A fiber optic imaging element for high-resolution ultraviolet detection and its preparation method and application
By forming a microporous structure in the core of the fiber image transmission element and filling it with perovskite quantum dot glass powder, the limitations of the ultraviolet detector in terms of ultraviolet detection efficiency and resolution are solved, and high-resolution fiber image transmission element for ultraviolet detection is prepared, which improves the detection efficiency and resolution, and is suitable for national defense, civilian and scientific research.
Patent Information
- Application Number
- CN202411624616.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-14
- Publication Date
- 2025-08-29
- Estimated Expiration
- 2044-11-14
AI Technical Summary
Existing ultraviolet detectors have limitations in ultraviolet detection efficiency and resolution, especially the visible light detection technology based on CCD has a strong absorption effect on light with a wavelength less than 400nm, making it difficult to effectively improve the detection efficiency and resolution of ultraviolet light.
Using the preparation method of optical fiber image transmission element for high-resolution ultraviolet detection, fiber image transmission element with high-precision microporous structures are formed by pickling the core of the optical fiber image transmission element, filling perovskite quantum dot glass powder, and providing a protective layer on its surface, fiber image transmission element with high precision microporous structure and high photoluminescent quantum yield is prepared.
It achieves high luminous intensity and long-term stability, improves the detection efficiency and detection resolution of ultraviolet detectors, and is suitable for national defense, civil and scientific research fields.
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Figure CN119644504B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of ultraviolet detection technology, and in particular to an optical fiber imaging element for high-resolution ultraviolet detection, a preparation method thereof, and applications thereof. Background Art
[0002] In modern photoelectric detection technology, ultraviolet radiation signals are generated by the corona phenomenon in outer space, flames, oil, and high-voltage lines. Therefore, ultraviolet detection has a wide range of application needs in aviation, communications, civil detection and other fields. Therefore, ultraviolet detection is receiving more and more attention and has become another extremely important technology developed after laser detection technology.
[0003] Visible light detection technology based on charge-coupled devices (CCDs) is highly mature, and mass-produced CCDs are already used in most industrial detection and civilian applications. Theoretically, CCDs have a certain response to wavelengths between 0.1 and 1100 nm. However, the detector's polysilicon electrodes strongly absorb light with wavelengths less than 400 nm, limiting their use in ultraviolet (UV) detection.
[0004] Therefore, how to improve the detection efficiency and detection resolution of ultraviolet light by ultraviolet detectors is of great significance to national defense, civilian use and scientific research fields. Summary of the Invention
[0005] The main purpose of the present invention is to provide a high-resolution ultraviolet detection optical fiber imaging element and its preparation method and application. The technical problem to be solved is how to improve the detection efficiency and detection resolution of ultraviolet light by the ultraviolet detector, so as to make it more suitable for practical use.
[0006] The purpose of the present invention and the technical problem solved are achieved by adopting the following technical solutions. According to the method for preparing a high-resolution ultraviolet detection optical fiber image transmission element proposed by the present invention, the steps include:
[0007] Acid-washing the cross section of one end of the optical fiber imaging element to form a microporous structure at the cross section, wherein the depth of the microporous structure is 10 to 50 μm, thereby obtaining an acid-washed optical fiber imaging element; wherein the core of the optical fiber imaging element is made of an acid-resistant material and the cladding is made of an acid-resistant material;
[0008] Filling the aforementioned microporous structure with perovskite quantum dot glass powder to obtain a filled optical fiber imaging element; and,
[0009] A protective layer is provided on the filling surface of the aforementioned filled optical fiber imaging element to obtain a high-resolution optical fiber imaging element for ultraviolet detection.
[0010] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures.
[0011] In some embodiments, according to the aforementioned method for preparing an optical fiber imaging element for high-resolution ultraviolet detection, the aforementioned perovskite quantum dot glass powder is CsPbX3 perovskite quantum dot glass powder; wherein X is at least one of Cl, Br and I.
[0012] In some embodiments, according to the aforementioned method for preparing an optical fiber imaging element for high-resolution ultraviolet detection, the components of the aforementioned CsPbX3 perovskite quantum dot glass powder, calculated in terms of oxide mass percentage, include: SiO2: 30-40%; H3BO3: 20-30%; ZnO: 15-20%; Cs2CO3: 10-15%; PbX2: 5-10%; and NaX: 5-10%.
