CN112521945A - Preparation method and application of infrared luminescent material hidden mark - Google Patents

Preparation method and application of infrared luminescent material hidden mark Download PDF

Info

Publication number
CN112521945A
CN112521945A CN202110173945.3A CN202110173945A CN112521945A CN 112521945 A CN112521945 A CN 112521945A CN 202110173945 A CN202110173945 A CN 202110173945A CN 112521945 A CN112521945 A CN 112521945A
Authority
CN
China
Prior art keywords
nayf
luminescent material
solution
phase
infrared luminescent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110173945.3A
Other languages
Chinese (zh)
Inventor
洪颖
陈国松
吴婷霞
王金陵
方静
朱园园
高蓉
薛鑫
陈建松
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Yangzi Inspection And Certification Co ltd
Jinling Customs Technical Center
Original Assignee
Jiangsu Yangzi Inspection And Certification Co ltd
Jinling Customs Technical Center
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Yangzi Inspection And Certification Co ltd, Jinling Customs Technical Center filed Critical Jiangsu Yangzi Inspection And Certification Co ltd
Priority to CN202110173945.3A priority Critical patent/CN112521945A/en
Publication of CN112521945A publication Critical patent/CN112521945A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7772—Halogenides
    • C09K11/7773—Halogenides with alkali or alkaline earth metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
    • G09F3/02—Forms or constructions
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
    • G09F3/02—Forms or constructions
    • G09F2003/0208—Indicia
    • G09F2003/0213—Concealed data

Abstract

The invention discloses a preparation method and application of an infrared luminescent material hidden mark, which comprises the following steps: step one, selecting a matrix material; step two, adjusting the concentration of rare earth doped ions; step three, magnetic stirring; step four, heating by a hydrothermal method; step five, controlling the particle form; step six, cooling and centrifugal separation; step seven, washing with water and ethanol; step eight, drying and grinding; and step nine, spraying marks. The NaYF with high luminous intensity can be prepared by adjusting the ion concentration and the hydrothermal temperature4：Yb3+，Er3+The micro-rod-shaped nanometer material is formed by spraying the infrared luminescent material on the surface of the security check baggage to form a hidden mark, which is beneficial toCatching on a servo; meanwhile, the method is used for criminal investigation sites, displays fingerprints in the form of small-particle suspension, and overcomes the defects that dust is raised by a powder method, the environment is polluted, and a moist or blister object cannot be displayed.

