CN113548894B - Ytterbium-yttria up-conversion luminescent transparent ceramic and preparation method thereof - Google Patents
Ytterbium-yttria up-conversion luminescent transparent ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses ytterbium-yttrium oxide up-conversion luminescent transparent ceramic and a preparation method thereof. Y is the Yb 2 O 3 The chemical composition of the up-conversion luminescent transparent ceramic is Y (2‑x‑y) Zr x Yb y O 3 Wherein x is more than or equal to 0.001 and less than or equal to 0.2, and y is more than or equal to 0.02 and less than 0.5. Y is Yb 2 O 3 The transmittance of the up-conversion luminescence transparent ceramic at 1100nm is 80-82%, and the transmittance at 600nm is 72-78%. Y is Yb 2 O 3 The up-conversion luminescence transparent ceramic excites blue light with the wavelength of 488nm at the waveband of 470-500 nm.
Description
Technical Field
The invention relates to ytterbium-yttrium oxide up-conversion luminescent transparent ceramic and a preparation method thereof, belonging to the technical field of transparent ceramic preparation.
Background
Recently, rare earth ion ytterbium doped yttrium oxide up-conversion transparent ceramics are receiving great attention. Stanciu et al (Stanciu G, Gheorghe L, Voicu F M, et al, Highly transparent Yb: Y in 2019 2 O 3 ceramic associated by solid-state interaction and combined structural procedure, ceramic International,2019,45(3):3217- 2 O 3 The preparation of transparent ceramics, but without mentioning the upconversion luminescence properties, the transmittance of the sample was low, and the transmittance at 1100nm of the sample with a Yb doping amount of 2 at.% was only 78.8%. In 2010 Xiaoui Hou et al (Xiaoui, Hou, and, et al.investment of the spectroscopic properties of high viscosity transgenic Yb (Y) 0.97 Zr 0.03 ) 2 O 3 ceramic[J]Optical Materials,2010,32(11):1435- 2 O 3 Blue light at 488nm can be excited under 980nm light excitation, but the transmittance is low, and the transmittance of a sample with Yb doping amount of 1 at.% at 1100nm is 78.1%. Thus, a Yb: Y having a high transmittance was developed 2 O 3 It is necessary to convert the luminescent transparent ceramic.
Current Yb: Y 2 O 3 The preparation method of the transparent ceramic mainly comprises vacuum sintering, hot isostatic pressing sintering and the like. In 2019 Lei Zhang (Zhang L, Yang J, Zhang Z, et al blue cooperative up-conversion luminescence of Yb: Y 2 O 3 transparent ceramics[J]Ceramics International,2019,45(7):9278- 2 O 3 The temperature required by vacuum sintering of the transparent ceramic is higher (above 1750 ℃) and the time required by vacuum sintering is longer (15 hours). Jun Wang et al (Wang J, Ma J, Zhang J, et al. Yb: Y) 2017 2 O 3 transparent ceramics processed with hot isostatic pressing[J]Optical Materials,2016: S0925346716302105.71:117-120.) reports Yb: Y prepared by vacuum sintering and hot isostatic sintering 2 O 3 Transparent ceramics, but the hot isostatic pressing process is relatively expensive to produce.
Disclosure of Invention
The yttrium oxide transparent ceramic has the characteristics of cubic phase structure, wide band gap, wide light-transmitting wave band, good chemical stability and good photochemical stability, and is often used as a matrix for doping rare earth ions in the field of luminescence, but the existing yttrium oxide transparent ceramic has the problems of higher melting point (2430 ℃), difficulty in sintering and densification and overhigh preparation cost. In order to solve the problems, the invention provides ytterbium-ytterbium trioxide up-conversion luminescent transparent ceramic and a preparation method thereof. The ytterbium-trioxide up-conversion luminescent transparent ceramic has high transmittance, the transmittance at 1100nm is 80-82%, the transmittance at 600nm is 72-77%, and blue light can be excited at 488nm under the excitation of light with the wavelength of 980 nm.
