CN110713828A - Sr for luminous ink2MgSi2O7Eu, Dy silicate system hollow luminescent ball and preparation method thereof - Google Patents
Sr for luminous ink2MgSi2O7Eu, Dy silicate system hollow luminescent ball and preparation method thereof Download PDFInfo
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- CN110713828A CN110713828A CN201810782002.9A CN201810782002A CN110713828A CN 110713828 A CN110713828 A CN 110713828A CN 201810782002 A CN201810782002 A CN 201810782002A CN 110713828 A CN110713828 A CN 110713828A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
Abstract
The invention discloses Sr for luminescent ink, belonging to the field of luminescent materials developed from functional materials2MgSi2O7: eu, Dy silicate system hollow luminescent ball and preparation method thereof. Said Sr2MgSi2O7: the raw materials of the Eu, Dy silicate system hollow luminescent ball comprise Sr (NO) in weight ratio3)290 to 100 parts of Mg (NO)3)2·6H2O50-60 parts, Eu2O30.1 to 0.2 part of Dy2O30.1 to 0.2 part of hydrogen peroxide and H3BO32-4 parts of citric acid, 14-16 parts of citric acid, 50-80 parts of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane coupling agent, 50-100 parts of ethyl silicate, 1-10 parts of pollen,100-200 parts of deionized water, 10-30 parts of absolute ethyl alcohol and concentrated HNO31-3 parts. The preparation method comprises the steps of coating a layer of silane coupling agent on rape pollen serving as a template agent, drying, soaking the rape pollen in Sr-Mg-Si-Eu-Dy sol, drying the pollen coated with the sol at a certain temperature, and finally performing heat treatment on a sample to remove the pollen template agent to obtain Sr2MgSi2O7: eu, Dy hollow luminescent ball. The method has simple process and low cost, and the prepared Sr2MgSi2O7: the Eu and Dy luminous hollow sphere is uniform, has few defects, light weight and good luminous performance.
Description
Technical Field
The invention belongs to the field of luminescent materials developed from functional materials, and particularly relates to Sr for luminescent ink2MgSi2O7: a Eu silicate system hollow luminous ball and a preparation method thereof.
Background
Sr2MgSi2O7: the Eu and Dy silicate system luminescent material has the advantages of high chemical stability, high temperature resistance, high luminous brightness and the like, and is considered to be a novel luminescent material which is extremely promising after an aluminate system. The material solves the problems of poor chemical stability, low brightness, single luminous color and the like of the traditional luminescent materials of a sulfide system and an aluminate system, thereby being widely regarded.
Synthesis of Sr by sol-gel method2MgSi2O7: eu and Dy are popular because of the advantages of low synthesis temperature, high product purity, good luminescence property and the like. But Sr is currently produced2MgSi2O7: the Eu and Dy luminescent materials have the defects that the Sr is influenced by the problems of irregular product appearance, serious agglomeration and the like2MgSi2O7: performance of Eu and Dy.
In the luminescent ink, the luminescent material accounts for 50 percent by mass and volume, the cost is high, and if the low-density hollow luminescent material can be prepared, the weight of the luminescent material is reduced, and the cost of the luminescent ink can be reduced. In addition. The large-particle long afterglow material has high luminous brightness, thick printing coating and less printing times, but is easy to settle in the printing ink, easy to break when being stirred and greatly reduced in brightness due to breaking; the small-particle long afterglow luminescent material is smooth in coating and not easy to settle, but the brightness is not high, and the number of times of printing is large, so that the long afterglow luminescent particles with proper size are one of the key points in the luminescent ink, and the particle size of the luminescent material in the luminescent ink is considered to be more proper to be controlled within 50-80 μm.
Therefore, the invention aims to prepare the hollow luminescent ball material with proper size, not only reduces the weight of the luminescent material to achieve the purpose of reducing the cost, but also ensures the luminescent brightness by directly using the luminescent material with proper size without crushing. One of the most effective methods for preparing hollow sphere materials in common use at present is an organic template method, and the types of templates are more, wherein the biological template has the advantages of simplicity, easy obtainment, low cost and the like, and is gradually applied by people.
Disclosure of Invention
Aiming at the problem of high cost caused by high specific gravity of luminescent materials in luminescent ink, the method for preparing the hollow silicate system hollow luminescent ball by using rape pollen as a template agent has the advantages of easy obtainment, low cost, unique and various structure, good appearance repeatability, easy removal, no environmental pollution and the like.
The invention provides Sr for luminescent ink2MgSi2O7: a hollow luminous ball of Eu, Dy silicate system is prepared through coating a layer of silane coupling agent on rape pollen as template agent, drying, immersing in Sr-Mg-Eu-Dy, drying the pollen coated with sol, and heat treating to remove pollen template agent to obtain Sr2MgSi2O7: eu, Dy hollow luminescent ball.
