CN101974333B - Method for manufacturing fine red fluorescent powder - Google Patents
Method for manufacturing fine red fluorescent powder Download PDFInfo
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- CN101974333B CN101974333B CN 201010518756 CN201010518756A CN101974333B CN 101974333 B CN101974333 B CN 101974333B CN 201010518756 CN201010518756 CN 201010518756 CN 201010518756 A CN201010518756 A CN 201010518756A CN 101974333 B CN101974333 B CN 101974333B
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Abstract
The invention discloses a method for manufacturing fine red fluorescent powder, which comprises: mixing yttrium europium oxide co-sediment with ammonium metavanadate and fluxing agent to obtain a mixture of raw materials, firing the mixture of the raw materials, cooling the mixture to room temperature, and passing the mixture through a dry sieve to obtain fired fluorescent powder; placing the fired fluorescent powder in a first alkali wash tank, performing alkali wash, and recovering alkaline solution to obtain first slurry; transferring the first slurry to a first rinsing tank, rinsing, settling, and pouring clear liquid out to obtain second slurry; filling the second slurry in a disperser, and dispersing to obtain third slurry; transferring the third slurry to a second alkali wash tank, and performing alkali wash to obtain fourth slurry; transferring the fourth slurry to a second rising tank, rinsing, settling, and pouring clear liquid out to obtain fifth slurry; and finally, dewatering the fifth slurry, drying, cooling to room temperature, and sieving to obtain finished red fluorescent powder. The red fluorescent powder manufactured by the invention has the advantages that: the particle size is small; and the light-emitting performance is high.
Description
Technical field
The present invention relates to a kind of manufacture method of fluorescent material, particularly a kind of manufacture method of fine red fluorescent powder.
Background technology
Yttrium Orthovanadate europium (YVO
4: Eu) as main red phosphor powder for high pressure mercury lamp, although it is effectively luminescent material under the 253.7nm shooting conditions, it has good temperature profile, maximum operating temperature can reach 330 ℃, chromaticity coordinates x value reaches 0.663 simultaneously, can guarantee good purity of color, and its characteristics of luminescence is basic and yttrium europium oxide (Y
2O
3: Eu) red fluorescence powder is suitable, but bigger than normal because of its granularity, generally at 8-10 μ m, but can't well be applied to fine-pipe-diameter energy-saving lamp and cold-cathode lamp, also can't with yttrium europium oxide (Y
2O
3: Eu) red fluorescence powder mixes application, has the poor shortcoming of luminescent properties.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of manufacture method of fine red fluorescent powder, can produce the center granularity is 4～6 μ m fine red fluorescent powders, is applied to fine-pipe-diameter energy-saving lamp and cold-cathode lamp, and can with Y
2O
3: the Eu red fluorescence powder mixes to be used, and the made red-emitting phosphors powder of the present invention has advantages of that luminescent properties is good.
In order to achieve the above object, the technical scheme taked of the present invention is:
A kind of manufacture method of fine red fluorescent powder comprises the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boric acid, boron oxide, bariumchloride, barium tetraborate, tetraboric acid magnesium or lithium tetraborate
(2) batch mixing
Y: V=1 in molar ratio: (1.0～1.2) get yttrium europium oxide codeposition body and ammonium meta-vanadate, and add 0.5～2% fusing assistant of yttrium europium oxide codeposition body quality, mix, and obtain mixture of raw material;
(3) burn till
Mixture of raw material calcination under the oxidizing atmosphere of 1050 ℃～1200 ℃ after 2～6 hours, is cooled to room temperature, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1 that fluor burns till product and weight percent: (4～6), the alkali cleaning temperature is 80～90 ℃, the alkali cleaning time is 20～40min, after reclaiming alkali lye, obtain the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, the weight ratio condition of 1: 5 of product and water of burning till by fluor is washed 5-8 time, outwells clear liquid after sedimentation and obtains the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, the weight ratio that fluor burns till product, ball and water is 1: (2～4): (2～4), disperseing rotating speed is 20～40 to turn/min, jitter time is 1～4 hour, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, fluor burns till product and weight percent is that 20% ammonia soln weight ratio is 1: (4～6), the alkali cleaning temperature is 80～90 ℃, the alkali cleaning time is 20～40min, after reclaiming alkali lye, obtains the 4th powder slurry;
(8) washing
Change the 4th powder slurry over to second washing bath, the weight ratio condition of 1: 5 of product and water of burning till by fluor is washed 4-6 time, outwells clear liquid after sedimentation and obtains the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 100～120 ℃ dry 8～12 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
The red-emitting phosphors powder granule made due to the present invention is little, and can produce the center granularity is 4～6 μ m fine red fluorescent powders, so have advantages of that luminescent properties is good.