In a first aspect, the present invention provides Yb: Y 2 O 3 Up-conversion luminescent transparent ceramics. Y is Yb 2 O 3 The chemical composition of the up-conversion luminescent transparent ceramic is Y (2-x-y) Zr x Yb y O 3 Wherein x is more than or equal to 0.001 and less than or equal to 0.2, and y is more than or equal to 0.02 and less than 0.5. x refers to the mole fraction of Zr and y refers to the mole fraction of Yb. Insufficient or excessive Zr can cause the change of the migration rate of the grain boundary in the sintering process, and further can reduce the visible light and near infrared light transmittance of the luminescent transparent ceramic. When Yb is insufficient, the upconversion luminescence property tends to be lowered due to a low Yb concentration. Excess Yb may be caused by Yb 3+ Ion radius (86.8pm) and Y 3+ Causes partial lattice defects to result in a decrease in transmittance, and excessively high Yb 3+ The ion concentration may cause quenching of the sample and decrease the luminescence of the upconverter.
Preferably, Yb: Y 2 O 3 The transmittance of the up-conversion luminescence transparent ceramic at 1100nm is 80-82%, and the transmittance at 600nm is 72-78%.
Preferably, the Yb: Y 2 O 3 The up-conversion luminescence transparent ceramic excites blue light with the wavelength of 488nm at the waveband of 470-500 nm.
In a second aspect, the present invention provides Yb: Y using any of the above 2 O 3 Preparation of up-conversion luminescent transparent ceramicsA method. The preparation method comprises the following steps: yb source, zirconium source and ytterbium source are mixed according to Y: Y 2 O 3 The Yb is powder Yb, Y is obtained by ball milling, drying, sieving and heat treatment after the stoichiometric ratio of the up-conversion luminescent transparent ceramic is weighed 2 O 3 Up-conversion luminescent transparent ceramics.
Preferably, the yttrium source is at least one of yttrium nitrate, yttrium oxide and yttrium chloride; the zirconium source is at least one of zirconium nitrate, zirconium oxide and zirconium acetate; the ytterbium source is at least one of ytterbium nitrate, ytterbium sulfate and ytterbium oxide.
Preferably, the temperature of the heat treatment is 800-.
Preferably, the preparation method further comprises: y is Yb in the form of powder 2 O 3 Forming the up-conversion luminescent transparent ceramic into a biscuit; sintering and annealing the biscuit to obtain Yb: Y 2 O 3 Up-conversion luminescent transparent ceramics.
Preferably, Yb: Y 2 O 3 The upper conversion luminescence transparent ceramics are formed into biscuit without cold isostatic pressing process.
Preferably, the sintering comprises pre-sintering and vacuum hot-pressing sintering after the pre-sintering; the presintering temperature is 1000-1400 ℃, and the presintering time is 0.5-2.5 hours; the sintering temperature of the vacuum hot-pressing sintering is 1400-1650 ℃, the sintering pressure is 20-60MPa, and the vacuum degree is 5 multiplied by 10 -1 -9×10 -1 Pa, hot-pressing sintering time is 0.5-3 hours.
Preferably, the annealing is heat preservation at 1200-1500 ℃ for 4-8 hours.
Y is Yb of the invention 2 O 3 The preparation method of the up-conversion luminescent transparent ceramic can still obtain good luminescent performance and light transmission performance under the conditions of relatively low sintering temperature and relatively short heat preservation time.
Drawings
FIG. 1 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 An X-ray diffraction pattern of the transparent ceramic material;
FIG. 2 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 A physical graph with the thickness of 2mm is obtained by polishing the two sides of the transparent ceramic material; it can be seen that the object images can clearly display the characters in the background picture;
FIG. 3 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 The transparent ceramic material is subjected to double-sided polishing to obtain a transmittance curve with the thickness of 2 mm;
FIG. 4 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 The transparent ceramic material has an up-conversion luminescence spectrum at 470-500 nm.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative of, and not restrictive on, the present invention. Unless otherwise specified, each percentage refers to an atomic percentage.
