X-ray scintillator thermal imaging film and application

Abstract

The invention discloses an X-ray scintillator thermal imaging film and application, and belongs to the field of fluorescence real-time imaging detection. ZrMgMo3O12: Dy fluorescent powder serves as an X-ray scintillator, PDMS liquid and the fluorescent powder are mixed to prepare an X-ray scintillator thermal imaging film, the fluorescent powder or the film is heated from 20 DEG C to 300 DEG C, an X-ray source is used for excitation, a thermal imaging picture can be obtained by detecting a fluorescent signal emitted by the film, an X-ray high-temperature thermal imaging mode is achieved, and the thermal imaging effect is good. The method is applied to the field of fluorescence real-time imaging detection. Besides, compared with an optical thermal imaging film with laser as an excitation source, the X-ray scintillator film has the advantages that the X-ray penetrating power is higher, the X-ray scintillator film can penetrate through the surface of an object and detect information in the object, the use temperature range is wider, thermal quenching does not occur at the temperature of 300 DEG C, and the application range of the film is widened.

Description

Technical Field

[0001] The invention belongs to the technical field of fluorescence real-time imaging detection, and in particular relates to an X-ray scintillator thermal imaging film and its application. Background Art

[0002] With the development of modern industry, the requirements for product quality are getting higher and higher. Fluorescence real-time imaging detection technology can perform high-precision detection of the appearance, size, defects, etc. of products to ensure that the products meet quality standards, improve production efficiency and reduce costs. Fluorescence real-time imaging detection is an interdisciplinary subject involving multiple fields such as optics, electronics, and computer science. Its basic principle is to use optical means to obtain the image or spectral information of the object to be detected, and then analyze and process this information to realize the detection, measurement, and identification of the object. At present, fluorescence real-time imaging detection technology mainly focuses on lasers and ultraviolet light as excitation sources. However, using lasers and ultraviolet light as excitation sources can only irradiate the surface of the object, and cannot detect the inside of the object. Moreover, due to the excessive power of the laser, some electronic components will be damaged. Since most industrial equipment and industrial devices work in a high-temperature environment, the optical signal of the fluorescent material is severely thermally quenched at high temperatures, so it is very important to maintain the luminescence performance at high temperatures. Summary of the invention

[0003] In view of the above-mentioned shortcomings of the prior art, the present invention provides an X-ray scintillator thermal imaging film and its application.

[0004] To achieve the above object, the technical solution adopted by the present invention is: an X-ray scintillator thermal imaging film is ZrMgMo3O 12 :Dy phosphor film;

[0005] The preparation method of the X-ray scintillator thermal imaging film comprises: mixing polydimethylsiloxane with a crosslinking agent, and then adding ZrMgMo3O 12 :Dy phosphor, then drop it on the glass, and after drying, you can get the X-ray scintillator thermal imaging film.

[0006] As a preferred embodiment of the present invention, the polydimethylsiloxane, the crosslinking agent and ZrMgMo3O 12 The mass percentages of :Dy phosphor are 55% to 65%, 5% to 7%, and 28% to 40% respectively.

[0007] Polydimethylsiloxane, crosslinker and ZrMgMo3O 12 :The sum of the mass percentages of Dy phosphor is 100%.

[0008] As a preferred embodiment of the present invention, the cross-linking agent is a platinum catalyst.

[0009] As a preferred embodiment of the present invention, the ZrMgMo3O 12 The preparation method of Dy phosphor comprises: adding Dy2O3 to a mixture of ZrO2, MgO and MoO3, adding ethanol and grinding to obtain a mixed material; then calcining the mixed material to obtain ZrMgMo3O 12 :Dy phosphor.

[0010] As a preferred embodiment of the present invention, the molar ratios of Dy2O3, ZrO2, MgO and MoO3 are 0.0025-0.025:0.495-0.45:0.5:1.5 respectively.

[0011] As a preferred embodiment of the present invention, the calcination temperature is 800° C. to 900° C., the time is 5 to 6 hours, the heating rate is 2 to 5° C. / min, and the atmosphere is air.

[0012] The present invention also claims to protect the application of the X-ray scintillator thermal imaging film in fluorescence real-time imaging detection.

