CN113249118A - Cyan mechanoluminescence material applied to low-temperature detection and preparation method and application thereof - Google Patents
Cyan mechanoluminescence material applied to low-temperature detection and preparation method and application thereof Download PDFInfo
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- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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- C09K11/0883—Arsenides; Nitrides; Phosphides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/16—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge
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- 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
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Abstract
The invention provides a cyan mechanoluminescence material, which can realize material damage detection under the low temperature condition of-270 ℃ to-50 ℃, and has the chemical general formula of Ba(1‑X)Si2O2N2:Eu2+ (X)Wherein, the value range of X is as follows: x is more than or equal to 0.0001 and less than or equal to 0.5, and the distribution range of traps is-270 ℃ to 400 ℃. The invention also provides a preparation method and application of the cyan mechanoluminescence material. The cyan mechanoluminescence material of the present invention, Eu is used2+The energy is stored in the electron trap as a light absorption center after absorbing visible light, is used for detection application under a low temperature condition, and is more beneficial to damage detection application under a very low temperature.
Description
Technical Field
The invention belongs to the technical field of material damage detection, and relates to a cyan mechanoluminescence material for realizing material damage detection under a low-temperature condition, and a preparation method and application thereof.
Background
With the increase of the load, the material has new damage phenomena of abrasion, fracture, abnormal deformation and the like, and the service life of the material is influenced, so that the monitoring of the damage of the material is an important means for guaranteeing related facilities. The mechanoluminescence material is one of common materials for monitoring material damage, and the principle is that a luminescence center and a trap energy level exist in the mechanoluminescence material, under specific illumination, light-excited electrons enter the trap energy level and are stored, when the mechanoluminescence material is subjected to external stress, electrons in the trap of the mechanoluminescence material absorb stress energy, the stress energy is released from the trap and returns to a luminescence center ion to realize luminescence, and the detection of the material damage can be realized by monitoring a light signal. For example, after the mechanoluminescence material on the detected material stores electrons in the trap through specific illumination, when the detected material is damaged, the released stress acts on the mechanoluminescence material, the electrons return to the luminescence center from the trap to realize local luminescence of the damaged position, and the detection system obtains a local luminescence signal to obtain information such as the position, the size, the damage degree and the like of the damaged part.
The depth of the trap energy level is an important property of the mechanoluminescence material, and the deeper the depth, the more mechanical energy the electrons need to be released, and the lower the sensitivity of detection. At the same time, in addition to mechanical energy, temperature can also cause electrons in traps to be released. The higher the temperature, the higher the energy of the electrons and the more likely they are to be released from the traps, a phenomenon known as thermal fluctuation of electrons. Therefore, the depth of the trap is usually described by temperature, the luminous brightness of the mechanoluminescence material is detected at different temperatures by heating the mechanoluminescence material, the brightness is regarded as the concentration of the trap, the temperature corresponding to the strongest luminous intensity is usually regarded as the depth of the trap, and therefore, the temperature is an important parameter for measuring the depth of the mechanoluminescence material trap. All current research focuses on room temperature, since most materials are used at room temperature, and the mechanoluminescence materials applied at low temperature, especially at very low temperature lower than-50 ℃, are only reported, and the relevant properties cannot be deduced from the materials applied at room temperature.
In practical application, a plurality of scenes of extremely low temperature application below room temperature exist, for example, projects such as railway laying, bridge building, cable and optical cable laying, scientific research station building and the like in plateau, mountain and polar regions face the risk of abnormal damage of materials, if the maintenance cannot be confirmed in time, on one hand, the risks are brought to related facility users, and on the other hand, the damage of large-scale infrastructure influences related basic activities. The lowest temperature of the Jolmus peak reaches-50 ℃, and the annual average temperature is-20 ℃; the lowest temperature in the desert river can reach-51 ℃; the lowest temperature of Antarctic can reach-89 ℃. In laboratories and factories, liquid nitrogen and liquid helium storage equipment and pipelines, and liquid nitrogen vaccine tanks, the temperature of which is reduced to-196 ℃ (liquid nitrogen) and-270 ℃ (liquid helium), and the stable maintenance of the equipment is also significant. When the satellite and the aerospace facility simulate the detection of materials at extreme temperatures, the low temperature needs to be detected to the low temperature limit, namely, the temperature is close to absolute zero (-273.15 ℃).
