CN100562554C - A kind of colorize method of blue cathode-ray luminescence material - Google Patents
A kind of colorize method of blue cathode-ray luminescence material Download PDFInfo
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- CN100562554C CN100562554C CNB2007100188701A CN200710018870A CN100562554C CN 100562554 C CN100562554 C CN 100562554C CN B2007100188701 A CNB2007100188701 A CN B2007100188701A CN 200710018870 A CN200710018870 A CN 200710018870A CN 100562554 C CN100562554 C CN 100562554C
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Abstract
A kind of colorize method of blue cathode-ray luminescence material is with ZnS, AgNO
3, fusing assistant and sulphur mix after the calcination mix with deionization the powder slurry, in the powder slurry, add potash water glass, ZnSO then
4Stir the sedimentation draining, washing, dewater powder agglomates, powder agglomates mixed with glass sphere, deionized water and silicate puts into ball mill ball milling, water elutration, after the standing and drying, the former powder of cathode-ray luminescence material usefulness blue powder; Then the former powder of blue powder is mixed obtaining the powder slurry with water, add cobalt blue dye, acrylic resin in the powder slurry again, use the sulphur acid for adjusting pH value, mix the back after dehydrating again with water and add gelatin, gum arabic, SiO
2And ZnSO
4, transfer pH to arrive with ammoniacal liquor, dehydrating sieves gets final product.After the present invention adopts that the surface treatment of former powder zinc silicate and twice are painted and namely uses earlier the painted drying and screening of latex, re-use gelatin and Arabic gum secondary coloring and Zn (OH)
2Surface treatment, thoroughly eliminate blue powder in use at green powder, blue powder on the graphite and residual on blue powder of rouge and powder.
Description
Technical field
The present invention relates to a kind of colorize method of cathode-ray luminescence material, be specifically related to a kind of colorize method of blue cathode-ray luminescence material.
Background technology
ZnS:Ag (Cl) is as the tricolour picture tube blue emitting 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; ZnS:Ag (Cl) is as blue colour fluorescent powder; for a long time; through regular meeting colour mixture problem (i.e. residual blue powder on green vermicelli appears in use; or on the blue powder bar residual rouge and powder); so that picture tube exists look to pollute, and is insider's question of common concern so take a kind of coloring process thoroughly to eliminate colour mixture always.
Summary of the invention
The purpose of this invention is to provide a kind of colorize method that can thoroughly eliminate the blue cathode-ray luminescence material of mixed color phenomenon.
For achieving the above object, the technical solution used in the present invention is: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.0-2.0%, the activator AgNO of 130ppm-180ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of after 890 ℃ of-960 ℃ of lower calcination 60-90 minutes, removing top after mixing and deionized water mix by 1: 3 mass ratio and 100-300 purpose screen cloth get powder and starch, the quality of pressing then the powder slurry stirs the KP1 that adds 12~20ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 120~200ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 12~16 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 10g~45g/kg by the quality of powder slurry, 1.0 the Acrylic Resin Emulsion of~8.0g/kg, be 2.0-4.5 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 0~2g/kg, the Arabic gum of 0.2g~2g/kg, the SiO of 1g~4g/kg successively again
2And the concentration of 10ml~40ml/kg is the ZnSO of 0.4mol/kg
4, transfer pH to 8.3~8.7 with ammoniacal liquor, dehydration and sieved after under 100~150 ℃ dry 12~24 hours 300 orders, 500 orders or 600 mesh sieves get final product.
The present invention adds ZnSO add KP1 in burning the finished powder slurry after again
4, stir, the sedimentation draining, i.e. former powder zinc silicate surface treatment and twice are painted namely use earlier the painted drying and screening of latex after, re-use gelatin and Arabic gum secondary coloring and Zn (OH)
2Be painted rear adding ZnSO
4, and to transfer with ammoniacal liquor be Zn (OH)
2Surface treatment, thus thoroughly eliminate blue powder in use at green powder, blue powder on the graphite and residual on blue powder of rouge and powder.
