CN107488448A - It is a kind of to light, heat, the more stimuli responsives of power self-activate luminescence material and preparation method thereof - Google Patents
It is a kind of to light, heat, the more stimuli responsives of power self-activate luminescence material and preparation method thereof Download PDFInfo
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- CN107488448A CN107488448A CN201710309971.8A CN201710309971A CN107488448A CN 107488448 A CN107488448 A CN 107488448A CN 201710309971 A CN201710309971 A CN 201710309971A CN 107488448 A CN107488448 A CN 107488448A
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
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Abstract
The present invention relates to it is a kind of to light, heat, the more stimuli responsives of power self-activate luminescence material and preparation method thereof, the chemical expression of the material is CaxZnyOS, wherein the ＜ y ＜ 1 of 0.9 ＜ x ＜ 1,0.9.The material sends bright pink under 250~300nm ultraviolet excitations, bright green light is sent under 325~350nm ultraviolet excitations, there is thermoluminescence performance under thermostimulation, there is stress irradiance performance under friction, collision, ultrasound and compression, naked eyes visible green light is sent, is that a kind of power, heat, light of collecting is stimulated in response to integral self-activation Multifunctional luminous material more.
Description
Technical field
The invention belongs to Material Physics technical field, be related to it is a kind of to light, heat, the more stimuli responsives of power self-activate luminescence material
Material and preparation method thereof.
Background technology
In the epoch that science and technology makes constant progress, increasing device products tend to intelligent and multifunction.More work(
The focus that energy material is always professional's concern, explores and study.Luminiferous material occupies important inside multifunctional material
Position.
Luminescent material is a kind of important functional material, is had in high-technology fields such as information, aerospace, detection and biologies
It is widely applied.In order to adapt to the fast development of current technical industry, meet the requirement of luminescent material multifunction, learn both at home and abroad
Person also tries to explore while further investigation performance original with constantly improve luminescent material and expands its New function, makes it by list
One function is to multi-functional transformation.In the evolution of nearest decades, luminescent material exploitation achieves considerable progress, ZnS：
Mn、SrAl2O4：Eu, Ce, SrMgAl6O11：Eu、ZrO2：Ti、Sr2MgSi2O7：Eu, Dy, ZnGa2O4：Mn、Ca2Al2SiO7：Ce、
(Ba, Ca) TiO3：Pr、Ca2Nb2O7：Pr、BaZrO3：Eu, Ti, BaSi2O2N2：Eu etc. more than tens plant luminescent material it is a certain or certain
There is excellent performance in a little performances.(Ba, Ca) TiO3：Pr materials have obvious red under ultraviolet excitation and compression
Light, but thermoluminescence efficiency is too low, and the mechanical stimulus that can be responded is single；Ca2Nb2O7：Although Pr materials can be in different ultraviolet lights
The lower conversion for realizing multiple color is excited, but the stress irradiance under thermoluminescence stimulates with multiple machine is weaker；SrAl2O4：
Eu, Dy material show excellent performance under light, thermostimulation, but only faint stress is responded；BaZrO3：Eu, Ti material
Material shows the orange-red light that brightness is high, monochromaticjty is good under light stimulus, but without luminescence response under heat and mechanical stimulus.Thus
It can be seen that most luminescent materials can only show good performance under some stimulations, it is difficult to realize collection power, heat, light thorniness
Swash the multifunction in response to one, limit the development and application of material to a certain extent.In order to realize that luminescent material exists
The practical application in Multifunction Sensor field, following requirement is proposed to luminescent material：Different wavelengths of light excites down, realizes luminous
The transformation of color；There are good luminescent properties under the effect of thermostimulation, ultrasound, friction, collision and compressor mechanical.
In addition, existing luminescent material generally needs outside doping lanthanide series or transition metal ions to be formed in the material
The effective centre of luminescence, environmental protection very urgent present limited in rare earth resources, exploitation do not need activator ion doping
Luminescent material be particularly important.Self-activate luminescence material do not need active ions doping, only by crystal itself the defects of
Can forms the centre of luminescence.Compared with the luminescent material of rare earth/transition metal doping, self-activate luminescence material has relatively low
Manufacturing cost, simpler production technology, gradually cause the extensive concern of people.
Therefore, develop has far reaching significance to the self-activate luminescence material of light, heat, the more stimuli responsives of power.
