CN113061432A - Preparation method and application of high-stability multifunctional whitlockite type fluorescent powder - Google Patents
Preparation method and application of high-stability multifunctional whitlockite type fluorescent powder Download PDFInfo
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- CN113061432A CN113061432A CN202110367103.1A CN202110367103A CN113061432A CN 113061432 A CN113061432 A CN 113061432A CN 202110367103 A CN202110367103 A CN 202110367103A CN 113061432 A CN113061432 A CN 113061432A
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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
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
- C09K11/7723—Phosphates
- C09K11/7724—Phosphates with alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M3/00—Printing processes to produce particular kinds of printed work, e.g. patterns
- B41M3/14—Security printing
- B41M3/144—Security printing using fluorescent, luminescent or iridescent effects
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- 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
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Abstract
The invention discloses a preparation method and application of high-stability multifunctional whitlockite fluorescent powder, wherein the chemical formula is (Ca)0.5Sr0.5)3‑yM0.07(PO4)2:0.07Ce3+,yMn2+Y is 0,0.01,0.03,0.05,0.07,0.09,0.11, and M is an alkali metal. The invention has good thermal stability and chemical stability, realizes spectrum excitation color development of 550-720nm red light and 720-900nm near-infrared light, can be tuned from purple to red, can be prepared into anti-counterfeiting ink excited by specific wavelength, and can display potential anti-counterfeiting patterns, printing of mobile phone quick response two-dimensional codes, near-infrared biological application and field emissionAnd the application prospect is good.
Description
Technical Field
The invention belongs to the technical field of fluorescent powder preparation, and particularly relates to a preparation method and application of high-stability multifunctional whitlockite fluorescent powder.
Background
Human perception of the luminescence of materials begins with the luminescence of natural minerals. The mineral luminescent materials can be divided into two categories: firstly, natural mineral luminescent material; the second is artificially synthesized luminescent material with mineral structure. The natural mineral usually contains rare earth quencher ions, and the luminescent performance of the natural mineral is greatly restricted by components and structures of the natural mineral, so the luminescent performance is generally poor. However, the material can be artificially synthesized to control the raw material, so that a mineral luminescent material with excellent performance can be obtained, and the material is widely applied to Light Emitting Diodes (LEDs), such as apatite type, pyroxene type, whitlockite type, yttrium aluminum garnet type luminescent materials, and the like. The mineral materials are widely used for White Light Emitting Diodes (WLEDs) such as apatite type, pyroxene type, limonite type and yttrium aluminum garnet type luminescent materials. Yellow light-emitting aluminate phosphor Y based on mineral prototypes3Al5O12：Ce3+Have been commercialized in WLED devices. Unfortunately, modern commercial phosphors still suffer from several recognized problems. For example, for a commercial combination of blue-colored and yellow-emitting phosphors, the absence of a red component in the emission spectrum may result in a lower color rendering index (Ra)<75) Higher color temperature (CCT)>4500K) Energy loss (>20%), color re-absorption and blue light hazards that may damage the retina and brain. These unacceptable fatal drawbacks indicate that red phosphor, an important component of WLED, still leaves much room for improvement to achieve healthy, efficient illumination levels. Much of the previous work has explored the use of red phosphors to improve the illumination quality of WLEDs. It includes the most widely used red nitride phosphor, CaAlSiN3：Eu2+And Sr2Si5N8：Eu2+. Although these phosphors achieve high quantum yields (IQE), the harsh synthesis conditions (high temperature and pressure) and deep red emission limit their large scale application in warm white light production. Moreover, spectral overlap is still an insurmountable threshold. Up to now, red-emitting Mn due to high IQE in blue4+Doped fluoride phosphors have attracted a great deal of attention. However, they also have two serious drawbacks: low Thermal Stability (TS) and use of large amounts of HFAnd (4) acid. Therefore, the development of high-quality red phosphor is still a challenge, and the design is needed.
In addition, no doubt, information security, health care and illumination display are the first major matters of the current society, and exploring how to apply the theoretical research of the fluorescent powder to the application of the fluorescent powder is the most critical innovation direction in the future. However, the research on the development of multifunctional application programs is still deficient at present, but some inventions have made fluorescent powder into anti-counterfeiting ink for anti-counterfeiting printing, but the excitation range of the anti-counterfeiting ink covers the visible light region or the ultraviolet excitation range is wider, so that the anti-counterfeiting and information security protection effects cannot be well embodied. Therefore, if the fluorescent powder with good chemical stability and color stability developed by the patent is made into anti-counterfeiting ink and is applied to printing anti-counterfeiting patterns and encrypted information, the excitation only at specific wavelengths (short-wave ultraviolet light and near ultraviolet light) can be realized. In particular, the current COVID-19 is subject to rapid information security technology in combination with phosphor anti-counterfeiting inks, which makes the health status and audit trails more stringent and rapid.