The present disclosure provides a Yb: Y 2 O 3 The up-conversion luminescent transparent ceramic comprises the following chemical components: y is (2-x-y) Zr x Yb y O 3 X is more than or equal to 0.001 and less than or equal to 0.2, and y is more than or equal to 0.02 and less than 0.5. Y compared with conventional Yb 2 O 3 A transparent ceramic of Yb: Y 2 O 3 The up-conversion luminescent transparent ceramic has higher transmission performance: the transmittance at 1100nm is 80-82%, and the transmittance at 600nm is 72-78%. In addition, Yb: Y 2 O 3 Yb is introduced into the up-conversion luminescent transparent ceramic to make Yb: Y 2 O 3 The up-conversion luminescence transparent ceramic has high-intensity up-conversion luminescence performance. For example, Yb: Y 2 O 3 The up-conversion luminescence transparent ceramic can excite blue light with the wavelength of 488nm in the range of 470-500nm wave band under the excitation of light with the wavelength of 980 nm. Y is the Yb 2 O 3 The up-conversion luminescent transparent ceramic is suitable for the fields of infrared detection, three-dimensional display, solid lasers, high-density data storage, laser medical treatment and the likeA domain. Preferably, 0.001. ltoreq. x.ltoreq.0.1 and 0.02. ltoreq. y.ltoreq.0.2.
Y is exemplified below 2 O 3 A method for preparing up-conversion luminescent transparent ceramics.
And (4) batching. According to Y (2-x-y) Zr x Yb y O 3 Weighing yttrium source, zirconium source and ytterbium source as raw material powder according to the stoichiometric ratio of x being more than or equal to 0.001 and less than or equal to 0.2 and y being more than or equal to 0.02 and less than 0.5. Yttrium sources include, but are not limited to, at least one of yttrium nitrate, yttrium oxide, yttrium chloride. The zirconium source includes, but is not limited to, at least one of zirconium nitrate, zirconium oxide, and zirconium acetate. The ytterbium source includes, but is not limited to, at least one of ytterbium nitrate, ytterbium sulfate, and ytterbium oxide. As an example, the yttrium source, the zirconium source and the ytterbium source are respectively yttrium nitrate, zirconium oxide and ytterbium nitrate.
The raw material powder is ball milled, preferably wet ball milled. The ball milling speed can be 210-250 rpm. The ball milling time may be 16-24 hours. As an example, a zirconium ball is used as a grinding ball, and raw material powder, the grinding ball and absolute ethyl alcohol are mixed according to a mass ratio of 1: 5: 2, performing ball milling.
The slurry formed by ball milling is dried. The drying temperature can be 55-70 deg.C, and the drying time can be 24-36 hr. Drying may be carried out in a drying oven. And sieving the dried powder. Preferably 120-mesh and 200-mesh. In some embodiments, each pass is performed twice.
And (4) carrying out heat treatment on the sieved powder so as to remove possible organic matters in the powder. The heat treatment is heat preservation for 1-5 hours at 800-1200 ℃.
Yb Y obtained by heat treatment 2 O 3 The particle size of the up-conversion luminescent transparent ceramic powder is uniform. The particle size may be 0.01-0.5 μm.
Yb is expressed as Y 2 O 3 And (3) forming the up-conversion luminescent transparent ceramic powder. The pressure can be maintained for 10 to 50 seconds under the pressure of 2 to 10MPa for molding. For example, Y is added to Yb at a pressure of 2-10MPa 2 O 3 And (3) pressurizing the upper conversion luminescent transparent ceramic material powder on two sides and keeping the pressure for 10 to 40 seconds to form a biscuit. This is because the mechanical stress generated during hot-press sintering acts as an additional driving force to promote Yb: Y 2 O 3 Sintering the up-conversion luminescent transparent ceramic biscuit. If the biscuit is subjected to cold isostatic pressing, the sample can obtain higher strength, but the shrinkage of the sample in the hot-pressing sintering process is not facilitated, which influences Yb: Y 2 O 3 The optical performance of the luminescent transparent ceramic is converted. Therefore, the process of forming the biscuit does not need cold isostatic pressing treatment.