The content of the invention
It is open a kind of to the stimulation more of light, heat, power it is an object of the invention to overcome existing luminescent material multifunction deficiency
Self-activate luminescence material of response and preparation method thereof.
The chemical expression of self-activate luminescence material disclosed in this invention to light, heat, the more stimuli responsives of power is
CaxZnyOS, wherein the ＜ y ＜ 1 of 0.9 ＜ x ＜ 1,0.9.
Self-activate luminescence material disclosed in this invention to light, heat, the more stimuli responsives of power is prepared using high temperature solid-state method.
Preparation process comprises the following steps：
A) appropriate amount of deionized water or absolute ethyl alcohol are added, after being fully ground than weighing raw material respectively by element chemistry metering
Drying obtains mixed powder；
B) powder obtained by step a) is calcined at 900~1100 DEG C in protective atmosphere, the time is 3~15 hours；
C) by pulverized after the cooling of calcined product that step b) is obtained obtain to light, heat, the more stimuli responsives of power from
Activate luminescent material.
Prepare to light, heat, the more stimuli responsives of power self-activate luminescence material, it is characterised in that Ca using its carbonate, oxygen
Compound, sulfide or peroxide are raw material, and Zn uses zinc oxide or zinc sulphide as raw material.
Prepare to light, heat, the more stimuli responsives of power self-activate luminescence material, it is characterised in that protective atmosphere is selected from N2、
One or more mixed gas in He, Ar.
Obtained by the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, it is characterised in that 250~
The pink of emitting bright under 300nm ultraviolet excitations, the green light of emitting bright under 325~350nm ultraviolet excitations.
Obtained by the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, it is characterised in that in Spurs
There is good thermoluminescence performance under swashing, the temperature range that can be responded is -150~50 DEG C.
Obtained by the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, it is characterised in that ultrasound,
Friction, collision and compressor mechanical effect are lower to have stress irradiance performance, sends naked eyes visible green light.
Obtained by the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, it is characterised in that material category
In the lossless luminescent material of trap control type, its thermoluminescence and stress irradiance can recover after ultraviolet light irradiation.
Beneficial effects of the present invention are：
(1) it is of the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, it is anti-using traditional solid phase
Prepared by induction method, preparation technology is simple, condition is easily controlled, equipment requirement is low, cost is cheap, without toxic gas in preparation process
Generation, it is environmentally safe.
(2) it is of the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, without outside doping activation
Agent ion, belong to self-activate luminescence material, that is, save resource, and environmental protection.
(3) obtained luminescent material and optically transparent macromolecular material are mixed and made into thin slice or cylindrical type resin
Body, also or coated on the parts to be tested surface, its suffered mechanical external force can be converted to light in the case where not destroying material structure
It can send.
(4) it is of the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, be light harvesting, heat, power thorniness
Swash the Multifunctional luminous material being integrated of response, have to multiple stimulation high-resolution, response in time, high excellent of luminosity
Point.
(5) it is of the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, swash available for single light source
The luminous of hair, display, imaging art, such as the polychromatic source and display of ultraviolet excitation；Available for single thermal excitation it is luminous,
It has been shown that, such as imaging art, thermoluminescence；The luminous, display that is excited available for various single mechanisms, imaging, testing field,
Stress irradiance such as under ultrasound, friction, collision and compressor mechanical effect.
(6) it is of the present invention to light, heat, the more stimuli responsives of power self-activate luminescence material, more can be used for above-mentioned list
One light source, single thermostimulation, the multi-color illumination of two kinds of single mechanical stimulus and two or more excitaton source shootings on group, display,
Imaging art, such as there is multi-color illumination, display, the imaging art of luminescence generated by light and stress irradiance function simultaneously, while there is light
The multi-color illumination of photoluminescence and thermoluminescence function, display, imaging, testing field, while there is stress irradiance and thermoluminescence
The multi-color illumination of function, display, imaging, testing field, at the same have luminescence generated by light, thermoluminescence, stress irradiance function it is more
Color illumination, display, imaging, testing field.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction figure of the sample of embodiment 1.
Fig. 2 is the electron scanning micrograph of the sample of embodiment 1.
Fig. 3 is the excitation spectrum (monitoring 610nm transmittings) and emission spectrum of the sample of embodiment 1 (285nm is excited).
Fig. 4 is the excitation spectrum (monitoring 520nm transmittings) and emission spectrum of the sample of embodiment 1 (355nm is excited).
