CN1281708C - Process for preparing cathode ray luminescent material - Google Patents
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- CN1281708C CN1281708C CN 200510042703 CN200510042703A CN1281708C CN 1281708 C CN1281708 C CN 1281708C CN 200510042703 CN200510042703 CN 200510042703 CN 200510042703 A CN200510042703 A CN 200510042703A CN 1281708 C CN1281708 C CN 1281708C
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Abstract
The present invention discloses a preparation method for a cathode ray luminescent material. The preparation method comprises the following steps: firstly, europium oxide, samarium oxide, sulfur, sodium carbonate and lithium phosphate are added in terbium yttrium oxide to be mixed and then be burnt; secondly, after an antioxidant layer on the upper part is removed, a power block is immersed in deionized water, soaked and washed by water, and the semi-dry power block is put in an acid pickling bath; thirdly, supernatant fluid is removed, and deionized water is added to be stirred; fourthly, when the electric conductivity of the supernatant fluid is from 10 to 50 muS/cm and after the mixture is dewatered, the power block is removed and ballmilled, and deionized water is added; fifthly, after ballmilling, powder slurry is discharged, dewatering is carried out, and the powder block is taken out; sixthly, the powder is dried, and a cathode ray luminescent material can be prepared. In the present invention, after samaric ions mixed in yttrium europium oxysulfide, the addition level of trivalent europium ions can be decreased, and thereby, cost is reduced. New fluorescent powder formed after mixture has the advantages of homogeneous granules, pure color and high luminescence and is a fluorescent substance effectively emitting red light, and the fluorescent powder can be used for the manufacture of color picture tubes and display tubes.
Description
Technical field
The present invention relates to a kind of method that is used to prepare the required cathode-ray luminescence material of colour picture tube (CPT), colour display tube (CDT), particularly a kind of preparation method who adopts europium as the negative ray red illuminating material of activator.
Background technology
The yttrium oxysulfide europium is as the tricolour picture tube red illuminating material, and application has reached more than 30 year; Its luminous efficiency height, the high praise that chemical stability is good, colour purity that sunset glow is suitable and good obtains people.
As everyone knows, the active material europium sesquioxide in the yttrium oxysulfide europium, for a long time, this red illuminating material holds at high price.In the yttrium oxysulfide europium except trivalent europium ion as the activator, also have trivalent terbium ion to play the sensitizing agent effect.For a long time, the illuminant colour coordinate and the europium addition in its material of red illuminating material are closely bound up, and promptly europium addition and chromaticity coordinates x value are proportional; That is to say to want to make red material luminous redder, then the europium addition will be more; Usually to make the illuminant colour coordinate of this red material reach x:0.660 ± 0.003; Y:0.340 ± 0.003.How to reduce the consumption of the active material europium sesquioxide in the yttrium oxysulfide europium, or be the problem that people pay close attention to always with the consumption that cheap rare earth partly substitutes europium sesquioxide.
In the prior art, the addition of activator trivalent europium ion must reach (Eu/Y more than 7.3%
2O
3), just can reach luminous requirement.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of cathode-ray luminescence material, reduce production costs, economical with materials.
Technical scheme of the present invention is achieved in that
At first in the terbium yttrium oxide, add the europium sesquioxide that accounts for its terbium yttrium oxide weight percent 6.1-7.0%, the Samarium trioxide of 0.1-0.4%, the sulphur of 40-50%, the yellow soda ash of 50-60%, the Trilithium phosphate of 5-15% mixes, mixing time is 1～3 hour, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, form powder agglomates, calcination temperature is 1100-1300 ℃, time 22-26 hour;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 10～20 hours; All clear liquors of top of draining then; Add deionized water, make powder agglomates and deionized water with 1: 6 weight ratio, stir, churning time is 2～10 hours; Treat the complete sedimentation of powder agglomates, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water once more, the weight ratio of powder slurry and deionized water 1: 6, stir be slurries after, cross 150 ± 50 order nylon mesh, continue then the powder slurry is washed with deionized water, washing times 3～5 times is 9～11 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making in the pickling tank powder slurry solution hydrochloric acid percentage concentration is 2.45～3.68%, and powder slurry solution temperature is 40～80 ℃, stirs 2～4 hours;
The venting supernatant liquor adds deionized water, washes 10～30 minutes, leaves standstill the venting supernatant liquor 1-2 hour; Add deionized water and stirring again; So repeat to wash four times, until specific conductivity 10～50 μ S/cm of supernatant liquor, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: deionized water is by weight=1: 1: 1, and 2～6 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 100～500 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 10-20 hour; Drying temperature: 80～220 ℃;
The dry powder that drying is good sieves, and 300～500 orders that sieve can make cathode-ray luminescence material.