And (4) pre-sintering. Yb to Y 2 O 3 The up-conversion luminescence transparent ceramic biscuit is pre-sintered for 0.5 to 2 hours at the temperature of 1000-1400 ℃. The pre-sintering may be performed in a high temperature furnace. The presintering atmosphere is air.
And (4) vacuum hot-pressing sintering. The sample obtained by air presintering is vacuum degree of 5X 10 -1 -9×10 -1 Hot-pressing and sintering for 0.5-3 hours under the conditions of Pa, pressure of 20-60MPa and temperature of 1400-1650 ℃.
And (6) annealing. And (3) carrying out heat preservation sintering on the sintered sample at the temperature of 1200-1500 ℃ for 4-8 hours. The annealing atmosphere is air.
The transparent ceramic capable of absorbing ultraviolet light provided by the invention has the advantages of higher visible light transmittance, high sintering density and up-conversion luminescence. In addition, the preparation method adopts a sintering process of air presintering, vacuum hot-pressing sintering and annealing, and takes yttria as a main body, and zirconia plays a role in promoting sintering in the sintering process, so that the transparent ceramic with high transmittance and up-conversion luminescence performance is prepared under the conditions of low hot-pressing sintering temperature (1400-1650 ℃) and short heat preservation time (0.5-3 hours).
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
And (3) preparing powder. According to Y (2-x-y) Zr x Yb y O 3 Weighing yttrium nitrate, zirconium oxide and ytterbium nitrate according to the stoichiometric ratio (atomic ratio) of the elements (wherein x is 0.02, y is 0.02, namely the doping amount of zirconium is 1 at.%, and the doping amount of ytterbium is 1 at.%), dissolving the yttrium nitrate, the zirconium oxide and the ytterbium nitrate in a proper amount of absolute ethyl alcohol, and uniformly mixing. The mass ratio of the total mass of the raw material powder to the absolute ethyl alcohol is 1: 2. The mixture of the raw material powder and the absolute ethyl alcohol was placed in a planetary ball mill and ball-milled at 210 rpm for 16 hours to form a slurry. The ball-milled slurry was dried in a 50 ℃ drying oven for 24 hours. Sieving the dried powder twice with 120 mesh sieve, and performing heat treatment on the sieved powder to obtain Yb: Y with proper and uniform particle size 2 O 3 And converting the luminescent transparent ceramic material powder. The heat treatment conditions were incubation at 800 ℃ for 1 hour.
And (5) forming ceramic material powder. Adopting a dry pressing forming process with the pressure of 2MPa and the dwell time of 10 seconds to obtain Yb: Y sintered by vacuum hot pressing 2 O 3 And converting the green body of the luminescent transparent ceramic material.
And (5) sintering the biscuit. Y is the formed Yb sintered by vacuum hot pressing 2 O 3 Pre-burning the transparent ceramic biscuit at 1000 deg.c for 0.5 hr, and final sintering at 1400 deg.c and vacuum degree of 9X 10 -1 And (4) sintering for 0.5 hour under the conditions of Pa and the pressure of 20 MPa.
And (6) annealing and heat treatment. Preserving the heat of the sample after vacuum hot-pressing sintering in a high-temperature furnace at 1200 ℃ for 4 hours to obtain the Yb: Y sintered by vacuum hot-pressing 2 O 3 (Y 1.96 Zr 0.02 Yb 0.02 O 3 ) An up-conversion luminescent transparent ceramic material.
