Rare earth doped tellurite material and liquid phase preparation method thereof

Abstract

The invention relates to the technical field of inorganic micro-nano material synthesis, and provides a rare earth doped tellurite material and a liquid phase preparation method thereof, the chemical formula of the obtained rare earth doped tellurite material is (R.E.) wTexOyClz, and R.E. Is a rare earth element and comprises one or more of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu. The method is simple in process, good in universality, low in energy consumption and flexible and adjustable in product component, and the mechanical stability and the chemical stability of the rare earth doped tellurite material are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of inorganic micro-nano material synthesis, and particularly relates to a rare earth doped tellurite material and a liquid phase preparation method thereof. BACKGROUND

[0002] The research on rare earth fluoride in the existing system is relatively mature, but there are problems of poor chemical stability and mechanical stability, and application limitations in some special conditions such as high temperature, humidity and corrosive environment. The research on high-performance up-conversion luminescence micro-nano materials based on oxide matrix materials urgently needs to seek an oxide-based micro-nano material with good development prospects. The preparation method of the rare earth oxide-based material is usually a high-temperature solid phase method, which needs a high sintering temperature and a long calcination time, and has the disadvantages of high energy consumption, long time, easy agglomeration and uncontrollable morphology. Compared with the high-temperature solid phase method, the liquid phase hydrothermal synthesis method has low energy consumption, and through controlling the reaction temperature, reaction time, precursor concentration, precursor solution pH and adding a suitable surfactant, the particle morphology and crystal phase can be accurately controlled to obtain the material with the best performance. SUMMARY

[0003] The present application aims to at least solve one of the technical problems in the related art. To this end, the present application provides a rare earth doped tellurite material and a liquid phase preparation method thereof, which has the advantages of simple process, low energy consumption, controllable particle morphology, high purity, and improved mechanical stability and chemical stability of the rare earth doped tellurite material.

[0004] The present application provides a rare earth doped tellurite material, and the chemical formula of the rare earth doped tellurite material is: (R.E.) w Te x O y Cl z Among them, R.E. is a rare earth element, including one or more of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.

[0005] According to the rare earth doped tellurite material provided by the present application, the chemical formula (R.E.) w Te x O y Cl z Among them: 0 < w < 6; 1 < x < 6; 1 < y < 20; 0 < z < 1 Among them, w, x, y and z are molar coefficients.

[0006] This invention also provides a liquid-phase preparation method for rare earth-doped tellurite materials, which is used to prepare the rare earth-doped tellurite materials as described above, and specifically includes the following steps: S100, weigh out rare earth compounds and tellurite; S200. Rare earth compounds and tellurite are added to deionized water to obtain aqueous solutions of rare earth compounds and tellurite. S300. Add the acid solution to the tellurite aqueous solution to obtain the first mixed solution; S400. Under ultrasonic conditions, the aqueous solution of rare earth compound is mixed with the first mixed solution to obtain the second mixed solution; S500: Transfer the second mixed solution into the reaction vessel and use hydrothermal treatment to obtain a suspension; S600: The suspension is subjected to solid-liquid two-phase separation treatment, the solid precipitate is collected, and rare earth doped tellurite solid phase product is obtained. S700: Wash the rare earth-doped tellurite solid phase product with ultrapure water by centrifugation and ultrasonication, and then dry the rare earth-doped tellurite solid phase product. S800: Grind the dried solid product to obtain rare earth-doped tellurite (RE). w Te x O y Cl z solid powder; S900. As needed, the rare earth-doped tellurite solid powder is calcined, and the calcined rare earth-doped tellurite solid powder is ground to obtain rare earth-doped tellurite material (RE). w Te x O y Cl z .

[0007] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein the rare earth compound may be a rare earth halide, a rare earth oxide, a rare earth hydroxide, a rare earth nitrate, a rare earth acetate, a rare earth phosphate, a rare earth carbonate, a rare earth chlorate, a rare earth sulfate, or a rare earth organic complex.

[0008] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein the tellurite can be telluric acid, sodium tellurite, or potassium tellurite.

[0009] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein the acid solution can be hydrochloric acid, nitric acid, sulfuric acid, or acetic acid.