The present invention is by changing the composition of this luminescent material; Thereby reduced the usage quantity of expensive rare earth material europium sesquioxide, reduced production cost, economical with materials, reduced consumption rare earth resources.In material, mix samaric ion Sm
3+After, can reduce trivalent europium ion Eu
3+Theoretical addition.The addition of activator trivalent europium ion can reduce to (Eu/Y below 6.7%
2O
3), usage quantity is saved more than 9% than original theoretical addition.
Embodiment
Embodiment one:
At first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.1% europium sesquioxide, 0.4% Samarium trioxide, 50% sulphur, 60% yellow soda ash, 15% Trilithium phosphate mixes, and mixing time is 2 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, form powder agglomates, calcination temperature is 1200 ℃, 23 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 10 hours; All clear liquors of top of draining; Add deionized water, powder agglomates: the weight ratio of deionized water=1: 6, stir, churning time is 2 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water, powder slurry: deionized water weight ratio=1: 6, stir and be slurries, cross 100 order nylon mesh, continuation is washed the powder slurry with deionized water, washing times 3 times is 9 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the half-dried powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the percentage concentration of powder slurry solution hydrochloric acid in the pickling tank is 2.45%, and powder slurry solution temperature is 40 ℃, stirs 2 hours;
The venting supernatant liquor adds deionized water, washes 10 minutes, leaves standstill the venting supernatant liquor 1 hour; Add deionized water and stirring again; So repeat to wash four times, until the specific conductivity 10 μ S/cm of supernatant liquor, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: water is by weight=1: 1: 1, and 4 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 100 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 10 hours; Drying temperature: 80 ℃;
The dry powder that drying is good sieves, and 300 orders that sieve can make cathode-ray luminescence material.
Embodiment two:
At first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.5% europium sesquioxide, 0.36% Samarium trioxide, 45% sulphur, 55% yellow soda ash, 10% Trilithium phosphate mixes, and mixing time is 2.5 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, form powder agglomates, carry out calcination, the temperature calcination is 1100 ℃, 25 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 15 hours; All clear liquors of top of draining; Add deionized water, powder agglomates: deionized water weight ratio=1: 6, stir, churning time is 8 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water, powder slurry: deionized water weight ratio=1: 6, stir and be slurries, cross 140 order nylon mesh, the powder slurry is washed in continuation, and washing times 4 times is 10 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the half-dried powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the percentage concentration of powder slurry solution hydrochloric acid in the pickling tank is 2.68%, and the temperature of powder slurry solution is 50 ℃, stirs 3 hours;
The venting supernatant liquor adds deionized water, washes 15 minutes, leaves standstill the venting supernatant liquor 2 hours; Add deionized water and stirring again; So repeat to wash four times, until specific conductivity 10～50 μ S/cm of supernatant liquor, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, alumina balls add deionized water, make powder agglomates: ball: water weight ratio=1: 1: 1,4 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 200 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 15 hours; Drying temperature: 100 ℃;
The dry powder that drying is good sieves, and 400 orders that sieve can make cathode-ray luminescence material.
Embodiment three:
At first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.7% europium sesquioxide, 0.32% Samarium trioxide, 55% sulphur, 50% yellow soda ash, 13% Trilithium phosphate mixes, and mixing time is 2 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, the temperature calcination is 1300 ℃, 26 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 20 hours; The upper clear supernate of draining; Add deionized water, powder agglomates: deionized water weight ratio=1: 6, stir, churning time is 8 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining keeps bottom powder slurry;
In the powder slurry, add deionized water, powder slurry: deionized water weight ratio=1: 6, stir and be slurries, cross 160 order nylon mesh, the powder slurry is washed in continuation, and washing times 5 times is 11 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the half-dried powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the concentration of hydrochloric acid of powder slurry solution in the pickling tank is 3.68%, and the temperature of powder slurry solution is 80 ℃, stirs 4 hours;
The venting supernatant liquor adds deionized water, washes 30 minutes, leaves standstill the venting supernatant liquor 1 hour; Add deionized water and stirring again; So repeat to wash four times,, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: water weight ratio=1: 1: 1,6 hours ball milling time until specific conductivity 10～50 μ S/cm of supernatant liquor;
After ball milling finishes, emit the powder slurry, cross 200 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 20 hours; Drying temperature: 220 ℃;
The dry powder that drying is good sieves, and 500 orders that sieve can make cathode-ray luminescence material.