Transmittance evaluation experiment: the prepared sample is subjected to a transmittance test in the range of 190-1100nm by a spectrophotometer.
Upper conversion luminescence evaluation experiment: the prepared sample is subjected to up-conversion luminescence test in the range of 470-500nm by a low-temperature absorption spectrometer.
Yb: Y sintered by vacuum hot pressing 2 O 3 Up-conversion luminescent transparent ceramic materialThe transmittance at 1100nm was 81.7%, the transmittance at 600nm was 77.2%, and converted luminescence on blue light was produced at 448 nm. Due to Yb of the present embodiment 3+ The ion concentration is small, so the up-conversion luminescence intensity is relatively low.
Example 2
And (3) preparing powder. According to Y (2-x-y) Zr x Yb y O 3 Weighing yttrium nitrate, zirconium oxide and ytterbium nitrate according to the stoichiometric ratio (atomic ratio) of the elements (wherein x is 0.02, y is 0.06, namely the doping amount of zirconium is 1 at.%, and the doping amount of ytterbium is 3 at.%), dissolving the yttrium nitrate, the zirconium oxide and the ytterbium nitrate in a proper amount of absolute ethyl alcohol, and uniformly mixing. The mass ratio of the total mass of the raw material powder to the absolute ethyl alcohol is 1: 2. The mixture of the raw material powder and the absolute ethyl alcohol is placed in a planetary ball mill and ball-milled for 18 hours at 220 revolutions per minute to form slurry. The ball-milled slurry was dried in a 55 ℃ dry box for 28 hours. Sieving the dried powder twice with a 140-mesh sieve, and performing heat treatment on the sieved powder to obtain Yb: Y with proper and uniform particle size 2 O 3 And converting the luminescent transparent ceramic material powder. The heat treatment condition is heat preservation for 2 hours at 900 ℃.
And (5) forming ceramic material powder. The Yb: Y sintered by vacuum hot pressing is obtained by adopting a dry pressing forming process with the pressure of 4MPa and the dwell time of 20 seconds 2 O 3 And converting the green body of the luminescent transparent ceramic material.
And (5) sintering the biscuit. Y is the formed Yb sintered by vacuum hot pressing 2 O 3 Pre-burning the green body in a high-temperature furnace at 1100 deg.c for 1 hr, and final treating at 1450 deg.c and vacuum degree of 8X 10 -1 Pa and a pressure of 30MPa for 1 hour.
And (6) annealing and heat treatment. Keeping the sample subjected to vacuum hot-pressing sintering in a high-temperature furnace at 1300 ℃ for 5 hours to obtain the Yb/Y subjected to vacuum hot-pressing sintering 2 O 3 (Y 1.92 Zr 0.02 Yb 0.06 O 3 ) An up-conversion luminescent transparent ceramic material.
Yb: Y sintered by vacuum hot pressing 2 O 3 The transmittance of the up-conversion luminescent transparent ceramic material at 1100nm is81.6%, and a transmittance at 600nm of visible light of 76.5%. The sample of this example has an enhanced intensity of converted luminescence at 448nm in blue light relative to the example.
Example 3
And (3) preparing powder. According to Y (2-x-y) Zr x Yb y O 3 Weighing yttrium nitrate, zirconium oxide and ytterbium nitrate according to the stoichiometric ratio (atomic ratio) of the elements (wherein x is 0.02, y is 0.10, namely the doping amount of zirconium is 1 at.%, and the doping amount of ytterbium is 5 at.%), dissolving the yttrium nitrate, the zirconium oxide and the ytterbium nitrate in a proper amount of absolute ethyl alcohol, and uniformly mixing. The mass ratio of the total mass of the raw material powder to the absolute ethyl alcohol is 1: 2. The mixture of the raw material powder and the absolute ethyl alcohol is placed in a planetary ball mill and ball-milled for 20 hours at 230 revolutions per minute to form slurry. The ball-milled slurry was dried in a 60 ℃ drying oven for 30 hours. Sieving the dried powder twice with 160 mesh sieve, and performing heat treatment on the sieved powder to obtain Yb: Y with proper and uniform particle size 2 O 3 And converting the luminescent transparent ceramic material powder. The heat treatment condition is heat preservation for 3 hours at 1000 ℃.
