CN113755165A - Manganese-doped 95MCT Yb and Ho up-conversion luminescence-dielectric bifunctional material and preparation method thereof - Google Patents
Manganese-doped 95MCT Yb and Ho up-conversion luminescence-dielectric bifunctional material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of photo-thermal dual-function materials, and discloses a manganese-doped 95MCT Yb Ho up-conversion luminescence-dielectric dual-function material, which has the following chemical expression: mnxYb0.01Ho0.01Mg0.95Ca0.05TiO(3.03+x)Wherein x is more than 0 and less than or equal to 0.05 and is the molar concentration of manganese ions; the photo-thermal bifunctional nano material is a hexagonal phase nanosphere, and the grain size is 21 nm-25 nm. The preparation method comprises the following steps of S1: dissolving tetrabutyl titanate into ethylene glycol; s2: dropping a citric acid aqueous solution into the solution obtained in the step S1; s3: sequentially dropping aqueous solutions of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate into the solution obtained from the S2; s4: heating the solution obtained in the step S3 to a certain temperature, preserving the temperature, and removing water; s5: grinding the brownish black solid obtained in the step S4 into powder, then placing the powder in a high-temperature furnace, heating to a certain temperature, and preserving heat to obtain a reaction product; s6: the reaction product obtained in S5 was cooled to room temperature to obtain the final productThe manganese-doped 95MCT is Yb and Ho up-conversion luminescent-dielectric bifunctional material.
Description
Technical Field
The invention belongs to the technical field of photo-thermal dual-function materials, and particularly relates to a manganese-doped 95 MCT-Yb-Ho up-conversion luminescence-dielectric dual-function material and a preparation method thereof.
Background
95MCT(0.95MgTiO3–0.05CaTiO3) Is a non-metal oxide material with excellent dielectric properties [ Journal of Alloys and Compounds 450(2008): 359-.]Commonly used in capacitors and dielectric resonators; the 95MCT ceramic has a relative dielectric constant of 20, a Q x f factor of 56000 (for 7GHz electromagnetic waves), and a temperature coefficient of resonance frequency (tau f) of 0. On the other hand, the rare earth ion doped dielectric material simultaneously exhibits the up-conversion luminescence-dielectric dual-function characteristics [ Journal of Alloys and Compounds 541(2012) 505-; angewandte Chemie 123(2011) 7008-.]Have received wide attention. Such as rare earth ion Er3+/Tm3+/Yb3+Doped CaTiO3Ceramics [ Journal of Alloys and Compounds 541(2012)505-]The material has excellent dielectric property, and can emit high-energy visible photons under the excitation of 980nm infrared light; rare earth ion Er3+/Yb3+Doped BaTiO3[Angewandte Chemie 123(2011)7008-7012]The material shows excellent dielectric and ferroelectric properties at different temperatures, and can emit green light under the excitation of 980nm infrared light. However, the up-conversion luminescence-dielectric bifunctional material reported at present generally has the problem of low luminescence efficiency, and the practical application thereof is severely restricted.
Disclosure of Invention
In view of the problems of the background art, the present invention provides a manganese-doped 95MCT: Yb, Ho up-conversion luminescent-dielectric bifunctional material and a preparation method thereof, wherein the bifunctional material has excellent up-conversion luminescent and dielectric effects, and the preparation method is simple in preparation process, low in cost, strong in operability, and capable of large-scale production.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a manganese-doped 95MCT Yb and Ho up-conversion luminescent-dielectric bifunctional material has the chemical expression as follows:
MnxYb0.01Ho0.01Mg0.95Ca0.05TiO(3.03+x)
wherein x is more than 0 and less than or equal to 0.05 and is the molar concentration of manganese ions; the photo-thermal bifunctional nano material is a hexagonal phase nanosphere, and the grain size is 21-25 nm.
A method for preparing a manganese-doped 95MCT, Yb and Ho up-conversion luminescent-dielectric bifunctional material comprises the following steps,
s1: dissolving tetrabutyl titanate into ethylene glycol, heating and stirring until the solution is clear;
s2: dripping citric acid aqueous solution into the solution obtained in the step S1, and continuously heating and stirring to form uniform solution;
s3: sequentially dropping aqueous solutions of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate into the solution obtained in the step S2, and heating and stirring to form a uniform solution;
s4: heating the solution obtained in the step S3 to a certain temperature, preserving the temperature, and removing water to obtain a brownish black solid;
s5: grinding the brownish black solid obtained in the step S4 into powder, then placing the powder in a high-temperature furnace, heating to a certain temperature, and preserving heat to obtain a reaction product;
s6: and naturally cooling the reaction product obtained in the step S5 to room temperature to obtain the final manganese-doped 95 MCT-Yb-Ho up-conversion luminescent-dielectric bifunctional material.
