CN101434837B - Ultraviolet excitated red fluorescent powder surface treating method - Google Patents
Ultraviolet excitated red fluorescent powder surface treating method Download PDFInfo
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- CN101434837B CN101434837B CN 200810232758 CN200810232758A CN101434837B CN 101434837 B CN101434837 B CN 101434837B CN 200810232758 CN200810232758 CN 200810232758 CN 200810232758 A CN200810232758 A CN 200810232758A CN 101434837 B CN101434837 B CN 101434837B
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Abstract
The invention relates to a surface disposal method of an ultraviolet excitation red fluorescent powder, belonging to the field of inorganic synthesis technique of optical function material. The method comprises the steps as follows: the surfactant raw material is screened by a screen of 400 meshes and ball-grinded; subsequently, the consistency of the solution is adjusted and the solution is mixed to gain the surfactant; subsequently, according to the mass percentage in occupation to yttrium europium oxide, 0.005-0.05 percent of surfactant is added into the red fluorescent powder of the yttrium europium oxide; under a mixing state, the surfactant and the red fluorescent powder of the yttrium europium oxide are mixed; the mixture is dehydrated, dried and screened, thus gaining the red fluorescent powder of the yttrium europium oxide with the surface disposed, wherein, according to the mass percentage, the surfactant is one of 5-20 percent Gama-Al2O3 solution, yttrium oxide, potassium silicate, zinc silicate or zinc sulfate. The surface disposal method can prepare the commercial red fluorescent powders which has good powder fluidity, good coating performance, good dispersion performance and good luminescence. The prepared red fluorescent powder of the yttrium europium oxide has the advantages of good fluidity, good coating performance, good dispersion performance and good luminescence.
Description
One, technical field
The present invention the invention belongs to the inorganic synthesis technical field of optical functional materials, is specifically related to a kind of surface treatment method of ultraviolet excitated red fluorescent powder.
Two, background technology
The yttrium europium oxide red fluorescence powder is a kind of important red illuminating material, middle 1960s, discovery is mixed with the yttrium oxide of europium can launch the narrow red fluorescence of spectral line under cathode-ray exciting, brightness is high and bright-coloured, this yttrium europium oxide red fluorescence powder is particularly suitable for doing the red fluorescence powder in the negative ray chromoscope, and yttrium europium oxide red fluorescence powder synthetic method commonly used has methods such as high temperature solid phase synthesis, sol-gel process, combustion synthesis method and microwave process for synthesizing.Simple owing to high temperature solid phase synthesis equipment at present, stable processing technique, yield is high and most widely used general.In recent years, along with technology rapid development, the yttrium europium oxide red fluorescence powder is good owing to luminosity height under vacuum ultraviolet (VUV), colour purity, stable to be widely used.At present commercial yttrium europium oxide ubiquity is in using coating process, and film quality is bad, apply evenly inadequately, so light efficiency is not high in luminescence process, and light decay is bigger.
Three, summary of the invention:
The objective of the invention is to, a kind of surface treatment method that can be applicable to the yttrium europium oxide red fluorescence powder of different coating methods is provided.
Present method can produce the good commercial red fluorescence powder of powder fluidity, screening characteristics, dispersiveness and luminous.
For achieving the above object, the manufacture method that the present invention adopts is: at first, the tensio-active agent raw material is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, the tensio-active agent raw material is γ-Al
2O
3, resulting tensio-active agent is that mass percent concentration is γ-Al of 5-20%
2O
3Solution; Secondly, in the yttrium europium oxide red fluorescence powder, add the tensio-active agent that accounts for yttrium europium oxide mass percent 0.005-0.05%, mixed surfactant and yttrium europium oxide red fluorescence powder under the state that stirs, with mixture dehydration, dry, sieve, can obtain surface treatment yttrium europium oxide red fluorescence powder.Because the γ-Al after handling
2O
3Yttrium oxide, potassium silicate, potassium silicate, zinc silicate has can be as the general character of tensio-active agent, and the characteristic that all has stupalith, it is through ball milling, cross 600 mesh sieves, all be that the solute granularity is less than 600 purpose solution after the stirring, (0.005-0.05%) tensio-active agent of trace joins (500 order) in the red fluorescence powder, improved the grain size distribution of red fluorescence powder, thereby can both play the effect that improves yttrium europium oxide red fluorescence powder performance, so the present invention also can adopt yttrium oxide, potassium silicate, a kind of in zinc silicate or the zinc sulfate as the tensio-active agent raw material, tensio-active agent can be the yttria solution of 1-15% for mass percent concentration, volumetric molar concentration is the potassium silicate solution of 1-10mol/l, volumetric molar concentration is a kind of in the zinc silicate solution of 1-10mol/l or the solution of zinc sulfate that volumetric molar concentration is 1-10mol/l.