[0013] In some embodiments, according to the aforementioned method for preparing a fiber optic imaging element for high-resolution ultraviolet detection, the aforementioned method for preparing the CsPbX3 perovskite quantum dot glass powder includes the following steps:
[0014] preparing glass raw materials, melting the aforementioned glass raw materials at 1000-1100° C. to obtain a glass melt;
[0015] pouring the aforementioned glass melt into a mold to obtain a precursor glass;
[0016] The precursor glass is annealed at 350-450° C. for 2-3 hours to obtain CsPbX3 perovskite quantum dot glass; and
[0017] The aforementioned CsPbX3 perovskite quantum dot glass is ground into powder to obtain the aforementioned CsPbX3 perovskite quantum dot glass powder.
[0018] In some embodiments, according to the aforementioned method for preparing a fiber optic imaging element for high-resolution ultraviolet detection, the method of filling the aforementioned perovskite quantum dot glass powder into the aforementioned microporous structure includes the following steps:
[0019] a. The aforementioned perovskite quantum dot glass powder is dispersed in an organic solvent to obtain a quantum dot dispersion;
[0020] b. The aforementioned microporous structure of the aforementioned pickled optical fiber imaging element is immersed in the aforementioned quantum dot dispersion, ultrasonically treated, and then the aforementioned pickled optical fiber imaging element is removed, the aforementioned quantum dot dispersion is scraped off the surface without pores, and dried;
[0021] Repeat step b multiple times until the aforementioned microporous structure is fully filled with the aforementioned perovskite quantum dot glass powder to obtain the aforementioned filled optical fiber imaging element.
[0022] In some embodiments, according to the aforementioned method for preparing an optical fiber imaging element for high-resolution ultraviolet detection, the size of the aforementioned perovskite quantum dot glass powder is 100-200 nm.
[0023] In some embodiments, according to the aforementioned method for preparing an optical fiber imaging element for high-resolution ultraviolet detection, the aforementioned protective layer includes an anti-reflection film.
[0024] In some embodiments, according to the aforementioned method for preparing an optical fiber imaging element for high-resolution ultraviolet detection, the aforementioned protective layer includes a quartz window, and the thickness of the aforementioned quartz window is 2 to 3 mm.
[0025] The purpose of the present invention and the solution to its technical problems are also achieved by adopting the following technical solutions. According to the present invention, a high-resolution ultraviolet detection optical fiber image transmission element is proposed, which includes:
[0026] An optical fiber imaging element, wherein the core of the optical fiber imaging element is made of an acid-etchable material and the cladding is made of an acid-resistant material, and the core of the optical fiber imaging element is recessed at a cross section at one end thereof, forming a microporous structure with a depth of 10 to 50 μm at the cross section;
[0027] Perovskite quantum dot glass powder, wherein the aforementioned perovskite quantum dot glass powder is filled in the aforementioned microporous structure; and
[0028] The protective layer is arranged on the cross section of the optical fiber imaging element filled with the perovskite quantum dot glass powder.
[0029] The purpose of the present invention and the technical problems solved therein are also achieved by adopting the following technical solutions: According to the present invention, an application of the aforementioned high-resolution ultraviolet detection optical fiber imaging element in the field of ultraviolet detection is proposed.
[0030] Through the above technical solution, the optical fiber image transmission element for high-resolution ultraviolet detection and its preparation method and application of the present invention have at least the following advantages:
[0031] The present invention proposes a method for preparing a fiber optic imaging element for high-resolution ultraviolet detection. The method employs an optical fiber imaging element with a core made of an acid-etchable material and a cladding made of an acid-resistant material. Using an acid-etching method, a high-precision, uniformly arranged microporous structure is created across the cross-section of the optical fiber imaging element. The depth of the microporous structure is controlled to be 10 to 50 μm, and the microporous structure is filled with perovskite quantum dot glass powder. Perovskite quantum dot glass powder has a high photoluminescence quantum yield, excellent color purity, and a tunable band gap. Controlling the filling thickness to 10 to 50 μm allows it to act as a UV-absorbing light-sensitive material, achieving high luminescence intensity and long-term stability, improving detection efficiency and lifetime. Furthermore, filling the perovskite quantum dot glass powder enables efficient luminescence from a single optical fiber, effectively improving detection resolution. Light converted from the quantum dot material within the microporous structure upon UV irradiation is transmitted by the corresponding optical fiber, with each optical fiber acting as a separate imaging unit. This significantly improves resolution compared to the diffusely reflected light from stimulated emission of traditional quantum dot materials. The high-resolution optical fiber imaging element for ultraviolet detection prepared by the present invention has the advantages of high brightness and high resolution, effectively improving the detection efficiency and detection resolution of ultraviolet detectors, and is of great significance to the fields of national defense, civil use and scientific research.
