CN107021520B - A kind of yttrium oxide powder and preparation method thereof - Google Patents

A kind of yttrium oxide powder and preparation method thereof Download PDF

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Publication number
CN107021520B
CN107021520B CN201710427928.1A CN201710427928A CN107021520B CN 107021520 B CN107021520 B CN 107021520B CN 201710427928 A CN201710427928 A CN 201710427928A CN 107021520 B CN107021520 B CN 107021520B
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yttrium oxide
preparation
oxide powder
yttrium
glycerine
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CN107021520A (en
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徐流杰
魏世忠
窦彩虹
周玉成
潘昆明
李秀青
李继文
刘伟
徐锐
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Harbin Peize Material Technology Co ltd
Sichuan Panyingda Technology Co ltd
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Henan University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Abstract

The present invention relates to a kind of yttrium oxide powders and preparation method thereof, belong to a kind of material preparation process.The preparation method of yttrium oxide powder of the present invention, comprising the following steps: 1) yttrium nitrate is dissolved in glycerine and water, then tune pH to pH=8~10, then in 160~170 DEG C of 14~16h of reaction, obtains reaction solution;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.The submicron order carambola shape yttrium oxide powder obtained using preparation method of the present invention, large specific surface area, when hardening constituent as metal material, the special groove structure of carambola shape yttrium oxide can be preferably fixed in the matrix of metal material, the more effectively growth of limitation matrix, keep crystal grain more tiny, there is widely application.

Description

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.

Claims (5)

1. a kind of yttrium oxide powder, which is characterized in that be prepared by method comprising the following steps:
1) by yttrium nitrate, glycerine, water be uniformly mixed solution is made, then adjust pH to 8 ~ 10, then 160 ~ 170 DEG C react 14 ~ 16h obtains reaction solution;
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, glycerine, water are uniformly mixed to the specific steps that solution is made are as follows: third is first added into yttrium nitrate in step 1) Triol 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).
2. yttrium oxide powder according to claim 1, which is characterized in that dry for 60 ~ 80 DEG C of vacuum drying 4 in step 2 ~6h。
3. yttrium oxide powder according to claim 1, which is characterized in that it is characterized in that, its shape is carambola shape.
4. a kind of preparation method of yttrium oxide powder, which comprises the following steps: 1) mix yttrium nitrate, glycerine, water Uniformly solution is made in conjunction, then adjusts pH to 8 ~ 10, then in 160 ~ 170 DEG C of 14 ~ 16h of reaction, obtain reaction solution;
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, glycerine, water are uniformly mixed to the specific steps that solution is made are as follows: third is first added into yttrium nitrate in step 1) Triol 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).
5. the preparation method according to claim 4, which is characterized in that in step 2 it is dry for 60 ~ 80 DEG C of vacuum drying 4 ~ 6h。
CN201710427928.1A 2017-06-08 2017-06-08 A kind of yttrium oxide powder and preparation method thereof Active CN107021520B (en)

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CN112194165A (en) * 2020-10-09 2021-01-08 上海第二工业大学 Yttrium oxide nanorod and preparation method thereof

Citations (1)

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CN104445354A (en) * 2014-12-13 2015-03-25 广西科技大学 Hydrothermal synthetic method of nano yttrium oxide powder

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Publication number Priority date Publication date Assignee Title
CN104445354A (en) * 2014-12-13 2015-03-25 广西科技大学 Hydrothermal synthetic method of nano yttrium oxide powder

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