Summary of the invention
The technical problems to be solved by the invention: fluorescence cover is prepared for current method, due to fluorescent powder in preparation process
Easily settled, material mixing is uneven, causes manufactured finished product light guide consistency poor, service life is short, the low disadvantage of light transmittance
End, provides a kind of by mixing and ball millings such as calcium carbonate, aluminum oxides, after dry, be sintered, crushed under hydrogen-nitrogen mixture gas
Sieve that CaAlSiN3:Eu3+ fluorescent powder is made is spare, then the stirring such as take ethyl orthosilicate, ethyl alcohol, filtration washing obtains monodisperse dioxy
SiClx, then using monodisperse silica as shell material and spare CaAlSiN3:Eu3+The stirring such as fluorescent powder is centrifuged, dries to be made and divide
The good fluorescent powder with core-shell structure of scattered property, finally by the method for itself and the obtained fluorescence cover of the equal mixed injection moldings of polycarbonate 3028.This hair
Bright preparation step is simple, and fluorescent powder occurs without sedimentation phenomenon in preparation process, and material is uniformly mixed, gained finished product light guide one
Good, the long service life of cause property, light transmittance are high.
In order to solve the above technical problems, the present invention is using technical solution as described below:
(1) 9.0~10.8g calcium carbonate is weighed, 10.2~12.2g aluminum oxide, 6.1~7.2g silica, 3.5~
4.2g europium oxide, 69.6~83.5g graphite and 0.04~0.05g barium chloride, are sequentially loaded into ball grinder, add 30~40mL
Mixture is placed in 70~80 DEG C of drying boxes dry 1~2h with 300~400r/min, 15~30min of ball milling by dehydrated alcohol,
Obtain rare-earth fluorescent ingredient;
(2) above-mentioned rare-earth fluorescent ingredient is fitted into tube furnace, is 0.1~1.0Pa to be evacuated to vacuum degree in furnace, with 100
It is 1:1 hydrogen-nitrogen mixture gas that~200mL/min, which is passed through volume ratio, and is heated to 600~700 DEG C with 20 DEG C/min, then with 10 DEG C/
Min is heated to 1400~1500 DEG C, and after 4~5h of heat preservation sintering, stopping is passed through hydrogen-nitrogen mixture gas, it is made to naturally cool to room
Temperature obtains sintered product, and sintered product is added in pulverizer and is crushed, and crosses 200 meshes, obtains CaAlSiN3:Eu3+Fluorescent powder, it is spare;
(3) 20~24mL ethyl orthosilicate is measured respectively, and 220~240mL ethyl alcohol forms solution, is fitted into beaker, with 300
~400r/min is stirred 10~20min, then adding 250~300mL mass fraction into beaker is 10% ammonium hydroxide, continues to stir
4~5h is mixed, is then filtered, is washed filter residue to cleaning solution with dehydrated alcohol and be in neutrality, obtain monodisperse silica;
(4) the spare CaAlSiN3:Eu3+ fluorescent powder of 1~2g step (2) is weighed, is 90% with 80~100mL mass fraction
Ethanol solution is uniformly mixed, and sequentially adds 8~10g polyethylene glycol, 0.1~0.5g citric acid, with 500~600r/min stirring
1~2h adds the above-mentioned monodisperse silica of 1~2g, continues 3~5h of stirring, then continue in centrifuge, 105~110
It dries at DEG C to constant weight, obtains fluorescent powder with core-shell structure;
(5) 5~8kg polycarbonate 3028 is weighed, is placed in drying box, at 105~110 DEG C after dry 8~10h, dress
Enter in mixing tank, into mixing tank be added the above-mentioned fluorescent powder with core-shell structure of 1~2g, with 300~400r/min premix 30~
40min, then mix with 5~8mL liquid paraffin, and be fitted into 1~2h of mixing in roller mill, then continues in injection molding machine, 280~
It is melted at 300 DEG C, obtains mixture, injected a mixture into injection molding in mold, be cooled to room temperature, demoulded, obtain fluorescence cover.
