CN113061362A - A kind of preparation method of stress luminescent coating of highly sensitive mechanical stimulus-responsive spheres - Google Patents

A kind of preparation method of stress luminescent coating of highly sensitive mechanical stimulus-responsive spheres Download PDF

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CN113061362A
CN113061362A CN202110371624.4A CN202110371624A CN113061362A CN 113061362 A CN113061362 A CN 113061362A CN 202110371624 A CN202110371624 A CN 202110371624A CN 113061362 A CN113061362 A CN 113061362A
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徐旭辉
吕鸿宇
刘志超
吴涛
余雪
邱建备
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Kunming University of Science and Technology
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Abstract

本发明涉及一种高灵敏机械刺激响应球体的应力发光涂层的制备方法，属于应力发光材料技术领域。本发明将高纯的SrCO3、Ga2O3和Tb4O7进行研磨混匀得到混合粉料A；混合粉料A置于温度为1300～1350℃、还原气氛中高温烧结6～8h，研磨得到SrGa2O4:Tb3+应力发光粉；SrGa2O4:Tb3+应力发光粉与PDMS胶体混合均匀得到混合液体，混合液体均匀涂覆在球体表面，保鲜膜包覆后加热固化涂覆层的胶体，得到高灵敏机械刺激响应球体的应力发光涂层。本发明SrGa2O4:Tb3+应力发光材料在紫外激发下具有优异的应力发光性能，其作为涂覆球体表面后可产生高灵敏机械刺激响应的应力发光。The invention relates to a preparation method of a stress luminescent coating of a highly sensitive mechanical stimulus responsive sphere, and belongs to the technical field of stress luminescent materials. In the present invention, high-purity SrCO 3 , Ga 2 O 3 and Tb 4 O 7 are ground and mixed to obtain a mixed powder A; Grinding to obtain SrGa 2 O 4 : Tb 3+ stress luminescent powder; SrGa 2 O 4 : Tb 3+ stress luminescent powder and PDMS colloid are evenly mixed to obtain a mixed liquid, the mixed liquid is uniformly coated on the surface of the sphere, and heated and cured after being covered with a plastic wrap Coated colloids to obtain stress-luminescent coatings on spheres that respond to highly sensitive mechanical stimuli. The SrGa 2 O 4 :Tb 3+ stress luminescent material of the present invention has excellent stress luminescence performance under ultraviolet excitation, and can generate stress luminescence with highly sensitive mechanical stimulation response after coating the surface of the sphere.

Description

Preparation method of stress luminescent coating of high-sensitivity mechanical stimulus response sphere
Technical Field
The invention relates to a preparation method of a stress luminescent coating of a high-sensitivity mechanical stimulus response sphere, belonging to the technical field of stress luminescent materials.
Background
The mechanically stimulated photons of the stress luminescent material are characteristic, which is of great importance in medical health diagnosis, biomechanical sensing, building structure inspection, and the application of activated light sources. Applications of the stress luminescent materials (CaAl) found at present2Si2O8:Eu2+、CaNb2O7:Pr3+Etc.) have the following disadvantages: (1) the efficiency of converting applied mechanical stimulation into light energy is low, stress luminescence with high brightness cannot be effectively generated, and the accuracy of the stress luminescence in the aspect of stress analysis application is greatly limited; (2) after the stress luminescent material and the colloid are mixed and packaged, the optical properties such as stress luminescence and the like are seriously reduced, and the bottleneck of the stress luminescent material in the field of coating film forming is formed; (3) as the traditional stress luminescent materials mostly belong to fractal luminescent materials, the stress luminescence is generated by the fracture of atomic bonds and chemical bonds, so that the repeatability is extremely poor, and the application potential is restricted.
Therefore, a high-sensitivity mechano-stimulus response spherical coating of a stress luminescent material with stability, high brightness, high sensitivity and repeatable performance is urgently needed to solve the problems of low brightness, insufficient packaging stability, poor repeatability and the like of the traditional stress luminescent material.
Disclosure of Invention
Aiming at the problem of mechanical stimulation of stress luminescent materials in the prior art, the invention provides a preparation method of a stress luminescent coating of a high-sensitivity mechanical stimulation response sphere2O4:Tb3+The stress luminescent coating has strong stress luminescent intensity, can repeatedly keep the original mechanical stimulus response luminescence for a long time, has high stress luminescence brightness and high stabilityQualitative property, high sensitivity and high transparency.