Fig. 5 is the thermoluminescence curve of the sample of embodiment 1.
Fig. 6 is the friction stree luminosity curve of the sample of embodiment 1.
Fig. 7 is the impact stresses luminosity curve of the sample of embodiment 1.
Fig. 8 is the ultrasonic stress irradiance curve of the sample of embodiment 1.
Fig. 9 is the compression stress luminosity curve of the sample of embodiment 1.
Figure 10 is the stress irradiance spectrum of the sample of embodiment 1.
Specific embodiment
Below by way of particular specific embodiment and with reference to accompanying drawing, the present invention will be described in more detail.It should be understood that this
The method and step that invention is mentioned does not repel also has other method and steps before and after the combination step, or is clearly carried at these
To the step of before can also insert other method and steps；It should also be understood that these embodiments are merely to illustrate the present invention and not had to
In limitation the scope of the present invention.Moreover, unless otherwise indicated, the numbering of various method steps is only to differentiate the facility of various method steps
Instrument, rather than ordering or the enforceable scope of the restriction present invention for limitation various method steps, the change of its relativeness
Or adjustment, in the case where changing technology contents without essence, when being also considered as the enforceable category of the present invention.
The present invention will be described in more detail by way of example and in conjunction with the accompanying drawings.
Specific embodiment of the invention 1-8 sample is prepared using high temperature solid phase synthesis, the material group of specific embodiment
Divide, raw material weight, protective atmosphere, calcining heat and time parameter are as shown in table 1.
Material component, raw material weight, calcining heat, time and the protective atmosphere of the embodiment 1-8 samples of table 1..
The luminescence generated by light, thermoluminescence, stress irradiance performance that specific embodiment of the invention 1-8 prepares material are as shown in table 2.
Luminescence generated by light, thermoluminescence and the stress irradiance performance of the embodiment 1-8 samples of table 2..
Sample appearance prepared by embodiment 1-8 is white, X-ray powder diffraction test result and CaZnOS powder diffraction marks
The diffraction data of quasi- card (01-072-3547) is consistent, and without dephasign, the sample for illustrating to obtain is pure phase CaZnOS structures.
Fig. 1 gives the X-ray powder diffraction figure of the sample of embodiment 1.Electron scanning micrograph shows that the present embodiment 1-8 prepares sample
Product are made up of closely coupled polycrystalline particle, and crystallite dimension is 2~5 μm.The scanning electron that Fig. 2 gives the sample of embodiment 1 shows
Micro mirror photo.As shown in table 2, embodiment 1-8 prepare sample and meanwhile have to light, heat, the more stimuli responsives of power luminescent properties.
The pink of embodiment 1-8 samples emitting bright under 250~300nm ultraviolet excitations.Fig. 3 gives the sample of embodiment 1
The photoemissive excitation spectrums of monitoring 610nm and the emission spectrum in the case where 285nm light excites.Embodiment 1-8 samples 325~
The green light of emitting bright under 350nm ultraviolet excitations.Fig. 3 gives the photoemissive exciting lights of sample monitoring 520nm of embodiment 1
Spectrum and the emission spectrum in the case where 355nm light excites.Embodiment 1-8 samples show thermoluminescence performance under thermostimulation, can respond
Temperature range be -150~50 DEG C.Fig. 5 gives the thermoluminescence curve of the sample of embodiment 1.Embodiment 1-8 samples are rubbing
Wipe, be respectively provided with stress irradiance performance under collision, ultrasound and compression, send macroscopic green light.Fig. 6-9 is provided respectively
Stress irradiance curve of the sample of embodiment 1 under friction, collision, ultrasound and compression.Figure 10 gives the sample of embodiment 1
Stress irradiance spectrum.
It is described above, it is only the explanation embodiment of the present invention, formal and substantial limitation not any to the present invention,
It should be pointed out that for those skilled in the art, on the premise of the inventive method is not departed from, that makes some changes
Enter and supplement and also should be regarded as protection scope of the present invention.All those skilled in the art, the spirit of the present invention is not being departed from
In the case of scope, the equivalent variations for a little variation, modification and evolution made using disclosed above technology contents,
For the equivalent embodiment of the present invention；Meanwhile any equivalent change that all substantial technologicals according to the present invention are done to above-described embodiment
The variation, modification and evolution of change, still fall within the scope of technical scheme.
