Efficient single-phase full-spectrum luminescent material

Abstract

The invention discloses an efficient single-phase full-spectrum luminescent metal halide luminescent material and a preparation method thereof. The chemical composition of the luminescent material is Cs2ZrCl6: Bi < 3 + > and Te < 4 + >. The method comprises the following steps: (1) weighing a proper amount of CsCl, ZrO2, BiCl3 and TeCl4 by using an electronic balance according to the stoichiometric ratio of materials, and putting the CsCl, ZrO2, BiCl3 and TeCl4 into a lining of a polytetrafluoroethylene reaction kettle; 2) adding a certain amount of concentrated HCl into the lining of the reaction kettle, and stirring for a certain time to dissolve all the raw materials; 3) taking out the stirrer, sealing the reaction kettle, placing the reaction kettle in an air dry oven, and reacting for a certain time at a certain temperature; and 4) washing the reaction product, and carrying out vacuum drying to obtain the Cs2ZrCl6: Bi < 3 + >, Te < 4 + > material. The material emits bright white light under the excitation of ultraviolet light. The synthesis method disclosed by the invention has the characteristics of low raw material cost, simple experimental operation, batch synthesis and the like; meanwhile, the obtained product is good in crystallinity, high in stability, environment-friendly and excellent in luminescent property; the method can be used in the technical fields of illumination display, anti-counterfeiting, photoelectric detection and the like.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of inorganic semiconductor luminescent materials, and relates to a Cs2ZrCl6:Bi 3+ , Te 4+ luminescent material and a preparation method, which provides a new thought and direction for the design and development of luminescent materials. BACKGROUND

[0002] Single-phase full-spectrum luminescent materials refer to luminescent materials that realize full-spectrum coverage in a single matrix, which can emit a continuous spectrum from blue light to red light, thereby generating white light. Such materials have important application prospects in the fields of optical materials and devices such as white light LED lighting and backlight display. At present, single-matrix full-spectrum luminescent materials are usually realized by rare earth ion doping, and the luminescent properties are regulated by co-doping of different ions or occupation of different crystallographic sites by ions. Although the luminescent efficiency of rare earth luminescent materials is generally high, in some applications such as white light LED lighting, the luminescent efficiency of single-phase fluorescent powder still has room for improvement. In addition, the mining and refining cost of rare earth elements is relatively high, especially some scarce rare earth elements such as europium (Eu) and neodymium (Nd), which leads to a relatively high price of rare earth luminescent materials. Therefore, it is necessary to develop new types of high-efficiency and low-cost full-spectrum luminescent materials.

[0003] Zero-dimensional metal halide white light luminescent materials have multiple advantages, which make them exhibit potential application prospects in the fields of solid-state lighting, display technology, etc. Most zero-dimensional metal halides have high photoluminescence quantum yield, wide spectrum emission, adjustable luminescent color, etc., so they are easy to realize single-phase high-efficiency full-spectrum emission. In addition, such materials also have good thermal stability, chemical stability, environmental friendliness, etc., which make them have important application potential in new lighting technology. SUMMARY

[0004] The purpose of the present application is to provide a Bi 3+ and Te 4+ co-doped Cs2ZrCl6 single-phase full-spectrum emission material and a preparation method thereof, which is high in efficiency and environmentally friendly.

[0005] The purpose of the present application is achieved by the following technical solutions:

[0006] A high-efficiency single-phase full-spectrum luminescent material refers to a Bi 3+ , Te 4+ doped Cs2ZrCl6 material, Bi 3+ , T e 4+ are doped into the Cs2ZrCl6 crystal lattice and replace the crystal sites of Zr, wherein Bi 3+ , Te 4+The doping amount of Cs2ZrCl6 is 0.05% to 11% of the Zr lattice site number (stoichiometric ratio) in the crystal structure of Cs2ZrCl6, preferably the doping amounts are 5% and 2% respectively.

