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A kind of preparation method of ferric niobate superfine powder
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A technology of ultra-fine powder and ultra-fine powder, which is applied in chemical instruments and methods, iron compounds, inorganic chemistry, etc., and can solve the problem of long synthesis process, inability to stably prepare ultra-fine ferric niobate powder, complex and cumbersome synthesis steps, etc. problems, to achieve the effects of short preparation time, good electrocatalytic activity, and short process flow
Active Publication Date: 2021-03-23
INNER MONGOLIA UNIVERSITY
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[0003] At present, one method of preparing ferric niobate is to use iron oxide and niobium pentoxide as raw materials, and adopt a calcination method in an air atmosphere. The temperature is as high as 1000 ° C, and the calcination time is as long as 24 hours. Preparation method; the other uses iron oxide and niobium trioxide as raw materials, the calcination temperature is 900-1250°C, and the calcination time is 48h; in addition, there is another method that first uses niobium pentoxide and molten potassium hydroxide as The raw material is a potassium niobate salt obtained by recrystallization, and then hydrothermally reacted with ferric sulfate at 180°C for 12 hours, and finally calcined at 800°C for 2 hours to obtain FeNb 2 o 6 products, but this method has a long synthesis process and complex and cumbersome synthesis steps; most importantly, none of the above methods can stably prepare spherical or rod-shaped iron niobate ultrafine powders
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Embodiment 1
[0032] (1) Accurately weigh 1.5g of FeCl 3 ·6H 2 O and 1.98g of Nb(OH) 5 , mix the two evenly, and ultrasonically disperse in 100ml absolute ethanol for 30min to form a homogeneous suspension;
[0033] (2) Then put the above suspension in an oven, dry it at 110°C for 10 hours, and grind the dried substance to obtain a yellow powder, which is the precursor;
[0034] (3) Place the precursor in a tube furnace, heat up to 800°C at a rate of 5°C / min in an Ar atmosphere, calcinate for 2 hours, and cool the furnace to room temperature naturally to obtain an ultrafine powder.
Embodiment 2
[0036] (1) Accurately weigh 1.5g of FeCl 3 ·6H 2 O and 1.98g of Nb(OH) 5 , mix the two evenly, and ultrasonically disperse in 100ml absolute ethanol for 30min to form a homogeneous suspension;
[0037] (2) Then put the above suspension in an oven, dry it at 110°C for 10 hours, and grind the dried substance to obtain a yellow powder, which is the precursor;
[0038] (3) Put the precursor in a tube furnace, raise the temperature to 800°C at a rate of 10°C / min in an Ar atmosphere, calcinate for 2 hours, and wait for the furnace to cool naturally to room temperature to obtain ultrafine powder.
Embodiment 3
[0040] (1) Accurately weigh 1.5g of FeCl 3 ·6H 2 O and 1.98g of Nb(OH) 5 , mix the two evenly, and ultrasonically disperse in 100ml absolute ethanol for 30min to form a homogeneous suspension;
[0041] (2) Then put the suspension in an oven, dry it at 100°C for 10 hours, and grind the dried substance to obtain a yellow powder, which is the precursor;
[0042] (3) Put the precursor in a tube furnace, raise the temperature to 900°C at a rate of 3°C / min in an Ar atmosphere, calcinate for 2h, and wait for the furnace to cool down to room temperature naturally to obtain an ultrafine powder.
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Abstract
The invention discloses a preparing method of iron niobate ultrafine powder. The preparing method comprises the steps of 1, preparing a precursor, and 2, preparing a finished product. The method for producing rodlike iron niobate is simple and low in cost and facilitates industrialization. Ferric trichloride and niobium hydroxide serve as raw materials, firstly, the precursor is prepared, then calcination is conducted at the temperature of 900 DEG C or below, and the rodlike large-specific-surface-area FeNb2O6 ultrafine powder can then be obtained. Through a solid-phase calcination method, theiron niobate ultrafine powder is synthesized in one step, the technological process is short, the synthesis steps are simple, and an electrocatalyst in an electrode material of a fuel cell has important practical significance.
Description
Technical field: [0001] The invention relates to a preparation method of ultrafine powder, in particular to a preparation method of iron niobate ultrafine powder. Background technique: [0002] Iron Niobate (FeNb 2 o 6 ) has good thermal stability and chemical stability. It is a semiconductor material with certain conductivity and certain magnetism. It is used as an electrode material and can improve the electrocatalytic activity of the electrode. It is used in fuel cells, supercapacitors, Lithium-ion batteries and other electrode materials have a wide range of applications. With the development of the human economy, the demand for fossil energy is increasing day by day, but the reserves of fossil energy are limited, and the energy crisis will be a major problem facing the world. In addition, fossil fuels cause environmental pollution and affect human health. Therefore, seeking sustainable and clean energy has become a major issue that countries around the world urgently...
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