Description

Preparation method and application of infrared luminescent material hidden mark
Technical Field
The invention relates to the field of marks, in particular to a preparation method and application of an infrared luminescent material hidden mark.
Background
The up-conversion luminescence refers to that a substance absorbs light with low wavelength and low frequency and emits light with high wavelength and short frequency, and an infrared luminescent material is an up-conversion luminescent material which emits visible light under the excitation of infrared light. The existing preparation of infrared luminescent materials has very high requirements on the environmental conditions of reaction and complex preparation conditions, and some infrared luminescent materials taking oxyfluoride, sulfide and other systems as matrix materials have certain harmfulness on the environment, have toxicity of different degrees and are not beneficial to physical and mental health of workers, and meanwhile, the prepared infrared luminescent materials have low stability.
For the evidence collection of customs security inspection and criminal investigation sites, an effective means for displaying the mark is lacked, which is not beneficial to implementing accurate and effective attack on the stolen goods of the suspect.
Therefore, a preparation method and application of the infrared luminescent material hidden mark are provided.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a preparation method and application of an infrared luminescent material hidden mark.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an infrared luminescent material hidden mark comprises the following steps:
step one, selecting a matrix material: the matrix material comprises 4 types of halide system, oxide system, oxyfluoride system and sulfide system, and Y is selected respectively2O3、ZrO2、NaYF4、YVO4、Y2O2S and GdOCI with phonon energy of 550cm-1、500cm-1、350cm-1、890cm-1、520cm-1And 500cm-1The lowest value is 350cm according to the phonon energy-1NaYF of4Er, Tb, Dy and Sm ions are used as activating agents as matrix materials;
step two, taking rare earth nitrate solution Y (NO)3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O、Gd(NO3)3·5H2Stirring O for 1h to form a mixed solution, wherein the concentration ratio (molar ratio) of the doped lanthanide ions is Y3+:Yb3+:Er3 +:Gd3+=78:18:2:2；
Step three, magnetic stirring: adding a certain amount of NaF into the mixed solution, then placing the mixed solution on a magnetic stirrer, stirring for 25min to form a complex solution, and adjusting the pH value of the solution to be 1.5-3;
step four, heating by a hydrothermal method: adding the complex solution into a high-pressure hydrothermal synthesis kettle, and heating for 14-20h at the temperature of 220 ℃ and 180-;
step five, controlling the particle form: the accurate control of the particle phase and the shape can be realized by controlling the hydrothermal reaction time, the temperature and the pH value of the solution, and the beta-NaYF is prepared4:Yb3+，Er3+A nano-luminescent material;
step six, cooling and centrifugal separation: naturally cooling the heated complexing solution at normal temperature, placing the cooled solution into a test tube, sealing with a cover, and then placing into a table-type high-speed refrigerated centrifuge, rotating at 3200r/min, and centrifuging for 8min to perform centrifugal separation on the raw materials;
step seven, water washing and ethanol washing: after separation, washing the raw materials with water for 3 times and washing with ethanol for 2 times, then adding a surfactant to improve the stability of the powder in a dispersing agent and slow down the sedimentation speed, and then drying the settled raw materials;
step eight, drying and grinding: putting the settled raw materials into a vacuum drying oven at 60 ℃ for drying for 12h, and grinding the dried sample into powder;
ninth, spraying a mark: the luminescent material powder is dissolved in sodium dodecyl benzene sulfonate to obtain a uniform and transparent dispersion system, and then the uniform and transparent dispersion system is sprayed on an article to form the hidden mark.
Preferably, in the second step, the rare earth ion is an activator, and the doped rare earth ion is Er3+、Tm3+And Ho3+Wherein, Er3+Has rich energy level and high up-conversion efficiency, and is used as the main activator of the up-conversion material.
Preferably, Gd is doped in the second step3+Can obtain NaYF with controllable crystal phase, size and luminescence property4Upconversion nanoparticles by addition of Gd3+The cubic phase to hexagonal phase transition is rapidly completed within 2 hours, and hexagonal phase NaYF with ultra-small size is obtained while the reaction temperature is reduced4Upconversion nanoparticles of Gd3+The addition of (b) accelerates the phase transition from cubic to hexagonal while decreasing the particle size, changing from large microtubes to small cubes.
Preferably, the surfactant in the seventh step is one or more of polyethyleneimine, ethylene diamine tetraacetic acid, cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate and oleic acid, and is chelated with cations to adjust the reaction concentration.