Application method of the invention: first filling built-in power, reassembles circuit board, to power panel welding electric wire, lamp plate electricity
Source inputs wire bonding, lamp cap welding, and each component is put into fluorescence cover produced by the present invention, internal plug is added, finally by lamp cap and aluminium
Fluorescent tube is made in profile material assembling.Light efficiency loss can be effectively reduced, prevention color temperature shift phenomenon occurs;Through detecting, fluorescence cover of the present invention
Thermal expansion coefficient is 7.0 × 10-5/ DEG C~7.2 × 10-5/ DEG C, optics light efficiency be 230~250lm/W, colour temperature be 2950~
3000K, light transmittance are up to 92.6% or more.
The present invention is compared with other methods, and advantageous effects are:
(1) preparation step of the present invention is simple, and fluorescent powder occurs without sedimentation phenomenon in preparation process, and material is uniformly mixed;
(2) gained finished product light guide consistency is good, and for service life up to 12~15 years, light transmittance was up to 92.6% or more.
Specific embodiment
Weigh 9.0~10.8g calcium carbonate first, 10.2~12.2g aluminum oxide, 6.1~7.2g silica, 3.5
~4.2g europium oxide, 69.6~83.5g graphite and 0.04~0.05g barium chloride, are sequentially loaded into ball grinder, add 30~
40mL dehydrated alcohol, with 300~400r/min, 15~30min of ball milling, mixture is placed in 70~80 DEG C of drying boxes dry 1~
2h obtains rare-earth fluorescent ingredient;Then above-mentioned rare-earth fluorescent ingredient is fitted into tube furnace, to be evacuated in furnace vacuum degree be 0.1~
1.0Pa is passed through volume ratio with 100~200mL/min as 1:1 hydrogen-nitrogen mixture gas, and is heated to 600~700 with 20 DEG C/min
DEG C, then be heated to 1400~1500 DEG C with 10 DEG C/min, after 4~5h of heat preservation sintering, stopping is passed through hydrogen-nitrogen mixture gas, make its from
It is so cooled to room temperature, obtains sintered product, sintered product is added in pulverizer and is crushed, cross 200 meshes, obtain CaAlSiN3:Eu3+
Fluorescent powder, it is spare;20~24mL ethyl orthosilicate is measured respectively, 220~240mL ethyl alcohol forms solution, is fitted into beaker, with
300~400r/min is stirred 10~20min, then adding 250~300mL mass fraction into beaker is 10% ammonium hydroxide, is continued
4~5h is stirred, is then filtered, is washed filter residue to cleaning solution with dehydrated alcohol and be in neutrality, obtain monodisperse silica;1 is weighed again
~2g spare CaAlSiN3:Eu3+ fluorescent powder is uniformly mixed with 80~100mL mass fraction for 90% ethanol solution, then successively
8~10g polyethylene glycol is added, 0.1~0.5g citric acid stirs 1~2h with 500~600r/min, adds the above-mentioned list of 1~2g
Dispersed silicon dioxide continues 3~5h of stirring, then continues in centrifuge, dries at 105~110 DEG C to constant weight, obtains nucleocapsid knot
Structure fluorescent powder;5~8kg polycarbonate 3028 is finally weighed, is placed in drying box, at 105~110 DEG C after dry 8~10h,
Be fitted into mixing tank, into mixing tank be added the above-mentioned fluorescent powder with core-shell structure of 1~2g, with 300~400r/min premix 30~
40min, then mix with 5~8mL liquid paraffin, and be fitted into 1~2h of mixing in roller mill, then continues in injection molding machine, 280~
It is melted at 300 DEG C, obtains mixture, injected a mixture into injection molding in mold, be cooled to room temperature, demoulded, obtain fluorescence cover.