Embodiment
Embodiment 1: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.0%, the activator AgNO of 150ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of removing top after 60 minutes 960 ℃ of lower calcinations after mixing and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches, the quality of pressing then the powder slurry stirs the KP1 that adds 18ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 170ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 14 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 45g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 5g/kg, be 3 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, add successively again the Arabic gum of 1.3g/kg, the SiO of 4g/kg by the quality of powder slurry
2With the concentration of 30ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.5 with ammoniacal liquor, dehydration and sieved after under 150 ℃ dry 12 hours 300 orders, 500 orders or 600 mesh sieves get final product.
Embodiment 2: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.6%, the activator AgNO of 170ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of removing top after 80 minutes 920 ℃ of lower calcinations after mixing and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches, the quality of pressing then the powder slurry stirs the KP1 that adds 15ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 130ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 12 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 30g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 1g/kg, be 4 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 1g/kg, the Arabic gum of 0.8g/kg, the SiO of 2g/kg successively again
2With the concentration of 10ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.3 with ammoniacal liquor, dehydration and sieved after under 130 ℃ dry 18 hours 300 orders, 500 orders or 600 mesh sieves get final product.
Embodiment 3: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.3%, the activator AgNO of 130ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of removing top after 90 minutes 890 ℃ of lower calcinations after mixing and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches, the quality of pressing then the powder slurry stirs the KP1 that adds 12ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 200ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 15 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 25g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 3g/kg, be 4.5 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 0.5g/kg, the Arabic gum of 0.2g/kg, the SiO of 1g/kg successively again
2With the concentration of 20ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.7 with ammoniacal liquor, dehydration and sieved after under 110 ℃ dry 20 hours 300 orders, 500 orders or 600 mesh sieves get final product.
Embodiment 4: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 2.0%, the activator AgNO of 180ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of removing top after 70 minutes 940 ℃ of lower calcinations after mixing and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches, the quality of pressing then the powder slurry stirs the KP1 that adds 20ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 120ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 16 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 10g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 8g/kg, be 2 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 2g/kg, the Arabic gum of 2g/kg, the SiO of 3g/kg successively again
2With the concentration of 40ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.4 with ammoniacal liquor, dehydration and sieved after under 100 ℃ dry 24 hours 300 orders, 500 orders or 600 mesh sieves get final product.
Claims (5)
1, a kind of colorize method of blue cathode-ray luminescence material is characterized in that:
1) at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.0-2.0%, the activator AgNO of 130ppm-180ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of after 890 ℃ of-960 ℃ of lower calcination 60-90 minutes, removing top after mixing and deionized water mix by 1: 3 mass ratio and 100-300 purpose screen cloth get powder and starch, the quality of pressing then the powder slurry stirs the KP1 that adds 12~20ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 120~200ml/kg concentration in the powder slurry be the ZnS0 of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 12~16 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder;
2) the former powder of blue powder and water are mixed by 1: 2 mass ratio obtain the powder slurry then, the cobalt blue dye that adds 10g~45g/kg again by the quality of powder slurry successively, 1.0 the acrylic resin latex of~8.0g/kg, with the sulphur acid for adjusting pH value is 2.0-4.5, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 0~2g/kg, the gum arabic of 0.2g~2g/kg, the SiO of 1g~4g/kg successively again
2And the concentration of 10ml~40ml/kg is the ZnSO of 0.4mol/kg
4, transfer pH to 8.3~8.7 with ammoniacal liquor, dehydration and sieved after under 100~150 ℃ dry 12~24 hours 300 orders, 500 orders or 600 mesh sieves get final product.