A preparation method of a stress luminescent coating of a high-sensitivity mechanical stimulus response sphere comprises the following specific steps:
(1) mixing high-purity SrCO3、Ga2O3And Tb4O7Grinding and uniformly mixing to obtain mixed powder A;
(2) placing the mixed powder A obtained in the step (1) at the temperature of 1300-1350 ℃ in a reducing atmosphere for high-temperature sintering for 6-8 h, and grinding to obtain SrGa2O4:Tb3+Stress luminescent powder;
(3) SrGa obtained in the step (2)2O4:Tb3+The stress luminescent powder and the PDMS colloid are uniformly mixed to obtain mixed liquid, the mixed liquid is uniformly coated on the surface of the sphere, and the colloid of the coating layer is heated and cured after the preservative film is coated, so that the stress luminescent coating of the high-sensitivity mechanical stimulus response sphere is obtained.
SrCO in the mixed powder A in the step (1) by taking the mole fraction of the mixed powder A as 100 percent340-50% of Ga2O350-60% of Tb4O7Accounting for 1-5%.
The reducing atmosphere in the step (2) is H2/N2Mixed reducing atmosphere, in volume fraction, H25-7 percent.
The step (3) SrGa2O4:Tb3+The mass ratio of the stress luminescent powder to the PDMS colloid is 1: 1.3-1.4.
The heating curing temperature in the step (3) is 80-100 ℃, and the curing time is 24-27 h.
The stress luminescence principle of the invention is as follows: SrGa of spherical surface2O4:Tb3+The stress magnitude and range of each point on the surface of the sphere are different in the process that the stress luminescent coating contacts with the object, and the SrGa2O4:Tb3+The stress luminescent material effectively converts mechanical stress stimulation into luminescence, the stress luminescent material is packaged in the colloid to be used as a coating to be coated on the surface of the sphere, the stress luminescent characteristic can be given to the sphere, and a user can combine optical detection according to the luminescence brightness of the sphere after being stressedThe device analyzes the stress condition of the ball body and provides a certain degree of illumination for the use of the ball body at night.
The invention has the beneficial effects that:
(1) the invention utilizes high-temperature solid phase sintering and film forming treatment to prepare SrGa which can be uniformly dispersed in a PDMS film and has high-sensitivity mechanical response2O4:Tb3+The stress luminous coating has stronger stress luminous intensity and can repeatedly keep the original mechanical stimulation response luminescence for a long time;
(2) SrGa of the invention2O4:Tb3+The stress luminescent material has excellent stress luminescent performance under ultraviolet excitation, and can generate stress luminescence with high-sensitivity mechanical stimulus response after being coated on the surface of a sphere;
(3) SrGa of the invention2O4:Tb3+The stress luminescent coating has the characteristics of high stress luminescent brightness, high stability, high sensitivity, high transparency and the like.
Drawings
FIG. 1 shows SrGa of example 12O4:Tb3+XRD pattern of the stress luminescent material;
FIG. 2 shows SrGa of example 12O4:Tb3+Photoluminescence spectra of stress luminescent materials;
FIG. 3 shows SrGa of example 12O4Matrix and SrGa2O4:Tb3+The thermoluminescent spectrum of (c);
FIG. 4 shows SrGa of example 12O4:Tb3+Mixing the gel with PDMS to package into colloid, and generating stress luminescence phenomenon by the colloid;
FIG. 5 is a diagram showing the internal structure of a sphere coated with a stress luminescent coating in example 1;
FIG. 6 is a schematic view of stress luminescence generated by applying the stress luminescence coating material on the surface of a sphere in example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a preparation method of a stress luminescent coating of a high-sensitivity mechanical stimulus response sphere comprises the following specific steps:
(1) mixing high-purity SrCO3、Ga2O3And Tb4O7Grinding and uniformly mixing to obtain mixed powder A; SrCO in the mixed powder A based on the mole fraction of 100 percent of the mixed powder A340-50% of Ga2O350-60% of Tb4O71-5% of the total;
(2) placing the mixed powder A obtained in the step (1) at the temperature of 1300-1350 ℃ in a reducing atmosphere for high-temperature sintering for 6-8 h, and grinding to obtain SrGa2O4:Tb3+Stress luminescent powder; wherein the reducing atmosphere is H2/N2Mixed reducing atmosphere, in volume fraction, H25-7% of the total;
(3) SrGa obtained in the step (2)2O4:Tb3+Uniformly mixing stress luminescent powder and PDMS colloid to obtain mixed liquid, uniformly coating the mixed liquid on the surface of the sphere, heating and curing the colloid of the coating layer after the preservative film is coated to obtain a stress luminescent coating of the high-sensitivity mechanical stimulus response sphere; wherein SrGa2O4:Tb3+The mass ratio of the stress luminescent powder to the PDMS colloid is 1: 1.3-1: 1.4; the heating curing temperature is 80-100 ℃, and the curing time is 24-27 h;
