A kind of yttrium oxide powder and preparation method thereof
Technical field
The present invention relates to a kind of yttrium oxide powders and preparation method thereof, belong to a kind of material preparation process.
Background technique
With the progress of science and technology, superconductor, ceramic material, fluorescent material are grown rapidly, the preparation of rare earth powder
It is also had received widespread attention with application.Rare earth oxide yttrium oxide in high temperature alloy there is stronger oxide dispersion intensifying to make
With, and using more in fluorescent material, high-strength alloy and superalloy.Therefore being prepared into for yttrium oxide powder is ground
One of hot spot studied carefully.
Wang Ying etc. has delivered one in 2013 about the " growth of the rodlike yttrium oxide powder of hydrothermal synthesis in functional material
The research of journey and growth mechanism " report, specifically the preparation method comprises the following steps: 0.58g yttrium nitrate hexahydrate is dissolved in 10ml deionization
In water, ammonium hydroxide is then added, is added in constant temperature blender with magnetic force and stirs in drop, gained colloidal substance tune pH to 9, hydro-thermal reaction
Temperature control obtains oxygen in 80~180 DEG C of 2~8h of reaction, cooled product centrifugation, washing, drying at room temperature, 600 DEG C of high-temperature heat treatment 4h
Change yttrium nanometer rods.
Nanometer rods yttrium oxide is small with alloy contact face in alloy preparation process, cannot preferably strengthen stabilized matrix phase.
Therefore, the application prospect that a kind of yttrium oxide powder of large specific surface area has had is researched and developed.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of yttrium oxide powder, have obtained a kind of poplar of large specific surface area
Peach shape yttrium oxide powder.
The present invention second is designed to provide a kind of yttrium oxide powder obtained using above-mentioned preparation method, and shape is
Carambola shape.
To achieve the above object, the technical scheme is that
A kind of preparation method of yttrium oxide powder, comprising the following steps:
1) yttrium nitrate, glycerine, water are uniformly mixed and solution is made, then adjust pH to 8~10, then is anti-at 160~170 DEG C
14~16h is answered, reaction solution is obtained;
2) reaction solution obtained by step 1) is filtered, gained precipitating it is washed, dry precursor powder;
3) by 600~700 DEG C of 2~3h of calcining of precursor powder obtained by step 2) to obtain the final product.
Yttrium nitrate is yttrium nitrate hexahydrate in step 1).Water is deionized water in step 1).
Yttrium nitrate, glycerine, water are uniformly mixed to the specific steps that solution is made are as follows: first add in step 1) into yttrium nitrate
Enter glycerine, adds water.
Every 5g yttrium nitrate is corresponding in step 1) is added 10~15mL glycerine and 40~45mL water.
PH is adjusted to use ammonium hydroxide in step 1).
It is 10 that pH is preferably adjusted in step 1).
After pH to 8~10 is adjusted in step 1), solution is placed in autoclave, then react at 160~170 DEG C 14~
16h.The volume of the autoclave is 100mL.The compactedness of solution is 50%~70% in above-mentioned autoclave.
Vacuum filtration is filtered into step 2).
Washing is with deionized water to washing of precipitate 5~6 times in step 2).
Dry in step 2) is 60~80 DEG C of 4~6h of vacuum drying.
Gained precursor powder ground processing before calcination in step 2).
In step 3) after 600~700 DEG C of 2~3h of calcining, it is air-cooled to room temperature.
A kind of yttrium oxide powder that the preparation method using above-mentioned yttrium oxide powder obtains, shape are carambola shape.It is described
Yttrium oxide powder length direction average-size is about 6 μm.The yttrium oxide powder transverse direction average-size is about 2 μm.
