CN104326500A - Preparation method of fluffy nano yttrium oxide powder - Google Patents

Preparation method of fluffy nano yttrium oxide powder Download PDF

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Publication number
CN104326500A
CN104326500A CN201410555047.4A CN201410555047A CN104326500A CN 104326500 A CN104326500 A CN 104326500A CN 201410555047 A CN201410555047 A CN 201410555047A CN 104326500 A CN104326500 A CN 104326500A
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preparation
yttrium
yttrium oxide
oxide powder
complexing agent
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CN104326500B (en
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吕文中
张晓荣
范桂芬
汪小红
王晓川
梁飞
雷文
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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

A kind of preparation method of fluffy state nano yttrium oxide powder
Technical field
The invention belongs to the preparation field of ultrafine powder, more specifically, relate to a kind of fluffy state nano yttrium oxide (comprising the yttrium oxide of doping) raw powder's production technology.
Background technology
Yttrium oxide is a kind of extremely important rare earth oxide, and water insoluble and alkali, dissolves in acid, in atmosphere easily absorbing carbon dioxide and water, has, 4f high as electricity price specific to rare earth element in addition r5d x6l 2the character of the excellences such as electron structure, radius are large, polarization force is strong, chemical property is active.Because its excellent heat-resisting, corrosion-resistant, high-temperature stability, specific inductivity are in high-quality characteristics such as 12-20, become important Industrial materials.At optical material, high-performance ceramics, battery material, magneticsubstance, the aspects such as luminescent material.For yttrium oxide nano-powder, there is high purity and specific surface area, little grain diameter, narrow size distribution are the preconditions that it is used widely.Existing report adopts solid phase method, the precipitator method etc. to prepare yttrium oxide nano-powder.
Chinese patent literature CN103539195 A discloses " a kind of preparation method of nano yttrium oxide powder ", the method utilizes the inorganic acid salt solution instillation containing yttrium to contain in the alcohol water mixed solution of precipitation agent and electrostatic stabilization agent, adding tensio-active agent subsequently, and calcine after ageing is just stirred to system, obtain the yttrium oxide powder of size distribution at 30 ~ 60nm.
Chinese patent literature CN1410353A discloses one " nano oxidized raw powder's production technology ", the method utilizes reacts under the condition introducing tensio-active agent containing ruthenium ion solution and basic solution, and after washing, oven dry, at 200 ~ 600 DEG C, calcining obtains the powder of particle diameter at 10 ~ 60nm.
Chinese patent literature CN103450899A discloses " a kind of preparation method of doped yttrium oxide nano-phosphor ", and the method is at Y (NO 3) 3with Eu (NO 3) 3mixing solutions in add NaOH solution, and regulate proper pH value to be load in reaction vessels after the NaOH adding equal mass after 6 ~ 8 again stirs, under temperature is 140 ~ 220 DEG C of conditions, reacts cooling after 4 ~ 6 hours obtains reaction product, subsequently through washing, precipitation, dries and obtains doped yttrium oxide nano-phosphor.
Preparation method's complex steps that above patent documentation uses, equipment is complicated, and need control comparatively multivariate, the large distribution of diameter of particle is wide, and powder granularity distributed area is non-adjustable and agglomeration is more serious.
Summary of the invention
For current Problems existing, the invention provides a kind of fluffy state nanometer Y 2o 3and RE:Y 2o 3raw powder's production technology.The present invention utilize New Chelating Agents by combustion method preparation reunite little, particle diameter is little and the nano yttrium oxide powder of narrowly distributing, the product of preparation is loose without the need to any broken thinning processing; The method is simple to operate, synthesis temperature is low, the cycle is short, be easy to industrialization; By controlling the add-on of New Chelating Agents, the nano-powder of different grain size interval distribution can be prepared.
