Method for preparing conductive powder by recoating aluminum-doped nano zinc oxide with aluminum

An aluminum-doped zinc oxide, conductive powder technology, applied in cable/conductor manufacturing, zinc oxide/zinc hydroxide, nanotechnology, etc., can solve the problems of high density and easy deposition, powder toxicity, serious particle agglomeration, etc. Achieving the effects of wide source of raw materials, alleviation of agglomeration and simple preparation process

Inactive Publication Date: 2014-02-12
JIANGSU DONGTAI FINE CHEM
6 Cites 9 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0002] Conductive powder mainly includes: ① metal powder such as gold, silver, copper, iron, nickel, etc., but because it is unstable in the air and easy to oxidize, its density is easy to deposit, which seriously affects its conductivity, so metal powder is gradually Replaced by emerging conductive powders; ②Carbon-based powders such as graphite, carbon black, etc., have better electrical conductivity, but because of their inherent blackness, their application range is greatly limited; ③Metal oxides such as tin oxide, oxide Antimony, indium oxide, tin-doped indium oxide (ITO), antimony-doped tin oxide (ATO), gallium-doped zinc oxide (ZGO), etc. Among them, the compounds for preparing tin oxide and antimony oxide have high or low toxicity , and ATO has blue-black color, indium oxide is very expensive, gallium and its compounds are highly toxic
[0003] Therefore, the application of the above-mentioned conductive powder is greatly limited, and aluminum-doped zinc oxide (ZAO) has many advantages such as wide source of raw materials, low cost, light color, non-toxicity, and high conductivity second only to ITO. And it is more and more favored by people, and will play an increasingly important role in the fields of electromagnetic wave shielding materials and anti-static coating materials...
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Abstract

The invention discloses a method for preparing conductive powder by recoating aluminum-doped nano zinc oxide with aluminum. The method comprises the following steps: firstly, preparing aluminum-doped zinc oxide powder; secondly, coating the aluminum-doped zinc oxide powder with an aluminum-containing film; finally, mixing the coated aluminum-doped zinc oxide powder with zinc powder, grinding, and calcining in an inert gas atmosphere to obtain the conductive powder. The method has the advantages that the zinc oxide conductive powder is prepared through primary aluminum doping and secondary aluminum coating, the primary aluminum doping improves the whiteness and the water dispersion of the nano zinc oxide and reduces the particle size of the nano zinc oxide, and the secondary aluminum coating further increases the defect concentration of zinc oxide crystals and improves the conductivity of the nano zinc oxide; the aluminum-doped zinc oxide is coated with a thin oxide film, so that zinc ions in water are unlikely to dissolve out, and the ball milling process of the zinc powder and the aluminum-doped zinc oxide is facilitated; the prepared conductive powder is high in conductive ability, small in particle size, light in color, wide in sources of raw materials, low in production cost, simple in preparation method, high in security, relatively light in environmental pollution, and suitable for industrial mass production.

Application Domain

Technology Topic

Examples

  • Experimental program(6)
  • Comparison scheme(4)

Example Embodiment

[0025] Example 1: (1) Add 1.2 kg of sodium lauryl sulfate to 100.0 kg of deionized water, stir and heat to 80°C, then add 518.4 g of aluminum sulfate and 28.8 kg of zinc sulfate to form a mixed solution, and then add to the mixed solution Add 1.0m/L sodium carbonate solution dropwise to it, control the pH of the system to 7 after the addition is complete, form a colloidal precipitation precursor, continue to stir and reflux for 2h, then wash, dry, and calcinate the colloidal precipitation precursor at 500℃ 2h to obtain aluminum-doped zinc oxide powder with an average particle size of 60nm;
[0026] (2) Add the obtained 14.6kg aluminum-doped zinc oxide powder to 146.0kg of deionized water to obtain aluminum-doped zinc oxide slurry with a solid content of 10%. The system is heated to 85°C, and the aluminum-doped zinc oxide is oxidized while stirring. Add 29.2L of 0.1m/L aluminum sulfate solution and 0.5m/L sodium carbonate solution in parallel to the zinc slurry to control the pH of the system to 8. After the addition, use 2.0m/L of sulfuric acid to adjust the pH of the system = 7, continue to stir and mature for 2h to obtain the precipitation precursor;
[0027] (3) Wash the obtained 14.9kg precipitation precursor with deionized water. When the conductivity of the filtrate is lower than 200μS/cm, end the washing and dry to obtain the white precursor; weigh 0.2kg zinc powder and the obtained white precursor Mix and grind into powder, and then calcinate under nitrogen atmosphere at 900℃ for 3h. After pulverization, aluminum-doped nano-zinc oxide re-coated aluminum conductive powder is obtained. Its average particle size is 80nm, volume resistivity is 10.0Ω·cm, and whiteness Is 75.1.