Preferably, the rare earth element Yb in the second step3+Has an excitation wavelength of 980nm, absorbs energy and transmits the energy to Er3+The up-conversion efficiency can be improved by 1-2 orders of magnitude, and the up-conversion sensitizer is used as an effective up-conversion sensitizer.
Preferably, the NaYF in the fourth step4Two crystal forms exist under normal state, one is cubic phase alpha-NaYF4The other is hexagonal phase beta-NaYF4When pH =2The reaction time is 0.5-14h, the crystal size is 500nm-5 mu m, and NaYF is added along with the increase of hydrothermal time4The cubic phase is changed into the hexagonal phase, and finally the micro-rod structure is grown.
The application of the infrared luminescent material hidden mark comprises the following specific steps:
luminous materials are respectively dissolved in different organic solvents and sodium dodecyl benzene sulfonate serving as an anionic surfactant, and the luminous materials are dissolved in the sodium dodecyl benzene sulfonate, so that a dispersion system with good concealment and stability can be obtained;
the dispersant used for marking is put into a handheld electric sprinkling can, and when customs security inspection marks luggage containing drugs, the dispersant is made into a hidden mark and sprayed on the luggage for marking; after the station is far away from the station crowd, capturing the station crowd without being perceived, and keeping the station crowd in a busy place;
the method can also be used for criminal investigation sites, shows fingerprints in the form of small-particle suspension, and overcomes the defects that dust is raised by a powder method, the environment is polluted, and moist or blister objects cannot be shown.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a simple and effective hydrothermal synthesis method, and NaYF with high luminous intensity can be prepared by adjusting the ion concentration and the hydrothermal temperature4：Yb3+，Er3+The material can emit strong green visible light visible to naked eyes under the irradiation of an infrared light source;
2. according to the hydrothermal synthesis method, complexing agents such as sodium citrate and the like are not required to be added, the accurate control of the particle phase and the shape of the luminescent material can be realized by changing the temperature and the pH value of the solution in the hydrothermal time, the high-intensity green visible light output is obtained, and the method is simple, convenient and efficient;
3. according to the invention, the infrared luminescent material is sprayed on the surface of the security inspection plum to form the hidden mark, so that the capturing and the dirty acquisition can be realized under the condition of no detection; meanwhile, the method is used for criminal investigation sites, displays fingerprints in the form of small-particle suspension, and overcomes the defects that dust is raised by a powder method, the environment is polluted, and a moist or blister object cannot be displayed.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention adopts the following scheme: a preparation method of an infrared luminescent material hidden mark comprises the following steps:
step one, selecting a matrix material: the matrix material comprises 4 types of halide system, oxide system, oxyfluoride system and sulfide system, and Y is selected respectively2O3、ZrO2、NaYF4、YVO4、Y2O2S and GdOCI with phonon energy of 550cm-1、500cm-1、350cm-1、890cm-1、520cm-1And 500cm-1The lowest value is 350cm according to the phonon energy-1NaYF of4Er, Tb, Dy and Sm ions are used as activating agents as matrix materials;
step two, taking rare earth nitrate solution Y (NO)3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O、Gd(NO3)3·5H2Stirring O for 1h to form a mixed solution, wherein the concentration ratio (molar ratio) of the doped lanthanide ions is Y3+:Yb3+:Er3 +:Gd3+=78:18:2:2；
Step three, magnetic stirring: adding a certain amount of NaF into the mixed solution, then placing the mixed solution on a magnetic stirrer, stirring for 25min to form a complex solution, and adjusting the pH value of the solution to be 1.5-3;
step four, heating by a hydrothermal method: adding the complex solution into a high-pressure hydrothermal synthesis kettle, and heating for 14-20h at the temperature of 220 ℃ and 180-;
step five, controlling the particle form: the accurate control of the particle phase and the shape can be realized by controlling the hydrothermal reaction time, the temperature and the pH value of the solution, and the beta-NaYF is prepared4:Yb3+，Er3+Nano hairAn optical material;
sixthly, cooling and centrifugal separation: naturally cooling the heated complexing solution at normal temperature, placing the cooled solution into a test tube, sealing with a cover, and then placing into a table-type high-speed refrigerated centrifuge, rotating at 3200r/min, and centrifuging for 8min to perform centrifugal separation on the raw materials;
step seven, water washing and ethanol washing: after separation, washing the raw materials with water for 3 times and washing with ethanol for 2 times, then adding a surfactant to improve the stability of the powder in a dispersing agent and slow down the sedimentation speed, and then drying the settled raw materials;
step eight, drying and grinding: and (3) putting the settled raw materials into a vacuum drying oven at 60 ℃ for drying for 12h, and grinding the dried sample into powder.