At very low temperatures, the application of conventional mechanoluminescence materials is limited because the depth of the trap, which facilitates the release of electrons, is a relative concept. For example, for a mechanoluminescence material having a trap depth of 50 ℃ relative to room temperature, at a low temperature of-50 ℃ the trap depth becomes 100 ℃ and sensitive detection of material damage is lost. The materials reported at present are mainly the mechanoluminescence materials applied at room temperature, which cause the application sensitivity to be reduced due to the lack of low-temperature trap energy level at low temperature and even lose the stress detection capability at extremely low temperature (such as-270 ℃). Therefore, it is necessary to research a novel mechanoluminescence material with a trap level depth lower than-50 ℃ and realize the application of material damage detection under low temperature conditions.
Disclosure of Invention
In view of the above, the present invention provides a cyan electroluminescent material, and a preparation method and an application thereof, wherein the cyan electroluminescent material has trap energy levels continuously distributed at-270 ℃ to 400 ℃, and can realize electroluminescent at a low temperature of-270 ℃ to-50 ℃, so as to realize material damage detection.
In order to achieve the above purpose, the present invention provides a cyan mechanoluminescence material for low temperature detection, wherein the low temperature is-270 ℃ to-50 ℃, and the chemical general formula of the material is Ba(1-X)Si2O2N2:Eu2+ (X)Wherein, the value range of X is as follows: x is more than or equal to 0.0001 and less than or equal to 0.5, and the distribution range of traps is-270 ℃ to 400 ℃.
The invention also provides a preparation method of the cyan mechanoluminescence material, which comprises the following steps:
(1) weighing the raw material BaCO according to the stoichiometric ratio3、SiO2、Eu2O3Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling for 24h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying for 19h at 60 ℃, taking out and sieving to obtain uniformly dispersed powder;
(2) putting the powder in a crucible, placing the crucible in a tubular furnace, introducing a mixed gas of 10% hydrogen and 90% nitrogen in volume ratio, and sintering at 1200 ℃ for 6h to obtain Ba(2-2X)SiO4:Eu2+ (2X)；
(3) Weighing raw material Ba according to stoichiometric ratio(2-2X)SiO4:Eu2+ (2X)、Si3N4(ii) a Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling 1.5h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying the slurry mixture for 19h at 60 ℃, taking out the slurry mixture, and sieving the slurry mixture to obtain uniformly dispersed powder;
(4) putting the powder into a crucible, putting the crucible into a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, sintering the powder for 3 to 6 hours at 1350 to 1500 ℃ to obtain Ba(1-X)Si2O2N2:Eu2+ (X)。
The invention also provides an application of the cyan mechanoluminescence material in material damage or abnormality detection, which comprises the following steps:
the cyan mechanoluminescence material is placed on the surface or inside of an object to be detected, and is excited for 5-15min by ultraviolet light with the wavelength of 254nm, the mechanoluminescence material is excited to emit light according to stress released when the object to be detected is damaged, and then the damage or abnormal condition of the object to be detected is evaluated by analyzing optical signals.
Further, the cyan mechanoluminescence material is placed on the surface or inside of the object to be detected, specifically:
preparing the cyan mechanoluminescence material into suspension, ink or paint of powder particles, and combining the suspension, ink or paint of powder particles with the surface of an object to be detected by adopting spraying, spin coating or printing technology;
or, the cyan mechanoluminescence material is directly doped in the synthesis process of the object to be detected and is combined in the object to be detected.