Example Embodiment

[0028] Example 2: (1) Add 2.0 kg of sodium dodecylbenzene sulfonate to 100.0 kg of deionized water, stir and heat to 45°C, then add 396.1 g of aluminum sulfate and 26.4 kg of zinc chloride to form a mixed solution, and then Add 3.0m/L ammonium bicarbonate solution dropwise to the mixed solution. After the addition, control the pH of the system to 9 to form a colloidal precipitation precursor. Continue stirring and reflux for 10 hours, and then wash, dry, and dry the colloidal precipitation precursor. Calcined at 300℃ for 2h to obtain aluminum-doped zinc oxide powder with an average particle size of 20nm;
[0029] (2) Add the obtained 15.8kg aluminum-doped zinc oxide powder to 79.0kg of deionized water to obtain an aluminum-doped zinc oxide slurry with a solid content of 20%. The system is heated to 50°C, and the aluminum-doped zinc oxide is oxidized while stirring. Add 2.96L 1.0m/L aluminum sulfate solution and 2.0m/L ammonium bicarbonate solution in parallel to the zinc slurry to control the pH of the system to 10. After the addition is complete, use 1.0m/L hydrochloric acid to adjust the system pH The value is 7, continue to stir and mature for 4h to obtain the precipitation precursor;
[0030] (3) Wash the obtained 16.1kg precipitated precursor with deionized water. When the conductivity of the filtrate is lower than 200μS/cm, end the washing and dry to obtain the white precursor; weigh 0.3kg of zinc powder and the obtained white precursor Mix and grind into powder, then calcined at 850℃ for 1h under nitrogen atmosphere, and obtain aluminum-doped nano-zinc oxide heavy-coated aluminum conductive powder after crushing. Its average particle size is 70nm, volume resistivity is 12.1Ω·cm, and whiteness It is 70.2.

Example Embodiment

[0031] Example 3: (1) Add 0.9kg of potassium higher fatty acid to 100.0kg of deionized water, stir and heat to 95°C, then add 519.2g of aluminum acetate and 25.9kg of zinc nitrate to form a mixed solution, and then add dropwise to the mixed solution 4.0m/L ammonia solution, control the pH of the system to 6 after the dropwise addition, form a colloidal precipitation precursor, continue to stir and reflux for 1 hour, then wash, dry, and calcinate the colloidal precipitation precursor at 600°C for 2 hours to obtain an average particle size Aluminum-doped zinc oxide powder with a diameter of 100nm;
[0032] (2) Add the obtained 7.2kg aluminum-doped zinc oxide powder to 48kg of deionized water to obtain an aluminum-doped zinc oxide slurry with a solid content of 15%. The system is heated to 95℃, and the aluminum-doped zinc oxide is added while stirring. Add 2.88L 0.5m/L aluminum sulfate solution and 2.0m/L ammonia solution to the slurry in parallel to control the pH of the system to 7, after the addition, adjust the pH of the system to 7 with 4.0m/L of acetic acid , Continue to stir and mature for 2h to obtain the precipitation precursor;
[0033] (3) Wash the obtained 7.4kg precipitated precursor with deionized water. When the conductivity of the filtrate is lower than 200μS/cm, finish the washing and dry to obtain the white precursor; weigh 0.1kg of zinc powder and the obtained white precursor It was mixed and ground into powder, and then calcined under argon atmosphere at 850℃ for 3h. After pulverization, aluminum-doped nano-zinc oxide re-coated aluminum conductive powder was obtained. Its average particle size was 100nm, volume resistivity was 13.4Ω·cm, white The degree is 73.5.
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PUM

PropertyMeasurementUnit
The average particle size60.0nm
The average particle size80.0nm
Volume resistivity10.0cm·Ω
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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