Embodiment
Embodiment 1
A kind of manufacture method of fine red fluorescent powder comprises the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boric acid;
(2) batch mixing
Y: V=1 in molar ratio: 1 gets yttrium europium oxide codeposition body and ammonium meta-vanadate, and adds 1% boric acid of yttrium europium oxide codeposition body quality, mixes, and obtains mixture of raw material;
(3) burn till
Mixture of raw material after 4.5 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1080 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1: 6 that fluor burns till product and weight percent, the alkali cleaning temperature is 90 ℃, the alkali cleaning time is 25min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, the weight ratio condition of 1: 5 of product and water of burning till by fluor is washed 8 times, outwells clear liquid after sedimentation and obtains the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, the weight ratio that fluor burns till product, ball and water is 1: 2: 2, and disperseing rotating speed is 20 to turn/min, and jitter time is 1.5 hours, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1: 4 that fluor burns till product and weight percent, and the alkali cleaning temperature is 80 ℃, and the alkali cleaning time is 20min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 5 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 120 ℃ dry 12 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
Embodiment 2
A kind of manufacture method of fine red fluorescent powder comprises the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boron oxide;
(2) batch mixing
Y: V=1 in molar ratio: 1.05 get yttrium europium oxide codeposition body and ammonium meta-vanadate, and add 1% boron oxide of yttrium europium oxide codeposition body quality, mix, and obtain mixture of raw material;
(3) burn till
Mixture of raw material after 4 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1100 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1: 5 that fluor burns till product and weight percent, the alkali cleaning temperature is 90 ℃, the alkali cleaning time is 20min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 7 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, the weight ratio that fluor burns till product, ball and water is 1: 2: 3, and disperseing rotating speed is 20 to turn/min, and jitter time is 2.5 hours, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1: 5 that fluor burns till product and weight percent, and the alkali cleaning temperature is 80 ℃, and the alkali cleaning time is 20min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 6 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 110 ℃ dry 12 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
Embodiment 3
A kind of manufacture method of fine red fluorescent powder comprises the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is lithium tetraborate;
(2) batch mixing
Y: V=1 in molar ratio: 1.1 get yttrium europium oxide codeposition body and ammonium meta-vanadate, and add 0.5% lithium tetraborate of yttrium europium oxide codeposition body quality to mix, and obtain mixture of raw material;
(3) burn till
Mixture of raw material after 4 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1130 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1: 4 that fluor burns till product and weight percent, the alkali cleaning temperature is 80 ℃, the alkali cleaning time is 40min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, the weight ratio condition of 1: 5 of product and water of burning till by fluor is washed 8 times, outwells clear liquid after sedimentation and obtains the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, it is to disperse at 1: 2: 4 by weight that fluor burns till product, ball and water, and disperseing rotating speed is 20 to turn/min, and jitter time is 3 hours, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1: 4 that fluor burns till product and weight percent, and the alkali cleaning temperature is 90 ℃, and the alkali cleaning time is 30min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 5 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 120 ℃ dry 9 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
Embodiment 4
A kind of manufacture method of fine red fluorescent powder comprises the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boric acid;
(2) batch mixing
Y: V=1 in molar ratio: 1.2 get yttrium europium oxide codeposition body and ammonium meta-vanadate, and add 1% boric acid of yttrium europium oxide codeposition body quality, obtain mixture of raw material;
(3) burn till
Mixture of raw material after 3 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1150 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1: 6 that fluor burns till product and weight percent, the alkali cleaning temperature is 90 ℃, the alkali cleaning time is 30min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 6 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, fluor burns till product: ball: water is to disperse at 1: 3: 4 by weight, and disperseing rotating speed is 30 to turn/min, and jitter time is 1.5 hours, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1: 6 that fluor burns till product and weight percent, and the alkali cleaning temperature is 85 ℃, and the alkali cleaning time is 40min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 6 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 110 ℃ dry 10 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
Embodiment 5
A kind of manufacture method of fine red fluorescent powder comprises the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is barium tetraborate;
(2) batch mixing
Y: V=1 in molar ratio: 1.0 get yttrium europium oxide codeposition body and ammonium meta-vanadate, and add 1% barium tetraborate of yttrium europium oxide codeposition body quality, obtain mixture of raw material;
(3) burn till
Mixture of raw material after 3 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1140 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1: 5 that fluor burns till product and weight percent, the alkali cleaning temperature is 85 ℃, the alkali cleaning time is 40min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 7 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, it is to disperse at 1: 2: 4 by weight that fluor burns till product, ball and water, and disperseing rotating speed is 25 to turn/min, and jitter time is 2 hours, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln is 1: 5 by weight that fluor burns till product and weight percent, and the alkali cleaning temperature is 90 ℃, and the alkali cleaning time is 30min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the weight ratio of the water condition of 1: 5 washing 4 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 120 ℃ dry 9 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
The chromaticity coordinates of each embodiment, brightness and center granularity are referring to subordinate list.