Further, when the cyan mechanoluminescence material is prepared into printing ink or coating, the addition amount of the cyan mechanoluminescence material is 1-30 wt%;
the ink or coating is an organic resin system;
when the cyan mechanoluminescence material is directly doped into the object to be detected, the addition amount is 1-30 wt%.
Further characterized in that the printing technique is selected from any one of dispensing, ink jet printing, water transfer printing, screen printing, and roll-to-roll printing.
Further, the object to be detected is a rigid object to be detected or a flexible object to be detected;
the object to be detected is any one of glass, silicon, metal alloy, ceramic, cement, wood and stone;
the flexible object to be detected is any one of a PDMS film, a PET film, a PS film, a PU film, a PI film and a PVA film.
Further, the method is suitable for application in crack prediction of the adhesive, and comprises the following steps:
the cyan mechanoluminescence material is directly doped in the synthesis process of the adhesive and is combined in the adhesive, after an adhesive layer is constructed and formed, the stress released when abnormality occurs is excited for 5-15min by ultraviolet light with the wavelength of 254nm to excite the mechanoluminescence material to emit light, and then the stress distribution in the adhesive layer is obtained through analysis of optical signals, so that the stress distribution is visualized, and the crack prediction of the adhesive is realized.
Further, the method is suitable for application in structural part degradation detection, and comprises the following steps:
the cyan mechanoluminescence material is placed on the surface of a structural member, and is excited for 5-15min by ultraviolet light with the wavelength of 254nm, the stress released when the structural member is degraded excites the mechanoluminescence material to emit light, further, the stress distribution of the structural member is obtained by analyzing optical signals, and a stress-strain curve is obtained by combining strain measurement results.
The invention adopts the technical scheme that the method has the advantages that:
the cyan mechanoluminescence material has trap energy levels continuously distributed at the temperature of-270 ℃ to 400 ℃, particularly has ultra-shallow trap energy levels at the temperature of-270 ℃ to-50 ℃, can obtain sensitive damage detection under the condition of ultra-low temperature through the electron capture capacity of the ultra-shallow energy levels at low temperature, and provides a material for detecting material damage for simulating the material tolerance detection under the ultra-low temperature of some low-temperature environments, such as bridges, railways and other infrastructure facilities in Qinghai-Tibet plateau, northeast region, polar region and the like, materials for maintaining the ultra-low temperature environment, satellites and aerospace facilities. Due to the fact that the material has the deep trap with the temperature of more than 150 ℃, the material can be moved to room temperature for maintenance operation such as replacement and maintenance after damage is found at low temperature, recheck during repair can be conducted through light excitation during maintenance, for example, under the irradiation of a 980nm wavelength laser, the damaged part can emit light obviously stronger than other parts, and the damaged part can be conveniently confirmed after moving. The damage of the material under the extreme low temperature condition can be remotely monitored in real time by monitoring the image or the luminous signal or simultaneously monitoring the image and the luminous signal, and the change of the material can be found as soon as possible.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a plot of the pyroelectric spectrum at-190 ℃ to 500 ℃ for the material synthesized in example 3;
FIG. 2 is an emission spectrum of the synthesized material in example 3 under excitation of light (L1 is an excitation spectrum of an emission peak monitored at a wavelength of 495nm at-190 ℃; L2 is an emission spectrum under excitation of light at a wavelength of 405nm at-190 ℃);
FIG. 3 is a spectrum of the material synthesized in example 3 (L3 is an afterglow spectrum at-190 ℃ for 5 minutes after excitation with a 254nm wavelength light; L4 is a mechanoluminescence spectrum at-190 ℃);
FIG. 4 is a plot of the pyroelectric spectrum at-270 ℃ to 0 ℃ for the material synthesized in example 3;
FIG. 5 is a pyroelectric spectrum at-190 ℃ to 300 ℃ of the synthetic materials of example 3 and comparative example (T1 is a pyroelectric spectrum of the synthetic material of example 3, and T0 is a pyroelectric spectrum of the synthetic material of comparative example).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The phenomenon of mechanoluminescence has been observed for a long time, but the excitation mechanism and the excitation state source of the mechanoluminescence have not been completely determined so far, and a person skilled in the art generally describes the phenomenon of mechanoluminescence, does not clarify the light-emitting source and mechanism of the mechanoluminescence, but only considers that factors influencing the mechanoluminescence are many, and even if substances of the same element have different preparation conditions (such as element concentration ratio, sintering temperature and sintering time during refining the substances), different pressures and different stress intensities, the mechanoluminescence performance has great difference. Therefore, it is of great theoretical and practical significance to research which factors are related to the mechanoluminescence, how to select the most suitable experimental conditions and synthesize the mechanoluminescence in a targeted manner.
