CN113403065B - Fluoride-based stress luminescent material, preparation method and application thereof - Google Patents
Fluoride-based stress luminescent material, preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 55
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910001428 transition metal ion Inorganic materials 0.000 claims abstract description 10
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 8
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 8
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 8
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 8
- -1 rare earth ions Chemical class 0.000 claims abstract description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 8
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 29
- 238000004020 luminiscence type Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 16
- 239000011572 manganese Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 229940093474 manganese carbonate Drugs 0.000 claims description 7
- 235000006748 manganese carbonate Nutrition 0.000 claims description 7
- 239000011656 manganese carbonate Substances 0.000 claims description 7
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 7
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000012856 weighed raw material Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 238000012827 research and development Methods 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 description 12
- 239000011575 calcium Substances 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 6
- 238000005166 mechanoluminescence Methods 0.000 description 5
- 238000004846 x-ray emission Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 235000015241 bacon Nutrition 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
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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
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/615—Halogenides
- C09K11/616—Halogenides with alkali or alkaline earth metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
- G01L1/241—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet by photoelastic stress analysis
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- Physics & Mathematics (AREA)
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- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention provides a fluoride-based stress luminescent material, a preparation method and application thereof. The general chemical formula of the fluoride-based stress luminescent material is M 1‑x F 2 :A x Or M 1‑x‑y F 2 :B x ,Mn 2+ y (ii) a Wherein x is more than or equal to 0 and less than or equal to 0.05,0 and less than or equal to 0.05, x and y respectively represent molar percentage content, and x and y are not zero at the same time; m is at least one of alkaline earth metals Mg and Ca; a is Bi or transition metal ions; the transition metal ions are Sc, ti, mn, cu or Zn and the like; b is at least one of rare earth ions Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb and the like. The stress luminescent material has excellent luminescent performance, and provides new possibility for further research and development of the stress luminescent mechanism.
Description
Technical Field
The invention relates to the field of novel inorganic luminescent materials, in particular to a fluoride-based stress luminescent material, a preparation method and application thereof.
Background
Stress luminescence has been discovered as early as the 16 th century, for example: the light can be emitted when earthquake or volcanic eruption occurs. Its earliest documented fact was written by Francis Bacon in 1605 in his work "The Advancement of Learning": "flashing is seen when a knife is used to quickly cut across the surface of the sugar cube". For many solid materials, they emit light when a mechanical stress is applied thereto, and this phenomenon is known as Mechanoluminescence (ML) or Tribouminescence (TL), and such a material emitting light under mechanical stress is called a stressor. The term stress luminescence was not used until 1978.
The popular saying is that: by collecting the light, the distribution of the light is converted into a distribution of stress. Stress refers to the mechanical force used to cause a material to luminesce and includes impact, tension, deformation, pressure, tension, shear, friction, fracture, and the like. In recent years, research on elastic stress luminescent materials has become a leading edge discipline. Although the conversion of mechanical stress into light distribution is quite complicated, some experiments have succeeded in applying the stress luminescence phenomenon to pressure sensors, mechanical force visualization and some other different kinds of intelligent systems, which have attracted worldwide attention, but: 1. the types of stress luminescent materials known today are very limited and are only seen in some silicates and piezoelectric materials; 2. the mechanism is not clear; 3. the trap type has not been specified.
Disclosure of Invention
The invention aims to provide a fluoride-based stress luminescent material, a preparation method and application thereof, which are used for supplementing new materials for the existing limited types of stress luminescent materials and increasing new research directions for research on the stress luminescent materials.
The invention is realized by the following steps: a fluoride-based stress luminescent material has a chemical general formula as shown in the following two expression forms, (1) M 1-x F 2 :A x Wherein x represents the mole percentage content, and x is more than 0 and less than or equal to 0.05; m is at least one of alkaline earth metals Mg and Ca; a is Bi or transition metal ions; the transition metal ions are Sc, ti, mn, cu or Zn and the like; (2) M 1-x-y F 2 :B x ,Mn 2+ y Wherein x is more than or equal to 0 and less than or equal to 0.05,0 and less than or equal to 0.05, x and y respectively represent molar percentage content, and x and y are not zero at the same time; m is at least one of alkaline earth metals Mg and Ca; b is at least one of rare earth ions Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb and the like.