The invention also provides Sr prepared by the method2MgSi2O7: of hollow Eu, Dy luminescent ballsThe process and the process parameters are as follows: soaking rape pollen with the particle size of 50-60 mu m in a 3- (2, 3-epoxypropoxy) propyl trimethoxy silane coupling agent in nitrogen protection for 20-30 min, and drying in an electrothermal blowing drying oven at 50-70 ℃ for 1-2 h; raw material Sr (NO)3)2、Mg(NO3)2·6H2O、Eu2O3、Dy2O3、H3BO3And citric acid and the like are put into an electric heating air blast drying oven to be dried for 5-6 hours at the temperature of 70-80 ℃, and then accurately weighed by an analytical balance according to the set mass. Sr (NO)3)2、Mg(NO3)2·6H2O、H3BO3And citric acid is poured into a beaker, a proper amount of deionized water is poured into the beaker, and the beaker is placed on a 60 ℃ constant temperature magnetic stirrer to be stirred. At the same time make Eu2O3And Dy2O3Dissolved in concentrated HNO3Medium, wait for Eu2O3And Dy2O3After complete dissolution, it was slowly poured into a beaker and stirred together. Adding a proper amount of absolute ethyl alcohol and ethyl silicate after 1-2H, beginning to drop at the speed of 1-2 ml/time, adding absolute ethyl alcohol at the speed of 5 ml/time, and after about 2-3 times, adopting H2SO4Adjusting the pH value to about 2 until the color of the solution becomes clear to prepare transparent Sr-Mg-Si-Eu-Dy sol; adding 1.0-1.5 g of pollen template agent into 100ml of sol, soaking for 1-2 h, drying the pollen coated with the sol for 2-3 h at 80-100 ℃, carrying out heat treatment on the sample for 1-14 h at 500-550 ℃, wherein the temperature is kept at 350 ℃ for 5-10 h to obtain Sr2MgSi2O7: eu, Dy silicate system hollow luminescent ball.
The invention has the characteristics that:
1. simple process and low cost.
2. Silane coupling agent is used as surface modifier and is used as silicon source to replace ethyl silicate as common silicon source material in solvent gel.
3. Prepared Sr2MgSi2O7: the Eu and Dy hollow luminescent sphere has uniform granularity, less defects and high luminescent brightness.
Detailed Description
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
The embodiment of the invention provides Sr for luminescent ink2MgSi2O7: the Eu, Dy silicate system hollow luminescent ball and the preparation method thereof, the method comprises the following steps:
s1: and (3) performing coating silane coupling agent pretreatment on the rape pollen template agent.
Soaking rape pollen with particle size of 56 μm in 3- (2, 3-epoxypropoxy) propyl trimethoxy silane coupling agent under nitrogen protection for 20 min;
drying in an electric heating forced air drying oven at 60 deg.C for 2 hr.
S2: preparing Sr-Mg-Si-Eu-Dy sol.
Raw material Sr (NO)3)2、Mg(NO3)2·6H2O、Eu2O3、Dy2O3、H3BO3Citric acid C6H8O7Drying in an electrothermal blowing drying oven at 80 deg.C for 5 hr;
weigh 0.04mol Sr (NO)3)2、0.02mol Mg(NO3)2·6H2O、20ml HNO3、0.004mol H3BO30.02mol of citric acid C6H8O7、0.00004mol Eu2O3，0.00004mol Dy2O3Is used as a raw material. Sr (NO)3)2、Mg(NO3)2·6H2O、H3BO3Pouring citric acid into a beaker, pouring 100ml of deionized water into the beaker, and placing the beaker on a 60-DEG C constant-temperature magnetic stirrer for stirring;
at the same time make Eu2O3And Dy2O3Dissolved in concentrated HNO3Medium, wait for Eu2O3And Dy2O3After completely dissolving, slowly pouring the mixture into a beaker and stirring the mixture;
after 1h, 25ml of absolute ethyl alcohol and ethyl silicate are addedStarting with 2 ml/time dropwise addition, adding 5 ml/time anhydrous ethanol, about 2 times later, adding 1 mol. L-1H of (A) to (B)2SO4Adjusting the pH value of the solution to about 2 until the color of the solution becomes clear to prepare transparent sol, and aging for later use.
S3: and (4) preparing the hollow luminous ball.