The invention provides a cyan mechanoluminescence material with the chemical general formula of Ba(1-X)Si2O2N2:Eu2+ (X)Wherein, the value range of X is as follows: x is more than or equal to 0.0001 and less than or equal to 0.5, and the distribution range of traps is-270 ℃ to 400 ℃.
The cyan mechanoluminescence material of the present invention, Eu is used2+As a light absorption center, energy is stored in the electron trap after absorbing visible light for subsequent detection applications. Further, Eu2+As luminescence center, the energy stored in the trap is returned to Eu2+The blue light is emitted, and the high-sensitivity damage detection of the material at extremely low temperature (lower than minus 50 ℃) can be realized.
The invention also provides a preparation method of the cyan mechanoluminescence material, which comprises the following steps:
(1) weighing the raw material BaCO according to the stoichiometric ratio3、SiO2、Eu2O3Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling for 24h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying for 19h at 60 ℃, taking out and sieving to obtain uniformly dispersed powder;
(2) putting the powder in a crucible, placing the crucible in a tubular furnace, introducing a mixed gas of 10% hydrogen and 90% nitrogen in volume ratio, and sintering at 1200 ℃ for 6h to obtain Ba(2-2X)SiO4:Eu2+ (2X)；
(3) Weighing raw material Ba according to stoichiometric ratio(2-2X)SiO4:Eu2+ (2X)、Si3N4(ii) a Using a planet ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling 1.5h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying the slurry mixture for 19h at 60 ℃, taking out the slurry mixture, and sieving the slurry mixture to obtain uniformly dispersed powder;
(4) putting the powder into a crucible, putting the crucible into a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, sintering the powder for 3 to 6 hours at 1350 to 1500 ℃ to obtain Ba(1-X)Si2O2N2:Eu2+ (X)。
The invention also provides an application of the cyan mechanoluminescence material in material damage or abnormality detection, which comprises the following steps:
the cyan mechanoluminescence material is placed on the surface or inside of an object to be detected, and is excited for 5-15min by ultraviolet light with the wavelength of 254nm, the mechanoluminescence material is excited to emit light according to stress released when the object to be detected is damaged, and then the damage or abnormal condition of the object to be detected is evaluated by analyzing optical signals.
Wherein, the cyan mechanoluminescence material is placed on the surface or inside of an object to be detected, the addition amount of the cyan mechanoluminescence material is 1-30 wt%, preferably 5-10 wt%, and specifically comprises the following steps: preparing the cyan mechanoluminescence material into suspension, ink or paint of powder particles, and combining the suspension, ink or paint of powder particles with the surface of an object to be detected by adopting spraying, spin coating or printing technology; or, the cyan mechanoluminescence material is directly doped in the synthesis process of the object to be detected and is combined in the object to be detected.
Specifically, a suspension of cyan mechanoluminescence material powder particles may be coated on the surface of the material to be detected, for example, a coating method such as spray coating, spin coating, or the like may be used, and a printing technique may also be used. The printing technique is preferably used to print a suspension of cyan mechanoluminescence material powder particles on the surface of the material to be detected. Wherein the printing technique may be selected from one of dispensing, ink jet printing, water transfer printing, screen printing, and roll-to-roll printing. When a suspension of cyan mechanoluminescence material powder particles is printed on the surface of a material to be detected by a printing technique, the suspension is preferably prepared into ink by blending and stirring or blending and ultrasonically dispersing the suspension.