And (5) forming ceramic material powder. Adopting a dry pressing forming process with the pressure of 6MPa and the dwell time of 30 seconds to obtain Yb: Y sintered by vacuum hot pressing 2 O 3 And converting the green body of the luminescent transparent ceramic material.
And (5) sintering the biscuit. Y is the formed Yb sintered by vacuum hot pressing 2 O 3 Pre-burning the green body in a high-temperature furnace at 1200 deg.c for 1.5 hr, and further treating at 1500 deg.c and 7X 10 vacuum degree -1 And Pa, the pressure is 40MPa, and the sintering is carried out for 1.5 hours.
And (4) annealing heat treatment. Keeping the sample after vacuum hot-pressing sintering in a high-temperature furnace at 1350 ℃ for 6 hours to obtain the Yb: Y sintered by vacuum hot-pressing 2 O 3 (Y 1.88 Zr 0.02 Yb 0.10 O 3 ) An up-conversion luminescent transparent ceramic material.
Yb: Y sintered by vacuum hot pressing 2 O 3 The transmittance of the up-conversion luminescent transparent ceramic material at 1100nm is 81.1%, and the transmittance at 600nm of visible light is 73.7%. This exampleThe intensity of converted luminescence on blue light at 448nm was enhanced compared to examples 1-2.
Example 4
And (3) preparing powder. According to Y (2-x-y) Zr x Yb y O 3 Weighing yttrium nitrate, zirconium oxide and ytterbium nitrate according to the stoichiometric ratio (atomic ratio) of the elements (wherein x is 0.02, y is 0.16, namely the doping amount of zirconium is 1 at.%, and the doping amount of ytterbium is 8 at.%), dissolving the yttrium nitrate, the zirconium oxide and the ytterbium nitrate in a proper amount of absolute ethyl alcohol, and uniformly mixing. The mass ratio of the total mass of the raw material powder to the absolute ethyl alcohol is 1: 2. The mixture of the raw material powder and the absolute ethyl alcohol was placed in a planetary ball mill and ball-milled at 240 revolutions per minute for 22 hours to form a slurry. The ball-milled slurry was dried in a drying oven at 65 ℃ for 32 hours. Sieving the dried powder twice with 180 mesh sieve, and performing heat treatment on the sieved powder to obtain Yb: Y with proper and uniform particle size 2 O 3 And converting the luminescent transparent ceramic material powder. The heat treatment conditions were heat preservation at 1100 ℃ for 4 hours.
And (5) forming ceramic material powder. Adopting a dry pressing forming process with the pressure of 8MPa and the dwell time of 40 seconds to obtain Yb: Y sintered by vacuum hot pressing 2 O 3 And converting the green body of the luminescent transparent ceramic material.
And (5) sintering the biscuit. Y is the Yb sintered by vacuum hot pressing after molding 2 O 3 Pre-burning the green body in a 1300 deg.c high temperature furnace for 2 hr, and final treating at 1600 deg.c and 6X 10 vacuum degree -1 And Pa and the pressure of 50MPa for 2 hours.
And (6) annealing and heat treatment. Keeping the sample after vacuum hot-pressing sintering in a high-temperature furnace at 1400 ℃ for 7 hours to obtain the Yb/Y sintered by vacuum hot-pressing 2 O 3 (Y 1.82 Zr 0.02 Yb 0.16 O 3 ) An up-conversion luminescent transparent ceramic material.
