80 ℃ and the stirring time is 1-4 h.
3. The method for preparing the nickel nano-powder for the ceramic capacitor as claimed in claim 1, wherein in the step 3, the drying temperature is 70-90 ℃.
4. The method for preparing the nickel nano powder for the ceramic capacitor as claimed in claim 1, wherein in the step 5, the reduction temperature is 250-350 ℃, the heat preservation time is 2-5 h, and the hydrogen flow is 100-200 ml/min.
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| CN101088962A (en) * | 2006-06-14 | 2007-12-19 | 中国科学院理化技术研究所 | Chemically excited combustion process for synthesizing Si3N4/SiC composite powder |
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| CN100363134C (en) * | 2005-11-25 | 2008-01-23 | 北京科技大学 | Method for preparing nano nickel powder by precipitation-hydrogen reduction process |
| KR101191970B1 (en) * | 2011-12-09 | 2012-10-17 | 한화케미칼 주식회사 | Phosphorous-doped nickel nano-particles and process for preparing the same |
| JP2015078425A (en) * | 2013-10-16 | 2015-04-23 | サムソン エレクトロ−メカニックス カンパニーリミテッド． | Nickel nano powder and production method thereof |
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Application publication date: 20190329 Assignee: Pucheng Zhenggong Gas Co.,Ltd. Assignor: XI'AN POLYTECHNIC University Contract record no.: X2023980034734 Denomination of invention: A Preparation Method of Nickel Nanoparticles for Ceramic Capacitors Granted publication date: 20211214 License type: Common License Record date: 20230419 |