Subordinate list
Claims (6)
1. the manufacture method of a fine red fluorescent powder is characterized in that: comprise the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boric acid, boron oxide, bariumchloride, barium tetraborate, tetraboric acid magnesium or lithium tetraborate;
(2) batch mixing
Y:V=1:(1.0～1.2 in molar ratio) get yttrium europium oxide codeposition body and ammonium meta-vanadate, and add 0.5～2% fusing assistant of yttrium europium oxide codeposition body quality, mix, obtain mixture of raw material;
(3) burn till
Mixture of raw material calcination under the oxidizing atmosphere of 1050 ℃～1200 ℃ after 2～6 hours, is cooled to room temperature, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1:(4～6 that fluor burns till product and weight percent), the alkali cleaning temperature is 80～90 ℃, the alkali cleaning time is 20～40min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till the condition of the weight ratio 1:5 of product and water by fluor and wash 5-8 time, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, the weight ratio that fluor burns till product, ball and water is 1:(2～4): (2～4), disperseing rotating speed is 20～40 to turn/min, jitter time is 1～4 hour, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1:(4～6 that fluor burns till product and weight percent), the alkali cleaning temperature is 80～90 ℃, the alkali cleaning time is 20～40min, after reclaiming alkali lye, obtains the 4th powder slurry;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till the condition of the weight ratio 1:5 of product and water by fluor and wash 4-6 time, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 100～120 ℃ dry 8～12 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
2. the manufacture method of a kind of fine red fluorescent powder according to claim 1 is characterized in that: comprise the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boric acid;
(2) batch mixing
Y:V=1:1 gets yttrium europium oxide codeposition body and ammonium meta-vanadate in molar ratio, and adds 1% boric acid of yttrium europium oxide codeposition body quality, mixes, and obtains mixture of raw material;
(3) burn till
Mixture of raw material after 4.5 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1080 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1:6 that fluor burns till product and weight percent, the alkali cleaning temperature is 90 ℃, the alkali cleaning time is 25min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till the condition of the weight ratio 1:5 of product and water by fluor and wash 8 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, the weight ratio that fluor burns till product, ball and water is 1:2:2, and disperseing rotating speed is 20 to turn/min, and jitter time is 1.5 hours, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1:4 that fluor burns till product and weight percent, and the alkali cleaning temperature is 80 ℃, and the alkali cleaning time is 20min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 5 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 120 ℃ dry 12 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
3. the manufacture method of a kind of fine red fluorescent powder according to claim 1 is characterized in that: comprise the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boron oxide;
(2) batch mixing
Y:V=1:1.05 gets yttrium europium oxide codeposition body and ammonium meta-vanadate in molar ratio, and adds 1% boron oxide of yttrium europium oxide codeposition body quality, mixes, and obtains mixture of raw material;
(3) burn till
Mixture of raw material after 4 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1100 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1:5 that fluor burns till product and weight percent, the alkali cleaning temperature is 90 ℃, the alkali cleaning time is 20min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 7 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, the weight ratio that fluor burns till product, ball and water is 1:2:3, and disperseing rotating speed is 20 to turn/min, and jitter time is 2.5 hours, obtains the 3rd powder slurry;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1:5 that fluor burns till product and weight percent, and the alkali cleaning temperature is 80 ℃, and the alkali cleaning time is 20min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 6 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 110 ℃ dry 12 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
4. the manufacture method of a kind of fine red fluorescent powder according to claim 1 is characterized in that: comprise the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is lithium tetraborate;
(2) batch mixing
Y:V=1:1.1 gets yttrium europium oxide codeposition body and ammonium meta-vanadate in molar ratio, and adds 0.5% lithium tetraborate of yttrium europium oxide codeposition body quality to mix, and obtains mixture of raw material;
(3) burn till
