CN106010529B - A kind of artificial schellite red fluorescence powder for adulterating manganese ion and preparation method thereof - Google Patents
A kind of artificial schellite red fluorescence powder for adulterating manganese ion and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of artificial schellite red fluorescence powder for adulterating manganese ion and preparation method thereof, chemical composition Ca1‑ xLa2WO7:xMn2+；Wherein, x takes 0.005~0.20, is made as follows：Step S1, by Ca1‑xLa2WO7:xMn2+Stoichiometric proportion weigh the mixture of oxide spinel calcium, lanthana, ammonium tungstate and manganese dioxide；Step S2, add fluxing agent and be ground, be ground to obtain mixture；Step S3, the mixture that step S2 is obtained load crucible, are sintered 4~6 hours under the conditions of reducing atmosphere and 1400~1600 DEG C in high temperature furnace, cool down and produce；Wherein, the addition of fluxing agent is the 0.7~0.9% of raw material weight, and the fluxing agent is the mixture of sodium acid carbonate and vulcanized sodium, and the weight ratio of sodium acid carbonate and vulcanized sodium is 6~8:1.The artificial schellite red fluorescence powder good dispersion of doping manganese ion provided by the invention, luminous intensity is high, and stability is high, and these advantages are relevant with sodium acid carbonate in fluxing agent and vulcanized sodium weight ratio, and the weight ratio of sodium acid carbonate and vulcanized sodium is 6~8:When 1, luminous intensity highest.
Description
Technical field
The invention belongs to field of light emitting materials, and in particular to a kind of artificial schellite red fluorescence powder and its system for adulterating manganese ion
Preparation Method.
Background technology
Obtained some colour rendering indexs of white light LEDs are low at present, and colour temperature is high, colder white light, be primarily due to lack feux rouges into
Point, therefore it is critically important to develop efficient red fluorescence powder.The rouge and powder used at present is mainly (Ca1-x, Srx) and S:Mn2+System,
Broadband excitation in blue region, broadband emission in red range, because its property is not sufficiently stable, environmental pollution when simultaneously synthesizing
It is very big, eventually it is eliminated.Nitride or the improvement of nitrogen oxides red light material colour temperature are fairly obvious, but the conjunction of this kind of fluorescent material
Into high temperature (1600~1800 DEG C), high pressure is needed, synthesis condition is more harsh, synthesizes high energy consumption.At present using more, effect compared with
The red fluorescence powder for getting well and reaching business application is mainly Y2O3:Mn3+, (Y, Gd) BO3:Mn3+And binary alkaline earth sulfide
MS：Mn2+(M=Ca, Ca, Sr, Ba), their fluorescence quantum efficiencies in similar fluorescent material are higher.But these rouge and powder are in reality
Some problems are remained in the application of border, as luminous efficiency is low, stability is not good enough, and particle is not thin etc. enough.
Tungstates is typical self-activating luminescent material, and luminescent spectrum is sufficiently stable, and intrinsic photoluminescent band is very wide, occupies
The major part of visible region, the cation in tungstates consumingly influence the position of transmitting band.Tungstates can be by some miscellaneous
Matter activates, and after these impurity are impregnated in tungstates dot matrix, can make it have the luminous of special nature.
The content of the invention
It is an object of the invention to provide a kind of artificial schellite red fluorescence powder for adulterating manganese ion and preparation method thereof.
The above-mentioned purpose of the present invention is achieved by following technical scheme：
A kind of artificial schellite red fluorescence powder for adulterating manganese ion, its chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x takes
It is worth for 0.005~0.20, is made by the steps and forms：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.005~0.20；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1400~1600 in high temperature furnace
Sintered 4~6 hours under the conditions of DEG C, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.7~0.9% of raw material weight, and the fluxing agent is sodium acid carbonate and vulcanization
The weight ratio of the mixture of sodium, sodium acid carbonate and vulcanized sodium is 6~8:1.
Further, described artificial schellite red fluorescence powder, its chemical composition are Ca1-xLa2WO7:xMn2+；Wherein, x takes
It is worth for 0.10, is made by the steps and forms：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.10；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1500 DEG C of conditions in high temperature furnace
Lower sintering 5 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.8% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 7:1.
Further, described artificial schellite red fluorescence powder, its chemical composition are Ca1-xLa2WO7:xMn2+；Wherein, x takes
It is worth for 0.005, is made by the steps and forms：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.005；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1400 DEG C of conditions in high temperature furnace
Lower sintering 6 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.7% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 6:1.