The preparation method of the fluoride-based stress luminescent material comprises the following steps: according to the general formula M 1-x F 2 :A x Or M 1-x-y F 2 :B x ,Mn 2+ y Weighing raw materials according to the chemical dose ratio of the elements; selecting corresponding fluoride as a raw material for the M element, selecting corresponding oxide as the raw material for the A element except Mn, and selecting manganese carbonate as the raw material if the A is Mn; b element is selected as the corresponding oxide of the element B as the raw material, and Mn element is selected as the raw material of manganese carbonate; putting the weighed raw materials into an agate mortar, adding ethanol to fully mix the raw materials, and fully grinding the raw materials to be in a powder state; the ground powder was placed in a crucible and placed in a high temperature atmosphere tube furnace under a weakly reducing atmosphere (5%H) 2 -95％N 2 ) Calcining at 1100 deg.C under nitrogen or argon gas protective atmosphere for 2 hr, and naturally cooling to roomTaking out the mixture at a high temperature, and grinding the mixture to obtain the required luminescent material.
The invention provides a fluoride-based stress luminescent material, which directly applies stress to powder or a film prepared by mixing the powder and an elastic high polymer material without carrying out prior ultraviolet light or visible light irradiation, and generates stress luminescence within the elastic limit of the material. On one hand, the luminescent performance of the stress luminescent material is excellent; on the other hand, the invention provides new possibility for further research and development of the mechanism of stress luminescence.
The fluoride-based stress luminescent material is prepared by adopting a traditional solid-phase reaction method, and has the advantages of simple process, low equipment requirement, easily controlled conditions, low cost, no toxic or harmful substances in the preparation process and environmental friendliness.
The stress luminescent material has high luminous efficiency and simple preparation method, and has potential application value in the application fields of structural damage detection, electronic signature systems, electronic skins and the like which relate to stress monitoring.
Drawings
Figure 1 is an XRD pattern of a sample of example 1 of the present invention.
FIG. 2 is an X-ray emission spectrum of a sample in example 1 of the present invention.
FIG. 3 is a diagram of an ML spectrum measured at a pressure of 40N for a sample in example 1 of the present invention.
FIG. 4 is a graph showing the relationship between the stress level and the luminescence intensity of the sample in example 1 of the present invention.
Figure 5 is an XRD pattern of the sample of example 2 of the invention.
FIG. 6 is an X-ray emission spectrum of a sample in example 2 of the present invention.
FIG. 7 is a real shot of stress luminescence phenomenon of six samples prepared in example 3 of the present invention.
FIG. 8 is a real shot of stress luminescence phenomenon of the samples prepared in examples 2 and 4 of the present invention.
Detailed Description
The fluoride-based stress luminescent material provided by the invention can realize luminescence adjustable stress luminescence by doping transition metal ions or different rare earth ions.
Specifically, the general chemical expression formula of the fluoride-based stress luminescent material of the present invention can be represented by the following two expression forms: (1) M 1-x F 2 :A x Wherein x represents the mole percentage content and is more than 0 and less than or equal to 0.05; m is at least one of alkaline earth metals Mg and Ca; a is transition metal ion or Bi; the transition metal ions are Sc, ti, mn, cu or Zn, etc. (2) M is a group of 1-x-y F 2 :B x ,Mn 2+ y Wherein x is more than or equal to 0 and less than or equal to 0.05,0 and less than or equal to 0.05, x and y represent molar percentage, and x and y are not zero at the same time; m is at least one of alkaline earth metals Mg and Ca; b is at least one of rare earth ions Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm or Yb.