Disclosure of Invention
The invention provides a preparation method and application of high-stability multifunctional whitlockite fluorescent powder.
The invention comprises the following steps:
the chemical formula of the high-stability multifunctional whitlockite fluorescent powder is (Ca)0.5Sr0.5)3-yM0.07(PO4)2:0.07Ce3+,yMn2+Y is 0,0.01,0.03,0.05,0.07,0.09,0.11, and M is an alkali metal.
Further, the alkali metal is one or more of Li, Na and K.
Further, the present invention comprises the steps of: in the matrix material beta-Ca3(PO4)2Adding sodium ion-containing compound (0.07mol) and Sr cation-containing compound SrCO3According to Ca2+:Sr2+The mol ratio is 1:1, and the high-stability multifunctional whitlockite is obtained by high-temperature solid phase synthesisA fluorescent powder.
Further, CaCO3、SrCO3、(NH4)2HPO4、Na2CO3、CeO2And MnCO3Preheating at 850 deg.C for 1h, and releasing NH in a muffle furnace in air3、H2O and CO2. After regrinding, at 5% H2、55％N2Is placed in a tube furnace and sintered for 10 hours at 1250 ℃. Slowly cooling to room temperature, and grinding into fine powder to obtain the high-stability multifunctional whitlockite type fluorescent powder.
Further, the compound containing sodium ions is one or more of sodium hydroxide, sodium carbonate and sodium bicarbonate; the compound containing Sr cation is one or more of strontium hydroxide, strontium carbonate or strontium bicarbonate.
Further, the high-stability multifunctional whitlockite type fluorescent powder is excited by one or more of ultraviolet light and near ultraviolet light to obtain the high-stability multifunctional whitlockite type fluorescent powder.
An application of high-stability multifunctional whitlockite fluorescent powder in anti-counterfeiting marks,
the invention has the beneficial effects that:
the invention has good thermal stability and chemical stability, realizes the spectrum excitation color development of 550-720nm red light and 720-900nm near-infrared light, can be tuned to red from purple, and has potential application prospect in near-infrared application and field emission display.
Drawings
Fig. 1 shows CNP with standard PDF cards according to the present invention: an XRD spectrum diagram of the Ce, yMn fluorescent powder;
fig. 2 shows a CNP of the present invention: a spectrum schematic diagram of a high-temperature XRD (X-ray diffraction) spectrum of Ce, 0.07Mn fluorescent powder at 25 ℃, 50 ℃, 100 ℃, 150 ℃, 200 ℃, 400 ℃, 600 ℃, 800 ℃ and 1000 ℃;
fig. 3 shows a CNP of the present invention: excitation (PL) and emission (PLE) spectra of Ce, 0.07Mn phosphor,
fig. 4 shows a CNP of the present invention: a CIE chromaticity coordinate diagram of Ce, 0.07Mn fluorescent powder, a tuning spectrum diagram of multifunctional whitlockite fluorescent powder with the color from purple to high stability;
fig. 5 shows a CNP of the present invention: ce, yMn (y ═ 0.07) phosphor shows decay profile at continuous I ═ 80mA, Va ═ 8 kV.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
As shown in fig. 1, the present embodiment includes the following steps:
in this example, CaCO was used as the raw material3(≥99.9％)、SrCO3(≥99.9％)、(NH4)2HPO4(≥99.9％)、Na2CO3(99.9％)、CeO2(≧ 99.99%) and MnCO3(99.99%) in the matrix material beta-Ca3(PO4)2Adding a compound containing sodium ions (0.07mol) and a compound containing Sr cations according to Ca2+:Sr2+The mixture is weighed according to the stoichiometric ratio and mixed in an agate mortar, and the mixture is thoroughly ground for 30 minutes. Placing the mixture in a corundum crucible, preheating at 850 deg.C for 1h, and releasing NH in a muffle furnace in air3、H2O and CO2. After regrinding, at 5% H2、55％N2Is placed in a tube furnace and sintered for 10 hours at 1250 ℃. After slowly cooling to room temperature, the product was ground into a fine powder for subsequent characterization.
