CN110791287B - Rare earth doped tungsten molybdate and preparation method and application thereof - Google Patents
Rare earth doped tungsten molybdate and preparation method and application thereof Download PDFInfo
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- CN110791287B CN110791287B CN201910922905.7A CN201910922905A CN110791287B CN 110791287 B CN110791287 B CN 110791287B CN 201910922905 A CN201910922905 A CN 201910922905A CN 110791287 B CN110791287 B CN 110791287B
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7759—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing samarium
- C09K11/7765—Vanadates; Chromates; Molybdates; Tungstates
Abstract
The invention discloses a rare earth doped tungsten molybdate with a chemical formula of Sr 1‑x Sm x (MoO 4 ) 0.5 (WO 4 ) 0.5 Wherein x is more than or equal to 0.05 and less than or equal to 0.25. The invention also discloses a preparation method of the rare earth doped tungsten molybdate, which comprises the following steps: s1, according to formula Sr 1‑ x Sm x (MoO 4 ) 0.5 (WO 4 ) 0.5 Respectively weighing samarium salt, strontium salt, tungstate and molybdate according to the stoichiometric ratio; s2, adding samarium salt and strontium salt into water to dissolve, adding tungstate and molybdate to dissolve and mix uniformly, then adjusting the pH to be more than or equal to 9, carrying out hydrothermal reaction, cooling to room temperature, centrifuging to obtain precipitate, washing and drying to obtain the rare earth doped tungsten molybdate. The invention also discloses application of the rare earth doped tungsten molybdate in solid electrolyte. The invention has good conductive performance and sintering compactness, low sintering temperature and good sintered body conductivity, and can be used for solid electrolyte.
Description
Technical Field
The invention relates to the technical field of self-activating luminescent materials, in particular to rare earth doped tungsten molybdate and a preparation method and application thereof.
Background
The tungsten molybdate powder does not need to dope some rare earth ions into the tungsten molybdate powder for activation, and can generate highly efficient fluorescence under the excitation of some special light, so that the luminous performance of the substrate can be remarkably improved by doping other activated ions into the substrate; the tungsten molybdate also has the properties of good stability, excellent ionic conductivity and the like under the condition of high temperature. Having ABO 4 Tungsten molybdate oxide of type scheelite (a ═ Ca, Sr, Ba, etc.; B ═ W, Mo) is a typical oxygen ion conductor. The tungsten molybdate is very suitable for being used as a luminescent material and has very important application in the fields of laser devices, ion conductors of oxides and the like.
At present, the preparation of tungsten molybdic acid powder mainly focuses on the traditional solid phase reaction method. However, the powder prepared by the method is easy to agglomerate and needs higher sintering temperature (generally 1150-. In order to improve the performance of the materials, the hydrothermal method, the sol-gel method and other soft chemical methods are being searched for preparing the materials, but at present, the tungsten molybdic acid powder prepared by the hydrothermal method is commonly used in the field of luminescent materials and is rarely used in electrolyte materials.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the rare earth doped tungsten molybdate and the preparation method and the application thereof, and the rare earth doped tungsten molybdate has good conductive performance and sintering compactness; the invention has smaller grain diameter, regular crystal appearance, uniform size and reasonable grain distribution, and the material pressed and densely formed can be sintered into a sintered body with compact structure, and the required sintering temperature is low, thus reducing the sintering energy consumption; and the prepared sintered body has good conductivity and can be used for solid electrolyte.
The invention provides a rare earth doped tungsten molybdate with a chemical formula of Sr 1-x Sm x (MoO 4 ) 0.5 (WO 4 ) 0.5 Wherein x is more than or equal to 0.05 and less than or equal to 0.25.
Preferably, x is 0.1.
The invention also provides a preparation method of the rare earth doped tungsten molybdate, which comprises the following steps:
s1 according to formula Sr 1-x Sm x (MoO 4 ) 0.5 (WO 4 ) 0.5 Respectively weighing samarium salt, strontium salt, tungstate and molybdate according to the stoichiometric ratio;
s2, adding samarium salt and strontium salt into water to dissolve, adding tungstate and molybdate to dissolve and mix uniformly, then adjusting the pH to be more than or equal to 9, carrying out hydrothermal reaction, cooling to room temperature, centrifuging to obtain precipitate, washing and drying to obtain the rare earth doped tungsten molybdate.
