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Method for producing rare earth ion doped yttrium aluminum garnet nano phosphor powder

A technology of yttrium aluminum garnet and nano-fluorescent powder, which is applied in chemical instruments and methods, luminescent materials, liquid injection devices, etc., and can solve problems such as harsh process requirements, irregular powder shapes, and large particles

Inactive Publication Date: 2009-12-16
NINGBO UNIV
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Problems solved by technology

[0004] The preparation method of rare earth ion-doped YAG phosphor mainly includes high-temperature solid-state reaction method [4] , sol-gel method [5] , polymer network gel method [6] , Solvothermal method [7] , combustion method [8] , spray pyrolysis [9] , coprecipitation method [10] etc., but these methods all have certain disadvantages, such as the high-temperature solid-state reaction method, the obtained powder needs ball milling, the particles are large and the particle size distribution is wide; the sol-gel method needs expensive raw materials, and the cost is high; The metal alkoxide in the glue method is generally not easy to obtain, and the cost is high, and the water must be strictly controlled during the reaction process, and the reaction conditions are harsh; the solvothermal method requires high synthesis temperature and pressure; the powder formed by the combustion method has different shapes. Rules; compared with other chemical methods, the co-precipitation method has the advantages of low cost, simple equipment and easy large-scale production, but the preparation method is cumbersome, demanding, and takes a long time
In addition to certain shortcomings in the process conditions, the above methods also have certain shortcomings in achieving high-concentration doping of rare earth ions, such as the sol-gel method, when Eu 3+ When the content reaches 0.06mol, Eu 3+ The luminescence reaches the strongest, and then with Eu 3+ decrease with the increase of the content, concentration quenching phenomenon occurs [11] ; Apply co-precipitation method, when Ce 3+ When the doping concentration in YAG is 4.8%, the fluorescence intensity reaches the maximum, Ce 3+ When the doping concentration is further increased, due to Ce 3+ Concentration quenching occurs due to the nonradiative relaxation between [12]

Method used

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  • Method for producing rare earth ion doped yttrium aluminum garnet nano phosphor powder
  • Method for producing rare earth ion doped yttrium aluminum garnet nano phosphor powder

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Embodiment 1

[0041] (1) First Al(NO 3 ) 3 , Y(NO 3 ) 3 and Eu(NO 3 ) 3 solution, according to the general formula (Y 0.98 Eu 0.02 ) 3 al 5 o 12 The stoichiometric ratio is formulated into a mother salt solution with a cation concentration of 0.2 mol / liter, and then a 0.6 mol / liter ammonium bicarbonate solution is prepared with deionized water, and the pH of the solution is adjusted to 10 with ammonia water, NH 4 HCO 3 The molar mass of (Y 1-χ ln χ ) 3 al 5 o 12 The ratio of the total molar weight of cations in the medium is 3:1;

[0042] (2) Adjust the valve so that the mother salt solution flows through the titanium alloy ultrasonic spray head with a pore size of 0.20 mm, and enters the ultrasonic atomization device at a flow rate of 300 ml / hour, and controls the spray flow rate so that the reaction is completed within 4 hours, at a frequency of 50KHz , Under the action of continuous ultrasound with a power of 45W, after ultrasonic atomization, it is added to the continuou...

Embodiment 2

[0048] (1) First Al(NO 3 ) 3 , Y(NO 3 ) 3 and Ce(NO 3 ) 3 solution, according to the general formula (Y 0.96 Ce 0.04 ) 3 al 5 o 12 The stoichiometric ratio is made into a mother salt solution with a cation concentration of 0.3 mol / liter, and then a 0.9 mol / liter ammonium bicarbonate solution is prepared with deionized water, and the pH of the solution is adjusted to 10 with ammonia water, NH 4 HCO 3 The molar mass of (Y 1-χ ln χ ) 3 al 5 o 12 The ratio of the total molar weight of cations in the medium is 3:1;

[0049] (2) Adjust the valve so that the mother salt solution flows through the titanium alloy ultrasonic spray head with a pore size of 0.20 mm, and enters the ultrasonic atomization device at a flow rate of 300 ml / hour, and controls the spray flow rate so that the reaction is completed within 4 hours, at a frequency of 50KHz , Under the action of continuous ultrasound with a power of 45W, after ultrasonic atomization, it is added to the continuously st...

Embodiment 3

[0055] (1) First Al(Ac) 3 、Y(Ac) 3 and Eu(Ac) 3 solution, according to the general formula (Y 0.94 Eu 0.06 ) 3 al 5 o 12 The stoichiometric ratio is made into a mother salt solution with a cation concentration of 0.15 mol / liter, and then a 0.45 mol / liter ammonium bicarbonate solution is prepared with deionized water, and the pH of the solution is adjusted to 10 with ammonia water, NH 4 HCO 3 The molar mass of (Y 1-χ ln χ ) 3 al 5 o 12 The ratio of the total molar weight of cations in the medium is 3:1;

[0056](2) Adjust the valve so that the mother salt solution flows through the titanium alloy ultrasonic spray nozzle with a pore size of 0.20 mm, and enters the ultrasonic atomization device at a flow rate of 200 ml / hour, and controls the spray flow rate so that the reaction is completed within 4 hours, at a frequency of 50KHz , Under the action of continuous ultrasound with a power of 45W, after ultrasonic atomization, it is added to the continuously stirring mix...

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Abstract

The invention discloses a method for producing a rare earth ion doped yttrium aluminum garnet nano phosphor powder. The general formula of the nano powder is (Y1-xLnx)3Al5O12, wherein Ln is one of rare earth elements Ce and Eu, x is more than or equal to 0.0 and less than or equal to 0.1, mixed solution of nitrates or acetates of Al, Y and Ln is used as a mother liquor of salt, and mixed solution of NH4HCO3 and NH3.H2O is used as solution of compound precipitator; the ammonia water is used for adjusting the pH value of the solution of compound precipitator to 10; and the mother liquor of salt undergoes ultrasonic atomization and then is sprayed in the solution of compound precipitator which is continuously stirred, and after complete reaction, the mixed solution if filtered, washed, dried, repeatedly ball-milled and calcined to obtain uniform and dispersed rare earth ion doped YAG nano phosphor powder. The method has the advantages that the produced nano phosphor powder is uniform and dispersed, the granularity is small (between 50 and 70 nanometers), and the generated phase is unitary; and the high-concentration uniform doping of the rare earth ions is realized, so that the rare earth ion doped yttrium aluminum garnet nano phosphor powder can be obtained in high efficiency.

Description

technical field [0001] The invention relates to a production method of yttrium aluminum garnet (YAG) fluorescent powder, in particular to a production method of rare earth ion-doped yttrium aluminum garnet (YAG) nano fluorescent powder. Background technique [0002] Phosphors with rare earth ions as the luminescent center have been widely used in many fields, such as lamp phosphors, medical phosphors, TV phosphors, etc. Due to the high added value and significant benefits of this product, it has become a rare earth high-tech development important areas. Although the amount of rare earth phosphor used is less than 4% of the total rare earth consumption, the output value accounts for 41% of the total sales of the rare earth application market, making it the hottest industry in the rare earth industry [1,2] . [0003] Yttrium aluminum garnet (yttrium aluminum garnet), the chemical formula is Y 3 Al 5 o 12 , referred to as YAG, has excellent optical properties and good mech...

Claims

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Application Information

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IPC IPC(8): C09K11/80B05B17/06B02C17/00B02C17/20
Inventor 夏海平邱杨王军王存宽
Owner NINGBO UNIV
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