Mixture of raw material after 4 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1130 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1:4 that fluor burns till product and weight percent, the alkali cleaning temperature is 80 ℃, the alkali cleaning time is 40min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till the condition of the weight ratio 1:5 of product and water by fluor and wash 8 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, fluor burns till product, ball and water by weight for 1:2:4 disperses, and disperseing rotating speed is 20 to turn/min, and jitter time is 3 hours, obtains the 3rd powder and starches;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is that 20% ammonia soln weight ratio is 1:4 that fluor burns till product and weight percent, and the alkali cleaning temperature is 90 ℃, and the alkali cleaning time is 30min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 5 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 120 ℃ dry 9 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
5. the manufacture method of a kind of fine red fluorescent powder according to claim 1 is characterized in that: comprise the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is boric acid;
(2) batch mixing
Y:V=1:1.2 gets yttrium europium oxide codeposition body and ammonium meta-vanadate in molar ratio, and adds 1% boric acid of yttrium europium oxide codeposition body quality, obtains mixture of raw material;
(3) burn till
Mixture of raw material after 3 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1150 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1:6 that fluor burns till product and weight percent, the alkali cleaning temperature is 90 ℃, the alkali cleaning time is 30min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 6 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, fluor burns till product: ball: water is by weight for 1:3:4 disperses, and disperseing rotating speed is 30 to turn/min, and jitter time is 1.5 hours, obtains the 3rd powder and starches;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, it is 1:6 with the 20% ammonia soln weight ratio that weight percent is that fluor burns till product, and the alkali cleaning temperature is 85 ℃, and the alkali cleaning time is 40min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 6 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 110 ℃ dry 10 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
6. the manufacture method of a kind of fine red fluorescent powder according to claim 1 is characterized in that: comprise the following steps:
(1) get the raw materials ready
The fusing assistant of purchasing yttrium europium oxide codeposition body, ammonium meta-vanadate, weight percent and being 30% potassium hydroxide solution, weight percent and be 20% ammonia soln and cross 100 mesh sieves, fusing assistant is barium tetraborate;
(2) batch mixing
Y:V=1:1.0 gets yttrium europium oxide codeposition body and ammonium meta-vanadate in molar ratio, and adds 1% barium tetraborate of yttrium europium oxide codeposition body quality, obtains mixture of raw material;
(3) burn till
Mixture of raw material after 3 hours, is cooled to room temperature in calcination under the oxidizing atmosphere of 1140 ℃, crosses 100 order dry screens, obtain fluorescent material and burn till product;
(4) alkali cleaning
Fluorescent material is burnt till product put into the first alkaline bath, and carry out alkali cleaning by following condition, it is that the weight ratio of 30% potassium hydroxide alkali lye is 1:5 that fluor burns till product and weight percent, the alkali cleaning temperature is 85 ℃, the alkali cleaning time is 40min, after reclaiming alkali lye, obtains the first powder slurry;
(5) washing
Change the first powder slurry over to first washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 7 times, outwell clear liquid after sedimentation and obtain the second powder slurry;
(6) disperse
With the second powder slurry dispersion machine of packing into, and disperse by following condition, fluor burns till product, ball and water by weight for 1:2:4 disperses, and disperseing rotating speed is 25 to turn/min, and jitter time is 2 hours, obtains the 3rd powder and starches;
(7) alkali cleaning
Change the 3rd powder slurry over to second alkaline bath, and carry out alkali cleaning by following condition, fluor burn till product and weight percent be 20% ammonia soln by weight being 1:5, the alkali cleaning temperature is 90 ℃, the alkali cleaning time is 30min, after reclaiming alkali lye, obtains the 4th powder and starches;
(8) washing
Change the 4th powder slurry over to second washing bath, burn till product by fluor: the condition washing of the weight ratio 1:5 of water 4 times, outwell clear liquid after sedimentation and obtain the 5th powder slurry;
(9) drying and screening
Remove contained moisture in the 5th powder slurry, and under take drying temperature as the condition of 120 ℃ dry 9 hours, temperature is crossed 160 mesh sieves after being down to room temperature, obtains finished products-red fluorescent material.
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