Yb: Y sintered by vacuum hot pressing 2 O 3 The transmittance of the up-conversion luminescent transparent ceramic material at 1100nm is 80.5%, and the transmittance at 600nm of visible light is 72.8%. The intensity of luminescence converted on blue light at 448nm for the sample of this example compared to example 1-3 is enhanced.
Comparative example 1
And (3) preparing powder. According to Y (2-x-y) Zr x Yb y O 3 Weighing yttrium nitrate and zirconium oxide according to the stoichiometric ratio (atomic ratio) of elements (wherein x is 0.02, y is 0, namely the doping amount of zirconium is 1 at.%, and the doping amount of ytterbium is 0 at.%), dissolving the yttrium nitrate and the zirconium oxide in a proper amount of absolute ethyl alcohol, and uniformly mixing. The mass ratio of the total mass of the raw material powder to the absolute ethyl alcohol is 1: 2. The mixture of the raw material powder and absolute ethyl alcohol was placed in a planetary ball mill and ball-milled at 250 revolutions per minute for 24 hours to form a slurry. The ball-milled slurry was dried in a drying oven at 70 ℃ for 36 hours. Sieving the dried powder twice with 200 mesh sieve, and performing heat treatment on the sieved powder to obtain vacuum hot-pressed sintered Y with proper and uniform particle size 2 O 3 Transparent ceramic material powder. The heat treatment condition is heat preservation at 1200 ℃ for 5 hours.
And (5) forming ceramic material powder. The vacuum hot-pressing sintered Y is obtained by adopting a dry pressing forming mode with the pressure of 10MPa and the pressure maintaining time of 50 seconds 2 O 3 A transparent ceramic biscuit.
And (5) sintering the biscuit. The formed Y is sintered by vacuum hot pressing 2 O 3 The transparent ceramic biscuit is preburnt in a high temperature furnace at 1400 deg.C for 2.5 hr, and then passed through a high temperature furnace at 1650 deg.C and a vacuum degree of 5 × 10 -1 Pa and 60MPa for 3 hours.
And (6) annealing and heat treatment. Keeping the sample after vacuum hot pressing sintering in a high temperature furnace at 1500 ℃ for 8 hours to obtain (Y) 1.98 Zr 0.02 O 3 ) Vacuum hot pressed sintered Y 2 O 3 (Y 1.98 Zr 0.02 O 3 ) A transparent ceramic material.
Vacuum hot pressed sintered Y 2 O 3 The transparent ceramic material has a transmittance of 81.8% at 1100nm and a transmittance of 77.7% at 600nm of visible light, and has no upconversion luminescence at 448 nm.
FIG. 1 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 X-ray diffraction pattern of transparent ceramic material. As can be seen from FIG. 1, Yb: Y was sintered by vacuum hot pressing 2 O 3 Up-conversion luminous transparent ceramic material and vacuum hot-pressed sintered Y 2 O 3 The transparent ceramic material has a single yttrium oxide structure, because ytterbium ions and zirconium ions enter the crystal lattice of yttrium oxide to replace the positions of yttrium ions, and the crystal structure of yttrium oxide is not changed.
FIG. 2 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 And (3) carrying out double-sided polishing on the transparent ceramic material to obtain a physical picture with the thickness of 2 mm. As can be seen from fig. 2, all samples were highly transparent, and the text under the samples was clearly visible.
FIG. 3 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 The transparent ceramic material is subjected to double-side polishing to obtain a transmittance curve with the thickness of 2 mm. As can be seen from FIG. 3, when the Yb doping amount was 0 at.%, Y was sintered by vacuum hot pressing 2 O 3 The transmittance of the transparent ceramic material at 1100nm is 81.8%; as the Yb concentration increased, the sample transmittance slightly decreased, and the transmittance at 1100nm was maintained at substantially 80% or more. The prepared samples of examples 1-4 have absorption in the 800-1100nm band, and the absorption intensity is enhanced along with the increase of the ytterbium doping concentration; however, when Yb is doped in an amount of 0 at.%, Y is sintered by vacuum hot pressing 2 O 3 The transparent ceramic material has no absorption in the 800-1100nm wave band.