the specific process parameters of the samples are shown in table 1,
TABLE 1 specific Process parameters for the samples
Figure BDA0003009528810000031
This example SrGa2O4:Tb3+The XRD pattern of the stress luminescent material is shown in figure 1, and as can be seen from figure 1, the series of samples doped with different Tb can be seen3+Diffraction peaks after concentration are all similar to SrGa2O4:Tb3+The standard card PDF NO.220905 is matched, which shows that the series of samples are SrGa2O4Pure phase;
this example SrGa2O4:Tb3+The photoluminescence spectrum of the stress luminescent material is shown in fig. 2, which shows that 395nm light can effectively excite the sample, and the sample can show 545nm yellow-green light emission under 395nm optimal excitation;
this example SrGa2O4Matrix and SrGa2O4:Tb3+The spectrum of the thermoluminescence is shown in FIG. 3, in which SrGa is shown2O4:0.03Tb3+Has deeper (100-3+The doping of the SrGa is further improved2O4The trap depth and the trap number of the semiconductor substrate, thereby optimizing the stress luminescence property;
this example SrGa2O4:Tb3+The stress luminescence phenomenon generated by the colloid is shown in figure 4, and the SrGa can be seen2O4:Tb3+The powder is packaged in the colloid uniformly and can generate obvious stress luminescence, and the L-shaped trace shows that the stress luminescence coating has a stress phosphorescence tailing phenomenon, so that the coating has good stress luminescence characteristics;
the internal structure diagram of the sphere coated with the stress luminescent coating is shown in fig. 5, the internal structure diagram and the physical diagram of the sphere coated with the stress luminescent coating are shown in the figure, the inner layer of the object is a sphere which can keep the intrinsic characteristic of the sphere, and the stress luminescent layer on the outer layer can endow the sphere with the stress luminescent characteristic, so that the sphere can emit light when being stressed;
the schematic diagram of stress luminescence generated by coating the stress luminescent coating material on the surface of the sphere in the embodiment is shown in fig. 6, before applying force to the sphere, the sphere maintains the performance of the sphere itself, when the sphere is in contact stress with the ground, the sphere displays stress luminescence due to the existence of the stress luminescent coating on the surface of the sphere, when the sphere is in contact with the hand again, the stress luminescence phenomenon can be repeatedly generated, and the stress luminescent coating endows the sphere with the stress luminescence performance while not affecting the use of the sphere itself; the method has great application potential in the field of stress analysis of objects.
Example 2: a preparation method of a stress luminescent coating of a high-sensitivity mechanical stimulus response sphere comprises the following specific steps:
(1) mixing high-purity SrCO3、Ga2O3And Tb4O7Grinding and uniformly mixing to obtain mixed powder A; SrCO in the mixed powder A based on the mole fraction of 100 percent of the mixed powder A340-50% of Ga2O350-60% of Tb4O71-5% of the total;
(2) placing the mixed powder A obtained in the step (1) at the temperature of 1300-1350 ℃ in a reducing atmosphere for high-temperature sintering for 6-8 h, and grinding to obtain SrGa2O4:Tb3+Stress luminescent powder; wherein the reducing atmosphere is H2/N2Mixed reducing atmosphere, in volume fraction, H25-7% of the total;
(3) SrGa obtained in the step (2)2O4:Tb3+Uniformly mixing stress luminescent powder and PDMS colloid to obtain mixed liquid, uniformly coating the mixed liquid on the surface of the sphere, heating and curing the colloid of the coating layer after the preservative film is coated to obtain a stress luminescent coating of the high-sensitivity mechanical stimulus response sphere; wherein SrGa2O4:Tb3+The mass ratio of the stress luminescent powder to the PDMS colloid is 1: 1.3-1: 1.4; the heating curing temperature is 80-100 ℃, and the curing time is 24-27 h;
the specific process parameters of the samples are shown in table 2,
TABLE 2 specific Process parameters for the samples
Figure BDA0003009528810000041
This example SrGa2O4:Tb3+The XRD pattern of the stress luminescent material shows that the series of samples are doped with different Tb3+Diffraction peaks after concentration are all similar to SrGa2O4:Tb3+The standard card PDF NO.220905 is matched, which shows that the series of samples are SrGa2O4Pure phase;
this example SrGa2O4:Tb3+The photoluminescence spectrum of the stress luminescent material shows that 395nm light can effectively excite the sample, and the sample can show 545nm yellow-green light emission under the optimal excitation of 395 nm;
this example SrGa2O4Matrix and SrGa2O4:Tb3+Shows SrGa in the thermoluminescent spectrum2O4:0.03Tb3+Has deeper (100-3+The doping of the SrGa is further improved2O4The trap depth and the trap number of the semiconductor substrate, thereby optimizing the stress luminescence property;