[0010] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein in steps S200, S300, and S400, one or more rare earth compounds are added to or dispersed in water to obtain an aqueous system of rare earth compounds; tellurite is added to or dispersed in water, and a predetermined amount of acid is added to obtain an aqueous system of tellurite; subsequently, the aqueous system of rare earth compounds is combined with H... + The combined tellurite aqueous system was mixed to obtain a mixture, which was then ultrasonically mixed for a set time to obtain the aqueous system of the precursor. Alternatively, one or more rare earth compounds are added to or dispersed in water to prepare an aqueous system of rare earth compounds; tellurite is added to or dispersed in water to prepare an aqueous system of tellurite; the aqueous system of rare earth compounds and the aqueous system of tellurite are mixed to obtain a mixture; a set amount of acid is added to the mixture to adjust the pH of the mixture; and ultrasonic mixing is performed for a set time to obtain an aqueous system of the precursor. Alternatively, one or more rare earth compounds are added to or dispersed in water to prepare an aqueous system of rare earth compounds; tellurite is directly added to the aqueous system of rare earth compounds and mixed to obtain a mixed solution; a set amount of acid is added to adjust the pH of the mixed solution; and ultrasonic mixing is performed for a set time to obtain an aqueous system of the precursor. Alternatively, one or more rare earth compounds can be added to or dispersed in water, and a set amount of acid can be added to prepare an aqueous system of rare earth compounds; tellurite can be directly added to the aqueous system of rare earth compounds; ultrasonic mixing can be performed for a set time to obtain an aqueous system of the precursor. Alternatively, tellurite can be added to or dispersed in water, and a set amount of acid can be added to prepare an aqueous system of tellurite; one or more rare earth compounds can be directly added to the aqueous system of tellurite; and ultrasonic mixing can be performed for a set time to obtain an aqueous system of the precursor. Alternatively, tellurite can be added to or dispersed in water, or one or more rare earth compounds can be directly added to the aqueous system of tellurite and mixed to obtain a mixture; a set amount of acid can be added to adjust the pH of the mixture; and ultrasonic mixing can be performed for a set time to obtain an aqueous system of the precursor.

[0011] According to the liquid-phase preparation method of rare earth-doped tellurite material provided by the present invention, in step S400, the molar ratio of tellurite to rare earth element in the aqueous solution of rare earth compound in the second mixed solution is (1~10):(1~10); the duration of ultrasonic environment is 10min~120min; and the volume of the second mixed solution is 5mL~200mL.

[0012] According to the liquid-phase preparation method of rare earth doped tellurite material provided by the present invention, in step S500, the temperature of the hydrothermal treatment is 40℃~300℃ and the treatment time is 0h~100h.

[0013] According to the liquid-phase preparation method of rare earth doped tellurite material provided by the present invention, in step S700, the drying temperature is 40℃~100℃ and the drying time is 4h~24h.

[0014] According to the liquid-phase preparation method of rare earth doped tellurite material provided by the present invention, in step S900, the calcination temperature is 240℃~1200℃ and the calcination time is 0h~24h.

[0015] The above-described one or more technical solutions in the embodiments of the present invention have at least one of the following technical effects: This invention utilizes a pure aqueous phase hydrothermal method to prepare rare earth-doped tellurite materials. Compared with traditional high-temperature solid-phase preparation methods, the preparation process is environmentally friendly, simple, energy-efficient, highly pure, easy to control and manipulate the growth environment, has good versatility, and is easy to scale up. This invention utilizes a pure aqueous phase hydrothermal method to prepare rare earth-doped tellurite materials. By precisely controlling synthesis parameters, including the pH, concentration, time, and temperature of the precursor solution, the crystal phase structure, particle size distribution, surface morphology, and various properties of the product can be regulated as needed. The rare earth-doped tellurite material prepared by the pure aqueous phase hydrothermal method of this invention has good mechanical and chemical stability, which can solve the problem of expanding the application of rare earth-doped fluoride materials under certain special conditions such as high temperature, humidity and corrosive environment. This invention relates to rare earth-doped tellurite materials prepared by a pure aqueous phase hydrothermal method, with the chemical formula (RE). w Te x O y Cl z By changing the types of trivalent rare earth dopants, bright emission of red, green and blue light under 980nm infrared light excitation can be achieved, which has good development prospects in the field of luminescent materials.

[0016] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0018] Figure 1 The X-ray diffraction test curve of the sample in Example 1 of this invention is shown.

[0019] Figure 2 The X-ray diffraction test curve of the sample in Example 2 of this invention is shown.

[0020] Figure 3 The X-ray diffraction test curve of the sample in Example 3 of this invention is shown.

[0021] Figure 4 The X-ray diffraction test curve of the sample in Example 4 of this invention is shown.

[0022] Figure 5 The X-ray diffraction test curve of the sample in Example 5 of this invention is shown.

[0023] Figure 6 The X-ray diffraction test curve of the sample in Example 6 of this invention is shown.

[0024] Figure 7 The X-ray diffraction test curve of the sample in Example 7 of this invention is shown.