When the cyan electroluminescent material is prepared into ink or paint, the ink comprises ink conventional components and cyan electroluminescent material powder, and the paint comprises paint conventional components and cyan electroluminescent material powder; the ink or coating is an organic resin system. The ink or the coating may be either aqueous or nonaqueous.
The object to be detected can be a rigid object to be detected or a flexible object to be detected. The rigid object to be detected may be selected from glass, silicon, metal or alloy, ceramic, cement, wood and stone, and the flexible object to be detected may be selected from PDMS (polydimethylsiloxane) film, PET (polyethylene terephthalate) film, PS (polystyrene) film, PU (polyurethane) film, PI (polyimide) film and PVA (polyvinyl alcohol) film.
The cyan mechanoluminescence material is contained on the outer surface of a polymer material such as general paper, synthetic paper, epoxy resin, polyethylene terephthalate, polyester, polypropylene, polyvinyl chloride, natural rubber or synthetic rubber, glass, ceramics, metal, wood, artificial fiber or natural fiber, concrete, or a combination thereof, or a processed product thereof, or the cyan mechanoluminescence material is contained in the interior of the container, whereby abnormality can be detected. The deterioration of various structures and members can be diagnosed by applying a shock wave (stress-strain detection, stress distribution measurement), for example, in a medium-high altitude area: large structures such as buildings, viaducts, bridges, roads, rails, pillars, towers, pipelines, tunnels, floor materials, tiles, wall materials, prefabricated plate materials, paving materials, building materials such as wood, steel, and concrete, transmission members such as gears and cams, exterior parts or interior parts (engine parts, tires, belts, and the like) used in bicycles, automobiles, electric trains, ships, and airplanes, bearing parts, bearing retainers, and connecting parts such as bearings with optical sensors, screws, nuts, and washers, and the like. Further, the internal stress distribution in the adhesive layer of the adhesive containing a cyan mechanoluminescence material can be visualized, and the cracking of the adhesive at low temperature can be grasped.
Comparative example:
to illustrate the effect of the cyan electroluminescent material of the present invention, SrAl was selected2O4Eu and Dy fluorescent powder is taken as a comparative example.
Example 1:
a cyan mechanoluminescence material was prepared as follows:
(1) in stoichiometric termsWeighing raw material BaCO3、SiO2、Eu2O3Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling the slurry mixture for 24 hours with alcohol at a ratio of 1:1:0.05, placing the obtained slurry mixture in an oven at 60 ℃, keeping the temperature and drying for 19 hours, taking out and sieving to obtain uniformly dispersed powder;
(2) putting the powder in a crucible, putting the crucible in a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, and sintering the powder at 1200 ℃ for 6 hours to obtain Ba1.9998SiO4:Eu2+ 0.0002；
(3) Weighing raw material Ba according to stoichiometric ratio1.9998SiO4:Eu2+ 0.0002、Si3N4(ii) a Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling 1.5h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying the slurry mixture for 19h at 60 ℃, taking out the slurry mixture, and sieving the slurry mixture to obtain uniformly dispersed powder;
(4) putting the powder in a crucible, putting the crucible in a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, and sintering the powder at 1430 ℃ for 4 hours to obtain Ba0.9999Si2O2N2:Eu2+ 0.0001。
The materials of the example 1 and the comparative example are uniformly mixed in polydimethylsiloxane according to 10 wt%, and are solidified for 120min at 120 ℃ to prepare soft films, the two soft films are placed in liquid nitrogen and are excited for 5min by ultraviolet light with the wavelength of 254nm, and the soft films in the liquid nitrogen are extruded, scratched, pulled and torn, so that the soft films of the materials of the example 1 can have obvious visible glow at stressed positions under the stress, and the soft films of the comparative example have no glow.