[0032] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 Schematic diagram of the structure of the optical fiber imaging element for high-resolution ultraviolet detection disclosed in Example 1 of the present invention;
[0034] Figure 2 Schematic diagram of the structure of the optical fiber imaging element for high-resolution ultraviolet detection disclosed in Example 2 of the present invention;
[0035] Figure 3 Schematic diagram of the structure of the optical fiber imaging element for high-resolution ultraviolet detection disclosed in Example 3 of the present invention;
[0036] Figure 4 This is a fluorescence spectrum of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in Example 1 of the present invention;
[0037] Figure 5 This is a fluorescence spectrum of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in Example 2 of the present invention;
[0038] Figure 6 This is a fluorescence spectrum of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in Example 3 of the present invention;
[0039] Figure 7 This is a fluorescence spectrum of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in Example 4 of the present invention;
[0040] Figure 8 This is a fluorescence spectrum of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in Example 5 of the present invention;
[0041] Figure 9 1 is a fluorescence spectrum diagram of the high-resolution ultraviolet detection optical fiber imaging element in Example 1 of the present invention and the P20 phosphor optical fiber imaging element in Comparative Example 2;
[0042] Figure 10 This is an X-ray diffraction test diagram of CsPbBr3 quantum dots in Example 1 of the present invention.
[0043] Description of reference numerals:
[0044] 1. Quartz window; 2. Alumina and hafnium oxide composite film; 3. CsPbBr3 perovskite quantum dot glass powder; 4. Acid-washed fiber optic panel; 5. Acid-washed fiber optic cone; 6. Acid-washed fiber optic image inverter. DETAILED DESCRIPTION
[0045] To further illustrate the technical means and effectiveness of the present invention in achieving its intended objectives, the following, in conjunction with the accompanying drawings and preferred embodiments, provides a detailed description of a high-resolution fiber optic imaging element for ultraviolet detection, its preparation method, and its specific implementation, structure, features, and effectiveness. In the following description, different references to "one embodiment" or "embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
[0046] The present invention provides these embodiments to make the present invention thorough and complete, and to fully express the scope of the present invention to those skilled in the art. It should be noted that: unless otherwise specifically stated, the relative arrangement of parts and steps, the composition of materials, numerical expressions and numerical values set forth in these embodiments should be interpreted as merely exemplary, and not as limiting.
[0047] The present invention proposes a method for preparing a high-resolution ultraviolet detection optical fiber image transmission element, such as Figures 1 to 3 As shown, the steps include:
[0048] Acid-washing the cross section of one end of the optical fiber imaging element to form a microporous structure at the cross section, wherein the depth of the microporous structure is 10 to 50 μm, thereby obtaining an acid-washed optical fiber imaging element; wherein the core of the optical fiber imaging element is made of an acid-resistant material and the cladding is made of an acid-resistant material;
[0049] Filling the aforementioned microporous structure with perovskite quantum dot glass powder to obtain a filled optical fiber imaging element; and,
[0050] A protective layer is provided on the filling surface of the aforementioned filled optical fiber imaging element to obtain a high-resolution optical fiber imaging element for ultraviolet detection.
[0051] Specifically, the optical fiber imaging element may be a fiber optic panel, an optical fiber light cone, or an optical fiber image invertor. Based on the acid resistance of the fiber core and the cladding, the acid solution used for pickling may be selected from at least one of 0.1 to 3.0 mol / L hydrochloric acid, nitric acid, citric acid, and sulfuric acid. The pickling method can produce a regularly arranged microporous structure with holes only at the fiber core position. This method can accurately prepare micropores at the fiber core position without destroying the cladding structure and causing optical crosstalk. In addition, the diameter of the micropores is controlled by regulating the fiber core diameter, and the depth of the micropores is controlled by adjusting the acid concentration and immersion time, thereby achieving a high-precision, highly uniform, regularly arranged micropore structure with adjustable micropore diameter and depth.