In a preferable embodiment of the invention, the volume ratio of tetrabutyl titanate to ethylene glycol in S1 is 1:1, and the reaction temperature is 60 +/-3 ℃.
In a preferred embodiment of the present invention, the molar ratio of citric acid to ethylene glycol in S2 is 1:1, and the reaction temperature is 60 ± 3 ℃.
In a preferable embodiment of the invention, the molar ratio of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate in S3 is x:0.01:0.01:0.95:0.05, wherein x is more than 0 and less than or equal to 0.05, and the reaction temperature is 60 +/-3 ℃.
As a preferable scheme of the invention, the reaction temperature in the S4 is 220 +/-10 ℃, and the reaction time is 115 min-125 min.
As a preferable scheme of the invention, the reaction temperature in the S5 is 800 +/-20 ℃, and the reaction time is 90-95 min.
As a preferable scheme of the invention, the cold pressing process is carried out for 10-15 min at the temperature of 20 +/-5 ℃.
The reaction principle of the invention is that nitric acid compound reacts with citric acid quickly to form citric acid complex, and the citric acid reacts with Ti (OH) released by butyl titanate under the control of glycol4Complexing and reacting at 220 ℃ to form a plastic jelly; after grinding, carrying out oxidative decomposition at 800 ℃ to obtain the final manganese-doped 95 MCT-Yb-Ho up-conversion luminescent-dielectric dual-function material;
compared with the prior art, the invention has the beneficial effects that:
1. the manganese-doped 95MCT prepared by the method comprises the following steps: the Yb and Ho up-conversion luminescence-dielectric dual-function material has high purity, good uniformity and excellent luminescence and dielectric properties;
2. the crystal field can be effectively regulated and controlled by controlling the proportion of manganese ions, so that the luminous efficiency is remarkably improved while the excellent dielectric property is maintained;
3. in the present invention, the doped holmium ions Ho3+And ytterbium ion Yb3+The molar percentage of the metal ions is 1 percent respectively, citric acid is used for complexing the metal ions, ethylene glycol is used for controlling the release of the metal ions and the growth rate of crystals, and the prepared sample has excellent photoluminescence characteristics and dielectric characteristics; the 95MCT crystal field can be effectively regulated and controlled by manganese doping, so that holmium ions Ho are generated3+The avalanche luminous efficiency is obviously improved, and the green light emission intensity is the reported BaTiO3:Yb3+/Er3+More than 70 times of the total weight of the composition.
Drawings
The invention is further illustrated by the non-limiting examples given in the accompanying drawings;
FIG. 1 shows BaTiO comparative example of the present invention3XRD patterns of Yb, Er;
FIG. 2 XRD pattern of manganese-doped 95MCT Yb, Ho in an example of the invention.
FIG. 3 comparative example BaTiO of the invention3Photoluminescence spectra of Yb, Er and example manganese-doped 95MCT Yb, Ho.
Detailed Description
In order that those skilled in the art can better understand the present invention, the following technical solutions are further described with reference to the accompanying drawings and examples.
The invention discloses a laminating process for a multilayer PCB, which comprises the following steps:
comparative example:
s1: adding tetrabutyl titanate and ethylene glycol into a three-neck flask according to the volume ratio of 1:1, wherein the total volume is 10ml, and then heating and stirring at 60 ℃ to form a uniform solvent;
s2: dripping citric acid aqueous solution into the solution obtained in the step S1, wherein the molar ratio of citric acid to glycol is 1:1, and continuously heating and stirring at 60 ℃ to form uniform solution;
s3: sequentially dripping aqueous solutions of ytterbium nitrate, erbium nitrate and barium nitrate with the molar ratio of 0.025:0.005:0.97 into the solution obtained in S2), and heating and stirring at 60 ℃ to form a uniform solution;
s4: heating the solution obtained in the step S3 to 220 ℃, preserving the temperature for 2 hours, and removing water to obtain a brownish black solid;
s5: grinding the brown-black solid obtained in the step S4) into powder, then placing the powder in a high-temperature furnace, and keeping the temperature at 800 ℃ for 1.5 hours to obtain a reaction product;
s6: naturally cooling the reaction product obtained in S5 to room temperature to obtain the final BaTiO3Yb and Er up-conversion luminescence-dielectric bifunctional material.