Example 1
9.0g calcium carbonate, 10.2g aluminum oxide, 6.1g silica, 3.5g europium oxide, 69.6g graphite are weighed first
It with 0.04g barium chloride, is sequentially loaded into ball grinder, adds 30mL dehydrated alcohol, with 300r/min ball milling 15min, will mix
Object is placed in 70 DEG C of drying boxes dry 1h, obtains rare-earth fluorescent ingredient;Then above-mentioned rare-earth fluorescent ingredient is fitted into tube furnace, to
It is 0.1Pa that vacuum degree is evacuated in furnace, is passed through volume ratio with 100mL/min as 1:1 hydrogen-nitrogen mixture gas, and with 20 DEG C/min heating
1400 DEG C are heated to 600 DEG C, then with 10 DEG C/min, and after heat preservation sintering 4h, stopping is passed through hydrogen-nitrogen mixture gas, keeps it naturally cold
But to room temperature, sintered product is obtained, sintered product is added in pulverizer and is crushed, 200 meshes is crossed, obtains CaAlSiN3:Eu3+ fluorescence
Powder, it is spare;20mL ethyl orthosilicate is measured respectively, and 220mL ethyl alcohol forms solution, is fitted into beaker, mixed with 300r/min stirring
10min is closed, then adding 250mL mass fraction into beaker is 10% ammonium hydroxide, continues to stir 4h, then filter, washed with dehydrated alcohol
It washs filter residue to cleaning solution to be in neutrality, obtains monodisperse silica;The spare CaAlSiN3:Eu3+ fluorescent powder of 1g is weighed again, with
80mL mass fraction is uniformly mixed for 90% ethanol solution, sequentially adds 8g polyethylene glycol, 0.1g citric acid, with 500r/min
1h is stirred, the above-mentioned monodisperse silica of 1g is added, continues to stir 3h, then continue in centrifuge, dried extremely at 105 DEG C
Constant weight obtains fluorescent powder with core-shell structure;5kg polycarbonate 3028 is finally weighed, is placed in drying box, at 105 DEG C after dry 8h,
Be fitted into mixing tank, into mixing tank be added the above-mentioned fluorescent powder with core-shell structure of 1g, with 300r/min premix 30min, then with 5mL
Liquid paraffin mixing, and it is fitted into mixing 1h in roller mill, it then continues in injection molding machine, is melted at 280 DEG C, obtain mixture, it will
Mixture injects injection molding in mold, is cooled to room temperature, and demoulds, obtains fluorescence cover.
Built-in power is first filled, circuit board is reassembled, electric wire, lamp plate power input wire bonding, lamp cap are welded to power panel
Welding, each component is put into fluorescence cover produced by the present invention, internal plug is added, and finally assembles lamp cap and aluminum profile and fluorescent tube is made.
Light efficiency loss can be effectively reduced, prevention color temperature shift phenomenon occurs;Through detecting, fluorescence cover thermal expansion coefficient of the present invention be 7.0 ×
10-5/ DEG C, optics light efficiency is 230lm/W, colour temperature 2950K, and light transmittance is up to 92.69%.
Example 2
9.9g calcium carbonate, 11.2g aluminum oxide, 6.6g silica, 3.9g europium oxide, 76.2g graphite are weighed first
It with 0.05g barium chloride, is sequentially loaded into ball grinder, adds 35mL dehydrated alcohol, with 350r/min ball milling 22min, will mix
Object is placed in 75 DEG C of drying boxes dry 2h, obtains rare-earth fluorescent ingredient;Then above-mentioned rare-earth fluorescent ingredient is fitted into tube furnace, to
It is 0.6Pa that vacuum degree is evacuated in furnace, is passed through volume ratio with 150mL/min as 1:1 hydrogen-nitrogen mixture gas, and with 20 DEG C/min heating
1450 DEG C are heated to 650 DEG C, then with 10 DEG C/min, and after heat preservation sintering 5h, stopping is passed through hydrogen-nitrogen mixture gas, keeps it naturally cold
But to room temperature, sintered product is obtained, sintered product is added in pulverizer and is crushed, 200 meshes is crossed, obtains CaAlSiN3:Eu3+Fluorescence
Powder, it is spare;22mL ethyl orthosilicate is measured respectively, and 230mL ethyl alcohol forms solution, is fitted into beaker, mixed with 350r/min stirring
15min is closed, then adding 275mL mass fraction into beaker is 10% ammonium hydroxide, continues to stir 5h, then filter, washed with dehydrated alcohol
It washs filter residue to cleaning solution to be in neutrality, obtains monodisperse silica;The spare CaAlSiN3:Eu3+ fluorescent powder of 2g is weighed again, with
90mL mass fraction is uniformly mixed for 90% ethanol solution, sequentially adds 9g polyethylene glycol, 0.3g citric acid, with 550r/min
2h is stirred, the above-mentioned monodisperse silica of 2g is added, continues to stir 4h, then continue in centrifuge, dried extremely at 108 DEG C
Constant weight obtains fluorescent powder with core-shell structure;7kg polycarbonate 3028 is finally weighed, is placed in drying box, at 108 DEG C after dry 9h,
Be fitted into mixing tank, into mixing tank be added the above-mentioned fluorescent powder with core-shell structure of 2g, with 350r/min premix 35min, then with 7mL
Liquid paraffin mixing, and it is fitted into mixing 2h in roller mill, it then continues in injection molding machine, is melted at 290 DEG C, obtain mixture, it will
Mixture injects injection molding in mold, is cooled to room temperature, and demoulds, obtains fluorescence cover.