Embodiment four:
At first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.9% europium sesquioxide, 0.4% Samarium trioxide, 50% sulphur, 60% yellow soda ash, 15% Trilithium phosphate mixes, and mixing time is 3 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, form powder agglomates, calcination temperature is 1300 ℃, 26 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 20 hours; All clear liquors of top of draining; Add deionized water, powder agglomates: deionized water weight ratio=1: 6, stir, churning time is 10 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water, powder slurry: the weight ratio of water=1: 6, stir and be slurries, cross 160 order nylon mesh, the powder slurry is washed in continuation, and washing times 5 times is 10 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the half-dried powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the concentration of hydrochloric acid of powder slurry solution in the pickling tank is 3.68%, and the temperature of powder slurry solution is 80 ℃, stirs 4 hours;
The venting supernatant liquor adds deionized water, washes 30 minutes, leaves standstill the venting supernatant liquor 2 hours; Add deionized water and stirring again; So repeat to wash four times, until specific conductivity 10～50 μ S/cm of supernatant liquor, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: the weight ratio of water is 1: 1: 1,6 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 300 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 20 hours; Drying temperature: 220 ℃;
The dry powder that drying is good sieves, and 400 orders that sieve can make cathode-ray luminescence material.
Claims (5)
1, a kind of preparation method of cathode-ray luminescence material, it is characterized in that, at first in the terbium yttrium oxide, add the europium sesquioxide that accounts for its terbium yttrium oxide weight percent 6.1-7.0%, the Samarium trioxide of 0.1-0.4%, the sulphur of 40-50%, the yellow soda ash of 50-60%, the Trilithium phosphate of 5-15%, mix, mixing time is 1～3 hour, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, form powder agglomates, calcination temperature is 1100-1300 ℃, time 22-26 hour;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 10～20 hours; All clear liquors of top of draining then; Add deionized water, make powder agglomates and deionized water with 1: 6 weight ratio, stir, churning time is 2～10 hours; Treat the complete sedimentation of powder agglomates, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water once more, the weight ratio of powder slurry and deionized water 1: 6, stir be slurries after, cross 150 ± 50 order nylon mesh, continue then the powder slurry is washed with deionized water, washing times 3～5 times is 9～11 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making in the pickling tank powder slurry solution hydrochloric acid percentage concentration is 2.45～3.68%, and powder slurry solution temperature is 40～80 ℃, stirs 2～4 hours;
The venting supernatant liquor adds deionized water, washes 10～30 minutes, leaves standstill the venting supernatant liquor 1-2 hour; Add deionized water and stirring again; So repeat to wash four times, until specific conductivity 10～50 μ S/cm of supernatant liquor, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: deionized water is by weight=1: 1: 1, and 2～6 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 100～500 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 10-20 hour; Drying temperature: 80～220 ℃;
The dry powder that drying is good sieves, and 300～500 orders that sieve can make cathode-ray luminescence material.
2, the preparation method of a kind of cathode-ray luminescence material according to claim 1, it is characterized in that, at first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.1% europium sesquioxide, 0.4% Samarium trioxide, 50% sulphur, 60% yellow soda ash, 15% Trilithium phosphate, mix, mixing time is 2 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, form powder agglomates, calcination temperature is 1200 ℃, 23 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 10 hours; All clear liquors of top of draining then; Add deionized water, powder agglomates: the weight ratio of water=1: 6, stir, churning time is 2 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water, powder slurry: deionized water weight ratio=1: 6, stir and be slurries, cross 100 order nylon mesh, continuation is washed the powder slurry with deionized water, washing times 3 times is 9 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the percentage concentration of powder slurry solution hydrochloric acid in the pickling tank is 2.45%, and powder slurry solution temperature is 40 ℃, stirs 2 hours;
The venting supernatant liquor adds deionized water, washes 10 minutes, leaves standstill the venting supernatant liquor 1 hour; Add deionized water and stirring again; So repeat to wash four times, until the specific conductivity 10 μ S/cm of supernatant liquor, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: water is by weight=1: 1: 1, and 4 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 100 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 10 hours; Drying temperature: 80 ℃;
The dry powder that drying is good sieves, and 300 orders that sieve can make cathode-ray luminescence material.
3, the preparation method of a kind of cathode-ray luminescence material according to claim 1, it is characterized in that, at first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.5% europium sesquioxide, 0.36% Samarium trioxide, 45% sulphur, 55% yellow soda ash, 10% Trilithium phosphate, mix, mixing time is 2.5 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, form powder agglomates, carry out calcination, the temperature calcination is 1100 ℃, 25 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 15 hours; All clear liquors of top of draining; Add deionized water, powder agglomates: water weight ratio=1: 6, stir, churning time is 8 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water, powder slurry: deionized water weight ratio=1: 6, stir and be slurries, cross 140 order nylon mesh, the powder slurry is washed in continuation, and washing times 4 times is 10 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the percentage concentration of powder slurry solution hydrochloric acid in the pickling tank is 2.68%, and the temperature of powder slurry solution is 50 ℃, stirs 3 hours;
The venting supernatant liquor adds deionized water, washes 15 minutes, leaves standstill the venting supernatant liquor 2 hours; Add deionized water and stirring again; So repeat to wash four times, until specific conductivity 10～50 μ S/cm of supernatant liquor, after the dehydration, remove powder agglomates, powder agglomates is put into ball mill, alumina balls add deionized water, make powder agglomates: ball: water weight ratio=1: 1: 1,4 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 200 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 15 hours; Drying temperature: 100 ℃;
The dry powder that drying is good sieves, and 400 orders that sieve can make cathode-ray luminescence material.