The fluoride-based stress luminescent material provided by the invention adopts a typical high-temperature solid phase method during preparation, and specifically comprises the following steps: selecting raw materials, namely selecting magnesium fluoride and calcium fluoride for alkaline earth metals Mg and Ca; selecting manganese carbonate for Mn element; selecting corresponding transition metal oxide for the transition metal ions; selecting bismuth oxide as Bi element; for rare earth ions, selecting corresponding rare earth ion oxides; after the raw materials are selected, weighing the raw materials according to the chemical dose ratio of each element in the chemical general formula; putting the weighed raw materials into an agate mortar, adding a proper amount of ethanol to fully mix, and fully grinding the mixture to be in a powder state. The ground powder was placed in a crucible and placed in a high temperature atmosphere tube furnace under a weakly reducing atmosphere (5%H) 2 -95％N 2 ) Or calcining at 1100 deg.C under nitrogen or argon gas protective atmosphere for 2h, naturally cooling to room temperature, taking out, and grinding to obtain the desired luminescent material.
Example 1 preparation of Mg 0.98 F 2 ：0.02Mn 2+ A stress luminescent material.
According to the formula Mg 0.98 F 2 ：0.02Mn 2+ (the doping amount of 0.02 is usually written before doping elements) weighing magnesium fluoride and manganese carbonate as raw materials according to the stoichiometric ratio of each element, putting the weighed raw materials into an agate mortar, adding a proper amount of ethanol to fully mix the raw materials, and fully grinding the raw materials into a powder state. Will be groundPlacing the ground powder in a crucible, placing the crucible in a high-temperature atmosphere tube furnace, calcining for 2h at 1100 ℃ under the protection of nitrogen, naturally cooling to room temperature, taking out, and grinding to obtain Mg 0.98 F 2 ：0.02Mn 2+ A stress luminescent material.
For Mg prepared in this example 0.98 F 2 ：0.02Mn 2+ The stress luminescent material was subjected to XRD and X-ray emission spectrum tests, and the results are shown in fig. 1 and 2. In FIGS. 1 and 2, for convenience of representation, a "MgF" is used 2 ：Mn 2+ "to show, the same is true below.
Mg prepared in this example 0.98 F 2 ：0.02Mn 2+ A40N pressure was applied to the stressed phosphor and the ML spectrum was measured as shown in FIG. 3.
The applied pressure was reduced to 30N and 20N, and then ML spectroscopy after light emission was performed in comparison with the pressure of 40N, and the results are shown in FIG. 4. Therefore, the stress luminescence intensity of the luminescent material is in a direct proportion relation with the applied stress, so that the application of the luminescent material to the detection of stress distribution is not problematic at all.
Example 2 preparation of Ca 0.98 F 2 ：0.02Mn 2+ A stress luminescent material.
According to the formula Ca 0.98 F 2 ：0.02Mn 2+ Weighing calcium fluoride and manganese carbonate as raw materials according to the stoichiometric ratio of the elements, putting the weighed raw materials into an agate mortar, adding a proper amount of ethanol to fully mix the raw materials, and fully grinding the raw materials to be in a powder state. Placing the ground powder in a crucible, placing the crucible in a high-temperature atmosphere tube furnace, calcining for 2h at 1100 ℃ under the protection of argon, naturally cooling to room temperature, taking out, and grinding to obtain Ca 0.98 F 2 ：0.02Mn 2+ A stress luminescent material.
Ca prepared in this example 0.98 F 2 ：0.02Mn 2+ The stress luminescent material was subjected to XRD and X-ray emission spectrum tests, and the results are shown in fig. 5 and 6.
Example 3 preparation of Mg 0.98 F 2 :0.02A stress luminescent material.
The preparation of the compound of the formula Mg according to the above method 0.98 F 2 :0.02A, wherein a is Bi, sc, ti, mn, cu, zn, thus six samples were prepared in total.
The prepared six samples were applied with a certain force (the force applied here was about the same) to obtain a stress luminescence phenomenon of each sample as shown in fig. 7.
Example 4 preparation of Ca 0.96 F 2 ：0.02B，0.02Mn 2+ A stress luminescent material.
The preparation method in this example can refer to the above description. B are Tb, eu, ho, ce, nd, er, tm, gd, sm, dy, yb and Pr, respectively, so that 12 samples in total were obtained.
The 12 samples of this example and the samples prepared in example 2 were tested in a stress luminescence experiment, and the luminescence phenomenon was shown in fig. 8.
