Preparation method of nanometer sized superfine ferro nickel alloy powder

A nickel-iron alloy, nano-level technology is applied in the field of preparation of nano-level ultra-fine nickel-iron alloy powder, which can solve the problems of inability to large-scale production, serious environmental pollution, large equipment investment, etc. The effect of narrow particle size distribution

Inactive Publication Date: 2005-03-16

UNIV OF SCI & TECH BEIJING

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Problems solved by technology

The aqueous solution reduction method can produce nano-scale (<100nm) nickel powder, but the cost is too high to be mass-produced

The carbonyl method is recognized in the world as an ideal method for producing ultrafine (0.5-6 μm) nickel powder and nickel-iron alloy powder, but its process is complicated, equipment investment is large, and en...

Abstract

The invention relates to a method of making nanometer ferronickel powder. Transform ferronickel sulfate solution or ferronickel azotate solution into nanometer NiO.FeO powder by low temperature supersound atomization hot transformation. Then wash the powder carefully, remove acid radical and the remnants water by centrifugation or heating to get the dry composite oxide. Then deoxidize the powder with hydrogen in tubing furnace at the low temperature of 650-700DEG C. Using the method, compound of the ferronickel is decided on the solution compound, and is well-proportioned. Grain size of average particle is equal as or bigger than 80mm. the particle is round and suited to mass production.

Technology Topic

Nanometer sizeComposite oxide +9

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Experimental program(2)

Example Embodiment

[0048] Example 1: Prepare 1kg of nano nickel-iron alloy powder, when the composition is Ni:Fe=3:1, it should be completed according to the following steps.

[0049] 1. Weigh 1244.52 grams of FeSO respectively 4 ·7H 2 O and 3357.8 grams of NiSO 4 ·6H 2 The O powder was added to 10 liters of distilled water, heated to 60°C and stirred continuously. After completely dissolved, the foreign impurities were filtered with a 40μm screen, and the solution was transferred to the atomizing liquid tank.

[0050] 2. Airflow ultrasonic spray thermal conversion, using annular slot resonance airflow ultrasonic atomizing nozzle with jet angle α=45°, jet pressure (air) 2.5MPa, hot air temperature 128℃, air jet velocity 2~2.5 Mach number, liquid flow The conveying speed is 200ml/min, and the dry precursor powder can be obtained after all the solution is atomized, and it is transferred to the repeated cleaning stage.

[0051] 3. Repeated cleaning, centrifugal separation, add distilled water to the precursor powder according to the mass ratio of powder: water = 1:5, keep stirring, and remove SO 2- 4 Sulfate ions are dissolved in the water, then the turbid liquid is continuously added to the continuous centrifuge to remove the waste liquid, and then fresh distilled water is added, and the centrifuge is repeatedly stirred, washed, and centrifuged until the waste liquid is BaCL 2 In the test, when there is no white precipitation, the cleaning is completed, and the powder is taken out of the centrifuge to air dry and transferred to reduction.

[0052] 4. The air-dried precursor powder is roasted in a roasting furnace at 360°C and 50 minutes air atmosphere to further decompose and remove the residual water and trace acid radicals in the precursor powder.

[0053] 5. Shearing and crushing, according to the mass ratio of precursor powder: industrial alcohol = 1:5, add industrial alcohol and pour into the liquid tank of the shearing machine, and press (15 minutes/100 grams of powder) at a speed of 10000 rpm Calculate the shearing time, discharge the slurry after shearing, and separate the industrial alcohol with a continuous centrifuge. The slurry can be air-dried naturally.

[0054] 6. In the tubular reduction furnace at 650℃, 60 minutes, use H 2 Gas reduction, H 2 Air cross-section flow 30ml/cm 2 After the reduction process, 1kg of nano-nickel-iron alloy powder can be obtained. The reduced powder should be put into acetone-oleic acid solution immediately to prevent spontaneous combustion.

[0055] 7. The obtained powder is tested for BET specific surface XRD phase composition, TEM particle size and particle morphology.

[0056] 8. Product vacuum aluminum bag packaging.

Example Embodiment

[0057] Example 2 When preparing 10kg of nano nickel-iron alloy powder, and the alloy composition is Ni:Fe=3:1, the following steps should be followed to complete.

[0058] 1. Weigh Ni(NO 3 ) 2 ·6H 2 O, 37.1487kg; Fe(NO 3 ) 3 ·9H 2 O, 18.0851kg, crystal powder, added to 120 liters of distilled water, heated to 50°C in a stainless steel reaction tank, and after constant stirring to completely dissolve, inject the solution into the liquid tank of the atomization tower through a 44μm screen filter pipeline with a liquid pump Perform spray heat conversion.

[0059] 2. Air spray heat conversion

[0060] Using the annular slot resonance airflow ultrasonic atomization nozzle with jet angle α=45°, jet pressure (air) 3.5MPa, hot air temperature 68°C, liquid flow rate 200ml/min, dry precursor can be obtained after all the solution is atomized The bulk powder is transferred to the roasting process.

[0061] 3. Put the precursor powder obtained in the above 2 directly into a calcining furnace for roasting at a temperature of 450°C in an air atmosphere for 30 minutes. After being cooled out of the furnace, a dry composite oxide powder can be obtained. The shearing and crushing process should be transferred.

[0062] 4. According to the mass ratio of composite oxide powder: industrial alcohol = 1:5, add industrial alcohol and pour into the shearing machine tank together, calculate the shearing time according to (15 minutes/100g powder), and release the slurry after shearing , Separate the industrial alcohol with a continuous centrifuge, and transfer to the reduction process after the slurry is air-dried naturally

[0063] 5. In the tubular reduction furnace, use H at 700℃ for 45 minutes 2 Gas reduction, H 2 Cross-sectional flow 50ml/cm 2 , And the rest is exactly the same as 5 in Example 1.

[0064] 6 and 7 are exactly the same as 7 and 8 in Example 1.

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Classification and recommendation of technical efficacy words

low cost

Method, apparatus and article for microfluidic control via electrowetting, for chemical, biochemical and biological assays and the like

InactiveUS7163612B2low cost

Owner:KECK GRADUATE INST OF APPLIED LIFE SCI

Preparation method of nanometer sized superfine ferro nickel alloy powder

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

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Example Embodiment

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Description & Claims & Application Information

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