FIG. 4 shows Yb: Y obtained in examples 1 to 4 2 O 3 Up-conversion luminescent transparent ceramic material and Y prepared in comparative example 1 2 O 3 The up-conversion luminescence spectrum of the transparent ceramic material at 470-500 nm. As can be seen from FIG. 4, Yb: Y 2 O 3 The sample has a blue light emission peak at 488nm, and the blue light emission intensity gradually increases along with the increase of the ytterbium concentration. However, when Yb is doped in an amount of 0 at.%, Y is vacuum hot-pressed and sintered 2 O 3 The transparent ceramic material has no blue light up-conversion luminescence phenomenon. This is because Yb is separatedThe coupled energy level formed by the photon when excited by 980nm light 2 F 5/2 - 2 F 5/2 And a synergistic light emitting effect is generated when the light transits back to the ground state energy level.
Claims (5)
1. Yb is Y 2 O 3 The up-conversion luminescent transparent ceramic is characterized in that Yb is Y 2 O 3 The chemical composition of the up-conversion luminescent transparent ceramic is Y (2-x-y) Zr x Yb y O 3 Wherein x is more than or equal to 0.001 and less than or equal to 0.2, and y is more than or equal to 0.02 and less than 0.5; y is Yb 2 O 3 The transmittance of the up-conversion luminescent transparent ceramic at 1100nm is 80-82%, and the transmittance at 600nm is 72-78%;
y is the Yb 2 O 3 The preparation method of the up-conversion luminescent transparent ceramic comprises the following steps: yb, Y is the ratio of yttrium source to zirconium source to ytterbium source 2 O 3 The Yb is obtained by ball milling, drying, sieving and heat treatment after the stoichiometric ratio of the up-conversion luminescent transparent ceramic is weighed 2 O 3 Up-conversion luminescent transparent ceramics; the preparation method further comprises the following steps: y is Yb in the form of powder 2 O 3 Forming the up-conversion luminescent transparent ceramic into a biscuit; sintering and annealing the biscuit to obtain Yb: Y 2 O 3 Up-conversion luminescent transparent ceramics; y is the Yb 2 O 3 The upper conversion luminescence transparent ceramics are formed into a biscuit without a cold isostatic pressing process; the sintering comprises pre-sintering and vacuum hot-pressing sintering after the pre-sintering; the presintering temperature is 1000-1400 ℃, and the presintering time is 0.5-2.5 hours; the sintering temperature of the vacuum hot-pressing sintering is 1400-1650 ℃, the sintering pressure is 20-60MPa, and the vacuum degree is 5 multiplied by 10 -1 -9×10 -1 Pa, and the hot-pressing sintering time is 0.5-3 hours.
2. Y is the Yb of claim 1 2 O 3 The up-conversion luminescent transparent ceramic is characterized in that Yb is Y 2 O 3 The up-conversion luminescence transparent ceramic excites blue light with the wavelength of 488nm at the wave band of 470-500 nm.
3. Root of herbaceous plantY is the Yb of claim 1 2 O 3 The up-conversion luminescent transparent ceramic is characterized in that the yttrium source is at least one of yttrium nitrate, yttrium oxide and yttrium chloride; the zirconium source is at least one of zirconium nitrate, zirconium oxide and zirconium acetate; the ytterbium source is at least one of ytterbium nitrate, ytterbium sulfate and ytterbium oxide.
4. Y is the Yb of claim 1 2 O 3 The up-conversion luminescent transparent ceramic is characterized in that the temperature of the heat treatment is 800-1200 ℃, and the heat preservation time of the heat treatment is 1-5 hours.
5. Y is the Yb of claim 1 2 O 3 The up-conversion luminescence transparent ceramic is characterized in that the annealing is carried out at the temperature of 1200-1500 ℃ for 4-8 hours.
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