Further, described artificial schellite red fluorescence powder, its chemical composition are Ca1-xLa2WO7:xMn2+；Wherein, x takes
It is worth for 0.20, is made by the steps and forms：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.20；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1600 DEG C of conditions in high temperature furnace
Lower sintering 4 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.9% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 8:1.
Further, the reducing atmosphere is Carbon monoxide reduction atmosphere.
Advantages of the present invention：
Artificial schellite red fluorescence powder good dispersion provided by the invention, luminous intensity is high, and stability is high, and these advantages are with helping
Sodium acid carbonate is relevant with vulcanized sodium weight ratio in flux, and the weight ratio of sodium acid carbonate and vulcanized sodium is 6~8:When 1, luminous intensity
Highest.
Embodiment
The essentiality content of the present invention is further illustrated with reference to embodiment, but present invention protection model is not limited with this
Enclose.Although being explained in detail with reference to preferred embodiment to the present invention, it will be understood by those within the art that, can be right
Technical scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention.
Embodiment 1：Adulterate the preparation of the artificial schellite red fluorescence powder of manganese ion
Chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x values are 0.10, are made by the steps and form：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.10；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1500 DEG C of conditions in high temperature furnace
Lower sintering 5 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.8% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 7:1.
Embodiment 2：Adulterate the preparation of the artificial schellite red fluorescence powder of manganese ion
Chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x values are 0.005, are made by the steps and form：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.005；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1400 DEG C of conditions in high temperature furnace
Lower sintering 6 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.7% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 6:1.
Embodiment 3：Adulterate the preparation of the artificial schellite red fluorescence powder of manganese ion
Chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x values are 0.20, are made by the steps and form：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.20；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1600 DEG C of conditions in high temperature furnace
Lower sintering 4 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.9% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 8:1.
Embodiment 4：Adulterate the preparation of the artificial schellite red fluorescence powder of manganese ion
Chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x values are 0.10, are made by the steps and form：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.10；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1500 DEG C of conditions in high temperature furnace
Lower sintering 5 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.8% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 6:1.
Embodiment 5：Adulterate the preparation of the artificial schellite red fluorescence powder of manganese ion
Chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x values are 0.10, are made by the steps and form：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.10；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1500 DEG C of conditions in high temperature furnace
Lower sintering 5 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.8% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 8:1.
Embodiment 6：The weight ratio of comparative example, sodium acid carbonate and vulcanized sodium is 5:1
Chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x values are 0.10, are made by the steps and form：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.10；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1500 DEG C of conditions in high temperature furnace
Lower sintering 5 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.8% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 5:1.
Embodiment 7：The weight ratio of comparative example, sodium acid carbonate and vulcanized sodium is 9:1
Chemical composition is Ca1-xLa2WO7:xMn2+；Wherein, x values are 0.10, are made by the steps and form：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is carbonic acid
Calcium, lanthana, the mixture of ammonium tungstate and manganese dioxide, wherein, x values are 0.10；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1500 DEG C of conditions in high temperature furnace
Lower sintering 5 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.8% of raw material weight, and the fluxing agent is the mixed of sodium acid carbonate and vulcanized sodium
The weight ratio of compound, sodium acid carbonate and vulcanized sodium is 9:1.
Embodiment 8：Effect example
The luminescent properties of fluorescent material prepared by testing example 1~7 respectively, different embodiment fluorescent material are excited and launched
The position of spectrum is basically identical, but luminous intensity, stability of photoluminescence and dispersiveness have relatively big difference, as a result such as table 1.Wherein, send out
Luminous intensity is set to 100 on the basis of embodiment 1, and remaining embodiment is the relative luminous intensity relative to embodiment 1.
The luminescent properties and dispersiveness of the different embodiment fluorescent material of table 1
| Luminous intensity | Stability of photoluminescence | Dispersiveness | |
| Embodiment 1 | 100 | It is highly stable | Dispersiveness is very good |
| Embodiment 4 | 99 | It is relatively stable | It is dispersed preferable |
| Embodiment 5 | 98 | It is relatively stable | It is dispersed preferable |
| Embodiment 6 | 63 | It is unstable | Poor dispersion |
| Embodiment 7 | 64 | It is unstable | Poor dispersion |
The test result and embodiment 4,5 of embodiment 2,3 are basically identical.