Ninth, spraying a mark: the luminescent material powder is dissolved in sodium dodecyl benzene sulfonate to obtain a uniform and transparent dispersion system, and then the uniform and transparent dispersion system is sprayed on an article to form the hidden mark.
In the second step, the rare earth ions are used as an activator, and the doped rare earth ions are Er3+、Tm3+And Ho3+Wherein, Er3+Has rich energy level and high up-conversion efficiency, and is used as the main activator of the up-conversion material.
Gd is doped in the second step3+Can obtain NaYF with controllable crystal phase, size and luminescence property4Upconversion nanoparticles by addition of Gd3+The cubic phase to hexagonal phase transition is rapidly completed within 2 hours, and hexagonal phase NaYF with ultra-small size is obtained while the reaction temperature is reduced4Upconversion nanoparticles of Gd3+The addition of (b) accelerates the phase transition from cubic to hexagonal while decreasing the particle size, changing from large microtubes to small cubes.
And seventhly, chelating the surfactant, which is Polyethyleneimine (PEI), Ethylene Diamine Tetraacetic Acid (EDTA), Cetyl Trimethyl Ammonium Bromide (CTAB), Sodium Dodecyl Benzene Sulfonate (SDBS) and Oleic Acid (OA), with the cation to adjust the reaction concentration.
In the second step, the rare earth element Yb3+Has an excitation wavelength of 980nm, absorbs energy and transmits the energy to Er3+The up-conversion efficiency can be improved by 1-2 orders of magnitude, and the up-conversion sensitizer is used as an effective up-conversion sensitizer.
NaYF in the fourth step4Two crystal forms exist under normal state, one is cubic phase alpha-NaYF4The other is hexagonal phase beta-NaYF4When the pH is =2, the reaction time is 0.5-14h, the crystal form size is 500nm-5 μm, and NaYF is increased along with the increase of hydrothermal time4The cubic phase is converted into the hexagonal phase, and finally a micro-rod structure is grown, and the luminescent material in the shape of the micro-rod has higher fluorescence intensity than other forms (cubes, rods, cubes and the like), so that the lanthanide-doped NaYF with the shape of a micro-tube is synthesized4To achieve fluorescence intensity enhancement;
in the specific embodiment, when the pH =2, the reaction time is 20h, the reaction temperature is 200 ℃, and a hydrothermal method is adopted to successfully prepare the beta-NaYF with regular appearance, uniform size and good dispersibility4:Yb3+，Er3+The luminescent material emits green light under the excitation of a 980nm infrared light source, and can be dissolved in sodium dodecyl benzene sulfonate to obtain a dispersion system with good concealment and stability.
The application of the infrared luminescent material hidden mark comprises the following specific steps:
luminescent materials are respectively dissolved in different organic solvents and sodium dodecyl benzene sulfonate serving as an anionic surfactant, and the luminescent materials are dissolved in the sodium dodecyl benzene sulfonate, so that a hidden and stable dispersion system can be obtained (the effects of the dispersion systems formed by different solvents are compared in a table 1);
the dispersant used for marking is put into a handheld electric sprinkling can, and when customs security inspection marks luggage containing drugs, the dispersant is made into a hidden mark and sprayed on the luggage for marking; after the station is far away from the station crowd, capturing the station crowd without being perceived, and keeping the station crowd in a busy place;
the method can also be used for criminal investigation sites, shows fingerprints in the form of small-particle suspension, and overcomes the defects that dust is raised by a powder method, the environment is polluted, and moist or blister objects cannot be shown.
TABLE 1 comparison of the effects of dispersions formed with different solvents
Figure DEST_PATH_IMAGE001
The rare earth up-conversion luminescent material is dissolved in sodium dodecyl benzene sulfonate, and the luminescent effect of the rare earth up-conversion luminescent material sprayed on paper textiles, plastics, glass and metal materials is weakened in sequence.
In conclusion, the optimum lanthanide ion concentration ratio at Y is obtained by researching the rare earth doping concentration ratio and the preparation process conditions3+:Yb3+:Er3+=80:18:2 (molar ratio); the hydrothermal synthesis method is utilized to prepare 18 percent Yb3+，2%Er3+Co-doped NaYF4The upconversion luminescence nanometer particles and the sample can realize upconversion luminescence without pre-charging at room temperature aiming at 980nm infrared laser.
The luminescent material is optimized by adjusting the hydrothermal synthesis time, the temperature, the ion concentration, the pH value of the initial solution and the like; the nanometer luminescent material with high luminescent performance is successfully prepared, the luminescent effect of the material reaches the expected requirement, and a dispersion system with good concealment and stability can be obtained by dissolving the nanometer luminescent material in sodium dodecyl benzene sulfonate.
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 able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.