The preparation method of a kind of nano yttrium oxide powder provided by the invention, is characterized in that, comprise the steps:
1st step will mix containing yttrium inorganic salt, deionized water and complexing agent, and at room temperature stir the slurries obtained containing yttrium, and wherein, the weight ratio containing yttrium inorganic salt and complexing agent is 8/0.5 ~ 8/10;
When target product is RE:Y 2o 3time, described containing in yttrium inorganic salt doped with rare earth ion;
2nd step is by described slurries, or the colloidal sol obtained by described slurries or xerogel are calcined at 400 DEG C ~ 900 DEG C, make it fully decompose, obtain fluffy state Y 2o 3or RE:Y 2o 3nano-powder.
Compared with prior art, the New Chelating Agents combustion method that the present invention adopts optimizes material preparation process, and powder granularity is little, narrow diameter distribution.Meanwhile, the yttrium oxide powder of a small amount of ion doping with precise stoichiometry ratio can effectively be synthesized (such as: Nd:Y 2o 3, Yb:Y 2o 3, Eu:Y 2o 3deng).Specifically, the present invention has the following advantages:
1. the method possess simultaneously simple to operate, the cycle is short, energy-conservation, easy industrialization, not by the advantage such as specific installation restriction
2. the present invention is when preparing yttrium oxide nano-powder, employs New Chelating Agents, and a small amount of adding of ratio complexing agent can make preparation temperature reduce, powder granularity little and be evenly distributed, specific surface area is large.
3. change the add-on of complexing agent, the distribution range of controlled powder process body, makes prepared Y 2o 3and RE:Y 2o 3it is adjustable that diameter of particle can be distributed in (as 10-30nm, 20-70nm etc.) in multiple comparatively close limit.
4. the inventive method can avoid because filtering, and the tedious steps such as washing make a small amount of dopant ion run off, and are conducive to the combined oxidation yttrium nano-powder preparing multiple doped element.
Accompanying drawing explanation
Fig. 1 is the preparation process of yttrium oxide nano-powder;
Nd:Y prepared by Fig. 2 embodiment 1-3 2o 3material phase analysis;
Y prepared by Fig. 3 embodiment 1 2o 3scanning electron microscope (SEM) photograph;
Y prepared by Fig. 4 embodiment 2 2o 3scanning electron microscope (SEM) photograph;
Y prepared by Fig. 5 embodiment 4-8 2o 3material phase analysis;
Y prepared by Fig. 6 embodiment 9-11 2o 3material phase analysis;
Y prepared by Fig. 7 embodiment 12-14 2o 3material phase analysis;
Y prepared by Fig. 8 embodiment 15-17 2o 3material phase analysis;
Yb:Y prepared by Fig. 9 embodiment 18-19 2o 3and Eu:Y 2o 3material phase analysis;
Y prepared by Figure 10 embodiment 21 2o 3scanning electron microscope (SEM) photograph;
The Y of Figure 11 prepared by embodiment 20 and 21 2o 3photo comparison schemes, and wherein, (a) is embodiment 20, and (b) is embodiment 21.
Embodiment
For current Problems existing, the present invention, by containing the inorganic salt solution of yttrium and the complex reaction of New Chelating Agents solution, considerably reduces sintering temperature, sample both can have been synthesized at 400 DEG C.
With Y (NO 3) 36H 2o is example, is dissolved in the yttrium nitrate solution formed in a small amount of deionized water; Take a certain amount of polyacrylic acid or ammonium polyacrylate (being about 10% ~ 130% of yttrium salt weight) joins in yttrium nitrate solution as complexing agent, stir with glass stick.Directly pour the reaction solution prepared into crucible, put into retort furnace and calcine, calcining temperature is at >=400 DEG C, and insulation >=0h can obtain fluffy ultra fine product.As the Y (NO as 8g 3) 36H 2the complexing agent adding 1g in O just can synthesize small particle size and the spherical yttrium oxide powder distributed within the scope of 20 ~ 70nm; When adding 2g complexing agent, just small particle size can be synthesized and the spherical yttrium oxide powder distributed within the scope of 10 ~ 30nm; When continuing to increase amount of complex, powder distribution range is less by what become, therefore by controlling the add-on of complexing agent, can control the particle size distribution of ball-type yttrium oxide product.