2, the colorize method of blue cathode-ray luminescence material according to claim 1 is characterized in that: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.0%, the activator AgNO of 150ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of removing top after 60 minutes 960 ℃ of lower calcinations after mixing and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches, the quality of pressing then the powder slurry stirs the KP1 that adds 18ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 170ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 14 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 45g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 5g/kg, be 3 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, add successively again the Arabic gum of 1.3g/kg, the SiO of 4g/kg by the quality of powder slurry
2With the concentration of 30ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.5 with ammoniacal liquor, dehydration and sieved after under 150 ℃ dry 12 hours 300 orders, 500 orders or 600 mesh sieves get final product.
3, the colorize method of blue cathode-ray luminescence material according to claim 1 is characterized in that: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.6%, the activator AgNO of 170ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, removes after 80 minutes that the oxide on top and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches in the burning 920 ℃ under after mixing, the quality of pressing then the powder slurry stirs the KP1 that adds 15ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 130ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 12 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 30g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 1g/kg, be 4 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 1g/kg, the Arabic gum of 0.8g/kg, the SiO of 2g/kg successively again
2With the concentration of 10ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.3 with ammoniacal liquor, dehydration and sieved after under 130 ℃ dry 18 hours 300 orders, 500 orders or 600 mesh sieves get final product.
4, the colorize method of blue cathode-ray luminescence material according to claim 1 is characterized in that: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 1.3%, the activator AgNO of 130ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of removing top after 90 minutes 890 ℃ of lower calcinations after mixing and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches, the quality of pressing then the powder slurry stirs the KP1 that adds 12ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 200ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 15 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 25g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 3g/kg, be 4.5 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 0.5g/kg, the Arabic gum of 0.2g/kg, the SiO of 1g/kg successively again
2With the concentration of 20ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.7 with ammoniacal liquor, dehydration and sieved after under 110 ℃ dry 20 hours 300 orders, 500 orders or 600 mesh sieves get final product.
5, the colorize method of blue cathode-ray luminescence material according to claim 1 is characterized in that: at first with ZnS, AgNO
3, flux and sulphur mixes, mix and add by mass percentage the flux of ZnS quality 2.0%, the activator AgNO of 180ppm take ZnS as matrix
3With 2% sulphur, said flux is: AlCl
3, Al
2(SO
4)
3With the mixture of NaCl, its mass ratio is AlCl
3: Al
2(SO
4)
3: NaCl=868: 378: 154, the oxide of removing top after 70 minutes 940 ℃ of lower calcinations after mixing and deionized water mix by 1: 3 mass ratio and mistake 100-300 purpose screen cloth gets powder and starches, the quality of pressing then the powder slurry stirs the KP1 that adds 20ml/kg in the powder slurry, the quality that starch by powder after 30 minutes at the interval again adds 120ml/kg concentration in the powder slurry be the ZnSO of 0.4mol/L
4, stirred the sedimentation draining 30 minutes, and wash, after the dehydration, powder agglomates is put into ball mill, and take powder agglomates: glass marble: deionized water adds glass marble and deionized water as 1: 1: 0.5 mass ratio, the quality of pressing simultaneously powder agglomates adds the silicate dispersant of 3.0ml/kg, ball milling 16 hours is emitted the powder slurry, water elutration then, after the standing and drying, cross 300~500 mesh sieves and get the cathode-ray luminescence material former powder of blue powder; Then the former powder of blue powder and water are mixed by 1: 2 mass ratio and obtain the powder slurry, the cobalt blue dye that adds successively again 10g/kg by the quality of powder slurry, the Acrylic Resin Emulsion of 8g/kg, be 2 with the sulphur acid for adjusting pH value, dehydrate, cross behind 300 mesh sieves with water by 1: 2 mass ratio mix the powder slurry, the quality by the powder slurry adds the gelatin of 2g/kg, the Arabic gum of 2g/kg, the SiO of 3g/kg successively again
2With the concentration of 40ml/kg be the ZnSO of 0.4mol/kg
4, transfer pH to 8.4 with ammoniacal liquor, dehydration and sieved after under 100 ℃ dry 24 hours 300 orders, 500 orders or 600 mesh sieves get final product.
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