Claims (7)

1. A preparation method of an infrared luminescent material hidden mark is characterized by comprising the following steps:
step one, selecting a matrix material: the matrix material comprises 4 types of halide system, oxide system, oxyfluoride system and sulfide system, and Y is selected respectively2O3、ZrO2、NaYF4、YVO4、Y2O2S and GdOCI with phonon energy of 550cm-1、500cm-1、350cm-1、890cm-1、520cm-1And 500cm-1The lowest value is 350cm according to the phonon energy-1NaYF of4Er, Tb, Dy and Sm ions are used as activating agents as matrix materials;
step two, taking rare earth nitrate solution Y (NO)3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O、Gd(NO3)3·5H2Stirring O for 1h to form a mixed solution, wherein the concentration of the doped lanthanide ions is matched with the molar ratio of Y3+:Yb3+:Er3+:Gd3+=78:18:2:2；
Step three, magnetic stirring: adding a certain amount of NaF into the mixed solution, then placing the mixed solution on a magnetic stirrer, stirring for 25min to form a complex solution, and adjusting the pH value of the solution to be 1.5-3;
step four, heating by a hydrothermal method: adding the complex solution into a high-pressure hydrothermal synthesis kettle, and heating for 14-20h at the temperature of 220 ℃ and 180-;
step five, controlling the particle form: the accurate control of the particle phase and the shape can be realized by controlling the hydrothermal reaction time, the temperature and the pH value of the solution, and the beta-NaYF is prepared4:Yb3+，Er3+A nano-luminescent material;
step six, cooling and centrifugal separation: naturally cooling the heated complexing solution at normal temperature, placing the cooled solution into a test tube, sealing with a cover, and then placing into a table-type high-speed refrigerated centrifuge, rotating at 3200r/min, and centrifuging for 8min to perform centrifugal separation on the raw materials;
step seven, water washing and ethanol washing: after separation, washing the raw materials with water for 3 times and washing with ethanol for 2 times, then adding a surfactant to improve the stability of the powder in a dispersing agent and slow down the sedimentation speed, and then drying the settled raw materials;
step eight, drying and grinding: putting the settled raw materials into a vacuum drying oven at 60 ℃ for drying for 12h, and grinding the dried sample into powder;
ninth, spraying a mark: the luminescent material powder is dissolved in sodium dodecyl benzene sulfonate to obtain a uniform and transparent dispersion system, and then the uniform and transparent dispersion system is sprayed on an article to form the hidden mark.
2. The method for preparing the covert mark of the infrared luminescent material of claim 1, wherein in the second step, the rare earth ion is an activator, and the doped rare earth ion is Er3+、Tm3+And Ho3+Wherein, Er3+Has rich energy level and high up-conversion efficiency, and is used as the main activator of the up-conversion material.
3. The method for preparing the covert marker of infrared luminescent material of claim 1, wherein Gd is doped in the second step3+Can obtain NaYF with controllable crystal phase, size and luminescence property4Upconversion nanoparticles by addition of Gd3+The cubic phase to hexagonal phase transition is rapidly completed within 2 hours, and hexagonal phase NaYF with ultra-small size is obtained while the reaction temperature is reduced4Upconversion nanoparticles of Gd3+The addition of (b) accelerates the phase transition from cubic to hexagonal while decreasing the particle size, changing from large microtubes to small cubes.
4. The method for preparing the covert marker of the infrared luminescent material of claim 1, wherein in the seventh step, the surfactant is one or more of polyethyleneimine, ethylene diamine tetraacetic acid, cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate and oleic acid, and is chelated with cations to adjust the reaction concentration.
5. The method of claim 1, wherein the second step is performed by using Yb as a rare earth element3+Has an excitation wavelength of 980nm, absorbs energy and transmits the energy to Er3+The up-conversion efficiency can be improved by 1-2 orders of magnitude, and the up-conversion sensitizer is used as an effective up-conversion sensitizer.
6. The method of claim 1, wherein NaYF is selected from the group consisting of4Two crystal forms exist under normal state, one is cubic phase alpha-NaYF4The other is hexagonal phase beta-NaYF4When the pH is =2, the reaction time is 0.5-14h, the crystal form size is 500nm-5 μm, and NaYF is increased along with the increase of hydrothermal time4The cubic phase is changed into the hexagonal phase, and finally the micro-rod structure is grown.
7. Use of an infrared luminescent material covert marker according to any one of claims 1 to 6, in particular as follows:
luminous materials are respectively dissolved in different organic solvents and sodium dodecyl benzene sulfonate serving as an anionic surfactant, and the luminous materials are dissolved in the sodium dodecyl benzene sulfonate, so that a dispersion system with good concealment and stability can be obtained;
the dispersant used for marking is put into a handheld electric sprinkling can, when customs security inspection marks luggage containing drugs, the dispersant is made into a hidden mark and sprayed on the luggage for marking, and the luggage is caught by a servo; it can also be used in criminal investigation sites to show fingerprints in the form of a small particle suspension sprayed from a spray can.
CN202110173945.3A 2021-02-09 2021-02-09 Preparation method and application of infrared luminescent material hidden mark Pending CN112521945A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110173945.3A CN112521945A (en) 2021-02-09 2021-02-09 Preparation method and application of infrared luminescent material hidden mark

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110173945.3A CN112521945A (en) 2021-02-09 2021-02-09 Preparation method and application of infrared luminescent material hidden mark

Publications (1)

Publication Number Publication Date
CN112521945A true CN112521945A (en) 2021-03-19

Family

ID=74975563

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110173945.3A Pending CN112521945A (en) 2021-02-09 2021-02-09 Preparation method and application of infrared luminescent material hidden mark

Country Status (1)

Country Link
CN (1) CN112521945A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116396755A (en) * 2023-06-01 2023-07-07 金陵海关技术中心 Nanometer invisible material and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102952547A (en) * 2012-10-30 2013-03-06 哈尔滨工程大学 Graphene and rare earth up-conversion fluorescent composite material and preparation method thereof
CN104458664A (en) * 2014-12-23 2015-03-25 武汉大学 Antibody functionalized rare earth luminescent material-based latent fingerprint detection probe, as well as preparation method and application thereof
CN111778029A (en) * 2020-07-28 2020-10-16 金陵海关技术中心 Preparation and application method of luggage hidden identification in travel inspection system