[0013] Compared with the prior art, the invention has the following beneficial effects: 12 :Dy phosphor is used as an X-ray scintillator, PDMS liquid is mixed with phosphor to prepare a film, the phosphor or X-ray scintillator film is excited by an X-ray source, the film is prompted to generate an optical signal, and the detection, measurement, and identification of objects are achieved by detecting the fluorescent signal, and it is applied to the field of real-time fluorescence imaging detection. In addition, compared with the optical thermal imaging film using laser as the excitation source, the X-ray scintillator film of the present invention has a stronger X-ray penetration ability, can penetrate the surface of objects such as plastics and rubber, detect the information inside the object, and has a higher temperature range. No thermal quenching occurs at 300°C, which improves the application range of the film and effectively solves the problem of thermal quenching of optical signals of fluorescent materials at high temperatures. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 The ZrMgMo3O prepared in Example 1 12 : Fluorescence spectra of Dy phosphor measured by fiber optic spectrometer at 20℃, 60℃, 100℃, 140℃, 180℃, 220℃, 260℃ and 300℃ under the excitation of X-ray source.

[0015] Figure 2 The actual image of the X-ray scintillator thermal imaging film prepared in Example 1; (a) is the actual image; (b) is the actual folding image.

[0016] Figure 3These are fluorescence imaging pictures of the X-ray scintillator thermal imaging film prepared in Example 1 under the excitation of an X-ray source at temperatures of 20°C, 60°C, 100°C, 140°C, 180°C, 220°C, 260°C, and 300°C. DETAILED DESCRIPTION

[0017] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0018] Example 1

[0019] A method for preparing an X-ray scintillator thermal imaging film comprises:

[0020] (1) Dy2O3 is added to ZrO2, MgO, and MoO3 in a molar ratio of 0.025:0.45:0.5:1.5, and then 0.2 mol of ethanol is added and ground to obtain a mixed material.

[0021] (2) The mixed material was calcined in air at 800°C for 6 hours to obtain ZrMgMo3O 12 :Dy phosphor.

[0022] (3) Mix the prepared polydimethylsiloxane with the platinum catalyst, and then add ZrMgMo3O 12 :Dy phosphor is added to the mixed PDMS liquid, then dripped on a flat glass plate, and a fluorescent film is obtained after drying; polydimethylsiloxane, crosslinking agent and ZrMgMo3O 12 :The mass percentage ratio of Dy phosphor is 62.5%:6.25%:31.25%.

[0023] Prepared ZrMgMo3O 12 :Dy phosphor or X-ray scintillator thermal imaging film is used as thermal imaging application, the steps are as follows:

[0024] (1) ZrMgMo3O 12 :Dy phosphor was heated at 20℃, 60℃, 100℃, 140℃, 180℃, 220℃, 260℃, and 300℃, and the fluorescence spectrum was obtained by using a fiber optic spectrometer under X-ray excitation. Figure 1 As shown, the yellow-green fluorescence of the phosphor did not undergo thermal quenching during the heating process, indicating that the phosphor has good thermal stability.

[0025] (2) The prepared X-ray scintillator film is heated at 20°C, 60°C, 100°C, 140°C, 180°C, 220°C, 260°C, and 300°C, a mask is placed on the film, and a thermal imaging pattern with distinct light and dark is obtained by taking a picture with a camera under X-ray excitation. Figure 3The film luminescence did not weaken during the heating process, and it still maintained bright fluorescence when heated to 300°C, indicating that its fluorescence thermal stability is good, its thermal imaging function is excellent, and it has application potential in real-time fluorescence imaging detection.

[0026] Example 2

[0027] A method for preparing an X-ray scintillator thermal imaging film comprises:

[0028] (1) Dy2O3 is added to ZrO2, MgO, and MoO3 in a molar ratio of 0.0025:0.495:0.5:1.5, and then 0.2 mol of ethanol is added and ground to obtain a mixed material.

[0029] (2) The mixture was calcined in air at 900°C for 5 hours to obtain ZrMgMo3O 12 :Dy phosphor.

[0030] (3) Mix the prepared polydimethylsiloxane with the platinum catalyst, and then add ZrMgMo3O 12 :Dy phosphor is added to the mixed PDMS liquid, then dripped on a flat glass plate, and a fluorescent film is obtained after drying; polydimethylsiloxane, crosslinking agent and ZrMgMo3O 12 :The mass percentage ratio of Dy phosphor is 55%:7%:38%.