Adding 1.5g of a pretreatment pollen template agent into 100ml of sol, soaking for 1h, and drying the pollen coated with the sol for 2h at 80 ℃;
the sample is thermally treated at 550 ℃ for 12h, wherein the temperature is kept at 350 ℃ for 8h, and Sr with good luminescence property can be obtained2MgSi2O7: eu, Dy silicate system hollow luminescent ball.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. Sr for luminous ink2MgSi2O7: the Eu, Dy silicate system hollow luminescent ball and the preparation method thereof are characterized in that: the raw material formula comprises Sr (NO) in a weight ratio3)290 to 100 parts of Mg (NO)3)2·6H2O50-60 parts, Eu2O30.1 to 0.2 part of Dy2O30.1 to 0.2 part of hydrogen peroxide and H3BO32-4 parts of citric acid, 14-16 parts of citric acid, 50-80 parts of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane coupling agent, 50-100 parts of ethyl silicate, 1-10 parts of pollen, 100-200 parts of deionized water, 10-30 parts of absolute ethyl alcohol, concentrated HNO31-3 parts.
2. Sr for luminous ink2MgSi2O7: eu, Dy silicate system hollow luminescent ball and preparation method thereof, characterized in that, the preparation method is used for preparing claim 1The preparation method of the hollow luminescent ball comprises the steps of coating a layer of silane coupling agent on rape pollen serving as a template agent, drying, soaking the rape pollen in Sr-Mg-Si-Eu-Dy sol, drying the pollen coated with the sol at a certain temperature, and finally, carrying out heat treatment on a sample to remove the pollen template agent to obtain Sr2MgSi2O7: eu, Dy hollow luminescent ball.
3. Sr for luminescent ink according to claim 22MgSi2O7: the Eu and Dy silicate system hollow luminescent ball is characterized by comprising the following steps:
performing coating silane coupling agent pretreatment on the rape pollen template agent;
preparing Sr-Mg-Si-Eu-Dy sol;
dipping the preprocessed rape pollen template agent in Sr-Mg-Si-Eu-Dy sol, drying and carrying out heat treatment to obtain the Sr2MgSi2O7: eu, Dy hollow luminescent ball.
4. Sr for luminescent ink according to claim 32MgSi2O7: the Eu and Dy silicate system hollow luminescent ball and the preparation method thereof are characterized in that in the step of carrying out coating silane coupling agent pretreatment on the rape pollen template agent, the method also comprises the following sub-steps:
rape pollen with the particle size of 50-60 mu m is soaked in a 3- (2, 3-epoxypropoxy) propyl trimethoxy silane coupling agent in nitrogen protection for 20-30 min;
drying in an electrothermal blowing drying oven at 50-70 deg.C for 1-2 hr.
5. Sr for luminescent ink according to claim 32MgSi2O7: the Eu, Dy silicate system hollow luminescent ball and the preparation method thereof are characterized in that in the preparation step of the Sr-Mg-Si-Eu-Dy sol, the preparation method also comprises the following sub-steps:
raw material Sr (NO)3)2、Mg(NO3)2·6H2O、Eu2O3、Dy2O3、H3BO3Drying citric acid and the like in an electric heating air blast drying oven at 70-80 ℃ for 5-6 h, and accurately weighing the dried citric acid and the like by using an analytical balance according to set mass;
sr (NO)3)2、Mg(NO3)2·6H2O、H3BO3Pouring citric acid into a beaker, pouring a proper amount of deionized water into the beaker, and placing the beaker on a 60 ℃ constant-temperature magnetic stirrer for stirring;
at the same time make Eu2O3And Dy2O3Dissolved in concentrated HNO3Medium, wait for Eu2O3And Dy2O3After completely dissolving, slowly pouring the mixture into a beaker and stirring the mixture;
adding a proper amount of absolute ethyl alcohol and ethyl silicate after 1-2H, beginning to drop at the speed of 1-2 ml/time, finally adding absolute ethyl alcohol at the speed of 5 ml/time, and after about 2-3 times, adopting H2SO4Adjusting the pH value to about 2 until the color of the solution becomes clear to prepare transparent Sr-Mg-Si-Eu-Dy sol.
6. Sr for luminescent ink according to claim 32MgSi2O7: the Eu and Dy silicate system hollow luminescent ball is characterized by further comprising the following steps in the preparation step of the hollow luminescent ball:
adding 1.0-1.5 g of the pretreated pollen template agent into 100ml of the sol, soaking for 1-2 h, and drying the pollen coated with the sol for 2-3 h at 80-100 ℃;
heat-treating the sample at 500-550 ℃ for 10-14 h, wherein the sample is kept at 350 ℃ for 5-10 h to obtain Sr2MgSi2O7: eu, Dy silicate system hollow luminescent ball.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114099675A (en) * | 2021-12-02 | 2022-03-01 | 兰州大学 | X-ray excited photodynamic cancer treatment nano composite particle and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114099675A (en) * | 2021-12-02 | 2022-03-01 | 兰州大学 | X-ray excited photodynamic cancer treatment nano composite particle and preparation method thereof |
| CN114099675B (en) * | 2021-12-02 | 2023-08-25 | 兰州大学 | X-ray excited photodynamic cancer treatment nano composite particle and preparation method thereof |
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