[0025] Figure 8 The X-ray diffraction test curve of the sample in Example 8 of this invention is shown.

[0026] Figure 9 This is a scanning electron microscope image of the sample from Example 1 of the present invention.

[0027] Figure 10 This is a scanning electron microscope image of the sample from Example 2 of the present invention.

[0028] Figure 11 This is a scanning electron microscope image of the sample from Example 3 of the present invention.

[0029] Figure 12 This is a scanning electron microscope image of the sample from Example 4 of the present invention.

[0030] Figure 13 This is a scanning electron microscope image of the sample from Example 5 of the present invention.

[0031] Figure 14 This is a scanning electron microscope image of the sample from Example 6 of the present invention.

[0032] Figure 15 This is a scanning electron microscope image of the sample from Example 8 of the present invention.

[0033] Figure 16 The photoluminescence spectrum of the sample in Example 8 of this invention under 980 nm infrared light excitation. Detailed Implementation

[0034] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention. The following embodiments are used to illustrate this invention but should not be used to limit the scope of this invention.

[0035] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0036] The following is combined Figures 1 to 16 This invention describes the rare earth-doped tellurite materials and their liquid-phase preparation method, along with related embodiments.

[0037] This invention provides a rare earth-doped tellurite material, the chemical formula of which is: (RE) w Te x O y Cl z RE represents rare earth elements, including one or more of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu.

[0038] According to the present invention, a rare earth-doped tellurite material is provided, wherein the chemical formula (RE) is... w Te x O y Cl z middle: 0 < w ≤ 6; 1 ≤ x ≤ 6; 1 ≤ y ≤ 20; 0 ≤ z ≤ 1 Where w, x, y, and z are all molar coefficients.

[0039] The rare earth-doped tellurite material (RE) of the present invention w Te x Oy Cl z The composition is flexible and adjustable, and the content and proportion of each rare earth element can be adjusted at will.

[0040] The rare earth-doped tellurite material (RE) of the present invention w Te x O y Cl z It has good mechanical and chemical stability.

[0041] It should be noted that the rare earth-doped tellurite material provided by this invention is a multifunctional optoelectronic material. It can achieve the performance required in the fields of upconversion emission and downconversion emission by precisely selecting and combining rare earth elements in the material. At the same time, it also has great application potential in the fields of energy storage, catalysis, optoelectronics and sensing.

[0042] The following describes a liquid-phase preparation method for a rare-earth-doped tellurite material provided by the present invention. The liquid-phase preparation method for a rare-earth-doped tellurite material described below can be referred to in correspondence with the rare-earth-doped tellurite material described above.

[0043] This invention also provides a liquid-phase preparation method for rare earth-doped tellurite materials, which is used to prepare the rare earth-doped tellurite materials as described above, and specifically includes the following steps: S100, weigh out tellurite and rare earth compounds; S200. Tellurite and rare earth compounds are added to or dispersed in a deionized aqueous solution, respectively. S300. Add the acid solution to the tellurite aqueous solution to obtain the first mixed solution; S400. Under ultrasonic conditions, the aqueous solution of rare earth compound is mixed with the first mixed solution to obtain the second mixed solution; S500: Transfer the second mixed solution into the reaction vessel and use hydrothermal treatment to obtain a suspension; S600: The suspension is subjected to solid-liquid two-phase separation treatment, the solid precipitate is collected, and rare earth doped tellurite solid phase product is obtained. S700: Wash the rare earth-doped tellurite solid phase product with ultrapure water by centrifugation and ultrasonication, and then dry the rare earth-doped tellurite solid phase product. S800: Grind the dried solid product to obtain rare earth-doped tellurite (RE). w Te x O y Cl z solid powder; S900. As needed, the rare earth-doped tellurite solid powder is calcined, and the calcined rare earth-doped tellurite solid powder is ground to obtain rare earth-doped tellurite material (RE). w Te x O y Cl z .

[0044] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein the rare earth compound may be a rare earth halide, a rare earth oxide, a rare earth hydroxide, a rare earth nitrate, a rare earth acetate, a rare earth phosphate, a rare earth carbonate, a rare earth chlorate, a rare earth sulfate, or a rare earth organic complex.

[0045] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein the tellurite can be telluric acid, sodium tellurite, or potassium tellurite.

[0046] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein the acid solution can be hydrochloric acid, nitric acid, sulfuric acid, or acetic acid.