Fig. 1 CNP with standard PDF cards attached: an XRD (X-ray diffraction) spectrum of the Ce, yMn fluorescent powder proves that the fluorescent powder is a single-phase whitlockite type mineral.
The fluorescent powder has good chemical stability and thermal stability, CL maintains 86.19 percent and 82.30 percent of initial strength after continuous electron radiation for 60min and 90min, and the fluorescent powder has potential application prospects in near infrared and FED. More importantly, the patent also combines a screen printing process to realize two application strategies of a dynamic two-dimensional code for epidemic prevention and an anti-counterfeiting pattern excited by near ultraviolet, which are combined with an information security technology.
In the synthesis and preparation of the fluorescent powder, the CNP: the XRD pattern of Ce, yMn, all well matched to the parent phase beta-Ca3(PO4)2(R3c), Powder Diffraction File (PDF) card number No. 09-0169, indicating that the synthesized sample was a single phase. Good thermal stability is a prerequisite for fluorescent powders to explore CNP: whether the structure of the Ce, yMn fluorescent powder is still stable under high temperature condition or not is determined by selecting CNP: ce, 0.07Mn, XRD patterns were recorded using high temperature X-ray diffraction techniques. Even if the temperature rises to 1000 degrees celsius, CNP: the single phase of the Ce, yMn phosphor did not change, but the position of the diffraction peak was slightly shifted to a small angle, further demonstrating that the stability of the phosphor structure may be responsible for good thermal stability. In addition, the fluorescent powder is tried to be dissolved in common aqueous solution, weak acid and organic solution such as DM, acetone and the like, the fluorescent powder cannot be dissolved in the solution, and the solution is filtered and tested for XPS, so that the signal of elements in the fluorescent powder cannot be detected, and the obtained fluorescent powder is proved to be capable of effectively resisting the corrosion of the weak acid and the organic solution and has good chemical stability.
CNP: the emission spectrum (PL) of a Ce, yMn sample under the excitation of near ultraviolet light 310nm is in two-peak broadband emission, the main peaks are 366nm and 636nm, wherein, the 366nm emission peak is from a Ce3+ center, and the energy transfer of the Ce3+ center enhances the 636nm orange-red emission of Mn2 +. The concentration of Ce3+ ions was fixed at 0.07, and as the concentration of Mn2+ was increased (y was 0,0.01,0.03,0.07,0.11), the intensity of the emission peak centered at 366nm gradually decreased, and the intensity of the emission peak centered at 636nm increased in order, and the color of the phosphor gradually changed from blue to red. But CNP when y is 0.11: ce, yMn concentration quenching occurred at 636nm peak intensity.
As shown in fig. 2, CNP: the high-temperature XRD pattern of Ce, 0.07Mn fluorescent powder at 25 deg.C, 50 deg.C, 100 deg.C, 150 deg.C, 200 deg.C, 400 deg.C, 600 deg.C, 800 deg.C and 1000 deg.C shows that the fluorescent powder has good thermal stability.
The experimental facts prove that the excitation energy can be effectively transferred to Mn2+ ions after being absorbed by Ce3+, and an energy transfer process exists between Ce3+ and Mn2 +. In addition, CNP was found preliminarily: ce, yMn has a near-infrared emission peak at 720nm-890nm, suggesting potential multifunctional applications in near-infrared near-LED bio-penetration, imaging, thermometry, and sensing.
As shown in fig. 3, CNP: the excitation (PL) and emission (PLE) spectra of the Ce, 0.07Mn phosphor showed the emission of 310-500nm near ultraviolet-blue violet light, 550-720nm red light, and 720-900nm near infrared light. SEM (scanning Electron microscope) and corresponding CL (electroluminescent Spectroscopy) mapping images show that the samples exhibit uniform emission, confirming that Ce3+、Mn2+The ions are uniformly distributed in the sample. As the probe current and acceleration voltage increased, the CL intensity gradually increased and no saturation effect was found, indicating that it was more effective for the application of FEDs. Compared with PL, the spectrum shape and the peak position have no obvious change, and two broadband points are shown at 370nm and 620nm and belong to Ce respectively3+And Mn2+The transmission band of light. The intensity of the two CL peaks is gradually reduced along with the increase of the bombardment time, the initial intensity is respectively maintained at 86.19 percent and 82.63 percent after continuous electron irradiation for 60min, and the initial intensity is respectively maintained at 82.30 percent and 81.61 percent after 90min, which are respectively superior to that of the commercial red phosphor Y2O3：Eu3+And Y2O2S：0.05Eu3+Under the same conditions, only 83 percent and 80 percent of strength values are remained, and the good ageing resistance is realized. In summary, experiments at appropriate times (90min) showed that CNP: the Ce, yMn fluorescent powder has good stability in CL strength under the bombardment of low-voltage electron beams, and shows potential advantages in FED application.