this example SrGa2O4:Tb3+Mixing with PDMS to package into colloid, and observing SrGa due to stress luminescence phenomenon generated by the colloid2O4:Tb3+The powder is packaged in the colloid uniformly and can generate obvious stress luminescence, and the L-shaped trace shows that the stress luminescence coating has a stress phosphorescence tailing phenomenon, so that the coating has good stress luminescence characteristics;
the inner layer of the sphere coated with the stress luminescent coating can maintain the intrinsic characteristic of the sphere, and the stress luminescent layer on the outer layer can endow the sphere with the stress luminescent characteristic, so that the sphere can emit light when being stressed;
the stress luminescent coating material is coated on the surface of a sphere, the sphere keeps the performance of the sphere before force is applied to the sphere, when the sphere is in contact stress with the ground, the sphere displays stress luminescence due to the existence of the stress luminescent coating on the surface of the sphere, and when the sphere is in contact with a hand again, the stress luminescence phenomenon can be repeatedly generated, and the stress luminescent coating endows the sphere with the stress luminescence performance while the use of the sphere is not influenced; the method has great application potential in the field of stress analysis of objects.
Example 3: a preparation method of a stress luminescent coating of a high-sensitivity mechanical stimulus response sphere comprises the following specific steps:
(1) will be provided withHigh purity SrCO3、Ga2O3And Tb4O7Grinding and uniformly mixing to obtain mixed powder A; SrCO in the mixed powder A based on the mole fraction of 100 percent of the mixed powder A340-50% of Ga2O350-60% of Tb4O71-5% of the total;
(2) placing the mixed powder A obtained in the step (1) at the temperature of 1300-1350 ℃ in a reducing atmosphere for high-temperature sintering for 6-8 h, and grinding to obtain SrGa2O4:Tb3+Stress luminescent powder; wherein the reducing atmosphere is H2/N2Mixed reducing atmosphere, in volume fraction, H25-7% of the total;
(3) SrGa obtained in the step (2)2O4:Tb3+Uniformly mixing stress luminescent powder and PDMS colloid to obtain mixed liquid, uniformly coating the mixed liquid on the surface of the sphere, heating and curing the colloid of the coating layer after the preservative film is coated to obtain a stress luminescent coating of the high-sensitivity mechanical stimulus response sphere; wherein SrGa2O4:Tb3+The mass ratio of the stress luminescent powder to the PDMS colloid is 1: 1.3-1: 1.4; the heating curing temperature is 80-100 ℃, and the curing time is 24-27 h;
the specific process parameters for the samples are shown in table 3,
TABLE 3 specific Process parameters for the samples
Figure BDA0003009528810000051
This example SrGa2O4:Tb3+The XRD pattern of the stress luminescent material shows that the series of samples are doped with different Tb3+Diffraction peaks after concentration are all similar to SrGa2O4:Tb3+The standard card PDF NO.220905 is matched, which shows that the series of samples are SrGa2O4Pure phase;
this example SrGa2O4:Tb3+The photoluminescence spectrum of the stress luminescent material shows that 395nm light can effectively excite the sample, and the sample can show 545nm yellow-green light emission under the optimal excitation of 395 nm;
this example SrGa2O4Matrix and SrGa2O4:Tb3+Shows SrGa in the thermoluminescent spectrum2O4:0.03Tb3+Has deeper (100-3+The doping of the SrGa is further improved2O4The trap depth and the trap number of the semiconductor substrate, thereby optimizing the stress luminescence property;
this example SrGa2O4:Tb3+Mixing with PDMS to package into colloid, and observing SrGa due to stress luminescence phenomenon generated by the colloid2O4:Tb3+The powder is packaged in the colloid uniformly and can generate obvious stress luminescence, and the L-shaped trace shows that the stress luminescence coating has a stress phosphorescence tailing phenomenon, so that the coating has good stress luminescence characteristics;
the inner layer of the sphere coated with the stress luminescent coating can maintain the intrinsic characteristic of the sphere, and the stress luminescent layer on the outer layer can endow the sphere with the stress luminescent characteristic, so that the sphere can emit light when being stressed;
the stress luminescent coating material is coated on the surface of a sphere, the sphere keeps the performance of the sphere before force is applied to the sphere, when the sphere is in contact stress with the ground, the sphere displays stress luminescence due to the existence of the stress luminescent coating on the surface of the sphere, and when the sphere is in contact with a hand again, the stress luminescence phenomenon can be repeatedly generated, and the stress luminescent coating endows the sphere with the stress luminescence performance while the use of the sphere is not influenced; the method has great application potential in the field of stress analysis of objects.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.