[0052] Perovskite quantum dot glass powder has a high photoluminescence quantum yield, excellent color purity, and an adjustable band gap. By controlling the depth of the microporous structure to 10-50 μm and the filling thickness to 10-50 μm, it acts as a UV-absorbing light-sensitive material, achieving high luminescence intensity and long-term stability, thereby improving detection efficiency and lifetime. Furthermore, filling the perovskite quantum dot glass powder enables efficient luminescence from a single optical fiber, effectively improving detection resolution. The light converted by the perovskite quantum dot glass powder within the microporous structure after ultraviolet irradiation is transmitted by the corresponding optical fiber, with each optical fiber acting as a separate imaging unit. Compared to the diffusely reflected light from stimulated emission of traditional quantum dot materials, the resolution is significantly improved. The perovskite quantum dot glass powder can be made of materials commonly used in the field, and can be either inorganic or organic perovskite quantum dot glass. Inorganic perovskite quantum dot glass is preferred; compared to organic perovskite quantum dot glass, inorganic perovskite quantum dot glass offers greater stability and is suitable for a wider range of environments. Preferably, the size of the perovskite quantum dot glass is 100 to 200 nm. The perovskite quantum dot glass powder can be filled by physical deposition or direct filling, which is not limited here.
[0053] The protective layer protects the perovskite quantum dot glass powder from contamination and shedding, isolates it from water and oxygen, and extends its service life and expands its scope of use. The protective layer can be made of transparent materials such as quartz, organic glass, and resin.
[0054] The high-resolution optical fiber imaging element for ultraviolet detection prepared by the method of the present invention has the advantages of high brightness and high resolution, effectively improving the detection efficiency and detection resolution of the ultraviolet detector, and is of great significance to the fields of national defense, civil use and scientific research.
[0055] In some embodiments, the aforementioned perovskite quantum dot glass powder is CsPbX3 perovskite quantum dot glass powder; wherein X is at least one of Cl, Br and I.
[0056] Specifically, CsPbX3 perovskite quantum dot glass has high hardness, excellent stability, and high transmittance, making the resulting fiber-optic imaging components brighter and suitable for a wider range of environments. Furthermore, by combining Cl, Br, and I ions, perovskite quantum dot materials can be produced that emit visible light of any wavelength.
[0057] In some embodiments, the components of the aforementioned CsPbX3 perovskite quantum dot glass powder include, in terms of oxide mass percentage: SiO2: 30-40%; H3BO3: 20-30%; ZnO: 15-20%; Cs2CO3: 10-15%; PbX2: 5-10%; and NaX: 5-10%.
[0058] In some embodiments, the method for preparing the aforementioned CsPbX3 perovskite quantum dot glass powder comprises the following steps:
[0059] preparing glass raw materials, melting the aforementioned glass raw materials at 1000-1100° C. to obtain a glass melt;
[0060] pouring the aforementioned glass melt into a mold to obtain a precursor glass;
[0061] The precursor glass is annealed at 350-450° C. for 2-3 hours to obtain CsPbX3 perovskite quantum dot glass; and
[0062] The aforementioned CsPbX3 perovskite quantum dot glass is ground into powder to obtain the aforementioned CsPbX3 perovskite quantum dot glass powder.
[0063] Specifically, the CsPbX3 perovskite quantum dot glass prepared using the method proposed in this invention features an amorphous glass component surrounding the outer ring of each perovskite grain, effectively preventing contact with water and oxygen and improving the long-term stability of the perovskite quantum dots. Annealing the precursor glass at 350-450°C for 2-3 hours can induce in-situ growth of CsPbX3 within the glass matrix. The CsPbX3 perovskite quantum dot glass can then be ground using conventional techniques in the art. For example, the CsPbX3 perovskite quantum dot glass can be placed in a ball mill, adjusted to a speed of 400-500 rpm, and milled for 5-6 hours to obtain a CsPbX3 perovskite quantum dot glass powder with a size of 100-200 nm.
[0064] In some embodiments, the method of filling the aforementioned perovskite quantum dot glass powder into the aforementioned microporous structure comprises the following steps:
[0065] a. The aforementioned perovskite quantum dot glass powder is dispersed in an organic solvent to obtain a quantum dot dispersion;
[0066] b. The aforementioned microporous structure of the aforementioned pickled optical fiber imaging element is immersed in the aforementioned quantum dot dispersion, ultrasonically treated, and then the aforementioned pickled optical fiber imaging element is removed, the aforementioned quantum dot dispersion is scraped off the surface without pores, and dried;
[0067] Repeat step b multiple times until the aforementioned microporous structure is fully filled with the aforementioned perovskite quantum dot glass powder to obtain the aforementioned filled optical fiber imaging element.