The surface treatment method of the yttrium europium oxide red fluorescence powder that the present invention proposes, its concrete steps are as follows:
(1), tensio-active agent preparation: the tensio-active agent raw material is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, wherein the tensio-active agent raw material is γ-Al
2O
3, tensio-active agent is that mass percent concentration is γ-Al of 5-20%
2O
3Solution, require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stirring, adding by the yttrium europium oxide mass percent in whipping process is the 0.005-0.05% tensio-active agent, churning time is 0.5-2.0 hour, the powder that stirs was starched 500 mesh sieves, dehydration, dry, sieve, can obtain surface treatment yttrium europium oxide red fluorescence powder.
The present invention also can adopt a kind of as the tensio-active agent raw material in yttrium oxide, potassium silicate, zinc silicate or the zinc sulfate, a kind of in the solution of zinc sulfate that tensio-active agent can be 1-10mol/l for mass percent concentration is the yttria solution of 1-15%, potassium silicate solution that volumetric molar concentration is 1-10mol/l, volumetric molar concentration is 1-10mol/l zinc silicate solution or volumetric molar concentration.
Because the present invention adopts unique surfactant formula and surface treatment method, thereby has made the good europium gadolinium yttrium oxide red fluorescent powder of flowability, screening characteristics, dispersiveness and luminous.Brightness according to the yttrium europium oxide red fluorescence powder of the present invention preparation is 105-107, and ó ln0.30-0.36 is significantly higher than the market like product.
Four, specific implementation method:
Embodiment 1:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 20%
2O
3Solution, require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.005% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 2:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 20%
2O
3Solution, require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.01% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens both must this red fluorescence powder, this powder brightness 106, ó ln 0.38.
Embodiment 3:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 20%
2O
3Solution requires to disperse ball to be herein
0.5-1.5mm agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.015% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens both must this red fluorescence powder, this powder brightness 107, ó ln 0.36.
Embodiment 4:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 20%
2O
3Solution, require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.02% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens both must this red fluorescence powder, this powder brightness 107, ó ln 0.33.
Embodiment 5:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 20%
2O
3Solution, require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.025% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens both must this red fluorescence powder, this powder brightness 107, ó ln 0.30.
Embodiment 6:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 20%
2O
3Solution requires to disperse ball to be herein
0.5-1.5mm agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.03% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens both must this red fluorescence powder, this powder brightness 107, ó ln 0.32.
Embodiment 7:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 5%
2O
3Solution requires to disperse ball to be herein
0.5-1.5mm agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.05% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 8:
(1), tensio-active agent preparation: with tensio-active agent raw material γ-Al
2O
3Cross 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is γ-Al of 10%
2O
3Solution requires to disperse ball to be herein
0.5-1.5mm agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.023% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 106, ó ln 0.38.
Embodiment 9:
(1), tensio-active agent preparation: tensio-active agent raw material yttrium oxide is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is 15% yttria solution, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.005% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 10:
(1), tensio-active agent preparation: tensio-active agent raw material yttrium oxide is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is 1% yttria solution, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.05% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 11:
(1), tensio-active agent preparation: tensio-active agent raw material yttrium oxide is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that mass percent concentration is 7% yttria solution, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.023% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 106, ó ln 0.38.
Embodiment 12:
(1), tensio-active agent preparation: tensio-active agent raw material potassium silicate is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and, obtain tensio-active agent solution high-speed stirring 12-24 hour, tensio-active agent is that volumetric molar concentration is the potassium silicate solution of 10mol/l, requires to disperse ball to be herein
0.5-1.5mm agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.005% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 13:
(1), tensio-active agent preparation: tensio-active agent raw material potassium silicate is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that volumetric molar concentration is the potassium silicate solution of 1mol/l, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.05% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 14:
(1), tensio-active agent preparation: tensio-active agent raw material potassium silicate is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and, obtain tensio-active agent solution high-speed stirring 12-24 hour, tensio-active agent is that volumetric molar concentration is the potassium silicate solution of 5mol/l, requires to disperse ball to be herein
0.5-1.5mm agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.023% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 106, ó ln 0.38.