As shown in fig. 4, CNP: the color of the Ce, 0.07Mn fluorescent powder realizes the tuning of the multifunctional whitlockite fluorescent powder from purple to high stability in a CIE chromaticity coordinate diagram. Mixing fluorescent powder and Polyvinyl Chloride (PVC) to prepare luminous ink, and printing a two-dimensional code and a school badge on the low-fluorescence paperboard by adopting a screen printing technology. Under the irradiation of natural light, the two-dimensional code and the pattern are not displayed and cannot be read; under the irradiation of ultraviolet light, patterns from purple to red and two-dimensional codes can be easily read. More noteworthy, the two-dimensional code can be read by a Quick Response (QR) scanning application program of the mobile phone, which includes information such as name, department, personal ID, health status, communication permission, and the like, only a simple light source or a flashlight equipped with an ultraviolet lamp is needed, or an ultraviolet lamp device can be added to the identifier, and the information reading is started during the identification. In addition, once the two-dimension code is generated without replacement, the real-time health state can be updated and the passing permission can be set in the background by utilizing the information communication technology, so that the dynamic epidemic prevention is realized. In addition, the use of a non-fluorescent base in actual production produces better results. In summary, with CNP: the anti-counterfeiting pattern made by Ce, yMn has important application prospect in the ultraviolet fluorescence anti-counterfeiting aspect of important documents such as traditional trademarks, certificates, currency and the like, and also provides a new strategy or can effectively realize dynamic epidemic prevention.
To sum up, this patent uses CNP: the anti-counterfeiting pattern made by Ce, yMn has important application prospect in the ultraviolet fluorescence anti-counterfeiting aspect of important documents such as traditional trademarks, certificates, currency and the like, and also provides a new strategy or can effectively realize dynamic epidemic prevention.
As shown in fig. 5, CNP: the decay behavior of the Ce, yMn (y is 0.07) fluorescent powder under continuous I is 80mA, Va is 8kV, the initial intensity of 86.19 percent and 82.63 percent is respectively maintained after 60min of continuous electron irradiation, and the initial intensity of 82.30 percent and 81.61 percent are respectively maintained after 90min, which shows that the fluorescent powder has good stability in CL intensity under low-voltage electron beam bombardment and shows potential advantages in FED application.
The fluorescent powder which has good chemical stability and can be effectively excited by specific wavelength is made into anti-counterfeiting ink, and then the screen printing technology is adopted for making luminous anti-counterfeiting patterns, or the two-dimensional code is made by combining the rapid information security technology and is printed on the passing permission certificate or card, so that the good effect can be obtained in the practical application of information protection, and the health state inquiry and the verification permission become stricter and quicker.
The patent provides a synthesis preparation method of high-stability multifunctional mineral fluorescent powder, which has good thermal stability and chemical stability, can be tuned to red from purple, and has potential application prospects in near-infrared application and field emission display. The fluorescent powder is prepared into anti-counterfeiting ink, and two practical applications are realized through a screen printing technology: (1) the dynamic two-dimensional code is combined with an information security technology and used for epidemic prevention; (2) anti-counterfeiting pattern excited by near ultraviolet. Under the irradiation of natural light, the two-dimensional code and the pattern are not displayed and cannot be read. Under the irradiation of ultraviolet light, patterns from purple to red and two-dimensional codes can be easily read. More noteworthy, the rapid response scanning application program of the mobile phone can read the information including name, department, personal ID, health state, communication permission and the like in the two-dimensional code, only one simple light source or flashlight with an ultraviolet lamp is needed, and ultraviolet lamp equipment can be added into the identifier, and the information reading is started during identification. In addition, once the two-dimension code is generated without replacement, the real-time health state can be updated and the passing permission can be set in the background by utilizing the information communication technology, so that the dynamic epidemic prevention is realized. With CNP: the anti-counterfeiting pattern made by Ce, yMn has important application prospect in the ultraviolet fluorescence anti-counterfeiting aspect of important documents such as traditional trademarks, certificates, currency and the like, and also provides a new strategy or can effectively realize dynamic epidemic prevention.
