Preparation method of fluffy nano yttrium oxide powder

Abstract

The invention discloses a preparation method of fluffy nano yttrium oxide powder, and belongs to the technical field of synthesis of superfine nano powder. The preparation method comprises steps of firstly mixing yttrium-containing inorganic salt, de-ionized water and a complexing agent, and uniformly stirring at room temperature to obtain slurry containing yttrium, wherein the weight ratio of the yttrium-containing inorganic salt to the complexing agent is 8 to (0.5-10), and when a target product is RE: Y2O3, the yttrium-containing inorganic salt is doped with rare earth ions; calcining the slurry or sol or xerogel obtained from the slurry at 400-900 DEG C, and decomposing sufficiently to obtain fluffy Y2O3 or RE: Y2O3 nano powder. By preparing the nano yttrium oxide which is small in agglomeration, small in grain size and narrow in distribution by the novel complexing agent through a calcining method, the preparation method disclosed by the invention can effectively avoid later treatment such as breaking and grinding on a prepared sample. The method is simple to operate, low in synthesis temperature, short in cycle and easy for industrialization; the method is beneficial for preparing multi-element doped composite yttrium oxide nano powder; and by controlling addition of the complexing agent, nano powder distributed in different grain size intervals can be prepared.

Description

technical field

[0001] The invention belongs to the field of preparation of ultrafine powders, and more specifically relates to a method for preparing fluffy nanometer yttrium oxide (including doped yttrium oxide) powder. Background technique

[0002] Yttrium oxide is an extremely important rare earth oxide, insoluble in water and alkali, soluble in acid, easy to absorb carbon dioxide and water in the air, and also has high electricity price, 4f unique to rare earth elements r 5d x 6l 2 Excellent properties such as electronic shell structure, large radius, strong polarizing force, and lively chemical properties. Because of its excellent heat resistance, corrosion resistance, high temperature stability, and dielectric constant of 12-20, it has become an important industrial material. In optical materials, high-tech ceramics, battery materials, magnetic materials, luminescent materials, etc. For yttrium oxide nanopowders, high purity and specific surface area, small partic...

Examples

example 1

[0047] Nd:Y as required 2 o 3 Weigh the corresponding Y(NO 3 ) 3 ·6H 2 O. The present invention weighs 7.871g Y(NO 3 ) 3 ·6H 2 O and 0.474g of Nd(NO 3 ) 3 ·6H 2 O as an example, dissolve it in a small amount of deionized water to form a nitrate solution; weigh 2g of polyacrylic acid as a complexing agent and fuel, add it to the fully dissolved yttrium nitrate solution, and stir evenly with a glass rod. Pour the prepared reaction solution directly into a crucible, put it into a muffle furnace for calcination, and calcine at a temperature of 500°C, and directly lower the temperature to obtain a fluffy ultrafine product.

[0048] The prepared nano-powder was subjected to X-ray diffraction analysis (XRD) to analyze the phase of the nano-powder, and the morphology and particle size of the powder were observed by using a transmission electron microscope (TEM).

[0049] The above Nd:Y 2 o 3 For XRD analysis of nano powder, see figure 2 In the lowermost curve, it can be...

example 2-21

[0052] The preparation process of Example 2-21 is the same as Example 1. The raw materials, complexing agents and process parameters used are shown in Table 1, and Example 21 is a comparative example.

[0053] Nd prepared by embodiment 2-3: Y 2 o 3 The XRD phase analysis such as figure 2 As shown, the graph does not show other impurity phases, the phase is pure, and the crystallinity is good. Y of instance 2 2 o 3 The scanning electron microscope picture is Figure 4 ,Compared Figure 10 It can be seen that the particles basically remain spherical, and the dispersibility is obviously improved. The particle size is between 20 and 70 nm, and the distribution range is narrow.

[0054] The Y prepared by embodiment 4-8 2 o 3 The XRD phase analysis such as Figure 5 Shown, the Y prepared by embodiment 9-11 2 o 3 The XRD phase analysis such as Image 6 Shown; Y prepared by embodiment 11-13 2 o 3 The XRD phase analysis such as Figure 7 Shown; Y prepared by embodiment ...

technical field

[0001] The invention belongs to the field of preparation of ultrafine powders, and more specifically relates to a method for preparing fluffy nanometer yttrium oxide (including doped yttrium oxide) powder. Background technique

[0002] Yttrium oxide is an extremely important rare earth oxide, insoluble in water and alkali, soluble in acid, easy to absorb carbon dioxide and water in the air, and also has high electricity price, 4f unique to rare earth elements r 5d x 6l 2 Excellent properties such as electronic shell structure, large radius, strong polarizing force, and lively chemical properties. Because of its excellent heat resistance, corrosion resistance, high temperature stability, and dielectric constant of 12-20, it has become an important industrial material. In optical materials, high-tech ceramics, battery materials, magnetic materials, luminescent materials, etc. For yttrium oxide nanopowders, high purity and specific surface area, small partic...

Examples

example 1

[0047] Nd:Y as required 2 o 3 Weigh the corresponding Y(NO 3 ) 3 ·6H 2 O. The present invention weighs 7.871g Y(NO 3 ) 3 ·6H 2 O and 0.474g of Nd(NO 3 ) 3 ·6H 2 O as an example, dissolve it in a small amount of deionized water to form a nitrate solution; weigh 2g of polyacrylic acid as a complexing agent and fuel, add it to the fully dissolved yttrium nitrate solution, and stir evenly with a glass rod. Pour the prepared reaction solution directly into a crucible, put it into a muffle furnace for calcination, and calcine at a temperature of 500°C, and directly lower the temperature to obtain a fluffy ultrafine product.

[0048] The prepared nano-powder was subjected to X-ray diffraction analysis (XRD) to analyze the phase of the nano-powder, and the morphology and particle size of the powder were observed by using a transmission electron microscope (TEM).

[0049] The above Nd:Y 2 o 3 For XRD analysis of nano powder, see figure 2 In the lowermost curve, it can be...

example 2-21

[0052] The preparation process of Example 2-21 is the same as Example 1. The raw materials, complexing agents and process parameters used are shown in Table 1, and Example 21 is a comparative example.

[0053] Nd prepared by embodiment 2-3: Y 2 o 3 The XRD phase analysis such as figure 2 As shown, the graph does not show other impurity phases, the phase is pure, and the crystallinity is good. Y of instance 2 2 o 3 The scanning electron microscope picture is Figure 4 ,Compared Figure 10 It can be seen that the particles basically remain spherical, and the dispersibility is obviously improved. The particle size is between 20 and 70 nm, and the distribution range is narrow.

[0054] The Y prepared by embodiment 4-8 2 o 3 The XRD phase analysis such as Figure 5 Shown, the Y prepared by embodiment 9-11 2 o 3 The XRD phase analysis such as Image 6 Shown; Y prepared by embodiment 11-13 2 o 3 The XRD phase analysis such as Figure 7 Shown; Y prepared by embodiment ...

Images