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Praseodymium ion-doped potassium strontium borate fluorescent powder and high-temperature solid-phase preparation method

A technology of high-temperature solid phase and fluorescent powder, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., and can solve the problems of electronegativity and the influence of radius luminescence

Active Publication Date: 2017-04-26
CHONGQING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in doping substitution, after impurity ions replace matrix ions, the defect effect caused by the difference in electronegativity and radius of ions will also have a significant impact on luminescence.
[0003] There is no potassium strontium borate phosphor powder doped with praseodymium ions at present, especially the relevant reports on blue light excitation doped potassium strontium borate red phosphor powder with praseodymium ions and its preparation process. Therefore, a kind of potassium borate doped with praseodymium ions is needed. Strontium phosphor and its high-temperature solid phase preparation method

Method used

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  • Praseodymium ion-doped potassium strontium borate fluorescent powder and high-temperature solid-phase preparation method
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  • Praseodymium ion-doped potassium strontium borate fluorescent powder and high-temperature solid-phase preparation method

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Experimental program
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Effect test

Embodiment 1

[0041] Such as figure 1 As shown, the high-temperature solid-phase preparation method of potassium strontium borate phosphor doped with praseodymium ions provided in this embodiment includes the following steps:

[0042] S1: Weighing Pr according to the stoichiometric ratio 2 o 3 , K 2 CO 3 , SrCO 3 , HBO 3 , Li 2 CO 3 and Na 2 CO 3 raw material;

[0043] S2: Grinding raw materials and fully mixing and grinding to obtain abrasives;

[0044] S3: putting the grinding material into a vacuum drying oven for drying to obtain a dry material;

[0045] S4: put the dried material into a high-temperature box-type resistance furnace for pre-calcination to obtain a pre-calcined material, the pre-calcined temperature is 400-600°C, and the pre-calcined time is 3-6 hours;

[0046] S5: After the temperature drops to room temperature, take out the pre-calcined material and grind it to obtain the re-ground material, and the grinding time is 0.8-1.2 hours;

[0047] S6: put the regri...

Embodiment 2

[0061] The specific steps of the high-temperature solid-phase preparation method of potassium strontium borate phosphor doped with praseodymium ions provided in this embodiment are as follows:

[0062] Weigh Pr according to the stoichiometric ratio 2 o 3 , K 2 CO 3 , SrCO 3 , HBO 3 , Li 2 CO 3 , Na 2 CO 3 raw material;

[0063] Grinding raw materials and thoroughly mixing the ground raw materials;

[0064] Dry the ground raw material in a vacuum drying oven;

[0065] Put it into a high-temperature box-type resistance furnace and pre-calcine at 500 ° C for 5 hours.

[0066] When the temperature drops to room temperature, take it out and grind it in an agate mortar for 1.1 hours.

[0067] Then move it into a corundum crucible, put it in a vacuum drying oven and dry it at 100°C for 1.1 hours,

[0068] Then put it into a high-temperature box-type resistance furnace, and perform high-temperature calcination at 850° C. for 16 hours.

[0069] When the temperature drops ...

Embodiment 3

[0080] The phosphor preparation method provided in this embodiment is to prepare potassium strontium borate phosphor doped with praseodymium ions by using a high-temperature solid-phase method. Replace potassium ions and strontium ions with praseodymium ions, replace strontium ions and praseodymium ions by doping charge compensators, the XRD pattern, SEM pattern, and spectrum of the sample, such as Figure 2-10 As shown; among them, SEM HV indicates the working voltage in ultra-high vacuum; SEMMAG indicates the magnification; WD indicates the working distance; Det:SE indicates the detector type; MIRA3 TESCAN indicates the model of thermal field emission scanning electron microscope; performance in nanospace indicates the operation mode .

[0081] (1) The XRD diffraction pattern of the experimental sample is compared with the pattern of the relevant literature, and the diffraction peaks are consistent, which shows that KSr was synthesized 4 (BO 3 ) 3 crystal, and the charge ...

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Abstract

The invention discloses a high-temperature solid-phase preparation method of praseodymium ion-doped potassium strontium borate fluorescent powder. The high-temperature solid-phase preparation method comprises the following steps: firstly, weighing raw materials according to a stoichiometric ratio; secondly, grinding the raw materials, thoroughly mixing and grinding to obtain the ground material, and drying; thirdly, putting the dried material into a high-temperature box-type resistance furnace, pre-calcining, taking out the pre-calcined material when the temperature is reduced to room temperature, grinding to obtain the reground material, and drying; fourthly, putting the redried material into the high-temperature box-type resistance furnace, and calcining at high temperature; finally, taking out the high-temperature calcined material when the temperature is reduced to room temperature, regrinding to obtain the required fluorescent powder. By the preparation method provided by the invention, the successful synthesis of samples can be ensured; in the samples, Pr3+ can substitute Sr2+ and K+, the strongest luminous intensity of a Sr2+-substituted sample is achieved when the doping amount is 1.5mol%, and the strongest luminous intensity of a K+- substituted sample is achieved when the doping amount is 1mol%; an experimental sample doped with a charge compensator (KSr4 (BO3)3: Pr3+, R+; R=Li, Na, K) has higher luminous intensity than a single-doped sample, and a sample doped with Li+ has the best effect. All samples emit red light.

Description

technical field [0001] The invention relates to the field of phosphor preparation, in particular to a method for preparing potassium strontium borate phosphor doped with praseodymium ions by a high-temperature solid-phase method. Background technique [0002] Rare earth-doped luminescent materials have a wide range of applications, which has attracted the attention of many researchers. Among them, the red phosphor plays a very important role in the application of LEDs. It can make up for the cold color of the white light formed after the blue chip and the yellow phosphor are packaged due to the lack of red light components. A large number of existing studies have shown that the chemically stable borate system is a kind of luminescent host material with excellent performance. where KSr 4 (BO 3 ) 3 It has a good orthorhombic lattice structure, and potassium atoms are in a lattice coordinated by eight oxygen atoms. Due to its wide application in luminescent materials and ot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/63
CPCC09K11/7712
Inventor 冯文林马诗章彭志清陈溶
Owner CHONGQING UNIV OF TECH
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