Example 2:
a cyan mechanoluminescence material was prepared as follows:
(1) weighing the raw material BaCO according to the stoichiometric ratio3、SiO2、Eu2O3Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling the slurry mixture for 24 hours with alcohol at a ratio of 1:1:0.05, placing the obtained slurry mixture in an oven at 60 ℃, keeping the temperature and drying for 19 hours, taking out and sieving to obtain uniformly dispersed powder;
(2) putting the powder in a crucible, putting the crucible in a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, and sintering the powder at 1200 ℃ for 6 hours to obtain Ba1.0SiO4:Eu2+ 1.0；
(3) Weighing raw material Ba according to stoichiometric ratio1.0SiO4:Eu2+ 1.0、Si3N4(ii) a Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling 1.5h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying the slurry mixture for 19h at 60 ℃, taking out the slurry mixture, and sieving the slurry mixture to obtain uniformly dispersed powder;
(4) putting the powder in a crucible, putting the crucible in a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, and sintering the powder at 1430 ℃ for 4 hours to obtain Ba0.5Si2O2N2:Eu2+ 0.5。
The cyan mechanoluminescence material is uniformly mixed in a glass batch according to 10 wt% to be fired into a glass rod containing the cyan mechanoluminescence material, the glass rod is excited for 15min by ultraviolet light with the wavelength of 254nm, the glass rod is placed in an environment with the temperature of 50 ℃ below zero, the glass rod is knocked, when the glass rod is cracked, obvious visible glow can be formed according to the cracked lines of the glass rod, and the glow can be detected by a spectrometer.
Example 3:
a cyan mechanoluminescence material was prepared as follows:
(1) weighing the raw material BaCO according to the stoichiometric ratio3、SiO2、Eu2O3Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling the slurry mixture for 24 hours with alcohol at a ratio of 1:1:0.05, placing the obtained slurry mixture in an oven at 60 ℃, keeping the temperature and drying for 19 hours, taking out and sieving to obtain uniformly dispersed powder;
(2) putting the powder in a crucible, putting the crucible in a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, and sintering the powder at 1200 ℃ for 6 hours to obtain Ba1.96SiO4:Eu2+ 0.04；
(3) Weighing raw material Ba according to stoichiometric ratio1.96SiO4:Eu2+ 0.04、Si3N4(ii) a By means of planetary ball millsThe raw materials by weight ratio: ball: ball-milling 1.5h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying the slurry mixture for 19h at 60 ℃, taking out the slurry mixture, and sieving the slurry mixture to obtain uniformly dispersed powder;
(4) putting the powder in a crucible, putting the crucible in a tubular furnace, introducing 10 percent hydrogen-nitrogen mixed gas, and sintering the powder at 1430 ℃ for 4 hours to obtain Ba0.98Si2O2N2:Eu2+ 0.02。
Since the properties of the composite materials of examples 1-2 and this example are similar, only the properties of the cyan electroluminescent material synthesized in this example will be described, and are characterized as follows:
FIG. 1 is a thermoluminescence spectrum of the synthesized material at-190 ℃ to 500 ℃, and it can be seen that the trap energy levels of the material are distributed in the temperature range of-190 ℃ to 400 ℃, wherein the lower the temperature, the greater the number of trap energy levels, and the higher the luminescence intensity of the low-temperature trap is than the room-temperature trap intensity, thus proving the advantage of the material in the extremely low-temperature detection.
FIG. 2 shows the emission spectrum of the synthesized material in this example under excitation of light (L1 is an excitation spectrum monitored at-190 ℃ for emission peak at 495nm wavelength; L2 is an emission spectrum under excitation of light at-190 ℃ for 405nm wavelength). FIG. 3 is a spectrum of the material synthesized in this example (L3 is an afterglow spectrum at-190 ℃ C. after excitation with 254nm wavelength light for 5 minutes; L4 is a mechanoluminescence spectrum at-190 ℃ C.). From fig. 2 and fig. 3, it can be known that the excitation emission spectrum, the afterglow and the force-induced emission spectrum obtain the wavelength position of the optical signal which can be monitored, and the instantaneous amplification of the peak intensity of the damage instantaneous emission spectrum can be obtained by monitoring the emission spectrum, so as to achieve the effect of detecting the damage.