Preferably, the pH is 9-11.
Preferably, the pH may be 9, 9.1, 9.2, 9.3, 9.4, 9.5, 9.6, 9.7, 9.8, 9.9, 10, 10.1, 10.2, 10.3, 10.4, 10.5, 10.6, 10.7, 10.8, 10.9 or 11.
Preferably, the pH is 9.
Preferably, the temperature of the hydrothermal reaction is 160-200 ℃, and the time of the hydrothermal reaction is 20-28 h.
Preferably, the temperature of the hydrothermal reaction is 180 ℃ and the time of the hydrothermal reaction is 24 h.
Preferably, the samarium salt is at least one of samarium nitrate and samarium nitrate hydrate.
Preferably, the strontium salt is at least one of strontium nitrate and strontium nitrate hydrate.
Preferably, the tungstate is at least one of ammonium tungstate and ammonium tungstate hydrate.
Preferably, the molybdate is at least one of ammonium molybdate and ammonium molybdate hydrate.
Preferably, the pH is adjusted with ammonia or nitric acid.
The invention also provides the application of the rare earth doped tungsten molybdate in the solid electrolyte.
According to the invention, Sm and Sr are adopted to dope tungsten molybdate, and proper doping amount is selected, so that the conductive material has good conductivity and sintering compactness; the rare earth doped tungsten molybdate is prepared by a hydrothermal method, and has a pure-phase scheelite structure and no other heterocrystal phase by adjusting the proper pH; the rare earth doped tungsten molybdate has smaller particle size, regular crystal morphology, uniform size and reasonable grain distribution through proper pH and hydrothermal reaction conditions, and the pressed and densely formed material can be sintered into a sintered body with compact structure, and the required sintering temperature is low, so that the sintering energy consumption can be reduced; and the prepared sintered body has good conductivity and can be used for solid electrolyte.
Drawings
FIG. 1 is a TG plot of rare earth doped tungsten molybdate.
FIG. 2 is an XRD diffraction pattern of rare earth doped tungsten molybdate obtained at different pH values.
FIG. 3 is a SME picture of a section of a rare earth doped tungsten molybdate sintered body obtained at different pH values.
FIG. 4 is a graph of conductivity versus temperature for tungsten molybdate doped with varying amounts Sm.
FIG. 5 is an Arrhenius plot of the ionic conductivity of tungsten molybdates doped with varying amounts of Sm.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of rare earth doped tungsten molybdate comprises the following steps:
s1, according to formula Sr 0.95 Sm 0.05 (MoO 4 ) 0.5 (WO 4 ) 0.5 Respectively weighing samarium salt, strontium salt, tungstate and molybdate according to the stoichiometric ratio;
s2, adding samarium salt and strontium salt into water to dissolve, adding tungstate and molybdate to dissolve and mix uniformly, then adjusting the pH to be more than or equal to 9, carrying out hydrothermal reaction, cooling to room temperature, centrifuging to obtain precipitate, washing and drying to obtain the rare earth doped tungsten molybdate.
Example 2
A preparation method of rare earth doped tungsten molybdate comprises the following steps:
s1, according to formula Sr 0.75 Sm 0.25 (MoO 4 ) 0.5 (WO 4 ) 0.5 Respectively weighing samarium nitrate, strontium nitrate, ammonium tungstate and ammonium molybdate according to the stoichiometric ratio;
s2, adding samarium nitrate and strontium nitrate into water to dissolve, adding ammonium tungstate and ammonium molybdate to dissolve, mixing uniformly, adjusting the pH to 11, carrying out hydrothermal reaction at 160 ℃ for 28h, cooling to room temperature, centrifuging at 2500rpm for 3min, taking precipitate, washing, and drying to obtain the rare earth doped tungsten molybdate.
Example 3
A preparation method of rare earth doped tungsten molybdate comprises the following steps:
s1, according to formula Sr 0.8 Sm 0.2 (MoO 4 ) 0.5 (WO 4 ) 0.5 Respectively weighing samarium nitrate, strontium nitrate, ammonium tungstate and ammonium molybdate according to the stoichiometric ratio;
s2, adding samarium nitrate and strontium nitrate into water to dissolve, adding ammonium tungstate and ammonium molybdate to dissolve, mixing uniformly, adjusting the pH value to 10, carrying out hydrothermal reaction at 200 ℃ for 20h, cooling to room temperature, centrifuging at 2500rpm for 3min, taking precipitate, washing, and drying to obtain the rare earth doped tungsten molybdate.