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102952547A (en) * 2012-10-30 2013-03-06 哈尔滨工程大学 Graphene and rare earth up-conversion fluorescent composite material and preparation method thereof
CN104458664A (en) * 2014-12-23 2015-03-25 武汉大学 Antibody functionalized rare earth luminescent material-based latent fingerprint detection probe, as well as preparation method and application thereof
CN111778029A (en) * 2020-07-28 2020-10-16 金陵海关技术中心 Preparation and application method of luggage hidden identification in travel inspection system

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
崔艳文: "Er3+，Yb3+共掺NaYF4及NaGdF4上转换发光材料的光学温度传感特性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116396755A (en) * 2023-06-01 2023-07-07 金陵海关技术中心 Nanometer invisible material and preparation method and application thereof

Similar Documents

Publication Publication Date Title
Yao et al. Large-scale synthesis and screen printing of upconversion hexagonal-phase NaYF 4: Yb 3+, Tm 3+/Er 3+/Eu 3+ plates for security applications
Lee et al. Ultraviolet radiation excited strong red-emitting LaAlO3: Eu3+ nanophosphors: Synthesis and luminescent properties
Liu et al. Upconversion/downconversion luminescence of color-tunable Gd2O3: Er3+ phosphors under ultraviolet to near-infrared excitation
Tang et al. Ion exchanged YVO4: Eu3+ nanocrystals and their strong luminescence enhanced by energy transfer of thenoyltrifluoroacetone ligands
Han et al. Controlled synthesis and luminescence properties of doped NaLa (WO4) 2 microstructures
Liu et al. Multifunctional β-NaGdF4: Ln3+ (Ln= Yb/Er/Eu) phosphors synthesized by L-arginine assisted hydrothermal method and their multicolor tunable luminescence
Li et al. Upconverting YbPO4: RE monospheres (RE= Ho, Er, Tm)
Qian et al. Tunable multicolor emission and energy transfer of cylindrical Gd2O3: Dy3+, Tb3+, Eu3+ particles
Liu et al. Screen printing of multi-mode emission NaYF 4: Yb, Er (Tm)/NaYF 4: Ce, Mn composites for anti-counterfeiting applications
CN112521945A (en) Preparation method and application of infrared luminescent material hidden mark
Wang et al. Reversible transformation of all-inorganic copper halide perovskite nanocrystals for anti-counterfeiting
Guo et al. Solvothermal synthesis and upconversion spectroscopy of monophase hexagonal NaYF4: Yb3+/Er3+ nanosized crystallines
Pratibha et al. Investigations of enhanced luminescence properties of Sm3+ doped LaAlO3 nanophosphors for field emission displays
Cao et al. Tuning the phase, morphology and size of monodisperse ScF 3 and NaScF 4 crystals through lanthanide doping
Kuisheng et al. Upconversion luminescence properties of Ho3+, Tm3+, Yb3+ co-doped nanocrystal NaYF4 synthesized by hydrothermal method
Yuan et al. Preparation and characterization of CaAl2O4: Eu2+, Nd3+ luminous phosphor synthesized by coprecipitation-sol-gel method
CN102344807B (en) Solvothermal synthesis method for NaLn(MoO4)2 micron crystal
Zhang et al. Multicolor luminescent GdVO4: Ln3+ (Ln= Eu, Dy and Sm) nanophosphors prepared by a protected calcination method
Ledoux et al. Upconversion phenomena in nanofluorides
Wang et al. Uniform Lu2 (C4H4O6) 3· 6H2O and Lu2O3: Ln (Ln= Eu3+, Tb3+) cauliflower-like microspheres: Facile synthesis and luminescent properties
Yang et al. Hydrothermal synthesis and luminescence properties of KLa (MoO 4) 2: Eu 3+ phosphor
CN103333689A (en) Method of thermosynthesis of SrWO4:Ln3<+> nanoribbon with solvent
Liang et al. Investigation of green emission of ScVO4: Yb3+/Er3+ sub-microcrystals with different morphologies
CN102559188A (en) Nano lamellar compound rare-earth hydroxide and preparation method thereof
CN106590643B (en) A kind of preparation method and applications of blue emission BCNO quantum dots

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20210319

RJ01 Rejection of invention patent application after publication