[0031] Prepared ZrMgMo3O 12 :Dy phosphor or X-ray scintillator thermal imaging film is used as thermal imaging application, the steps are as follows:

[0032] (1) ZrMgMo3O 12 :Dy phosphor was heated at 20℃, 60℃, 100℃, 140℃, 180℃, 220℃, 260℃, and 300℃, and the fluorescence spectrum was obtained by using a fiber optic spectrometer under X-ray excitation. The yellow-green fluorescence of the phosphor did not undergo thermal quenching during the heating process, indicating that the phosphor has good thermal stability.

[0033] (2) The prepared X-ray scintillator film was heated at 20°C, 60°C, 100°C, 140°C, 180°C, 220°C, 260°C, and 300°C, and a mask was placed on the film. Under X-ray excitation, a camera was used to obtain a thermal imaging pattern with distinct light and dark. The film did not emit light during the heating process, and it still maintained bright fluorescence when heated to 300°C, indicating that it has good thermal stability of fluorescence and excellent thermal imaging function, and has potential for application in real-time fluorescence imaging detection.

[0034] Comparative Example 1

[0035] A method for preparing an X-ray scintillator thermal imaging film comprises:

[0036] (1) Eu2O3, ZrO2, MgO and MoO3 are mixed in a molar ratio of 0.025:0.45:0.5:1.5, and then ethanol is added and ground to obtain a mixed material.

[0037] (2) The mixed material was calcined in air at 800°C for 6 hours to obtain ZrMgMo3O 12 :Eu phosphor.

[0038] (3) Mixing the base polymer for preparing PDMS with a crosslinking agent, and then 12 :Eu phosphor is added to the mixed PDMS liquid, then dripped on a flat glass, and a fluorescent film is obtained after drying; polydimethylsiloxane, crosslinking agent and ZrMgMo3O 12 :The mass percentage ratio of Eu phosphor is 62.5%:6.25%:31.25%.

[0039] Prepared ZrMgMo3O 12 : The application of Eu phosphor or X-ray scintillator thermal imaging film as thermal imaging includes the following steps:

[0040] (1) ZrMgMo3O 12 :Eu phosphor was heated at 20℃, 60℃, 100℃, 140℃, 180℃, 220℃, 260℃, and 300℃, and the fluorescence spectrum was obtained by using a fiber optic spectrometer under X-ray excitation. The red fluorescence intensity of the phosphor gradually decreased with the increase of temperature during the heating process, and the material luminescence disappeared at 220℃, indicating that the thermal stability of the phosphor was poor.

[0041] (2) The prepared X-ray scintillator film was heated at 20°C, 60°C, 100°C, 140°C, 180°C, 220°C, 260°C, and 300°C, a mask was placed on the film, and a thermal imaging pattern was obtained by using a camera under X-ray excitation. During the heating process, the luminescence intensity of the film gradually decreased with the increase in temperature, and the luminescence of the material disappeared at 220°C, indicating that its fluorescence thermal stability was poor, the application temperature range of the thermal imaging function was limited, the thermal imaging function was not as good as that of Example 1, and it had poor application ability in real-time fluorescence imaging detection.

[0042] Comparative Example 2

[0043] A method for preparing an X-ray scintillator thermal imaging film comprises:

[0044] (1) Tb4O7, ZrO2, MgO and MoO3 are mixed in a molar ratio of 0.025:0.45:0.5:1.5, and then ethanol is added and ground to obtain a mixed material.

[0045] (2) The mixed material was calcined in air at 800°C for 6 hours to obtain ZrMgMo3O 12 :Tb phosphor.

[0046] (3) Mixing the base polymer for preparing PDMS with a crosslinking agent, and then 12 :Tb phosphor is added to the mixed PDMS liquid, then dripped on a flat glass, and a fluorescent film is obtained after drying; polydimethylsiloxane, crosslinking agent and ZrMgMo3O 12 :The mass percentage ratio of Tb phosphor is 62.5%:6.25%:31.25%.

[0047] Prepared ZrMgMo3O 12 : The application of Tb phosphor or X-ray scintillator thermal imaging film as thermal imaging includes the following steps:

[0048] (1) ZrMgMo3O 12 :Tb phosphor was heated at 20℃, 60℃, 100℃, 140℃, 180℃, 220℃, 260℃, and 300℃, and the fluorescence spectrum was obtained by using a fiber optic spectrometer under X-ray excitation. The green fluorescence intensity of the phosphor gradually decreased with the increase of temperature during the heating process, and the luminescence disappeared at 180℃, indicating that the thermal stability of the phosphor was poor.