The crystal structure of the fluoride-based stress luminescent material prepared by the invention belongs to a tetragonal system. Stress luminescence occurs when stress is directly applied on the fluoride-based stress luminescent material; the powder can be directly stressed, and a film or a cylinder prepared by mixing the powder and the elastic high polymer material can be stressed, so that stress luminescence can occur within the elastic limit of the material. Furthermore, the stress luminescence intensity of the fluoride-based stress luminescent material has a linear relationship with the magnitude of the applied stress. The applied stress includes, but is not limited to, friction, compression, tension, bending, impact, torsion, ultrasound, and the like.
The stress luminescent material has high luminous efficiency and simple preparation method, and has potential application value in the application fields of structural damage detection, electronic signature systems, electronic skins and the like which relate to stress monitoring.
Claims (5)
1. The application of the fluoride-based stress luminescent material in the fields of structural damage detection, electronic signature systems and electronic skin and relates to the stress monitoring aspect is characterized in that the chemical general formula of the fluoride-based stress luminescent material is M 1-x F 2 : A x Wherein x isRepresents the mole percentage content, and x is more than 0 and less than or equal to 0.05; m is one of alkaline earth metals Mg and Ca; a is Bi or transition metal ions;
the transition metal ions are Sc, ti, mn, cu or Zn;
the preparation method of the fluoride-based stress luminescent material comprises the following steps: according to the general formula M 1-x F 2 : A x Weighing raw materials according to the chemical dose ratio of the elements; selecting corresponding fluoride as a raw material for the M element, selecting corresponding oxide as the raw material for the A element except Mn, and selecting manganese carbonate as the raw material if the A is Mn; putting the weighed raw materials into an agate mortar, adding ethanol to fully mix the raw materials, and fully grinding the raw materials to be in a powder state; placing the ground powder in a crucible, placing the crucible in a high-temperature atmosphere tube furnace, calcining the 2h at 1100 ℃ in a weak reducing atmosphere and a nitrogen or argon protective atmosphere, naturally cooling to room temperature, taking out, and grinding to obtain the required luminescent material;
the fluoride-based stress luminescent material can generate stress luminescence within the elastic limit of the material by directly applying stress without carrying out the prior ultraviolet light or visible light irradiation.
2. Use according to claim 1, wherein x is in particular 0.02.
3. Use according to claim 1, characterized in that the weakly reducing atmosphere is 5% by volume of H 2 And 95% of N 2 。
4. The application of the fluoride-based stress luminescent material in the fields of structural damage detection, electronic signature systems and electronic skin and relates to the stress monitoring aspect is characterized in that the chemical general formula of the fluoride-based stress luminescent material is M 1-x -y F 2 :B x ,Mn 2+ y Wherein x is more than or equal to 0 and less than or equal to 0.05,0 and more than or equal to y is less than or equal to 0.05, and x and y respectively represent the mole percentage content; m is one of alkaline earth metals Mg and Ca; b is one of rare earth ions;
the rare earth ions are Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm and Yb;
the preparation method of the fluoride-based stress luminescent material comprises the following steps: according to the general formula M 1-x -y F 2 :B x ,Mn 2+ y Weighing raw materials according to the chemical dose ratio of the elements; the element M is selected to be the corresponding fluoride as the raw material, the element B is selected to be the corresponding oxide as the raw material, and the element Mn is selected to be manganese carbonate as the raw material; putting the weighed raw materials into an agate mortar, adding ethanol to fully mix the raw materials, and fully grinding the raw materials to be in a powder state; placing the ground powder in a crucible, placing the crucible in a high-temperature atmosphere tube furnace, calcining the 2h at 1100 ℃ in a weak reducing atmosphere and a nitrogen or argon protective atmosphere, naturally cooling to room temperature, taking out, and grinding to obtain the required luminescent material;
the fluoride-based stress luminescent material can generate stress luminescence within the elastic limit of the material by directly applying stress without carrying out the prior ultraviolet light or visible light irradiation.
5. Use according to claim 4, wherein x and y are each 0.02.
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