[0047] According to the present invention, a liquid-phase preparation method for rare earth-doped tellurite materials is provided, wherein in steps S200, S300, and S400, one or more rare earth compounds are added to or dispersed in water to obtain an aqueous system of rare earth compounds; tellurite is added to or dispersed in water, and a predetermined amount of acid is added to obtain an aqueous system of tellurite; subsequently, the aqueous system of rare earth compounds is combined with H... + The combined tellurite aqueous system was mixed to obtain a mixture, which was then ultrasonically mixed for a set time to obtain the aqueous system of the precursor. Alternatively, one or more rare earth compounds are added to or dispersed in water to prepare an aqueous system of rare earth compounds; tellurite is added to or dispersed in water to prepare an aqueous system of tellurite; the aqueous system of rare earth compounds and the aqueous system of tellurite are mixed to obtain a mixture; a set amount of acid is added to the mixture to adjust the pH of the mixture; and ultrasonic mixing is performed for a set time to obtain an aqueous system of the precursor. Alternatively, one or more rare earth compounds are added to or dispersed in water to prepare an aqueous system of rare earth compounds; tellurite is directly added to the aqueous system of rare earth compounds and mixed to obtain a mixed solution; a set amount of acid is added to adjust the pH of the mixed solution; and ultrasonic mixing is performed for a set time to obtain an aqueous system of the precursor. Alternatively, one or more rare earth compounds can be added to or dispersed in water, and a set amount of acid can be added to prepare an aqueous system of rare earth compounds; tellurite can be directly added to the aqueous system of rare earth compounds and mixed to obtain a mixture; ultrasonic mixing for a set time can be used to obtain an aqueous system of the precursor. Alternatively, tellurite can be added to or dispersed in water, and a predetermined amount of acid can be added to prepare an aqueous system of tellurite; one or more rare earth compounds can be directly added to the aqueous system of tellurite and mixed to obtain a mixture; ultrasonic mixing for a predetermined time can then be used to obtain an aqueous system of the precursor. Alternatively, tellurite can be added to or dispersed in water, or one or more rare earth compounds can be directly added to the aqueous system of tellurite and mixed to obtain a mixture; a set amount of acid can be added to adjust the pH of the mixture; and ultrasonic mixing can be performed for a set time to obtain an aqueous system of the precursor.

[0048] According to the liquid-phase preparation method of rare earth-doped tellurite material provided by the present invention, in step S400, the molar ratio of tellurite in the second mixed solution to rare earth elements in the rare earth compound aqueous solution is (1~10):(1~10); the duration of the ultrasonic environment is 10 min~120 min; and the volume of the second mixed solution is 5 mL~200 mL.

[0049] According to the liquid-phase preparation method of rare earth doped tellurite material provided by the present invention, in step S500, the temperature of the hydrothermal treatment is 40℃~300℃ and the treatment time is 0h~100h.

[0050] According to the liquid-phase preparation method of rare earth-doped tellurite material provided by the present invention, in step S700, the rare earth-doped tellurite solid product needs to be washed multiple times, preferably three times, to ensure the removal effect of impurities and improve the purity of the rare earth-doped tellurite solid product; furthermore, the drying temperature is 40℃~100℃, and the drying time is 4h~24h.

[0051] According to the liquid-phase preparation method of rare earth doped tellurite material provided by the present invention, in step S900, the calcination temperature is 240℃~1200℃ and the calcination time is 0h~24h.

[0052] This invention utilizes a pure aqueous phase hydrothermal method to prepare rare earth-doped tellurite materials. Compared with traditional high-temperature solid-phase preparation methods, the preparation process is environmentally friendly, simple, energy-efficient, and has good versatility. This invention utilizes a pure aqueous phase hydrothermal method to prepare rare earth-doped tellurite materials, and the morphology and crystal phase of the product can be controlled by adjusting the temperature and pH of the solution. This invention utilizes a pure aqueous phase hydrothermal method to prepare rare earth-doped tellurite materials. The reaction temperature is adjustable, and the morphology and crystallinity of the product can be controlled by adjusting the hydrothermal reaction temperature and reaction time of the solution. The rare earth-doped tellurite materials prepared by the hydrothermal method in pure aqueous phase have good mechanical and chemical stability, which can solve the problem of expanding the application of rare earth-doped fluoride materials under certain special conditions such as high temperature, humidity and corrosive environment; at the same time, the special electronic structure and unique physicochemical properties of rare earth ions endow the materials with many excellent properties, such as good electrical conductivity, excellent optical properties and magnetism.

[0053] This invention relates to rare earth-doped tellurite materials prepared by a pure aqueous phase hydrothermal method, with the chemical formula (RE). w Te x O y Cl z By changing the types of trivalent rare earth dopants, bright emission of red, green and blue light under 980nm infrared light excitation can be achieved, which has good development prospects in the field of luminescent materials.