[0049] (2) The prepared X-ray scintillator film was heated at 20°C, 60°C, 100°C, 140°C, 180°C, 220°C, 260°C, and 300°C, and a mask was placed on the film. Under X-ray excitation, a thermal imaging pattern with distinct light and dark was obtained by taking a picture with a camera. During the heating process, the luminescence intensity of the film gradually decreased with the increase in temperature until the luminescence disappeared at 180°C, indicating that its fluorescence thermal stability was poor, the application temperature range of the thermal imaging function was limited, the thermal imaging function was not as good as in the embodiment, and its application potential in real-time fluorescence imaging detection was poor.

[0050] Comparative Example 3

[0051] A method for preparing an X-ray scintillator thermal imaging film comprises:

[0052] (1) Dy2O3 was added to Y2O3 and MoO3 in a molar ratio of 0.025:0.45:0.5:1.5, and then 10 ml of ethanol was added and ground to obtain a mixed material.

[0053] (2) The mixed material was calcined in air at 800°C for 6 hours to obtain Y2Mo3O 12 :Dy phosphor.

[0054] (3) Mix the prepared polydimethylsiloxane with the platinum catalyst, and then 12 :Dy phosphor is added to the mixed PDMS liquid, then dripped on a flat glass plate, and a fluorescent film is obtained after drying; polydimethylsiloxane, crosslinking agent and Y2Mo3O 12 :The mass percentage ratio of Dy phosphor is 62.5%:6.25%:31.25%.

[0055] The prepared Y2Mo3O 12 :Dy phosphor or X-ray scintillator thermal imaging film is used as thermal imaging application, the steps are as follows:

[0056] (1) Y2Mo3O 12 :Dy phosphor is heated at 20℃, 60℃, 100℃, 140℃, 180℃, 220℃, 260℃, and 300℃, but cannot be excited to emit light under X-ray excitation.

[0057] (2) The prepared X-ray scintillator film is heated at 20°C, 60°C, 100°C, 140°C, 180°C, 220°C, 260°C, and 300°C, and a mask is placed on the film. When excited by X-rays, the film cannot be excited to emit light, and imaging cannot be performed, and the film cannot be used for real-time fluorescence imaging detection.

[0058] Compared with Example 1, the effect of Comparative Example 1-2 is poor, because Dy is doped in ZrMgMo3O 12 In the matrix, the oxygen vacancies in the material in Example 1 gradually increase during the heating process, making it easier for excited electrons to be captured and produce an anti-thermal quenching effect, while Eu and Tb doped in ZrMgMo3O 12 In the matrix, oxygen vacancies did not increase during the heating process, resulting in thermal quenching. 12 It cannot absorb the energy of X-rays, resulting in it being unable to be excited after being doped with Dy.

[0059] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. An X-ray scintillator thermal imaging film, characterized in that: ZrMgMo3O 12 :Dy phosphor film; The preparation method of the X-ray scintillator thermal imaging film comprises: mixing polydimethylsiloxane with a crosslinking agent, and then adding ZrMgMo3O 12 :Dy phosphor, then drop it on the glass, and after drying, you can get the X-ray scintillator thermal imaging film.

2. The X-ray scintillator thermal imaging film according to claim 1, characterized in that: The polydimethylsiloxane, the crosslinking agent and the ZrMgMo3O 12 The mass percentages of :Dy phosphor are 55% to 65%, 5% to 7%, and 28% to 40% respectively.

3. The X-ray scintillator thermal imaging film according to claim 1, characterized in that: The cross-linking agent is a platinum catalyst.

4. The X-ray scintillator thermal imaging film according to claim 1, characterized in that: The ZrMgMo3O 12 The preparation method of Dy phosphor comprises: adding Dy2O3 to a mixture of ZrO2, MgO and MoO3, adding ethanol and grinding to obtain a mixed material; then calcining the mixed material to obtain ZrMgMo3O 12 :Dy phosphor.

5. The X-ray scintillator thermal imaging film according to claim 4, characterized in that: The molar ratios of Dy2O3, ZrO2, MgO and MoO3 are 0.0025-0.025:0.495-0.45:0.5:1.5 respectively.

6. The X-ray scintillator thermal imaging film according to claim 4, characterized in that: The calcination temperature is 800° C. to 900° C., the time is 5 to 6 hours, the heating rate is 2 to 5° C. / min, and the atmosphere is air.

7. Application of the X-ray scintillator thermal imaging film according to any one of claims 1 to 6 in fluorescence real-time imaging detection.

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