[0007] The preparation method of the single-phase full-spectrum luminescent material comprises the following steps: 1) according to the stoichiometric ratio of the material, a proper amount of CsCl, ZrO2, BiCl3 and TeCl4 are weighed by using an electronic balance and put into a polytetrafluoroethylene reaction kettle liner; 2) a certain amount of concentrated HCl is added into the reaction kettle liner, and stirring is performed for a certain time to dissolve all the raw materials; 3) the stirrer is taken out, the reaction kettle is sealed, and placed in a blast drying oven to react for a certain time at a certain temperature; 4) after the reaction product is washed and vacuum dried, Cs2ZrCl6:Bi 3+ , Te 4+ material is obtained.

[0008] Preferably, the luminescent material presents bright white light emission under ultraviolet light excitation, and the highest fluorescence quantum efficiency is up to 84.2%.

[0009] Preferably, in step 1), in order to ensure the purity and luminescent efficiency of the material, the input stoichiometric ratio of the metal chloride raw material is CsCl:(ZrO2+BiCl3+TeCl4)=2:1, wherein BiCl3:(ZrO2+BiCl3+TeCl4)=(0.01-0.11):1, preferably 0.05, and TeCl4:(ZrO2+BiCl3+TeCl4)=(0.005-0.07):1, preferably 0.02.

[0010] Preferably, in step 1), the amount of concentrated hydrochloric acid is 20% of the capacity of the reaction kettle.

[0011] Preferably, in step 2), the certain temperature is 160-200°C, preferably 180°C.

[0012] Preferably, in step 3), the certain time is 2-24h, preferably 12h.

[0013] Preferably, in step 4), the reaction product is washed, and the solvent of the washed product is a pure low-polarity organic solvent.

[0014] Compared with the prior art, the present application has the following beneficial effects:

[0015] (1) The solvothermal preparation method adopted in the present application is simple to operate, can be synthesized in one step in batches, has low requirements on experimental conditions, and requires low-cost experimental equipment and raw materials.

[0016] (2) The preparation method adopted in the present application can successfully dope Bi 3+ , Te 4+By incorporating it into the Cs₂ZrCl₆ lattice and substituting Zr at lattice sites, Cs₂ZrCl₆∶Bi is formed. 3+ Te 4+ The luminescent material has a highest fluorescence quantum efficiency of 84.2%.

[0017] (3) The single-phase full-spectrum emission material described in this invention is obtained by reaction under high temperature and high pressure conditions, which not only makes the material highly crystallizable, but also helps to improve the stability of the material. Attached Figure Description

[0018] Figure 1 The Cs2ZrCl6∶Bi synthesized under the conditions shown in Example 8 of this invention 3+ Te 4+ X-ray diffraction (XRD) pattern of the sample.

[0019] Figure 2 Preparation of Cs2ZrCl6∶Bi in Example 8 of the present invention 3+ Te 4+ Fluorescence emission spectrum of the sample under 365nm ultraviolet light excitation. Detailed Implementation

[0020] Comparative Example 1:

[0021] Weigh 2 mmol of CsCl and 1 mmol of ZrO2 and pour them into a 25 ml polytetrafluoroethylene (PTFE) liner. Add 5 ml of concentrated hydrochloric acid and stir for at least 30 min to completely dissolve the reactants. Remove the stir bar. Seal the reactor containing the reactants and place it in a 180°C drying oven for 12 h. After the reaction, allow the reactor to cool to room temperature naturally. Open the reactor, discard the supernatant, add 4 ml of n-butanol solution, and centrifuge at 5000 rpm for 5 min. Repeat the washing twice. Then, replace the n-butanol with n-hexane and wash once using the same method. Place the washed sample in a 60°C vacuum oven to dry for 12 h. After the temperature drops to room temperature, collect the sample in a reagent bottle for subsequent testing. XRD analysis confirmed that the product is Cs₂ZrCl₆. Excitation and emission spectroscopy and fluorescence quantum efficiency tests showed that the reaction product obtained in this comparative example emits weak blue light under ultraviolet light, with a fluorescence quantum efficiency of 8.1%.