[0054] Example 1: Flower-like morphology of Y2Te4O 11 Preparation S100, the raw materials selected are sodium tellurite and rare earth yttrium chloride hexahydrate, according to Y2Te4O 11 The stoichiometric ratio of Y and Te elements in the selected raw materials is determined by weighing yttrium chloride hexahydrate and sodium tellurite in a ratio of 0.5:1. S200, Sodium tellurite and yttrium chloride are separately dispersed in deionized water; S300, according to H + With a Te ratio of 1:2, HCl solution was added to sodium tellurite aqueous solution and ultrasonically mixed for 10 min to obtain the first mixed solution; S400. Under ultrasonic conditions, yttrium chloride aqueous solution is added to the first mixed solution and ultrasonically mixed for 30 min to obtain the second mixed solution with a volume of 10 mL. S500. The second mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 120℃ and the reaction time is 6h. S600 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S700. The solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S800, the dried solid product is ground to obtain rare earth-doped tellurite Y2Te4O 11 Solid powder.

[0055] X-ray diffraction was used to analyze the rare earth-doped tellurite material Y2Te4O. 11 Analysis was performed, and its X-ray diffraction pattern was obtained as follows:Figure 1 As shown, the results indicate that the material is a single, pure phase, free of impurities, and exhibits slightly weak crystallinity. Scanning electron microscopy was used to examine the obtained rare-earth-doped tellurite material Y2Te4O. 11 Perform analysis, such as Figure 9 As shown, the sample particles have a diameter of approximately 5µm and a uniform micron-sized flower-like morphology.

[0056] Example 2: Flower-like morphology of Y2Te4O 11 Preparation S100, the raw materials selected are sodium tellurite and rare earth yttrium nitrate hexahydrate, according to Y2Te4O 11 The stoichiometric ratio of Y and Te elements in the selected raw materials is determined by weighing yttrium nitrate hexahydrate and sodium tellurite in a ratio of 0.5:1. S200, Sodium tellurite and yttrium nitrate are separately dispersed in deionized water; S300, according to H + With a Te ratio of 1:2, HNO3 solution was added to sodium tellurite aqueous solution and ultrasonically mixed for 10 min to obtain the first mixed solution; S400. Under ultrasonic conditions, yttrium nitrate aqueous solution is added to the first mixed solution and ultrasonically mixed for 30 min to obtain the second mixed solution with a volume of 10 mL. S500. The second mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 120℃ and the reaction time is 6h. S600 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S700. The solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S800, the dried solid product is ground to obtain rare earth-doped tellurite Y2Te4O 11 Solid powder.

[0057] X-ray diffraction was used to analyze the rare earth-doped tellurite material Y2Te4O. 11 Analysis was performed, and its X-ray diffraction pattern was obtained as follows: Figure 2 As shown, the results indicate that the material is a single, pure phase, free of impurities, and exhibits slightly weak crystallinity. Scanning electron microscopy was used to examine the obtained Y₂Te₄O₂. 11 Perform analysis, such as Figure 10 As shown, the sample particles have a diameter of approximately 5µm and a uniform micron-sized flower-like morphology.

[0058] Example 3: Rod-shaped Y2Te4O 11 Preparation S100, the raw materials selected are sodium tellurite and yttrium chloride hexahydrate, according to Y2Te4O 11 The stoichiometric ratio of Y and Te elements in the selected raw materials is determined by weighing yttrium chloride hexahydrate and sodium tellurite in a ratio of 0.5:1. S200, Sodium tellurite and yttrium chloride are separately dispersed in deionized water; S300, according to H + With a Te ratio of 1:2, HCl solution was added to sodium tellurite aqueous solution and ultrasonically mixed for 10 min to obtain the first mixed solution; S400. Under ultrasonic conditions, yttrium chloride aqueous solution is added to the first mixed solution and ultrasonically mixed for 30 min to obtain the second mixed solution with a volume of 10 mL. S500. The second mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 240℃ and the reaction time is 6h. S600 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S700. The solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S800, the dried solid product is ground to obtain rare earth-doped tellurite Y2Te4O 11 Solid powder.

[0059] X-ray diffraction was used to analyze the rare earth-doped tellurite material Y2Te4O. 11 Analysis was performed, and its X-ray diffraction pattern was obtained as follows: Figure 3 As shown, the results indicate that the material is a single, pure phase, free of impurities, and exhibits high crystallinity. The obtained Y₂Te₄O₂ was analyzed using scanning electron microscopy. 11 Perform analysis, such as Figure 11 As shown, the sample particles have a diameter of approximately 1 µm and a short rod-like morphology.