Example 4
A preparation method of rare earth doped tungsten molybdate comprises the following steps:
s1, according to formula Sr 0.9 Sm 0.1 (MoO 4 ) 0.5 (WO 4 ) 0.5 Respectively weighing samarium nitrate hexahydrate, strontium nitrate, ammonium tungstate hydrate and ammonium molybdate tetrahydrate according to a stoichiometric ratio;
s2, adding samarium nitrate hexahydrate and strontium nitrate into water to dissolve, adding ammonium tungstate hydrate and ammonium molybdate tetrahydrate to dissolve and mix uniformly, adjusting the pH to 9, carrying out hydrothermal reaction at 180 ℃ for 24h, cooling to room temperature, centrifuging at 2500rpm for 3min, taking precipitate, washing, and drying to obtain the rare earth doped tungsten molybdate.
The above rare earth doped tungsten molybdate is taken for TG analysis, the result is shown in figure 1, figure 1 is a TG curve diagram of the rare earth doped tungsten molybdate, and the results can be known from figure 1: the mass loss in the powder heating process can be roughly divided into three stages: first, the loss of the sample is about 0.5% at room temperature to 200 ℃ mainly due to evaporation of crystal water contained therein and volatilization of a small amount of volatile impurities. When the temperature is programmed from 200 ℃ to 550 ℃, the rapid decrease process of the TG curve can be obviously seen, and the loss amount of the sample is about 2.75 percent, which is probably caused by the decomposition of nitrate and the like contained in the powder along with the increase of the temperature. Above 500 c, the mass of the powder slowly decreased until unchanged, indicating that the reactions were substantially complete and a stable solid solution was formed.
Example 5
The pH was 7, otherwise the same as in example 4.
Example 6
The pH was 11, otherwise the same as in example 4.
For the rare earth doped tungsten molybdate, SrWO, of examples 4-6 4 、SrMoO 4 As shown in fig. 2, at different pH, a hetero peak exists between crystal plane (101) and crystal plane (112), and gradually decreases with increasing pH, the hetero peak significantly decreases when pH is 9, and decreases to a very low value, and the hetero peak does not exist when pH is 11; meanwhile, the XRD pattern can also obviously reflectThe peak height is more obvious when the pH value is increased in the hydrothermal reaction process. Therefore, the pH value of a reaction sample is increased as much as possible in the process of preparing powder by a hydrothermal method so as to reduce the existence of a foreign peak and improve the crystallization property to obtain better powder, and therefore, the pH value is selected to be more than or equal to 9.
Sintered bodies were prepared according to example 4 and example 6, respectively, and the preparation method of the sintered bodies was: and (2) taking rare earth doped tungsten molybdate, adding a drop of ethanol solution of polyvinyl alcohol, grinding until no powder is attached to the wall of the grinding pot, taking 1.2g of ground powder, tabletting, heating to 650 ℃ at the speed of 2 ℃/min, preserving heat for 3h, heating to 845 ℃ at the speed of 1.5 ℃/min, and preserving heat for 2h to obtain the rare earth doped tungsten molybdate sintered body.
SME scanning is performed on the sections of the rare earth doped tungsten molybdate sintered bodies prepared in the embodiments 4 and 6, and the result is shown in FIG. 3, wherein FIG. 3 is a SME picture of the section of the rare earth doped tungsten molybdate sintered body obtained at different pH values, and it can be seen from FIG. 3 that the smaller the crystal grain generated in the hydrothermal reaction process of the sample with higher pH value 1, the closer the grain size of the crystal grain is to the nanometer level; 2. when the sintering temperature was the same, pH 9 showed no significant pores in the sintered body cross section, indicating that the sintered body was dense enough to meet the requirements for use as a solid battery electrolyte material, while pH 11 showed a large number of pores in the sintered body cross section SEM. This shows that the higher the pH during the hydrothermal reaction, the smaller the grain size and the higher the temperature required for the sintering process.
Example 7
The chemical formula of the rare earth doped tungsten molybdate is Sr 0.95 Sm 0.05 (MoO 4 ) 0.5 (WO 4 ) 0.5 The preparation method is the same as example 4.