As shown in Figure 1, the preparation method that example of the present invention provides specifically comprises following process:
(1) will deionized water be added containing yttrium inorganic salt and stir, obtain containing yttrium inorganic acid salt solution; Add a certain amount of complexing agent wherein again, obtain the slurries containing yttrium.
The target product of preparation can be Y 2o 3or RE:Y 2o 3, when target product is RE:Y 2o 3time, to containing doped with rare earth ion in yttrium inorganic salt, its subsequent products is also doped with rare earth ion accordingly.
The described concentration containing yttrium inorganic acid salt solution can from close to saturated until infinite dilution can, the rare earth ion adulterated can be multiple, as Nd 3+, Yb 3+, Eu 3+deng, can single ion doping, also can different kinds of ions doping.
Complexing agent is at least one in polyacrylic acid (PAA) and ammonium polyacrylate (PAM), and reaction is carried out at normal temperatures and pressures.
The mode that complexing agent adds containing the inorganic acid salt solution of yttrium can dropwise add, and also can directly pour into; Meanwhile, the addition sequence of metal-salt, water, complexing agent is interchangeable.
Closing containing the inorganic acid salt solution of yttrium and the part by weight of complexing agent is Y/P=8/0.5 ~ 8/10, and from the viewpoint of energy-saving and environmental protection and properties of sample, it is 8/1 ~ 8/3 that preferred proportion closes, more preferably 8/2.
Mainly refer to the nitric acid metal-salt of Yttrium trinitrate and doping containing yttrium inorganic salt, as Yttrium trinitrate, neodymium nitrate etc., preferred yttrium nitrate solution, or the mixing solutions of rare earth nitrate and Yttrium trinitrate, concentration is close to saturated.
(2) after reinforced, stirred by slurries under normal temperature and pressure conditions with glass stick, direct remarks or slurries are evaporated excessive moisture at a certain temperature, remove portion moisture forms colloidal sol or removes all moisture and forms xerogel.
Vaporization temperature is general not higher than 100 DEG C.
Above-mentioned homogeneous solution evaporates excessive moisture, forms colloidal sol or all moisture formation xerogel by the equipment such as heating in water bath or baking oven for heating heating remove portion.
(3) slurries in step (2) or colloidal sol or xerogel are carried out calcination processing, obtain the little and uniform spherical yttrium oxide product of particle diameter.
Calcining temperature is that 400 DEG C ~ 900 DEG C (from the viewpoint of energy-conserving and environment-protective, preferably 500 DEG C ~ 900 DEG C, being more preferably 500 DEG C) make sample fully decompose, and is possessed the little and narrowly distributing of particle diameter, the nano yttrium oxide powder of soilless sticking simultaneously.
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further.It should be noted that at this, the explanation for these embodiments understands the present invention for helping, but does not form limitation of the invention.In addition, if below in described each embodiment of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
Example of the present invention adopts deionized water as solvent, adopts nitrate and complexing agent as starting material, under the condition of differential responses temperature and different complexing agent addition, has prepared Y by combustion method 2o 3and RE:Y 2o 3nano-powder.
The present invention adopts combustion method reason to be New Chelating Agents in the process of decomposing to release gas to make, and synthesized powder is loose to expand, diameter of particle is little and even, simultaneously, thermopositive reaction in metal-salt and complexing agent decomposition course can make ambient temperature increase sharply, thus without the need to indirect heating, sample can synthesize at a lower temperature.In order to improve the purity of sample, utilize the raw material of analytical pure rank.
Example 1
Nd:Y as required 2o 3nano-powder quality takes corresponding Y (NO 3) 36H 2o.The present invention is to take 7.871g Y (NO 3) 36H 2nd (the NO of O and 0.474g 3) 36H 2o is example, is dissolved in the nitrate solution formed in a small amount of deionized water; The polyacrylic acid taking 2g joins as complexing agent and fuel in the yttrium nitrate solution fully dissolved, and stirs with glass stick.Directly pour the reaction solution prepared into crucible, put into retort furnace and calcine, calcining temperature is 500 DEG C, directly lowers the temperature, and can obtain fluffy ultra fine product.
