A kind of yttrium oxide powder and preparation method thereof
Technical field
The present invention relates to a kind of yttrium oxide powder and preparation method thereof, belong to a kind of material preparation process.
Background technology
With the progress of science and technology, superconductor, ceramic material, fluorescent material fast development, the preparation of rare earth powder
Extensive concern is also received with application.Rare earth oxide yittrium 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 the preparation of yttrium oxide powder turns into and ground
One of focus studied carefully.
Wang Ying etc. delivered in 2013 in functional material one on《The growth of the bar-shaped yttrium oxide powder of Hydrothermal Synthesiss
The research of journey and growth mechanism》Report, its specific preparation method is:The water yttrium nitrates of 0.58g six are dissolved in 10ml deionizations
In water, ammoniacal liquor is then added, is added in constant temperature blender with magnetic force and stirs in drop, gained colloidal substance adjusts pH to 9, hydro-thermal reaction
Temperature control reacts 2~8h at 80~180 DEG C, and cooled product centrifugation, washing, drying at room temperature, 600 DEG C of high-temperature heat treatment 4h obtain oxygen
Change yttrium nanometer rods.
Nanometer rods yittrium oxide is small with alloy contact face in alloy preparation process, it is impossible to preferably strengthen stabilized matrix phase.
Therefore, the application prospect that a kind of big yttrium oxide powder of specific surface area has had is researched and developed.
The content of the invention
It is an object of the invention to provide a kind of preparation method of yttrium oxide powder, a kind of big poplar of specific surface area has been obtained
Peach shape yttrium oxide powder.
Second purpose of the invention be to provide a kind of yttrium oxide powder obtained using above-mentioned preparation method, and its profile is
Carambola shape.
To achieve the above object, the technical scheme is that:
A kind of preparation method of yttrium oxide powder, comprises the following steps:
1) yttrium nitrate, glycerine, water are well mixed and solution is made, then adjust pH to 8~10, then it is anti-at 160~170 DEG C
14~16h is answered, reaction solution is obtained;
2) by step 1) gained reacting liquid filtering, scrubbed, dry the precursor powder of gained precipitation;
3) by step 2) 2~3h of gained 600~700 DEG C of precursor powder calcining produce.
Step 1) in yttrium nitrate be six water yttrium nitrates.Step 1) reclaimed water be deionized water.
Step 1) in by yttrium nitrate, glycerine, water is well mixed that concretely comprising the following steps for solution is made:First add into yttrium nitrate
Enter glycerine, add water.
Step 1) in per 5g yttrium nitrates, correspondence adds 10~15mL glycerine and 40~45mL water.
Step 1) in adjust pH use ammoniacal liquor.
Step 1) in preferred adjust pH to be 10.
Step 1) in adjust pH to 8~10 after, solution is placed in autoclave, then 160~170 DEG C react 14~
16h.The volume of the autoclave is 100mL.The compactedness of solution is 50%~70% in above-mentioned autoclave.
Step 2) in be filtered into vacuum filtration.
Step 2) in washing be with deionized water to washing of precipitate 5~6 times.
Step 2) in dry for 60~80 DEG C vacuum drying 4~6h.
Step 2) middle gained precursor powder ground processing before calcination.
Step 3) in 600~700 DEG C calcining 2~3h after, be air-cooled to room temperature.
A kind of yttrium oxide powder that preparation method using above-mentioned yttrium oxide powder is obtained, its profile is carambola shape.It is described
Yttrium oxide powder length direction average-size is about 6 μm.The horizontal average-size of the yttrium oxide powder is about 2 μm.
The preparation of yttrium oxide powder of the present invention, using hydrothermal synthesis method, adds organic solvent glycerine and hinders intercrystalline
Reunite, realize the transformation of shape, and glycerine is not involved in the precipitation reaction of yttrium nitrate and ammoniacal liquor.Obtained using preparation method of the present invention
The submicron order carambola shape yttrium oxide powder arrived, specific surface area is big, has strong binding ability with metal material, is used as metal material
During the hardening constituent of material, the special groove structure of carambola shape yittrium oxide preferably can be fixed in the matrix of metal material, more had
The growth of the limitation matrix of effect, makes crystal grain more tiny, with wider application.
Brief description of the drawings
Fig. 1 is the XRD of the gained yttrium oxide powder of embodiment 1;
Fig. 2 schemes for the SEM of the gained yttrium oxide powder of embodiment 1.
Embodiment
Embodiments of the present invention are described further below in conjunction with the accompanying drawings.
Embodiment 1
The preparation method of the present embodiment yttrium oxide powder, comprises the following steps:
1) six water yttrium nitrate 5g are weighed, glycerine 10mL is added, then adds 45mL deionized waters, obtain solution A, to
Ammoniacal liquor is instilled in solution A and adjusts pH=8, mixed solution B is obtained;
2) by step 1) obtained mixed solution B is put into the autoclave of 100mL polytetrafluoroethyllining linings, in baking oven
In 170 DEG C of reaction 15h, obtained precipitation will be reacted and be filtered by vacuum, be washed with deionized 5 times, 60 DEG C in drying box
4h is dried in vacuo, precursor powder is obtained;
3) by step 2) grinding of obtained precursor powder, 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, comprises the following steps:
1) six water yttrium nitrate 5g are weighed, glycerine 15mL is added, then adds 40mL deionized waters, obtain solution A, to
Ammoniacal liquor is instilled in solution A and adjusts pH=9, mixed solution B is obtained;
2) by step 1) obtained mixed solution B is put into the autoclave of 100mL polytetrafluoroethyllining linings, in baking oven
In 160 DEG C of reaction 14h, obtained precipitation will be reacted and be filtered by vacuum, be washed with deionized 5 times, 70 DEG C in drying box
5h is dried in vacuo, precursor powder is obtained;
3) by step 2) grinding of obtained precursor powder, 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, comprises the following steps:
1) six water yttrium nitrate 5g are weighed, glycerine 12mL is added, then adds 42mL deionized waters, obtain solution A, to
Ammoniacal liquor is instilled in solution A and adjusts pH=10, mixed solution B is obtained;
2) by step 1) obtained mixed solution B is put into the autoclave of 100mL polytetrafluoroethyllining linings, in baking oven
In 170 DEG C of reaction 16h, obtained precipitation will be reacted and be filtered by vacuum, be washed with deionized 6 times, 60 DEG C in drying box
4h is dried in vacuo, precursor powder is obtained;
3) by step 2) grinding of obtained precursor powder, 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 tests are carried out to the gained yttrium oxide powder of embodiment 1, as a result as shown in Figure 1.As shown in Figure 1, X-ray diffraction
Figure is completely the same with Jade standard cards (NO.43-1036), and it is Y to react obtained powder2O3。
Embodiment 2
SEM tests are carried out to the gained yttrium oxide powder of embodiment 1, as a result as shown in Fig. 2 as shown in Figure 2, gained yittrium oxide
Powder is carambola shape, with groove structure, and particle is uniform, and specific surface area is big.