[0022] Comparative Example 2:

[0023] Weigh 2 mmol of CsCl, 0.95 mmol of ZrO2, and 0.05 mmol of BiCl3, and pour them into a 25 ml polytetrafluoroethylene (PTFE) liner. Add 5 ml of concentrated hydrochloric acid and stir for at least 30 min to completely dissolve the reactants. Remove the stir bar. Seal the reactor containing the reactants and place it in a 180°C drying oven for 12 h. After the reaction, allow the reactor to cool to room temperature naturally. Open the reactor, discard the supernatant, add 4 ml of n-butanol solution, and centrifuge at 5000 rpm for 5 min. Repeat the washing twice. Then, replace the n-butanol with n-hexane and wash once using the same method. Place the washed sample in a 60°C vacuum oven to dry for 12 h. After cooling to room temperature, collect the sample in a reagent bottle for subsequent testing. XRD analysis confirmed that the product is Cs2ZrCl6. Excitation and emission spectra and fluorescence quantum efficiency tests revealed that the reaction product obtained in this comparative example emits bright blue light under ultraviolet light, with a fluorescence quantum efficiency of 90%.

[0024] Comparative Example 3:

[0025] Weigh 2 mmol of CsCl, 0.98 mmol of ZrO2, and 0.02 mmol of TeCl4, and pour them into a 25 ml polytetrafluoroethylene (PTFE) liner. Add 5 ml of concentrated hydrochloric acid and stir for at least 30 min to completely dissolve the reactants. Remove the stir bar. Seal the reactor containing the reactants and place it in a 180°C drying oven for 12 h. After the reaction, allow the reactor to cool to room temperature naturally. Open the reactor, discard the supernatant, add 4 ml of n-butanol solution, and centrifuge at 5000 rpm for 5 min. Repeat the washing twice. Then, replace the n-butanol with n-hexane and wash once using the same method. Place the washed sample in a 60°C vacuum oven to dry for 12 h. After cooling to room temperature, collect the sample in a reagent bottle for subsequent testing. XRD analysis confirmed that the product is Cs2ZrCl6. Excitation and emission spectra and fluorescence quantum efficiency tests revealed that the reaction product obtained in this comparative example emits bright yellow light under ultraviolet light, with a fluorescence quantum efficiency of 77.4%.

[0026] Example 1:

[0027] Take 2 mmol of CsCl, 0.99 mmol of Zr02, and 0.01 mmol of TeCl4, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is naturally cooled to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits yellow light under ultraviolet light excitation, and the fluorescence quantum efficiency is 53.5%.

[0028] Example 2:

[0029] Take 2 mmol of CsCl, 0.99 mmol of Zr02, and 0.01 mmol of TeCl4, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is naturally cooled to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits yellow light under ultraviolet light excitation, and the fluorescence quantum efficiency is 53.5%.

[0030] Example 3:

[0031] Take 2 mmol of CsCl, 0.98 mmol of Zr02, 0.02 mmol of TeCl4, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is naturally cooled to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. The product is proved to be Cs2ZrCl6 by XRD test. The sample emits yellow light under ultraviolet light excitation, and the fluorescence quantum efficiency is 77%.

[0032] Example 4:

[0033] Take 2 mmol of CsCl, 0.98 mmol of Zr02, 0.02 mmol of TeCl4, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is naturally cooled to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. The product is proved to be Cs2ZrCl6 by XRD test. The sample emits yellow light under ultraviolet light excitation, and the fluorescence quantum efficiency is 77%.

[0034] Example 5:

[0035] Take 2 mmol of CsCl, 0.93 mmol of Zr02, 0.07 mmol of TeCl4, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is naturally cooled to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. The product is proved to be Cs2ZrCl6 by XRD test. The sample emits yellow light under ultraviolet light excitation, and the fluorescence quantum efficiency is 53.7%.

[0036] Example 6:

[0037] Take 2 mmol of CsCl, 0.93 mmol of Zr02, 0.07 mmol of TeCl4, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is naturally cooled to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. The product is proved to be Cs2ZrCl6 by XRD test. The sample emits yellow light under ultraviolet light excitation, and the fluorescence quantum efficiency is 53.7%.

[0038] Example 7:

[0039] Take 2 mmol of CsCl, 0.95 mmol of Zr02, 0.02 mmol of TeCl4, 0.03 mmol of BiCl3, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is allowed to naturally cool to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits yellowish white light under ultraviolet light excitation, and the fluorescence quantum efficiency is 81.5%.