FIG. 4 is a thermoluminescence spectrum of the synthesized material at-270 ℃ to 0 ℃, from which it can be observed that the trap level distribution exists in the material at-270 ℃ to 0 ℃, and the strongest peak of the trap level distribution is located at-255 ℃, which proves the advantage of the material in the detection of extremely low temperature.
The cyan mechanoluminescence material in this example was uniformly mixed in an epoxy resin in an amount of 10% by weight and cured at 120 ℃ for 20min to prepare a film fixed on a glass plate. The film is excited by ultraviolet light with the wavelength of 254nm for 5min at room temperature, extruded and scratched, weak glow can be seen, and weak images and luminescent signals can be acquired along cracks of broken glass sheets; the soft film is placed in liquid nitrogen (-190 ℃), is excited for 5min by ultraviolet light with the wavelength of 254nm, is extruded and scratched, and bright glow can be observed, and strong images and luminous signals can be acquired along cracks of broken glass sheets.
For comparison, the comparative example material 10 wt% was uniformly mixed in an epoxy resin under the same conditions, and cured at 120 ℃ for 20min to prepare a film fixed on a glass plate. The film is excited by ultraviolet light with the wavelength of 254nm for 5min at room temperature, extruded and scratched, bright glow can be seen, and weak images and luminescent signals can be acquired along cracks of broken glass sheets; the soft film is placed in liquid nitrogen (-190 ℃), is excited for 5min by ultraviolet light with the wavelength of 254nm, is extruded and scratched, and is not observed with glow, and broken glass sheets can not be observed with luminescence along cracks of the glass sheets and can not be acquired with images and luminescence signals.
Comparing the pyroelectric spectrograms of the two materials at-190 ℃ to 300 ℃, namely, fig. 5, it can be seen from the figures that the difference of traps of the two materials at low temperature (-190 ℃ to-50 ℃) is obvious, which shows that the cyan mechanoluminescence material in the embodiment can realize low-temperature detection, while the material in the comparative example has better force-induced detection performance at normal temperature, but cannot be applied in low-temperature detection, and the cyan mechanoluminescence material in the embodiment has outstanding beneficial effects.
The cyan mechanoluminescence material has trap levels continuously distributed at the temperature of-270 ℃ to 400 ℃, particularly has ultra-shallow trap levels at the temperature of-270 ℃ to-50 ℃, can obtain sensitive damage detection under the condition of ultra-low temperature through the electron capture capacity of the ultra-shallow trap levels at low temperature, and provides material damage detection for infrastructure facilities of bridges, railways and the like in some low-temperature environments, such as Qinghai-Tibet plateau, northeast region, polar region and the like. Due to the fact that the material has the deep trap with the temperature of more than 150 ℃, the material can be moved to room temperature for maintenance operation such as replacement and maintenance after damage is found at low temperature, recheck during repair can be conducted through light excitation during maintenance, for example, under the irradiation of a 980nm wavelength laser, the damaged part can emit light obviously stronger than other parts, and the damaged part can be conveniently confirmed after moving. The damage of the material under the extremely low temperature condition can be remotely monitored in real time by monitoring the image or the luminous signal or monitoring the image and the luminous signal simultaneously, and the change of the material can be found as soon as possible.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The cyan mechanoluminescence material applied to low-temperature detection is characterized in that the low temperature is-270 ℃ to-50 ℃, and the chemical general formula of the material is Ba(1-X)Si2O2N2:Eu2+ (X)Wherein, the value range of X is as follows: x is more than or equal to 0.0001 and less than or equal to 0.5, and the distribution range of traps is-270 ℃ to 400 ℃.