Claims (5)

1.一种高灵敏机械刺激响应球体的应力发光涂层的制备方法，其特征在于，具体步骤如下：1. a preparation method of the stress luminescent coating of a highly sensitive mechanical stimulus responsive sphere, is characterized in that, concrete steps are as follows: (1)将高纯的SrCO3、Ga2O3和Tb4O7进行研磨混匀得到混合粉料A；(1) grinding and mixing high-purity SrCO 3 , Ga 2 O 3 and Tb 4 O 7 to obtain mixed powder A; (2)将步骤(1)混合粉料A置于温度为1300～1350℃、还原气氛中高温烧结6～8h，研磨得到SrGa2O4:Tb3+应力发光粉末；(2) placing the mixed powder A in step (1) at a temperature of 1300-1350° C. and sintering at a high temperature in a reducing atmosphere for 6-8 hours, and grinding to obtain SrGa 2 O 4 :Tb 3+ stress luminescent powder; (3)将步骤(2)SrGa2O4:Tb3+应力发光粉与PDMS胶体混合均匀得到混合液体，混合液体均匀涂覆在球体表面，保鲜膜包覆后加热固化涂覆层的胶体，得到高灵敏机械刺激响应球体的应力发光涂层。(3) mixing step (2) SrGa 2 O 4 :Tb 3+ stress luminescent powder and PDMS colloid uniformly to obtain a mixed liquid, the mixed liquid is uniformly coated on the surface of the sphere, and the colloid of the coating layer is heated and cured after being covered with a fresh-keeping film, Stress-luminescent coatings of highly sensitive mechanical stimuli-responsive spheroids were obtained. 2.根据权利要求1所述高灵敏机械刺激响应球体的应力发光涂层的制备方法，其特征在于：以混合粉料A的摩尔分数为100％计，步骤(1)混合粉料A中SrCO3占40～50％、Ga2O3占50～60％和Tb4O7占1～5％。2. the preparation method of the stress luminescent coating of the highly sensitive mechanical stimulation responsive sphere according to claim 1, is characterized in that: taking the mole fraction of mixed powder A as 100%, step (1) in mixed powder A SrCO 3 accounts for 40-50%, Ga 2 O 3 accounts for 50-60% and Tb 4 O 7 accounts for 1-5%. 3.根据权利要求1所述高灵敏机械刺激响应球体的应力发光涂层的制备方法，其特征在于：步骤(2)还原气氛为H2/N2混合还原气氛，以体积分数计，H2占5～7％。3. The preparation method of the stress luminescent coating of the highly sensitive mechanical stimulus responsive sphere according to claim 1, characterized in that: the reducing atmosphere in step (2) is a H 2 /N 2 mixed reducing atmosphere, in terms of volume fraction, H 2 Accounted for 5 to 7%. 4.根据权利要求1所述高灵敏机械刺激响应球体的应力发光涂层的制备方法，其特征在于：步骤(3)SrGa2O4:Tb3+应力发光粉与PDMS胶体的质量比为1:1.3～1.4。4. the preparation method of the stress luminescent coating of the highly sensitive mechanical stimulus responsive sphere according to claim 1, is characterized in that: the mass ratio of step (3) SrGa 2 O 4 :Tb 3+ stress luminescent powder and PDMS colloid is 1 : 1.3 to 1.4. 5.根据权利要求1所述高灵敏机械刺激响应球体的应力发光涂层的制备方法，其特征在于：步骤(3)加热固化温度为80～100℃，固化时间为24～27h。5 . The method for preparing a stress luminescent coating of a highly sensitive mechanical stimulus responsive sphere according to claim 1 , wherein in step (3), the heating and curing temperature is 80-100° C., and the curing time is 24-27 h. 6 .
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