The nano-powder of preparation is carried out X-ray diffraction analysis (XRD) to the material phase analysis of nano-powder, utilize pattern and the particle size of transmission electron microscope (TEM) analysis and observation powder.
Above-mentioned Nd:Y 2o 3the XRD analysis of nano-powder is shown in the curve of the bottom in Fig. 2, therefrom can find out that the product of example 1 is Nd:Y 2o 3pure phase is consistent with card JCPDS 83-0927.Compare the wide in range not sharp-pointed peak (curve see Fig. 5 bottom) of the sample XRD after 400 DEG C of calcinings, the sharp intensity that after 500 DEG C of process, the XRD diffraction peak of sample becomes increases.Collection of illustrative plates does not show the diffraction peak of other dephasign, and crystallization is better.
The TEM figure of example 1 sample is shown in Fig. 3, and as can be seen from Fig., the basic soilless sticking phenomenon of powder, the border of particle is more clear, and particle keeps spherical substantially, and particle diameter is little to be evenly distributed, and particle size is between 10 ~ 30nm.
Example 2-21:
Example 2-21 preparation process is as example 1, and the starting material adopted, complexing agent and processing parameter etc. are specifically in table 1, and wherein example 21 is comparative example.
Nd:Y prepared by embodiment 2-3 2o 3xRD material phase analysis as shown in Figure 2, collection of illustrative plates does not show other dephasign, and thing is mutually pure, and degree of crystallinity is better.The Y of example 2 2o 3scanning electron microscope (SEM) photograph is Fig. 4, and contrast Figure 10 can find out that particle keeps spherical substantially, and dispersiveness obviously improves, and particle size is between 20 ~ 70nm, and distributed area is narrower.
Y prepared by embodiment 4-8 2o 3xRD material phase analysis as shown in Figure 5, the Y prepared by embodiment 9-11 2o 3xRD material phase analysis as shown in Figure 6; Y prepared by embodiment 11-13 2o 3xRD material phase analysis as shown in Figure 7; Y prepared by embodiment 13-17 2o 3xRD material phase analysis as shown in Figure 8.
Can clearly learn from Fig. 5 to Fig. 8, polyacrylic acid and ammonium polyacrylate can as complexing agents, and can synthesis of nano yttrium oxide powder at a lower temperature, and powder purity is high, exist, and degree of crystallinity is better without other dephasign.As can be seen from Figure 5, sample just defines Y at 400 DEG C 2o 3diffraction peak.
Yb:Y prepared by example 18 and 19 2o 3and Eu:Y 2o 3material phase analysis as shown in Figure 9, is the diffraction peak of pure phase material in figure, exists without other dephasign, illustrates that this method can prepare multiple RE:Y 2o 3pure phase material.
Figure 10 is the Y prepared by comparative example (embodiment 21, does not add complexing agent) 2o 3transmission electron microscope picture, as can be seen from the figure, sample is laminar coacervate, and reunion degree is very large.
Comparative example 21 (Figure 10) and embodiment 2 (Fig. 4); can find out that powder reuniting phenomenon almost disappears from embodiment 1 (Fig. 3); the border of particle is more clear; particle keeps spherical substantially; particle diameter is little and distribution is very even, and particle size is between 10 ~ 30nm.Contrast Figure 10, Fig. 4 and Fig. 3 can also learn, the add-on of suitable increase complexing agent, the particle diameter of powder can be made to diminish, and distribution range narrows.
Figure 11 for embodiment 20 (namely a) and embodiment 21 (namely b) prepared by Y 2o 3photo, obviously can find out the Y adding complexing agent and prepare from figure 2o 3fluffy, and the sample powder of the complexing agent do not added, reunite serious, be bonded in crucible bottom, become to harden phenomenon.
Equipment used in the preparation of above-mentioned example and test process is as follows: 1, beaker, glass stick, corundum crucible etc.; 2, Sai Duolisi bs124s electronic balance: MAX:120g, d=0.1mg; 3, X-ray diffractometer: Japanese Shimadzu Corporation, XRD-7000S; 4, transmission electron microscope: Japanese JEM-2100.