[0068] Specifically, the method for filling perovskite quantum dot glass powder is easy to operate, and the powder is evenly and compactly filled and not easy to fall off. Preferred are volatile, low-toxic organic solvents, such as acetone, anhydrous ethanol or isopropyl alcohol. The method of dispersing the powder in the organic solvent can be mechanical stirring, shaking or ultrasonic methods. For example, the perovskite quantum dot glass powder is evenly dispersed in an acetone solvent by ultrasonication for 30-50 minutes, the acid-washed optical fiber imaging element is immersed in the quantum dot dispersion and ultrasonically treated for 30-50 minutes, and then the acid-washed optical fiber imaging element is pulled out of the quantum dot dispersion at a speed of 1-3 mm / s, and the quantum dot dispersion on the non-porous position of the surface is scraped off with a scraper, and then the quantum dot glass powder is placed in an oven at 50-70°C and dried for 10-20 minutes to fill the microporous structure. This is repeated many times until the perovskite quantum dot glass powder fills the microporous structure.
[0069] In some embodiments, the size of the aforementioned perovskite quantum dot glass powder is 100-200 nm.
[0070] Specifically, when the size of perovskite quantum dot glass powder is less than 100nm, excessive perovskite grains are exposed, affecting the long-term stability of the perovskite quantum dots. When the size of perovskite quantum dot glass powder is greater than 200nm, it affects resolution. Therefore, the size of perovskite quantum dot glass powder is controlled between 100 and 200nm.
[0071] In some embodiments, the aforementioned protective layer includes an anti-reflection film.
[0072] Specifically, providing an antireflection coating can further increase the brightness of the optical fiber imaging element. The antireflection coating can be an aluminum oxide and hafnium oxide composite film 2. The aluminum oxide and hafnium oxide composite film 2 has the advantages of high hardness and high transmittance. For example, the film structure of the aluminum oxide and hafnium oxide composite film 2 and the thickness of each film layer are: HfO2 (115-118nm)-Al2O3 (70-72nm)-HfO2 (120-122nm)-Al2O3 (40-42nm)-HfO2 (72-74nm)-Al2O3 (80-82nm)-filled optical fiber imaging element.
[0073] In some embodiments, the aforementioned protective layer includes a quartz window 1 , and the thickness of the aforementioned quartz window 1 is 2 to 3 mm.
[0074] Specifically, when the protective layer includes both an antireflection film and a quartz window 1, the protective layer is installed as follows: an antireflection film is plated on the filling surface of the optical fiber imaging element, and then the surface of the antireflection film and the quartz window 1 are polished to a roughness of 5 to 10 nm. The quartz window 1 is then placed on the surface of the antireflection film and heated to increase the activation energy of the molecules and atoms on the surface of the antireflection film and the protective layer, so that the two are bonded into a single entity. Preferably, the heating temperature is 200 to 250°C.
[0075] The present invention provides a high-resolution ultraviolet detection optical fiber imaging element, which comprises:
[0076] An optical fiber imaging element, wherein the core of the optical fiber imaging element is made of an acid-etchable material and the cladding is made of an acid-resistant material, and the core of the optical fiber imaging element is recessed at a cross section at one end thereof, forming a microporous structure with a depth of 10 to 50 μm at the cross section;
[0077] Perovskite quantum dot glass powder, wherein the aforementioned perovskite quantum dot glass powder is filled in the aforementioned microporous structure; and
[0078] The protective layer is arranged on the cross section of the optical fiber imaging element filled with the perovskite quantum dot glass powder.
[0079] The present invention proposes an application of the aforementioned high-resolution ultraviolet detection optical fiber imaging element in the field of ultraviolet detection. For example, the high-resolution ultraviolet detection optical fiber imaging element proposed by the present invention can be installed on an ultraviolet detector for use.
[0080] The present invention will be further described below with reference to specific embodiments, but this should not be construed as limiting the scope of protection of the present invention. Non-essential improvements and adjustments made to the present invention by those skilled in the art based on the above-mentioned contents of the present invention still fall within the scope of protection of the present invention.
[0081] Unless otherwise specified, the materials and reagents mentioned below are commercially available products familiar to those skilled in the art. Unless otherwise specified, the methods described are all well-known methods in the art. Unless otherwise defined, technical or scientific terms used shall have the same meanings as those commonly understood by those skilled in the art.