[0060] Example 4: Er2Te4O 11 Preparation S100, the raw materials selected are sodium tellurite and erbium chloride hexahydrate, according to Er2Te4O 11 The stoichiometric ratio of Er and Te elements in the selected raw materials is determined by weighing Erbium chloride hexahydrate and sodium tellurite in a ratio of 0.5:1. S200, Sodium tellurite and erbium chloride are separately dispersed in deionized water; S300. Under ultrasonic conditions, erbium chloride aqueous solution is added to sodium tellurite aqueous solution and ultrasonically mixed for 30 minutes to obtain the first mixed solution. S400, according to H + With a Te ratio of 1:2, HCl solution was added to the first mixed solution, and the mixture was ultrasonically mixed for 30 minutes to obtain the second mixed solution, with a solution volume of 50 mL. S500. The second mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 240℃ and the reaction time is 6h. S600 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S700. The solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S800, the dried solid product is ground to obtain rare earth-doped tellurite Er2Te4O 11 Solid powder.

[0061] The rare earth-doped tellurite material Er2Te4O obtained by X-ray diffraction 11 Analysis was performed, and its X-ray diffraction pattern was obtained as follows: Figure 4 As shown, the results indicate that the material is a single, pure phase, free of impurities, and exhibits high crystallinity. Scanning electron microscopy was used to examine the obtained Er2Te4O... 11 Perform analysis, such as Figure 12 As shown, the sample particles have a diameter of approximately 1 µm and an irregular short rod-like morphology.

[0062] Example 5: Tb2Te4O 11 Preparation S100, the raw materials selected are sodium tellurite and terbium chloride hexahydrate, according to Tb2Te4O 11 The stoichiometric ratio of Tb and Te elements in the selected raw materials is determined by weighing terbium chloride hexahydrate and sodium tellurite in a ratio of 0.5:1. S200, Sodium tellurite and terbium chloride are separately dispersed in deionized water; S300. Under ultrasonic conditions, terbium chloride aqueous solution is added to sodium tellurite aqueous solution and ultrasonically mixed for 30 minutes to obtain the first mixed solution. S400, according to H + With a Te ratio of 1:2, HCl solution was added to the first mixed solution, and the mixture was ultrasonically mixed for 30 minutes to obtain the second mixed solution, with a solution volume of 50 mL. S500. The second mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 240℃ and the reaction time is 6h. S600 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S700. The solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S800, the dried solid product is ground to obtain rare earth-doped tellurite Tb2Te4O 11 Solid powder.

[0063] X-ray diffraction was used to analyze the rare earth-doped tellurite material Tb2Te4O. 11 Analysis was performed, and its X-ray diffraction pattern was obtained as follows: Figure 5 As shown, the results indicate that the material is a single, pure phase, free of impurities, and exhibits high crystallinity. Scanning electron microscopy was used to examine the obtained Tb₂Te₄O₂. 11 Perform analysis, such as Figure 13 As shown, the sample particles have a diameter of approximately 1 µm and an irregular short rod-like morphology.

[0064] Example 6: Tm2Te6O 15 Preparation S100, the raw materials selected are sodium tellurite and thulium hexahydrate, according to Tm2Te6O 15 The stoichiometric ratio of Tm and Te elements in the selected raw materials is determined by weighing thulium chloride hexahydrate and sodium tellurite in a ratio of 1:3. S200, Sodium tellurite and thulium chloride are separately dispersed in deionized water; S300. Under ultrasonic conditions, add thulium chloride aqueous solution to sodium tellurite aqueous solution and mix ultrasonically for 30 min to obtain a mixed solution with a volume of 10 mL. S400. The mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 280℃ and the reaction time is 6h. S500 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S600, the solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S700. The dried solid product is ground to obtain rare earth-doped tellurite Tm2Te6O. 15 Solid powder.

[0065] X-ray diffraction was used to analyze the rare earth-doped tellurite material Tm2Te6O. 15 Analysis was performed, and its X-ray diffraction pattern was obtained as follows: Figure 6 As shown, the results indicate that the material is a single, pure phase, free of impurities, and exhibits high crystallinity. The obtained Tm2Te6O was analyzed using scanning electron microscopy. 15Perform analysis, such as Figure 14 As shown, the sample particles have a diameter of approximately 1 µm and a spherical shape.