From the XRD pattern of fig. 1, the sample is a cubic phase BaTiO3 crystal. The curve of BaTiO3 Yb and Er in the photoluminescence spectrum of FIG. 3 shows that the sample can emit green light with the central wavelength of 539nm under the excitation of 978nm infrared light;
example 1:
s1: adding tetrabutyl titanate and ethylene glycol into a three-neck flask according to the volume ratio of 1:1, wherein the total volume is 10ml, and then heating and stirring at 60 ℃ to form a uniform solvent;
s2: dripping citric acid aqueous solution into the solution obtained in the step S1, wherein the molar ratio of citric acid to glycol is 1:1, and continuously heating and stirring at 60 ℃ to form uniform solution;
s3: sequentially dripping aqueous solutions of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate in a molar ratio of 0.01:0.01:0.95:0.05 into the solution obtained by S2, and heating and stirring at 60 ℃ to form a uniform solution;
s4: heating the solution obtained in the step S3 to 220 ℃, preserving the temperature for 2 hours, and removing water to obtain a brownish black solid;
s5: grinding the brown-black solid obtained in the step S4 into powder, then placing the powder in a high-temperature furnace, and keeping the temperature at 800 ℃ for 1.5 hours to obtain a reaction product;
s6: naturally cooling the reaction product obtained in S5 to room temperature to obtain the final manganese-doped 95MCT: yb and Ho up-conversion luminescent-dielectric bifunctional material.
As can be seen from the curve a in FIG. 2, the sample is a eutectic formed by MgTiO3 in a triangular phase and CaTiO3 in a monoclinic phase; lattice parameters calculated from XRD diffraction peaks indicate that the ratio of the two eutectics, the trigonal MgTiO3 and the monoclinic CaTiO3, is 94.1: 5.9, the ratio of the components is close to 95: 5; the error mainly comes from the doped Yb3+/Ho3+Ions and Mg2+、Ca2+The radius difference of the ions;
mn in a molar ratio of 0.01 is shown by the 95MCT: Yb, Ho,0.01Mn curve in the photoluminescence spectrum of FIG. 32+Doped 95MCT: the Yb and Ho up-conversion luminescence-dielectric bifunctional material can emit green light with the central wavelength of 538nm under the excitation of 978nm infrared light, and the luminous intensity of the material is about 53 times of that of the comparative example BaTiO3 Yb and Er.
Example 2:
s1: adding tetrabutyl titanate and ethylene glycol into a three-neck flask according to the volume ratio of 1:1, wherein the total volume is 10ml, and then heating and stirring at 60 ℃ to form a uniform solvent;
s2: dripping citric acid aqueous solution into the solution obtained in the step S1, wherein the molar ratio of citric acid to glycol is 1:1, and continuously heating and stirring at 60 ℃ to form uniform solution;
s3: sequentially dripping aqueous solutions of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate in a molar ratio of 0.03:0.01:0.01:0.95:0.05 into the solution obtained from S2, and heating and stirring at 60 ℃ to form a uniform solution;
s4: heating the solution obtained in the step S3 to 220 ℃, preserving the temperature for 2 hours, and removing water to obtain a brownish black solid;
s5: grinding the brown-black solid obtained in the step S4 into powder, then placing the powder in a high-temperature furnace, and keeping the temperature at 800 ℃ for 1.5 hours to obtain a reaction product;
s6: naturally cooling the reaction product obtained in S5 to room temperature to obtain the final manganese-doped 95MCT: yb and Ho up-conversion luminescent-dielectric bifunctional material.
As can be seen from the curve b in FIG. 2, the sample is a eutectic formed by MgTiO3 in a trigonal phase and CaTiO3 in a monoclinic phase; lattice parameters calculated according to XRD diffraction peaks show that the ratio of the triangular MgTiO3 eutectic to the monoclinic CaTiO3 eutectic is 94.9:5.1, which is close to the original component ratio of 95: 5; the error mainly comes from the doped Yb3+/Ho3+Ions and Mg2+、Ca2+The radius difference of the ions;
mn in a molar ratio of 0.03 is shown by the 95MCT: Yb, Ho,0.03Mn curve in the photoluminescence spectrum of FIG. 32+Doped 95MCT: the Yb and Ho up-conversion luminescence-dielectric bifunctional material can emit green light with the central wavelength of 538nm under the excitation of 978nm infrared light, and the luminous intensity of the material is about 71 times that of the comparative example BaTiO3 Yb and Er.
Example 3:
s1: adding tetrabutyl titanate and ethylene glycol into a three-neck flask according to the volume ratio of 1:1, wherein the total volume is 10ml, and then heating and stirring at 60 ℃ to form a uniform solvent;
s2: dripping citric acid aqueous solution into the solution obtained in the step S1, wherein the molar ratio of citric acid to glycol is 1:1, and continuously heating and stirring at 60 ℃ to form uniform solution;
s3: sequentially dripping aqueous solutions of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate with the molar ratio of 0.05:0.01:0.01:0.95:0.05 into the solution obtained from S2, and heating and stirring at 60 ℃ to form a uniform solution;
s4: heating the solution obtained in the step S3 to 220 ℃, preserving the temperature for 2 hours, and removing water to obtain a brownish black solid;
s5: grinding the brown-black solid obtained in the step S4 into powder, then placing the powder in a high-temperature furnace, and keeping the temperature at 800 ℃ for 1.5 hours to obtain a reaction product;
s6: naturally cooling the reaction product obtained in S5 to room temperature to obtain the final manganese-doped 95MCT: yb and Ho up-conversion luminescent-dielectric bifunctional material.