[0040] Example 8:

[0041] Take 2 mmol of CsCl, 0.95 mmol of Zr02, 0.02 mmol of TeCl4, 0.03 mmol of BiCl3, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction raw materials, and place it in a 180°C air drying oven for 12 h. After the reaction is completed, the reaction kettle is allowed to naturally cool to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash once in the same way. The washed sample is placed in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, the sample is collected in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits yellowish white light under ultraviolet light excitation, and the fluorescence quantum efficiency is 81.5%.

[0042] Example 8: Figure 1 The XRD pattern of the 2% Te 4+ and 5% Bi 3+ co-doped C s2 ZrCl6 metal halide luminescent material is shown in Figure 1 , all the diffraction peaks match with Cs2ZrCl6 with PDF number 74-0505, proving that the synthesized material is pure Cs2ZrCl6 phase. The excitation and emission spectra are shown in Figure 2 .

[0043] Example 9:

[0044] Take 2 mmol of CsCl, 0.93 mmol of ZrO2, 0.02 mmol of TeCl4, and 0.05 mmol of BiCl3, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction materials, and place it in a 180°C air drying oven for 6 h. After the reaction is completed, allow the reaction kettle to naturally cool to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge for 5 min at 5000 rpm, repeat the washing for 2 times, and then replace the n-butanol with n-hexane and wash once in the same way. Place the washed sample in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, collect the sample in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits white light under ultraviolet light excitation, and the fluorescence quantum efficiency is 61.3%.

[0045] Example 10:

[0046] Take 2 mmol of CsCl, 0.93 mmol of ZrO2, 0.02 mmol of TeCl4, and 0.05 mmol of BiCl3, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction materials, and place it in a 180°C air drying oven for 6 h. After the reaction is completed, allow the reaction kettle to naturally cool to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge for 5 min at 5000 rpm, repeat the washing for 2 times, and then replace the n-butanol with n-hexane and wash once in the same way. Place the washed sample in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, collect the sample in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits white light under ultraviolet light excitation, and the fluorescence quantum efficiency is 61.3%.

[0047] Example 11:

[0048] Take 2 mmol of CsCl, 0.93 mmol of ZrO2, 0.02 mmol of TeCl4, and 0.05 mmol of BiCl3, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction materials, and place it in a 160°C air drying oven for 12 h. After the reaction is completed, allow the reaction kettle to naturally cool to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge for 5 min at 5000 rpm, repeat the washing for 2 times, and then replace the n-butanol with n-hexane and wash once in the same way. Place the washed sample in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, collect the sample in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits white light under ultraviolet light excitation, and the fluorescence quantum efficiency is 58.2%.

[0049] Example 12:

[0050] Take 2 mmol of CsCl, 0.93 mmol of ZrO2, 0.02 mmol of TeCl4, and 0.05 mmol of BiCl3, pour them into a 25 ml polytetrafluoroethylene reaction kettle liner, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction materials uniformly, and take out the stirrer. Seal the reaction kettle containing the above reaction materials, and place it in a 160°C air drying oven for 12 h. After the reaction is completed, allow the reaction kettle to naturally cool to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge for 5 min at 5000 rpm, repeat the washing for 2 times, and then replace the n-butanol with n-hexane and wash once in the same way. Place the washed sample in a vacuum oven at 60°C for 12 h, and after the temperature drops to room temperature, collect the sample in a reagent bottle for subsequent testing. XRD test proves that the product is Cs2ZrCl6. The sample emits white light under ultraviolet light excitation, and the fluorescence quantum efficiency is 58.2%.