2. A method of preparing a cyan mechanoluminescence material as claimed in claim 1, characterized by comprising the steps of:
(1) weighing the raw material BaCO according to the stoichiometric ratio3、SiO2、Eu2O3Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball-milling for 24h with alcohol at a ratio of 1:1:0.05 to obtain a slurry mixture, placing the slurry mixture in an oven, keeping the temperature and drying for 19h at 60 ℃, taking out and sieving to obtain uniformly dispersed powder;
(2) putting the powder in a crucible, placing the crucible in a tubular furnace, introducing a mixed gas of 10% hydrogen and 90% nitrogen in volume ratio, and sintering at 1200 ℃ for 6h to obtain Ba(2-2X)SiO4:Eu2+ (2X)；
(3) Weighing raw material Ba according to stoichiometric ratio(2-2X)SiO4:Eu2+ (2X)、Si3N4(ii) a Using a planetary ball mill to prepare the following raw materials in percentage by weight: ball: ball milling 1.5h with 1:1:0.05 alcohol to obtain slurry mixture, placing in oven, and oven drying at 60 deg.CDrying for 19h, taking out and sieving to obtain uniformly dispersed powder;
(4) putting the powder in a crucible, placing the crucible in a tubular furnace, introducing mixed gas of 10% hydrogen and 90% nitrogen in volume ratio, and sintering at 1350-1500 ℃ for 3-6 h to obtain Ba(1-X)Si2O2N2:Eu2+ (X)。
3. Use of a cyan mechanoluminescence material according to claim 1 for the detection of damage or abnormality to a material comprising the steps of:
the cyan mechanoluminescence material is placed on the surface or inside of an object to be detected, and is excited for 5-15min by ultraviolet light with the wavelength of 254nm, the cyan mechanoluminescence material is excited to emit light according to stress released when the object to be detected is damaged, and then the damage or abnormal condition of the object to be detected is evaluated by analyzing optical signals.
4. Use according to claim 3, wherein the cyan mechanoluminescence material is placed on the surface or inside the object to be detected, in particular:
preparing the cyan mechanoluminescence material into suspension, ink or paint of powder particles, and combining the suspension, ink or paint of powder particles with the surface of an object to be detected by adopting spraying, spin coating or printing technology;
or, the cyan mechanoluminescence material is directly doped in the synthesis process of the object to be detected and is combined in the object to be detected.
5. The use according to claim 4, wherein the cyan electroluminescent material is added in an amount of 1-30 wt% when the cyan electroluminescent material is made into an ink or a coating;
the ink or the coating is an organic resin system;
when the cyan mechanoluminescence material is directly doped into the object to be detected, the addition amount is 1-30 wt%.
6. Use according to claim 4, wherein the printing technique is selected from any one of dispensing, ink jet printing, water transfer printing, screen printing and roll-to-roll printing.
7. The use according to claim 3, wherein the object to be detected is a rigid object to be detected or a flexible object to be detected;
the object to be detected is any one of glass, silicon, metal alloy, ceramic, cement, wood and stone;
the flexible object to be detected is any one of a PDMS film, a PET film, a PS film, a PU film, a PI film and a PVA film.
8. Use according to claim 3, for use in crack prediction of adhesives, comprising the steps of:
the cyan mechanoluminescence material is directly doped in the synthesis process of the adhesive and is combined in the adhesive, after an adhesive layer is constructed and formed, the ultraviolet light with the wavelength of 254nm excites for 5-15min, the stress released when abnormality occurs excites the mechanoluminescence material to emit light, and then the stress distribution in the adhesive layer is obtained through analysis of a material luminescence image and an optical signal, so that the stress distribution is visualized, and the crack prediction of the adhesive is realized.
9. The use according to claim 3, adapted for use in structural component degradation detection, comprising the steps of:
the cyan mechanoluminescence material is placed on the surface of a structural member, and is excited for 5-15min by ultraviolet light with the wavelength of 254nm, the stress released when the structural member is degraded excites the mechanoluminescence material to emit light, further, the stress distribution of the structural member is obtained by analyzing a material luminescence image and an optical signal, a stress-strain curve is obtained by combining a strain measurement result, and the degradation degree is evaluated.
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