Claims (2)
1. it is a kind of to light, heat, the more stimuli responsives of power self-activate luminescence material, it is characterised in that the chemical expression of the material
For CaxZnyOS, wherein the ＜ y ＜ 1 of 0.9 ＜ x ＜ 1,0.9；The powder of material emitting bright under 250~300nm ultraviolet excitations
Red light；The green light of material emitting bright under 325~350nm ultraviolet excitations；The material has heat under thermostimulation
Release luminescent properties；The material has stress irradiance performance under friction, collision, ultrasound and compression, sends main peak and is located at
Naked eyes visible green light at 520nm；The material can be used as stimulating the multifunctional sensing in response to one in collection power, heat, light more
Device.
2. as claimed in claim 1 to light, heat, the more stimuli responsives of power self-activate luminescence material preparation method, its feature
It is, Ca uses its carbonate, oxide, sulfide or peroxide as raw material, and Zn uses zinc oxide or zinc sulphide as raw material,
In N2, one or more mixed gas in He, Ar protective atmosphere in prepared using solid phase synthesis process, preparation process includes
Following steps：
A) appropriate amount of deionized water or absolute ethyl alcohol are added, is dried after being fully ground than weighing raw material respectively by element chemistry metering
Obtain mixed powder；
B) powder obtained by step a) is calcined at 900~1100 DEG C in protective atmosphere, the time is 3~15 hours；
C) by the self-activation obtained to light, heat, the more stimuli responsives of power of being pulverized after the cooling of calcined product that step b) is obtained
Luminescent material.
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| CN201710309971.8A CN107488448A (en) | 2017-04-28 | 2017-04-28 | It is a kind of to light, heat, the more stimuli responsives of power self-activate luminescence material and preparation method thereof |
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| CN201710309971.8A CN107488448A (en) | 2017-04-28 | 2017-04-28 | It is a kind of to light, heat, the more stimuli responsives of power self-activate luminescence material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061362A (en) * | 2021-04-07 | 2021-07-02 | 昆明理工大学 | Preparation method of stress luminescent coating of high-sensitivity mechanical stimulus response sphere |
| US11203714B2 (en) | 2018-07-19 | 2021-12-21 | Qingdao University | Luminescent material and preparation method thereof |
| CN114316954A (en) * | 2022-01-13 | 2022-04-12 | 山东大学 | Metal oxysulfide free of activated ion force luminescence, preparation method and application thereof |
| WO2022186378A1 (en) * | 2021-03-05 | 2022-09-09 | 国立研究開発法人産業技術総合研究所 | Stress-stimulated luminescent material and method for producing said stress-stimulated luminescent material |
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| CN105400511A (en) * | 2015-09-15 | 2016-03-16 | 青岛大学 | Multifunctional luminescent material with adjustable light color and high brightness as well as application thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105400511A (en) * | 2015-09-15 | 2016-03-16 | 青岛大学 | Multifunctional luminescent material with adjustable light color and high brightness as well as application thereof |
Non-Patent Citations (2)
| Title |
|---|
| BOLONG HUANG: "Energy harvesting and conversion mechanisms for intrinsic upconverted mechano-persistent luminescence in CaZnOS", 《PHYSICAL CHEMISTRY CHEMICAL PHYSICS》 * |
| R.I.GULYAEVA ET AL: "Chemism and Kinetics of the Oxidation of Zinc–Calcium Oxysulfide", 《RUSSIAN METALLURGY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11203714B2 (en) | 2018-07-19 | 2021-12-21 | Qingdao University | Luminescent material and preparation method thereof |
| WO2022186378A1 (en) * | 2021-03-05 | 2022-09-09 | 国立研究開発法人産業技術総合研究所 | Stress-stimulated luminescent material and method for producing said stress-stimulated luminescent material |
| CN113061362A (en) * | 2021-04-07 | 2021-07-02 | 昆明理工大学 | Preparation method of stress luminescent coating of high-sensitivity mechanical stimulus response sphere |
| CN113061362B (en) * | 2021-04-07 | 2021-12-14 | 昆明理工大学 | Preparation method of stress luminescent coating of high-sensitivity mechanical stimulus response sphere |
| CN114316954A (en) * | 2022-01-13 | 2022-04-12 | 山东大学 | Metal oxysulfide free of activated ion force luminescence, preparation method and application thereof |
| CN114316954B (en) * | 2022-01-13 | 2022-11-15 | 山东大学 | Metal oxysulfide free of activated ion force luminescence, preparation method and application thereof |
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