Example 8
The chemical formula of the rare earth doped tungsten molybdate is Sr 0.85 Sm 0.15 (MoO 4 ) 0.5 (WO 4 ) 0.5 The preparation method is the same as example 4.
Example 9
The chemical formula of the rare earth doped tungsten molybdate is Sr 0.8 Sm 0.2 (MoO 4 ) 0.5 (WO 4 ) 0.5 The preparation method is the same as example 4.
Example 10
The chemical formula of the rare earth doped tungsten molybdate is Sr 0.75 Sm 0.25 (MoO 4 ) 0.5 (WO 4 ) 0.5 The preparation method is the same as example 4.
Sintered bodies were prepared according to example 4 and examples 7 to 10, respectively, and the preparation method of the sintered bodies was: and (2) taking rare earth doped tungsten molybdate, adding a drop of ethanol solution of polyvinyl alcohol, grinding until no powder is attached to the wall of the grinding pot, taking 1.2g of ground powder, tabletting, heating to 650 ℃ at the speed of 2 ℃/min, preserving heat for 3h, heating to 845 ℃ at the speed of 1.5 ℃/min, and preserving heat for 2h to obtain the rare earth doped tungsten molybdate sintered body.
The electric conductivity and ionic conductivity arrhenius curves of the sintered bodies obtained in example 4 and examples 7-10 were measured, and the results are shown in fig. 4 and 5, wherein fig. 4 is a graph of the electric conductivity of tungsten molybdate doped with different amounts of Sm as a function of temperature, and fig. 5 is an arrhenius graph of the ionic conductivity of tungsten molybdate doped with different amounts of Sm;
as can be seen from FIG. 4, the conductivity gradually increases as the Sm content increases, because Sm content increases 3+ Substituted Sr 2+ In order to keep the electric neutrality, oxygen is discharged from crystal lattices to form oxygen vacancies, and further the ionic conductivity of the crystal lattices is greatly improved, so that the ionic conductivity is improved, and when the Sm content exceeds 0.1, the conductivity is reduced, because excessive oxygen vacancies can cause the association between the oxygen vacancies and solid-dissolved cations, and the conductivity is reduced; when the Sm content is 0.1, the rare earth doped tungsten molybdate reaches the highest conductivity at 800 ℃, and the highest conductivity is 5.9 multiplied by 10 -2 S·cm -1 ；
As can be seen from fig. 5, the change of the conductivity activation energy has the same rule as the change of the conductivity, and when the Sm content exceeds 0.1, the conductivity activation energy is increased; when the Sm content is 0.1, the activation energy is the lowest.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. The preparation method of the rare earth doped tungsten molybdate is characterized in that the chemical formula of the rare earth doped tungsten molybdate is Sr 1-x Sm x （MoO 4 ） 0.5 （WO 4 ） 0.5 Wherein x = 0.1;
the preparation method specifically comprises the following steps:
s1, according to formula Sr 1-x Sm x （MoO 4 ） 0.5 （WO 4 ） 0.5 Respectively weighing samarium salt, strontium salt, tungstate and molybdate according to the stoichiometric ratio;
s2, adding samarium salt and strontium salt into water for dissolving, adding tungstate and molybdate for dissolving and mixing uniformly, then adjusting the pH to be =9-11, carrying out hydrothermal reaction at the temperature of 160-200 ℃ for 20-28h, cooling to room temperature, centrifuging to obtain precipitate, washing and drying to obtain the rare earth doped tungsten molybdate.
2. The method for preparing rare earth-doped tungstomolybdate as claimed in claim 1, characterized in that the temperature of hydrothermal reaction is 180 ℃ and the time of hydrothermal reaction is 24 h.
3. The method for preparing rare earth-doped tungstomolybdate in accordance with claim 1 wherein samarium salt is at least one of samarium nitrate and samarium nitrate hydrate; the strontium salt is at least one of strontium nitrate and strontium nitrate hydrate.
4. The method for preparing rare earth doped tungsten molybdate according to claim 1, wherein the tungstate is at least one of ammonium tungstate and ammonium tungstate hydrate; the molybdate is at least one of ammonium molybdate and ammonium molybdate hydrate.
5. The method of claim 1, wherein the pH is adjusted with ammonia or nitric acid.
6. Use of the rare earth-doped tungstomolybdate prepared by the method of claims 1 to 5 in a solid electrolyte.
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