It is intercrystalline that organic solvent glycerine obstruction is added using hydrothermal synthesis method in the preparation of yttrium oxide powder of the present invention
Reunite, realizes the transformation of shape, and glycerine is not involved in the precipitation reaction of yttrium nitrate and ammonium hydroxide.It is obtained using preparation method of the present invention
The submicron order carambola shape yttrium oxide powder arrived, large specific surface area have strong binding ability with metal material, as metal material
When the hardening constituent of material, the special groove structure of carambola shape yttrium oxide can be preferably fixed in the matrix of metal material, more be had
The growth of the limitation matrix of effect, keeps crystal grain more tiny, has widely application.
Detailed description of the invention
Fig. 1 is the XRD diagram of 1 gained yttrium oxide powder of embodiment;
Fig. 2 is that the SEM of 1 gained yttrium oxide powder of embodiment schemes.
Specific embodiment
Embodiments of the present invention are described further with reference to the accompanying drawing.
Embodiment 1
The preparation method of the present embodiment yttrium oxide powder, comprising the following steps:
1) yttrium nitrate hexahydrate 5g is weighed, glycerine 10mL is added, then adds 45mL deionized water, obtains solution A, to
Ammonium hydroxide tune pH=8 is instilled in solution A, obtains mixed solution B;
2) the mixed solution B that step 1) obtains is put into the autoclave of 100mL polytetrafluoroethyllining lining, in baking oven
In 170 DEG C of reaction 15h, the obtained precipitating of reaction is filtered by vacuum, is washed with deionized 5 times, 60 DEG C in drying box
It is dried in vacuo 4h, obtains precursor powder;
3) precursor powder for obtaining step 2) is ground, and then 600 DEG C of calcining 3h in Muffle furnace, are air-cooled to room temperature,
Obtain carambola shape yttrium oxide powder.
Embodiment 2
The preparation method of the present embodiment yttrium oxide powder, comprising the following steps:
1) yttrium nitrate hexahydrate 5g is weighed, glycerine 15mL is added, then adds 40mL deionized water, obtains solution A, to
Ammonium hydroxide tune pH=9 is instilled in solution A, obtains mixed solution B;
2) the mixed solution B that step 1) obtains is put into the autoclave of 100mL polytetrafluoroethyllining lining, in baking oven
In 160 DEG C of reaction 14h, the obtained precipitating of reaction is filtered by vacuum, is washed with deionized 5 times, 70 DEG C in drying box
It is dried in vacuo 5h, obtains precursor powder;
3) precursor powder for obtaining step 2) is ground, and then 700 DEG C of calcining 2h in Muffle furnace, are air-cooled to room temperature,
Obtain carambola shape yttrium oxide powder.
Embodiment 3
The preparation method of the present embodiment yttrium oxide powder, comprising the following steps:
1) yttrium nitrate hexahydrate 5g is weighed, glycerine 12mL is added, then adds 42mL deionized water, obtains solution A, to
Ammonium hydroxide tune pH=10 is instilled in solution A, obtains mixed solution B;
2) the mixed solution B that step 1) obtains is put into the autoclave of 100mL polytetrafluoroethyllining lining, in baking oven
In 170 DEG C of reaction 16h, the obtained precipitating of reaction is filtered by vacuum, is washed with deionized 6 times, 60 DEG C in drying box
It is dried in vacuo 4h, obtains precursor powder;
3) precursor powder for obtaining step 2) is ground, and then 600 DEG C of calcining 2h in Muffle furnace, are air-cooled to room temperature,
Obtain carambola shape yttrium oxide powder.
Experimental example 1
XRD test is carried out to 1 gained yttrium oxide powder of embodiment, as a result as shown in Figure 1.As shown in Figure 1, X-ray diffraction
Figure is completely the same with Jade standard card (NO.43-1036), and the powder reacted is Y2O3。
Embodiment 2
SEM test is carried out to 1 gained yttrium oxide powder of embodiment, as a result as shown in Fig. 2, as shown in Figure 2, gained yttrium oxide
Powder is carambola shape, has groove structure, particle is uniform, large specific surface area.