Preparation of red fluorescent powder Zn2SiO4:Eu3+

A red fluorescent powder, eu2o3 technology, applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of inapplicable silicate, urea low reducing ability, low reducing ability, etc., to overcome the reaction activation energy barrier, product The crystal shape becomes better and the effect of increasing the heat release of combustion

Inactive Publication Date: 2008-10-08
SHANGHAI NORMAL UNIVERSITY
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Problems solved by technology

[0006] Traditional combustion agents include urea, citric acid, glycine, etc. Glycine is often used as a complexing agent for metal ions because it has a carboxyl group at one end and an amino group at the other end. The structural characteristics of this zwitterion can prevent selective deposition and make various components The combination is uniform, but this characteristic cannot be applied to SiO 2 above; citric acid is also unsuitable for silicates due to the need to form complexes with metal ions; urea has low reducing power and produces less gas (10.5kJ / g), glycine has moderate reducing power But it can produce more gas (13kJ / g). When urea is used as the combustion agent, due to its low reducing ability at very high temperature and the amount of gas produced is small, the product appears as large particles

Method used

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  • Preparation of red fluorescent powder Zn2SiO4:Eu3+
  • Preparation of red fluorescent powder Zn2SiO4:Eu3+
  • Preparation of red fluorescent powder Zn2SiO4:Eu3+

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preparation example Construction

[0027] like figure 1 The process flow diagram shown, a red phosphor Zn 2 SiO 4 :Eu 3+ The preparation method, its steps are as follows:

[0028] 1) the Eu 2 o 3 and ZnO according to the composition ratio (n Eu 2 o 3 : nZnO=0.06:1) dissolved in nitric acid with a volume of 1:1 concentration and mixed evenly;

[0029] 2) Add a certain amount (the content is 2% to 3% of the total mass of other solid raw materials added) of boric acid, urea and combustion aid NH 4N o 3 , in the case of solution boiling SiO 2 (n SiO 2 : nZnO=1:2) was slowly added, and then ultrasonically dispersed for 5-10 minutes;

[0030] 3) Move the solution directly into a high-temperature furnace pre-heated to 600°C. With the evaporation of water, the solution begins to expand and bubble, releasing a large amount of gas; the gas is ignited and burns violently, and the flame is yellow-white. It can be maintained for about 30s;

[0031] 4) Collect the obtained fluffy and foamy products, grind and mi...

Embodiment 1

[0036] According to the composition ratio n(ZnO):n(Eu 2 o 3 )=1:0.06 Weigh ZnO, Eu 2 o 3 Dissolve 0.1mol (8.1380g) and 0.002mol (0.7040g) respectively in nitric acid at a concentration of 1:1 (volume ratio), and mix them uniformly. Add about 0.17-0.18g (0.1768g) of boric acid, 50.7271g of urea and an appropriate amount of combustion aid NH 4 NO 3 , 0.1mol (6.0080g) SiO 2 Add slowly, then ultrasonically disperse for 10min. Move the solution directly into a high-temperature furnace preheated to 600°C. As the water evaporates, the solution begins to expand and bubble, releasing a large amount of gas. After the gas is ignited, it will burn violently, the flame is yellowish white, and the burning process can last for about 30s. Collect the obtained fluffy and foamy products, place them in an agate mortar, grind and mix them, and finally place them in a high-temperature resistance furnace at 1100° C. for 2 hours. The calcined product is slightly ground to obtain a powder sam...

Embodiment 2

[0038] According to the composition ratio n(ZnO):n(Eu 2 o 3 )=1:0.06 Weigh ZnO, Eu 2 o 3 0.1mol (8.1380g) and 0.002mol (0.7040g), respectively, were dissolved in nitric acid at a concentration of 1:1 (volume ratio), and mixed uniformly. Add about 0.17-0.18g (0.1768g) of boric acid, 40.5817g of urea and an appropriate amount of combustion aid NH 4 NO 3 , 0.1mol (6.0080g) SiO 2 Add slowly, then ultrasonically disperse for 10min. Move the solution directly into a high-temperature furnace preheated to 600°C. As the water evaporates, the solution begins to expand and bubble, releasing a large amount of gas. After the gas is ignited, it will burn violently, the flame is yellowish white, and the burning process can last for about 30s. Collect the obtained fluffy and foamy products, place them in an agate mortar, grind and mix well, and finally place them in a high-temperature resistance furnace at 1100° C. for 3 hours. The calcined product is slightly ground to obtain a powde...

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Abstract

The invention discloses the preparation method of red phosphor Zn2SiO4:Eu3+, which adopts the combustion method as the novel preparation method; Urea is used as the incendiary agent to synthesize the red phosphor Zn2SiO4:Eu3+ successfully; the combustion thermal discharge is improved and excessive combustion gas is generated through the addition of a small quantity of combustion auxiliary agent ammonium nitrate so that the combustion product is ensured to be looser; the combustion auxiliary agent is combusted in the interior of the mixture to catalyze the whole combustion reaction, facilitating the system to overcome high reaction activation potential barrier; the raw product is combusted within the temperature range of the experiment; after the continuous heat preservation; the product has small morphological changes; the crystal formation of the product is good, avoiding the decreasing of the luminescent property caused by the damage of the crystal lattice after grinding and crushing.

Description

technical field [0001] The invention relates to a red fluorescent powder Zn 2 SiO 4 :Eu 3+ The preparation method, specifically for the preparation of red phosphor Zn by combustion method 2 SiO 4 :Eu 3+ method. Background technique [0002] Usually Eu 3+ The emission spectrum is in the red region. These lines have many important applications in lighting and display (color television). These lines correspond to 4f 6 excited state 5 D. 0 energy level to 7 f J (J = 0, 1, 2, 3, 4, 5 and 6) energy level transition emission. because 5 D. 0 The energy levels are not split by the crystal field (J=0), the splitting of the emission transition is by 7 f J It is caused by crystal splitting of energy levels. In addition to these lines, it can also be observed from the higher 5D energy level (i.e. 5 D. 1 , 5 D. 2 even 5 D. 3 ) emission. [0003] In the past few decades, for Eu 3+ There have been quite a lot of reports on the synthesis methods of various systems o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/79
Inventor 彭子飞罗彩芹余军保
Owner SHANGHAI NORMAL UNIVERSITY
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