Built-in power is first filled, circuit board is reassembled, electric wire, lamp plate power input wire bonding, lamp cap are welded to power panel
Welding, each component is put into fluorescence cover produced by the present invention, internal plug is added, and finally assembles lamp cap and aluminum profile and fluorescent tube is made.
Light efficiency loss can be effectively reduced, prevention color temperature shift phenomenon occurs;Through detecting, fluorescence cover thermal expansion coefficient of the present invention be 7.1 ×
10-5/ DEG C, optics light efficiency is 240lm/W, colour temperature 2975K, and light transmittance is up to 92.81%.
Example 3
10.8g calcium carbonate, 12.2g aluminum oxide, 7.2g silica, 4.2g europium oxide, 83.5g graphite are weighed first
It with 0.05g barium chloride, is sequentially loaded into ball grinder, adds 40mL dehydrated alcohol, with 400r/min ball milling 30min, will mix
Object is placed in 80 DEG C of drying boxes dry 2h, obtains rare-earth fluorescent ingredient;Then above-mentioned rare-earth fluorescent ingredient is fitted into tube furnace, to
It is 1.0Pa that vacuum degree is evacuated in furnace, is passed through volume ratio with 200mL/min as 1:1 hydrogen-nitrogen mixture gas, and with 20 DEG C/min heating
1500 DEG C are heated to 700 DEG C, then with 10 DEG C/min, and after heat preservation sintering 5h, stopping is passed through hydrogen-nitrogen mixture gas, keeps it naturally cold
But to room temperature, sintered product is obtained, sintered product is added in pulverizer and is crushed, 200 meshes is crossed, obtains CaAlSiN3:Eu3+ fluorescence
Powder, it is spare;24mL ethyl orthosilicate is measured respectively, and 240mL ethyl alcohol forms solution, is fitted into beaker, mixed with 400r/min stirring
20min is closed, then adding 300mL mass fraction into beaker is 10% ammonium hydroxide, continues to stir 5h, then filter, washed with dehydrated alcohol
It washs filter residue to cleaning solution to be in neutrality, obtains monodisperse silica;The spare CaAlSiN3:Eu3+ fluorescent powder of 2g is weighed again, with
100mL mass fraction is uniformly mixed for 90% ethanol solution, sequentially adds 10g polyethylene glycol, 0.5g citric acid, with 600r/
Min stirs 2h, adds the above-mentioned monodisperse silica of 2g, continues to stir 5h, then continue in centrifuge, does at 110 DEG C
It is dry to constant weight, obtain fluorescent powder with core-shell structure;8kg polycarbonate 3028 is finally weighed, is placed in drying box, it is dry at 110 DEG C
It after 10h, is fitted into mixing tank, the above-mentioned fluorescent powder with core-shell structure of 2g is added into mixing tank, with 400r/min premix 40min,
It is mixed again with 8mL liquid paraffin, and is fitted into mixing 2h in roller mill, then continued in injection molding machine, melted at 300 DEG C, obtained mixed
Material is closed, injection molding in mold is injected a mixture into, is cooled to room temperature, demoulds, obtains fluorescence cover.
Built-in power is first filled, circuit board is reassembled, electric wire, lamp plate power input wire bonding, lamp cap are welded to power panel
Welding, each component is put into fluorescence cover produced by the present invention, internal plug is added, and finally assembles lamp cap and aluminum profile and fluorescent tube is made.
Light efficiency loss can be effectively reduced, prevention color temperature shift phenomenon occurs;Through detecting, fluorescence cover thermal expansion coefficient of the present invention be 7.2 ×
10-5/ DEG C, optics light efficiency is 250lm/W, colour temperature 3000K, and light transmittance is up to 93.18%.