As can be seen from the curve c in FIG. 2, the sample is a eutectic formed by MgTiO3 in the trigonal phase and CaTiO3 in the monoclinic phase; lattice parameters calculated according to XRD diffraction peaks show that the ratio of the triangular MgTiO3 eutectic to the monoclinic CaTiO3 eutectic is 94.2:5.8, which is close to the original component ratio of 95: 5; the error mainly comes from the doped Yb3+/Ho3+Ions and Mg2+、Ca2+The radius difference of the ions;
mn in a molar ratio of 0.05 is shown by the 95MCT: Yb, Ho,0.05Mn curve in the photoluminescence spectrum of FIG. 32+Doped 95MCT: the Yb and Ho up-conversion luminescence-dielectric bifunctional material can emit green light with the central wavelength of 538nm under the excitation of 978nm infrared light, and the luminous intensity of the material is about 45 times of that of the comparative example BaTiO3 Yb and Er.
The foregoing embodiments are merely illustrative of the principles of the present invention and its efficacy, and are not to be construed as limiting the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. A manganese-doped 95MCT Yb and Ho up-conversion luminescent-dielectric bifunctional material is characterized in that: the chemical expression is as follows:
MnxYb0.01Ho0.01Mg0.95Ca0.05TiO(3.03+x)
wherein x is more than 0 and less than or equal to 0.05 and is the molar concentration of manganese ions; the photo-thermal bifunctional nano material is a hexagonal phase nanosphere, and the grain size is 21-25 nm.
2. The method for preparing the manganese-doped 95MCT Yb Ho up-conversion luminescent-dielectric bifunctional material as claimed in claim 1, wherein the method comprises the following steps: comprises the following steps of (a) carrying out,
s1: dissolving tetrabutyl titanate into ethylene glycol, heating and stirring until the solution is clear;
s2: dripping citric acid aqueous solution into the solution obtained in the step S1, and continuously heating and stirring to form uniform solution;
s3: sequentially dropping aqueous solutions of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate into the solution obtained in the step S2, and heating and stirring to form a uniform solution;
s4: heating the solution obtained in the step S3 to a certain temperature, preserving the temperature, and removing water to obtain a brownish black solid;
s5: grinding the brownish black solid obtained in the step S4 into powder, then placing the powder in a high-temperature furnace, heating to a certain temperature, and preserving heat to obtain a reaction product;
s6: and naturally cooling the reaction product obtained in the step S5 to room temperature to obtain the final manganese-doped 95 MCT-Yb-Ho up-conversion luminescent-dielectric bifunctional material.
3. The method for preparing the manganese-doped 95MCT Yb Ho up-conversion luminescent-dielectric bifunctional material as claimed in claim 2, wherein the method comprises the following steps: the volume ratio of tetrabutyl titanate to ethylene glycol in the S1 is 1:1, and the reaction temperature is 60 +/-3 ℃.
4. The method for preparing the manganese-doped 95MCT Yb Ho up-conversion luminescent-dielectric bifunctional material as claimed in claim 2, wherein the method comprises the following steps: the molar ratio of the citric acid to the ethylene glycol in the S2 is 1:1, and the reaction temperature is 60 +/-3 ℃.
5. The method for preparing the manganese-doped 95MCT Yb Ho up-conversion luminescent-dielectric bifunctional material as claimed in claim 2, wherein the method comprises the following steps: the molar ratio of manganese nitrate, ytterbium nitrate, holmium nitrate, magnesium nitrate and calcium nitrate in the S3 is x:0.01:0.01:0.95:0.05, wherein x is more than 0 and less than or equal to 0.05, and the reaction temperature is 60 +/-3 ℃.
6. The method for preparing the manganese-doped 95MCT Yb Ho up-conversion luminescent-dielectric bifunctional material as claimed in claim 2, wherein the method comprises the following steps: the reaction temperature in the S4 is 220 +/-10 ℃, and the reaction time is 115-125 min.
7. The method for preparing the manganese-doped 95MCT Yb Ho up-conversion luminescent-dielectric bifunctional material as claimed in claim 2, wherein the method comprises the following steps: the reaction temperature in the S5 is 800 +/-20 ℃, and the reaction time is 90-95 min.
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