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Nickel powder and production method thereof

A manufacturing method, micropowder technology, applied in the direction of transportation and packaging, metal processing equipment, etc., can solve the problems of shrinkage characteristics without any disclosure, thick oxide film thickness, difficult to form thickness, etc., to prevent discontinuity or peeling, crystallinity Excellent, prevent cracking or peeling effect

Active Publication Date: 2012-09-12
SUMITOMO METAL MINING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0023] However, in this proposal, although the oxidation resistance of the obtained nickel powder is evaluated, there is no disclosure on the shrinkage characteristics during firing.
In addition, nothing is said about the decomposition behavior of the above-mentioned debinders
In addition, since the fine nickel powder is brought into contact with an oxidizing gas at a high temperature, the nickel powder may spontaneously ignite due to rapid oxidation.
Therefore, the thickness of the oxide film becomes thick, and it is presumed that it is difficult to form an appropriate thickness.

Method used

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  • Nickel powder and production method thereof
  • Nickel powder and production method thereof
  • Nickel powder and production method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0137] Ignite the high-frequency plasma with the plasma input power of about 60kW, adjust the total amount of argon to 209L / min, hydrogen to 45L / min, and ambient gas pressure to 60kPa to obtain a stable plasma flame. A nickel raw material was supplied to the inside of the plasma flame at 1 kg / hr by carrying gas (argon 10 liters / minute) to prepare fine powder.

[0138] In addition, as a nickel raw material, 90 mass % of nickel powder (nickel, Type 255, average particle diameter of 2.2 to 2.8 μm, manufactured by Inco Special Products and Inco Limited) was mixed with 10 mass % of nickel oxide (approximately 2 mass % sulfur) nickel raw material. The sulfur content in the nickel raw material was 0.2% by mass, and the oxygen content was 2% by mass.

[0139] The temperature of the plasma is 10000° C. or higher, so the nickel raw material powder evaporates and gasifies instantaneously, and then condenses in the low-temperature plasma tail flame to be pulverized. The obtained microni...

Embodiment 2

[0143] Except having changed the hydrogen gas supplied to the plasma to 9 L / min, it carried out similarly to Example 1, obtained nickel fine powder, and evaluated it. The BET diameter of nickel fine powder is 152nm. Analyze this nickel micropowder by XRD, adopt the grain size that Scherrer method obtains to be The crystal grain size was 85% of the BET diameter, and it was found that nickel fine powder having a crystallinity close to a single crystal was formed. The sulfur and oxygen contents were 0.24% by mass and 1.0% by mass, respectively. Based on the measurement results of TMA, the shrinkage initiation temperature was about 360° C., and the shrinkage rate was 7.9%. Each evaluation result is shown in Table 1 together with other examples.

[0144] Furthermore, as a result of FE-AES analysis, the thickness of the oxygen-containing coating layer was as thin as 14 nm. Also, the thickness of the sulfur-containing layer was 8 nm. The thickness of each layer is shown togethe...

Embodiment 3

[0146] Except having used the following nickel powder as nickel powder, it carried out similarly to Example 1, obtained the nickel fine powder, and evaluated it. Add 4kg of nickel powder (nickel, Type255, average particle size 2.2-2.8μm, manufactured by Inco Special Products and Inco Limited) to 16L of pure water adjusted to 50°C, add 18g of sodium hydrosulfide hydrate (Sodium hydrosulfide n- hydrate), stirred for 30 minutes. Then, repulp (Repulp) was performed once, and after filtering and vacuum-drying (36 hours), it crushed and was used as a nickel raw material. The sulfur content in the nickel raw material was 0.2% by mass, and the oxygen content was 0.4% by mass.

[0147] The BET diameter of nickel micropowder is 125nm. Analyze this nickel micropowder by XRD, adopt the grain size that Scherrer method obtains to be The crystal grain size was 75% of the BET diameter, and it was found that nickel fine powder having a crystallinity close to a single crystal was formed. T...

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Abstract

Disclosed is a nickel powder having excellent crystallinity and a high shrink temperature, inhibiting sintering contraction even at high temperatures without affecting the decomposition temperature of the resin binder. Also provided is a production method for the nickel powder. The average particle diameter of the nickel powder is 0.05 - 0.3[Mu]m, crystalline diameter is 60% - 90% of specific surface area diameter, sulphur content is 0.1% - 0.5% by weight, and oxygen content is 0.4% - 1.5% by weight. The powder has a 2 - 15nm thick oxygen-containing surface coating layer with an outermost surface formed from a mixture of a nickel-sulphur compound and a nickel-oxygen compound. Furthermore, in x-ray photoelectron spectroscopy analysis, the outermost layer should preferably have an abundance ratio of 50% - 100% nickel sulphide in the sulphur compound and an abundance ratio of 0% - 50% of nickel hydroxide in the nickel-oxygen compound.

Description

technical field [0001] The invention relates to a nickel micropowder and a manufacturing method thereof. More specifically, it relates to nickel fine powder used as an electrode material for electronic components such as internal electrodes of a multilayer ceramic capacitor, and a method for producing the same. [0002] This application claims priority based on Japanese Patent Application No. "Japanese Patent Application No. 2009-219286" filed on September 24, 2009 in Japan, and the above application is cited for reference in this application. Background technique [0003] In recent years, there has been a demand for miniaturization of electronic devices, and in order to meet this demand, finer nickel powders used as materials for components of electronic devices have also been required to be more finely divided. For example, in multilayer ceramic capacitors (MLCC: Multilayer Ceramic Capacitor), it is required to reduce the particle size of nickel fine powder in order to co...

Claims

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Application Information

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IPC IPC(8): B22F1/02B22F1/00B22F9/02B22F1/16
CPCB22F9/12B22F2999/00C22C19/03B22F1/16B22F2202/13B22F9/02B22F2301/15
Inventor 川上裕二石田荣治田中宏幸冈田美香金子勋
Owner SUMITOMO METAL MINING CO LTD
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