Embodiment 15:
(1), tensio-active agent preparation: tensio-active agent raw material zinc silicate is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that volumetric molar concentration is the zinc silicate solution of 10mol/l, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.005% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 16:
(1), tensio-active agent preparation: tensio-active agent raw material zinc silicate is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and, obtain tensio-active agent solution high-speed stirring 12-24 hour, tensio-active agent is that volumetric molar concentration is the zinc silicate solution of 1mol/l, requires to disperse ball to be herein
0.5-1.5mm agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.05% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 17:
(1), tensio-active agent preparation: tensio-active agent raw material zinc silicate is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that volumetric molar concentration is the zinc silicate solution of 5mol/l, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.023% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 106, ó ln 0.38.
Embodiment 18:
(1), tensio-active agent preparation: tensio-active agent raw material sulphuric acid zinc is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that volumetric molar concentration is the solution of zinc sulfate of 10mol/l, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.005% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 19:
(1), tensio-active agent preparation: tensio-active agent raw material sulphuric acid zinc is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that volumetric molar concentration is the solution of zinc sulfate of 1mol/l, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.05% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 105, ó ln 0.40.
Embodiment 20:
(1), tensio-active agent preparation: tensio-active agent raw material sulphuric acid zinc is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and with solution high-speed stirring 12-24 hour, obtain tensio-active agent, tensio-active agent is that volumetric molar concentration is the solution of zinc sulfate of 5mol/l, and require to disperse ball is the 0.5-1.5mm agate ball herein;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the qualified powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add and account for yttrium europium oxide mass percent 0.023% tensio-active agent, churning time is 2.0 hours, the powder that stirs was starched the dehydration of 500 mesh sieves, dry down at 110-120 ℃, dried powder is crossed 200 eye mesh screens must this red fluorescence powder, this powder brightness 106, ó ln 0.38.
Claims (1)
1. the surface treatment method of a yttrium europium oxide red fluorescence powder is characterized in that:
(1), tensio-active agent preparation: the tensio-active agent raw material is crossed 400 eye mesh screens, remove the screening reject on 400 eye mesh screens, all the other powder that obtain are packed in the ball milling bottle, according to mass percent with powder: ball: water is 1: 2: 2 ratio ball milling 12-48 hour, the solution that ball milling obtains is crossed 600 mesh sieves, adjust strength of solution and, obtain tensio-active agent, require to disperse ball to be herein solution high-speed stirring 12-24 hour
Agate ball;
(2), yttrium europium oxide red fluorescence powder pre-treatment: the pulp of yttrium europium oxide red fluorescence powder is handled, crossed 500 eye mesh screens, remove the screening reject on 500 eye mesh screens, all the other powder that obtains slurries are washed qualified powder pulp-water 2-5 time for qualified powder slurry;
(3), yttrium europium oxide red fluorescence powder preparation: the powder slurry that washing is good is got rid of the upper water washing lotion, stir, in whipping process, add the tensio-active agent of yttrium europium oxide mass percent 0.005-0.05%, churning time is 0.5-2.0 hour, the powder that stirs was starched 500 mesh sieves, and dehydration, crossing 200 eye mesh screens at temperature 110-120 ℃ drying, dried powder must this red fluorescence powder;
The tensio-active agent raw material is γ-Al in the step 1
2O
3, a kind of in yttrium oxide, potassium silicate, zinc silicate or the zinc sulfate, tensio-active agent is that mass percent concentration is γ-Al of 20%
2O
3A kind of in the solution of zinc sulfate that zinc silicate solution that solution, mass percent concentration are the yttria solution of 1-15%, potassium silicate solution that volumetric molar concentration is 1-10mol/l, volumetric molar concentration is 1-10mol/l or volumetric molar concentration are 1-10mol/l.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20060127669A1 (en) * | 2003-01-24 | 2006-06-15 | Hisao Kogoi | Surface modification method for inorganic oxide powder, powder produced by the method and use of the powder |
| CN1995275A (en) * | 2006-12-19 | 2007-07-11 | 江门市科恒实业有限责任公司 | Nano grade high temperature disperser applied to Y2O3: Eu red powder and its preparation method |
| CN101173169A (en) * | 2007-11-30 | 2008-05-07 | 彩虹集团电子股份有限公司 | Fluorescent powder dispersion method |
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| US20060127669A1 (en) * | 2003-01-24 | 2006-06-15 | Hisao Kogoi | Surface modification method for inorganic oxide powder, powder produced by the method and use of the powder |
| CN1995275A (en) * | 2006-12-19 | 2007-07-11 | 江门市科恒实业有限责任公司 | Nano grade high temperature disperser applied to Y2O3: Eu red powder and its preparation method |
| CN101173169A (en) * | 2007-11-30 | 2008-05-07 | 彩虹集团电子股份有限公司 | Fluorescent powder dispersion method |
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