And programming the target information by using an internet program to generate the two-dimensional code. Manufacturing a screen printing plate (200 meshes) by using the school badge pattern and the two-dimensional code according to a design drawing, and fully mixing fluorescent powder and ss-110 type PVC screen printing ink to prepare fluorescent printing ink, wherein the mass ratio of the powder to the glue is 1: and 2, using a low-fluorescence paperboard as a substrate, placing the screen printing plate above the substrate, uniformly scraping the fluorescent ink with a coating plate, and drying for 10 hours. And placing the obtained card paper under an ultraviolet short-wave light source, and clearly displaying the school badge pattern and the two-dimensional code. The two-dimensional code is scanned by a quick response scanning application program of the mobile phone, so that personal information, health status and passing permission information can be obtained.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. High stabilityThe qualitative multifunctional whitlockite type fluorescent powder is characterized in that the chemical formula of the fluorescent powder is (Ca)0.5Sr0.5)3-yM0.07(PO4)2:0.07Ce3+,yMn2+Y is 0,0.01,0.03,0.05,0.07,0.09,0.11, and M is an alkali metal ion.
2. The highly stable multifunctional whitlockite-type phosphor according to claim 1, wherein the alkali metal is one or more of Li, Na and K.
3. The method for preparing the highly stable multifunctional whitlockite type phosphor according to any one of claims 1 to 2, comprising the steps of: in the matrix material beta-Ca3(PO4)2Adding compound Na containing sodium ion2CO3(0.07mol) and a compound SrCO containing Sr cation3According to Ca2+:Sr2+The high-stability multifunctional whitlockite fluorescent powder is synthesized by a high-temperature solid phase method according to the mol ratio of 1: 1.
4. The method for preparing highly stable multifunctional whitlockite phosphor as claimed in claim 3, wherein CaCO is added3、SrCO3、(NH4)2HPO4、Na2CO3、CeO2And MnCO3Preheating at 850 deg.C for 1h, and releasing NH in a muffle furnace in air3、H2O and CO2(ii) a After regrinding, at 5% H2、55％N2In a reducing atmosphere, placing the mixture in a tubular furnace and sintering the mixture for 10 hours at 1250 ℃; slowly cooling to room temperature, and grinding into fine powder to obtain the high-stability multifunctional whitlockite type fluorescent powder.
5. The method for preparing high-stability multifunctional whitlockite-type phosphor according to claim 3, wherein the compound containing sodium ions is one or more of sodium hydroxide, sodium carbonate and sodium bicarbonate; the compound containing Sr cation is one or more of strontium hydroxide, strontium carbonate or strontium bicarbonate.
6. Use of the highly stable multifunctional whitlockite-type phosphor according to any one of claims 1 to 2, wherein the highly stable multifunctional whitlockite-type phosphor is obtained by exciting the highly stable multifunctional whitlockite-type phosphor according to any one of claims 1 to 2 by one or more of ultraviolet light and near ultraviolet light.
7. An application of high-stability multifunctional whitlockite fluorescent powder in plant growth illumination.
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| CN113580806A (en) * | 2021-07-21 | 2021-11-02 | 中钞印制技术研究院有限公司 | Security element and security document |
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| CN105176529A (en) * | 2015-09-19 | 2015-12-23 | 青岛科技大学 | Europium-manganese coactivated phosphate white light fluorescent powder and preparation method thereof |
| CN111978960A (en) * | 2020-07-10 | 2020-11-24 | 贺州学院 | Synthesis method of broadband excitation phosphate red fluorescent powder |
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| Title |
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| XIAOFANG YU， XIAOYUN MI: "Color-Tunable Luminescence and Energy Transfer Properties of Dy3+/Eu3+ Co-doped Ca1.5Sr1.5(PO4)2 Phosphor for white LED Applications", 《2020 IEEE 3RD INTERNATIONAL CONFERENCE ON ELECTRONICS TECHNOLOGY (ICET)》 * |
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| CN113580806A (en) * | 2021-07-21 | 2021-11-02 | 中钞印制技术研究院有限公司 | Security element and security document |
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