The foregoing is only best case study on implementation of the present invention, not in order to limit the present invention, all amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., be all included within protection scope of the present invention.
Table 1: combustion method prepares Y 2o 3and RE:Y 2o 3the embodiment parameter of powder
Note: Y (NO 3) 36H 2o is abbreviated as YN; Nd (NO 3) 36H 2o is abbreviated as NdN; Yb (NO 3) 35H 2o is abbreviated as YbN; Eu (NO 3) 36H 2o is abbreviated as EuN.

Claims (11)

1. a preparation method for nano yttrium oxide powder, is characterized in that, comprises the steps:
1st step will mix containing yttrium inorganic salt, deionized water and complexing agent, and at room temperature stir the slurries obtained containing yttrium, and wherein, the weight ratio containing yttrium inorganic salt and complexing agent is 8/0.5 ~ 8/10;
When target product is RE:Y 2o 3time, described containing in yttrium inorganic salt doped with rare earth ion;
2nd step is by described slurries, or the colloidal sol obtained by described slurries or xerogel are calcined at 400 DEG C ~ 900 DEG C, make it fully decompose, obtain fluffy state Y 2o 3or RE:Y 2o 3nano-powder.
2. the preparation method of nano yttrium oxide powder according to claim 1, is characterized in that, adjust described amount of complex according to diameter of particle Spreading requirements.
3. the preparation method of nano yttrium oxide powder according to claim 1, it is characterized in that, described complexing agent is at least one in polyacrylic acid PAA and ammonium polyacrylate PAM.
4. according to the preparation method of described nano yttrium oxide powder arbitrary in claims 1 to 3, it is characterized in that, described is Yttrium trinitrate containing yttrium inorganic salt, or the nitric acid metal-salt of Yttrium trinitrate and doping.
5. according to the preparation method of described nano yttrium oxide powder arbitrary in claims 1 to 3, it is characterized in that, the rare earth ion of described doping is single ion doping or different kinds of ions doping.
6. according to the preparation method of described nano yttrium oxide powder arbitrary in claims 1 to 3, it is characterized in that, the mode that described complexing agent adds is for dropwise adding or directly pouring into.
7. according to the preparation method of described nano yttrium oxide powder arbitrary in claims 1 to 3, it is characterized in that, the described addition sequence containing yttrium inorganic salt, deionized water and complexing agent is any.
8.. according to the preparation method of described nano yttrium oxide powder arbitrary in claims 1 to 3, it is characterized in that, is 8/1 ~ 8/3 containing the inorganic salt solution of yttrium and the weight ratio of complexing agent, is preferably 8/2.
9. according to the preparation method of described fluffy state nano yttrium oxide powder arbitrary in claims 1 to 3, it is characterized in that, described calcining temperature is 500 DEG C ~ 900 DEG C, is preferably 500 DEG C.
10. according to the preparation method of described nano yttrium oxide powder arbitrary in claims 1 to 3, it is characterized in that, process isothermal holding after firing, soaking time preferably 1 to 3 hour.
11., according to the preparation method of described nano yttrium oxide powder arbitrary in claims 1 to 3, is characterized in that, described colloidal sol or xerogel by by described slurries≤100 DEG C time evaporation section or all moisture obtain.
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CN106927497A (en) * 2017-04-13 2017-07-07 镧明新材料科技（上海）有限公司 The preparation method and its product of environment-friendly type nano yttrium oxide powder, application
CN109366039A (en) * 2018-11-27 2019-02-22 浙江大学 A kind of preparation method of the yttrium oxide microballoon for titanium alloy vacuum brazing stop-off gent
CN114873625A (en) * 2022-04-28 2022-08-09 中国航空制造技术研究院 Preparation method of ash-like light nano yttrium oxide powder

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CN106927497A (en) * 2017-04-13 2017-07-07 镧明新材料科技（上海）有限公司 The preparation method and its product of environment-friendly type nano yttrium oxide powder, application
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CN114873625B (en) * 2022-04-28 2023-08-22 中国航空制造技术研究院 Preparation method of ash-shaped light nano yttrium oxide powder

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