[0066] Example 7: Preparation of LuTeO3Cl S100: The raw materials are sodium tellurite and lutetium chloride hexahydrate, which are weighed in a ratio of 1:4. S200, Sodium tellurite and lutetium chloride are separately dispersed in deionized water; S300. Under ultrasonic conditions, add the rare earth lutetium chloride aqueous solution to the sodium tellurite aqueous solution and mix ultrasonically for 30 min to obtain a mixed solution with a volume of 10 mL. S400. The mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 280℃ and the reaction time is 6h. S500 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S600, the solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S700: Grind the dried solid product to obtain rare earth-doped tellurite LuTeO3Cl solid powder.

[0067] The rare-earth-doped tellurite material LuTeO3Cl was analyzed by X-ray diffraction, and its X-ray diffraction pattern is shown below. Figure 7 As shown, the results indicate that the material is a single pure phase without impurities.

[0068] Example 8: Y 1.78 Yb 0.2 Er 0.02 Te4O 11 Preparation S100, the raw materials selected are sodium tellurite and three rare earth compounds (rare earth yttrium nitrate hexahydrate, rare earth ytterbium chloride hexahydrate, and rare earth erbium acetate tetrahydrate), according to Y 1.78 Yb 0.2 Er 0.02 Te4O 11 The stoichiometric ratio of RE and Te elements in the selected raw materials is determined by weighing Yttrium nitrate hexahydrate, ytterbium chloride hexahydrate, erbium acetate tetrahydrate, and sodium tellurite in a ratio of 0.89:0.1:0.01:1. S200, Sodium tellurite and rare earth compounds are dispersed separately in deionized water; S300, according to H +With a Te ratio of 1:2, HCl solution was added to sodium tellurite aqueous solution and ultrasonically mixed for 10 min to obtain the first mixed solution; S400. Under ultrasonic conditions, the aqueous solution of rare earth compound is added to the first mixed solution and ultrasonically mixed for 30 minutes to obtain the second mixed solution with a volume of 10 mL. S500. The second mixed solution is transferred to a reaction vessel for hydrothermal treatment, wherein the reaction temperature is 240℃ and the reaction time is 6h. S600 After the reaction is complete, cool to room temperature to obtain a suspension. Take out the suspension and perform solid-liquid two-phase separation treatment to collect the solid precipitate. S700. The solid product was centrifuged and ultrasonically washed three times with ultrapure water to obtain rare earth-doped tellurite, which was then placed in a vacuum oven and vacuum dried at 60°C for 8 hours. S800, The dried solid product is ground to obtain rare earth-doped tellurite Y. 1.78 Yb 0.2 Er 0.02 Te4O 11 Solid powder.

[0069] X-ray diffraction was used to analyze the rare earth-doped tellurite material Y. 1.78 Yb 0.2 Er 0.02 Te4O 11 Analysis was performed, and its X-ray diffraction pattern was obtained as follows: Figure 8 As shown, the result Y 1.78 Yb 0.2 Er 0.02 Te4O 11 It is a single, pure phase, free of impurities, and exhibits high crystallinity. The obtained rare-earth-doped tellurite material Y was analyzed using scanning electron microscopy. 1.78 Yb 0.2 Er 0.02 Te4O 11 Perform analysis, such as Figure 15 As shown, the sample particles have a diameter of approximately 1 µm and an irregular short rod-like morphology. The photoluminescence spectrum under 980 nm infrared excitation was measured, as shown below. Figure 16 As shown, the sample can emit bright green light.

[0070] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A rare earth doped tellurite material, characterized in that, The obtained rare earth doped tellurite material has a chemical formula as follows: wherein R.E. is a rare earth element, including one or more of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu. (R.E.) w Te x O y Cl z 2. The rare earth doped tellurite material obtained according to claim 1, wherein the rare earth doped tellurite material has a chemical formula as follows: 0 < w ≤ 6; 1 ≤ x ≤ 6; 1 ≤ y ≤ 20; 0 ≤ z ≤ 1 in the chemical formula (R.E.) w Te x O y Cl z in: w, x, y, and z are all molar coefficients. wherein To prepare the rare earth doped tellurite material according to any one of claims 1 to 2, the method specifically comprises the following steps:

3. A method for the liquid phase preparation of a rare earth doped tellurite material, characterized in that, S100, weighing the tellurite and the rare earth compound; S200, adding or dispersing the tellurite and the rare earth compound into a deionized water solution respectively; S300, adding an acid solution into the tellurite water solution to obtain a first mixed solution; S400, mixing the rare earth compound water solution with the first mixed solution under an ultrasonic environment to obtain a second mixed solution; S500, transferring the second mixed solution into a reaction kettle, and using a hydrothermal treatment method to obtain a suspension; S600, performing a solid-liquid two-phase separation treatment on the suspension, collecting a solid phase precipitate, and obtaining a rare earth doped tellurite solid phase product; S700, centrifugally and ultrasonically washing the rare earth doped tellurite solid phase product with ultrapure water, and then drying the rare earth doped tellurite solid phase product; The rare earth compound can be a rare earth halide, a rare earth oxide, a rare earth hydroxide, a rare earth nitrate, a rare earth acetate, a rare earth phosphate, a rare earth carbonate, a rare earth chlorate, a rare earth sulfate, or a rare earth organic complex. The tellurite can be tellurous acid, sodium tellurite, or potassium tellurite. S800: Grind the dried solid product to obtain rare earth-doped tellurite solid powder (RE). w Te x O y Cl z ; S900、According to the need, the rare earth doped tellurite solid powder is subjected to calcination treatment, and the rare earth doped tellurite solid powder after the calcination treatment is ground to obtain a high-crystallinity rare earth doped tellurite material (R.E.) w Te x O y Cl z .

4. The process for the liquid phase preparation of a rare earth doped tellurite material according to claim 3, characterized in that, The acid solution can be hydrochloric acid, nitric acid, sulfuric acid, or acetic acid.

5. The method of claim 3, wherein the liquid phase preparation of a rare earth doped tellurite material is characterized by, Alternatively, one or more rare earth compounds are added or dispersed in water to prepare a water system of the rare earth compound; the tellurite is added or dispersed in water to prepare a water system of the tellurite; the water system of the rare earth compound and the water system of the tellurite are mixed to obtain a mixed solution; a set amount of acid is added to the mixed solution to adjust the pH of the mixed solution; and the mixed solution is ultrasonically mixed for a set time to obtain a water system of the precursor; 6. The process for the liquid phase preparation of a rare earth doped tellurite material according to claim 3, characterized in that, Alternatively, one or more rare earth compounds are added or dispersed in water to prepare a water system of the rare earth compound; the tellurite is directly added into the water system of the rare earth compound to obtain a mixed solution; a set amount of acid is added to adjust the pH of the mixed solution; and the mixed solution is ultrasonically mixed for a set time to obtain a water system of the precursor; 7. The method of claim 3, wherein the liquid phase preparation of a rare earth doped tellurite material is characterized by, In the steps S200, S300, S400, one or more rare earth compounds are added or dispersed in water to obtain a water system of the rare earth compound; the tellurite is added or dispersed in water, and a certain amount of acid is added to obtain a water system of the tellurite; then, the water system of the rare earth compound and the water system of the tellurite combined with H + The mixed solution is obtained by mixing the water system of the tellurite combined with H Alternatively, one or more rare earth compounds are added or dispersed in water to prepare a water system of the rare earth compound; the tellurite is directly added into the water system of the rare earth compound to obtain a mixed solution; a set amount of acid is added to adjust the pH of the mixed solution; and the mixed solution is ultrasonically mixed for a set time to obtain a water system of the precursor; Alternatively, one or more rare earth compounds are added or dispersed in water to prepare a water system of the rare earth compound; the tellurite is directly added into the water system of the rare earth compound to obtain a mixed solution; a set amount of acid is added to adjust the pH of the mixed solution; and the mixed solution is ultrasonically mixed for a set time to obtain a water system of the precursor; ​ ​ Or, the tellurite is added or dispersed in water, one or several rare earth compounds are directly added into the tellurite water system, and the mixture is obtained; a certain amount of acid is added to adjust the pH of the mixture; and the mixture is ultrasonically mixed for a certain time to obtain a precursor water system.

8. The process according to claim 3, wherein the liquid phase preparation of rare earth doped tellurite materials is characterized by, In the S400 step, the molar ratio of tellurite in the second mixed solution to rare earth elements in the rare earth compound aqueous solution is (1-10):(1-10); the maintenance time of the ultrasonic environment is 10 min-120 min; and the volume of the second mixed solution is 5 mL-200 mL.

9. The method of claim 3, wherein the liquid phase preparation of a rare earth doped tellurite material is characterized by, In the S500 step, the reaction temperature of the hydrothermal treatment method is 40℃-300℃, and the hydrothermal treatment reaction time is 0h-100h.

10. The process of claim 3, wherein the process is characterized by, In the S700 step, the rare earth-doped tellurite solid-phase product needs to be washed multiple times, preferably 3 times, to ensure the removal of impurities and improve the purity of the rare earth-doped tellurite solid-phase product; further, the drying temperature is 40℃-100℃, and the drying time is 4h-24h.

11. The method of claim 3, wherein the liquid phase preparation of a rare earth doped tellurite material is characterized by, In the S900 step, the calcination temperature is 240℃-1200℃, and the calcination time is 0h-24h.

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