4, the preparation method of a kind of cathode-ray luminescence material according to claim 1, it is characterized in that, at first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.7% europium sesquioxide, 0.32% Samarium trioxide, 55% sulphur, 50% yellow soda ash, 13% Trilithium phosphate, mix, mixing time is 2 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, the temperature calcination is 1300 ℃, 26 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 20 hours; The upper clear supernate of draining; Add deionized water, powder agglomates: water weight ratio=1: 6, stir, churning time is 8 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining keeps bottom powder slurry;
In the powder slurry, add deionized water, powder slurry: water weight ratio=1: 6, stir and be slurries, cross 160 order nylon mesh, the powder slurry is washed in continuation, and washing times 5 times is 11 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the concentration of hydrochloric acid of powder slurry solution in the pickling tank is 3.68%, and the temperature of powder slurry solution is 80 ℃, stirs 4 hours;
The venting supernatant liquor adds deionized water, washes 30 minutes, leaves standstill the venting supernatant liquor 1 hour; Add deionized water and stirring again; So repeat to wash four times,, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: water weight ratio=1: 1: 1,6 hours ball milling time until specific conductivity 10～50 μ S/cm of supernatant liquor;
After ball milling finishes, emit the powder slurry, cross 200 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 20 hours; Drying temperature: 220 ℃;
The dry powder that drying is good sieves, and 500 orders that sieve can make cathode-ray luminescence material.
5, the preparation method of a kind of cathode-ray luminescence material according to claim 1, it is characterized in that, at first in the terbium yttrium oxide, add and account for its terbium yttrium oxide weight percent and be: 6.9% europium sesquioxide, 0.4% Samarium trioxide, 50% sulphur, 60% yellow soda ash, 15% Trilithium phosphate, mix, mixing time is 3 hours, makes raw material;
With the raw material that the mix high purity aluminium oxide crucible of packing into, and cover one deck oxidation inhibitor on the top of raw material, carry out calcination, form powder agglomates, calcination temperature is 1300 ℃, 26 hours time;
Remove after the oxidation inhibitor layer on top, powder agglomates is immersed in the deionized water, soaked 20 hours; All clear liquors of top of draining; Add deionized water, powder agglomates: water weight ratio=1: 6, stir, churning time is 10 hours; Treat the complete sedimentation of powder, the upper clear supernate of draining, the powder that keeps the bottom is starched;
In the powder slurry, add deionized water, powder slurry: the weight ratio of water=1: 6, stir and be slurries, cross 160 order nylon mesh, the powder slurry is washed in continuation, and washing times 5 times is 10 until the pH of supernatant liquor value, till specific conductivity 200 μ S/cm～400 μ S/cm, the powder agglomates of washing is dropped in the pickling tank;
Add hydrochloric acid in pickling tank, making the concentration of hydrochloric acid of powder slurry solution in the pickling tank is 3.68%, and the temperature of powder slurry solution is 80 ℃, stirs 4 hours;
The venting supernatant liquor adds deionized water, washes 30 minutes, leaves standstill the venting supernatant liquor 2 hours; Add deionized water and stirring again; So repeat to wash four times, until specific conductivity 10～50 μ S/cm of supernatant liquor, after the dehydration, take out powder agglomates, powder agglomates is put into ball mill, add alumina balls, add deionized water, make powder agglomates: ball: the weight ratio of water is 1: 1: 1,6 hours ball milling time;
After ball milling finishes, emit the powder slurry, cross 300 mesh sieves, powder agglomates is taken out in dehydration;
With powder drying, time of drying: 20 hours; Drying temperature: 220 ℃;
The dry powder that drying is good sieves, and 400 orders that sieve can make cathode-ray luminescence material.
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|---|---|---|---|
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|---|---|---|---|
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| CN101565618B (en) * | 2009-06-01 | 2012-10-10 | 彩虹集团电子股份有限公司 | Method for preparing red phosphor for CCFL |
| CN112342022A (en) * | 2020-11-19 | 2021-02-09 | 陕西彩虹新材料有限公司 | Method for manufacturing laser display yellow fluorescent powder |
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