[0051] Example 13:

[0052] Take 2 mmol of CsCl, 0.93 mmol of ZrO2, 0.02 mmol of TeCl4, 0.05 mmol of BiCl3, pour it into a 25 ml polytetrafluoroethylene reaction kettle lining, add 5 ml of concentrated hydrochloric acid, stir for at least 30 min, mix the reaction raw materials uniformly, and take out the stirrer. The reaction kettle containing the above reaction raw materials is sealed and placed in a 200 DEG C air drying oven for 12 h. After the reaction is completed, the reaction kettle is naturally cooled to room temperature. Open the reaction kettle, pour off the supernatant, add 4 ml of n-butanol solution and centrifuge at 5000 rpm for 5 min, repeat the washing for 2 times, then replace the n-butanol with n-hexane and wash it once in the same way. The washed sample is placed in a vacuum oven at 60 DEG C for 12 h, and after the temperature decreases to room temperature, the sample is collected in a reagent bottle for subsequent testing. It is proved by XRD test that the product is Cs2ZrCl6. The sample emits yellowish white light under ultraviolet light excitation, and the fluorescence quantum efficiency is 75.6%.

[0053] The embodiments of the present application do not exhaust the technical scope of the claimed technical range, and the new technical solutions formed by the same or multiple technical features in the technical solutions of the embodiments are also within the scope of the claimed technical range; at the same time, in all the embodiments of the present application, the parameters in the same embodiment only represent one example (i.e. a feasible scheme) of the technical solution, and there is no strict cooperation and limitation relationship between the parameters, and the parameters can be replaced with each other without violating the axioms and the claims of the present application, except for the special declaration.

[0054] The technical means disclosed in the present application is not limited to the technical means disclosed in the above technical means, but also includes the technical solutions composed of any combination of the above technical features. The above is the specific embodiment of the present application, and it should be pointed out that for ordinary skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, and these improvements and refinements are also considered as the protection scope of the present application.

[0055] The specific embodiments described herein are merely illustrative of the spirit of the present application. Those skilled in the art of the present application can make various modifications or supplements to the described specific embodiments or use similar ways to replace them, but without departing from the spirit of the present application or exceeding the scope defined by the appended claims.

Claims

1. A highly efficient single phase full spectrum emitting metal halide luminescent material and a method for its preparation, having a chemical composition of: Cs2ZrCl6:Bi 3+ 4+ Te. The method of the present invention comprises the following steps: 1) According to the stoichiometric ratio of the material, the appropriate amount of CsCl, ZrO2, BiCl3, TeCl4 is weighed by using an electronic balance and put into a polytetrafluoroethylene reaction kettle liner; 2) A certain amount of concentrated HCl is added to the reaction kettle liner, and stirred for a certain time to dissolve all the raw materials; 3) Take out the stirrer, seal the reaction kettle, and place it in a blast drying oven for a certain time at a certain temperature; 4) After washing and vacuum drying the reaction product, Cs2ZrCl6∶Bi 3+ 4+ material is obtained. The material presents bright white light emission under ultraviolet light excitation.​ ​​ 2. The method for preparing a single-phase full-spectrum luminescent material according to claim 1, characterized in that: In step 1), the input stoichiometric ratio of the metal chloride raw material is CsCl:(ZrO2+BiCl3+TeCl4)=2:1, wherein BiCl3:(ZrO2+BiCl3+TeCl4)=(0.01-0.11):1, preferably 0.05, and wherein TeCl4:(ZrO2+BiCl3+TeCl4)=(0.005-0.07):1, preferably 0.

02.

3. The method for preparing a single-phase full-spectrum luminescent material according to claim 1, characterized in that: In step 1), the amount of methanol solvent is 20% of the capacity of the reaction kettle.

4. The method for preparing a single-phase full-spectrum luminescent material according to claim 1, characterized in that: In step 3), the certain temperature is preferably 180℃.

5. The method for preparing a single-phase full-spectrum luminescent material according to claim 1, characterized in that: In step 3), the certain time is preferably 12h.

6. The method for preparing a single-phase full-spectrum luminescent material according to claim 1, characterized in that: In step 4), the solvent for washing the product is a pure low-polarity organic solvent.

7. The single-phase full-spectrum luminescent material of claim 1 exhibits bright white light emission under ultraviolet light excitation.

8. Use of the single-phase full-spectrum luminescent material according to claim 1, characterized in that: It can be used in technical fields such as illumination display, anti-counterfeiting, and photoelectric detection.

Images