It is above-mentioned test result indicates that, it is provided by the invention doping manganese ion artificial schellite red fluorescence powder good dispersion, hair
Luminous intensity is high, and stability is high, and these advantages are relevant with sodium acid carbonate in fluxing agent and vulcanized sodium weight ratio, sodium acid carbonate and vulcanization
The weight ratio of sodium is 6~8:When 1, luminous intensity highest.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but the protection of the present invention is not limited with this
Scope.It will be understood by those within the art that technical scheme can be modified or equivalent substitution,
Without departing from the essence and protection domain of technical solution of the present invention.
Claims (5)
1. a kind of preparation method for the artificial schellite red fluorescence powder for adulterating manganese ion, the chemical composition of the fluorescent material is Ca1- xLa2WO7:xMn2+；Wherein, x values are 0.005~0.20, it is characterised in that are comprised the following steps：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is calcium carbonate, oxidation
The mixture of lanthanum, ammonium tungstate and manganese dioxide, wherein, x values are 0.005~0.20；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained loads crucible, in reducing atmosphere and 1400~1600 DEG C of bars in high temperature furnace
Sintered 4~6 hours under part, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.7~0.9% of raw material weight, and the fluxing agent is sodium acid carbonate and vulcanized sodium
The weight ratio of mixture, sodium acid carbonate and vulcanized sodium is 6~8:1.
2. preparation method according to claim 1, the chemical composition of the fluorescent material is Ca1-xLa2WO7:xMn2+；Wherein, x
Value is 0.10, it is characterised in that is comprised the following steps：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is calcium carbonate, oxidation
The mixture of lanthanum, ammonium tungstate and manganese dioxide, wherein, x values are 0.10；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained load crucible, burnt in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Knot 5 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.8% of raw material weight, and the fluxing agent is the mixing of sodium acid carbonate and vulcanized sodium
The weight ratio of thing, sodium acid carbonate and vulcanized sodium is 7:1.
3. preparation method according to claim 1, the chemical composition of the fluorescent material is Ca1-xLa2WO7:xMn2+；Wherein, x
Value is 0.005, it is characterised in that is comprised the following steps：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is calcium carbonate, oxidation
The mixture of lanthanum, ammonium tungstate and manganese dioxide, wherein, x values are 0.005；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained load crucible, burnt in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Knot 6 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.7% of raw material weight, and the fluxing agent is the mixing of sodium acid carbonate and vulcanized sodium
The weight ratio of thing, sodium acid carbonate and vulcanized sodium is 6:1.
4. preparation method according to claim 1, the chemical composition of the fluorescent material is Ca1-xLa2WO7:xMn2+；Wherein, x
Value is 0.20, it is characterised in that is comprised the following steps：
Step S1, by chemical composition Ca1-xLa2WO7:xMn2+Stoichiometric proportion weigh raw material, the raw material is calcium carbonate, oxidation
The mixture of lanthanum, ammonium tungstate and manganese dioxide, wherein, x values are 0.20；
Step S2, add fluxing agent and be ground, be ground to obtain mixture；
Step S3, the mixture that step S2 is obtained load crucible, burnt in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Knot 4 hours, cool down the artificial schellite red fluorescence powder for producing the doping manganese ion；
Wherein, the addition of fluxing agent is the 0.9% of raw material weight, and the fluxing agent is the mixing of sodium acid carbonate and vulcanized sodium
The weight ratio of thing, sodium acid carbonate and vulcanized sodium is 8:1.
5. according to any described preparation method of Claims 1 to 4, it is characterised in that：The reducing atmosphere be carbon monoxide also
Primordial Qi atmosphere.
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2016
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| CN104804738A (en) * | 2015-05-18 | 2015-07-29 | 厦门砺德光电科技有限公司 | Near-ultraviolet-excited white-light LED (light-emitting diode) fluorescent powder and preparation method thereof |
| CN105199728A (en) * | 2015-06-01 | 2015-12-30 | 井冈山大学 | Novel Eu<3+> and Mn<2+> co-doped tungstate red fluorescent material and preparation method thereof |
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| Enhancement of luminescence properties via the substitution of Ba2+ by Sr2+ and Ca2+ in the white phosphors Ba1-yMyLa2-xWO7:xDy3+ (M=Sr, Ca)(x=0.01–0.4, y=0–0.4);Shao-An Yan et al.;《Journal of Luminescence》;20120307;1867-1872 * |
| Synthesis and luminescence properties of Ln3+ (Ln3+ = Er3+, Sm3+)-doped barium lanthanum tungstate BaLa2WO7 phosphors;Shao-An Yan et al.;《Optical Materials》;20110823;147-151 * |
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