[0082] In the following embodiments, the core of the optical fiber imaging element is made of an acid-etchable material. The core composition, calculated by mole percentage of oxides, includes: SiO2: 30.3-36.4%; B2O3: 18.9-20.2%; La2O3: 5.9-6.1%; the total content of BaO and CaO is 33.7-39.4%; Al2O3: 1.6-2.3%; TiO2: 2.0-2.9%; and the cladding of the optical fiber imaging element is 1.6-2.3%. Acid-resistant materials are used, and the cladding components, calculated by molar percentage of oxides, include: SiO2: 70.5~74.5%; PbO: 12.0~12.5%; Bi2O3: 0~2.0%; the total content of Na2O, K2O, Rb2O and Cs2O is: 5.8~7.7%; the total content of BaO and MgO is: 4.6~6.7%; Al2O3: 1.1~3.0%; TiO2: 0~2.0%.
[0083] Example 1:
[0084] This embodiment provides a high-resolution ultraviolet detection optical fiber image transmission element and its preparation method. Figure 1 .
[0085] The fiber optic imaging element in this embodiment uses a fiber optic panel with a core diameter of 10 μm and a thickness of 10 mm. The cross section of the fiber optic panel was immersed in a 1 L 0.5 mol / L nitric acid solution for 2 hours to form a regularly arranged microporous structure with a diameter of 10 μm and a depth of 10 μm in the cross section of the fiber optic panel, thereby obtaining an acid-washed fiber optic panel 4.
[0086] The perovskite quantum dot glass powder in this example is CsPbBr3 perovskite quantum dot glass powder 3, which has a green fluorescent color. The CsPbBr3 perovskite quantum dot glass composition, by oxide mass percentage, is 30% SiO2; 30% H3BO3; 20% ZnO; 10% Cs2CO3; 5% PbBr2; and 5% NaBr. Approximately 10g of high-purity raw materials are thoroughly mixed and melted in air at 1050°C for 12 minutes to produce a uniform glass melt. The melt is then poured into a brass mold to produce a precursor glass. Finally, the precursor glass is annealed by heating at 400°C for 2 hours to induce in-situ growth of CsPbBr3 within the glass matrix, yielding the CsPbBr3 perovskite quantum dot glass. The CsPbBr3 perovskite quantum dot glass was placed in a ball mill, the rotation speed was adjusted to 500 rpm, and the time was 5 hours to obtain CsPbBr3 perovskite quantum dot glass powder 3 with a size of 150 nm.
[0087] CsPbBr3 perovskite quantum dot glass powder 3 was added to an acetone solvent and sonicated for 30 minutes to uniformly disperse it, resulting in a quantum dot dispersion. An acid-washed optical fiber panel 4 was immersed in the quantum dot dispersion and sonicated for 30 minutes. The panel was then pulled out of the solution at a speed of 1 mm / s. The quantum dot dispersion on the surface without pores was scraped off with a scraper. The panel was then dried in an oven at 50°C for 10 minutes to fill the micropores with the CsPbBr3 perovskite quantum dot glass powder 3. This process was repeated multiple times until the micropores were completely filled with quantum dot glass powder, resulting in a filled optical fiber panel.
[0088] An aluminum oxide and hafnium oxide composite film 2 is plated on the filling surface of the fiber optic panel. A 2mm thick quartz window 1 is then placed on the surface of the anti-reflection film. A temperature of 230°C is applied to activate the molecules and atoms on the quartz window 1 and the surface of the anti-reflection film, bonding the two together to form a single unit. This results in a high-resolution optical fiber imaging element for ultraviolet detection. The film structure and thickness of the aluminum oxide and hafnium oxide composite film 2 are as follows:
[0089] Quartz window 1-HfO2 (115~118nm)-Al2O3 (70~72nm)-HfO2 (120~122nm)-Al2O3 (40~42nm)-HfO2 (72~74nm)-Al2O3 (80~82nm)-filled optical fiber faceplate.
[0090] 0.2 ml of the aforementioned quantum dot dispersion was dripped onto the surface of a quartz substrate with a thickness of 12 mm, and the rotation speed was controlled to 800 rpm for 60 s by spin coating. After spin coating, the substrate was heated in an oven at 60°C for 30 min to form a quantum dot glass film with a thickness of 10 μm on the surface of the quartz substrate to obtain a quantum dot glass film quartz plate.
[0091] The prepared CsPbBr3 quantum dot glass was subjected to X-ray diffraction test, and the results were as follows: Figure 10 As shown in the figure, it can be seen that the peaks correspond one to one with the PDF standard comparison card, proving that high-purity CsPbBr3 quantum dots have been successfully synthesized.
[0092] The fluorescence spectra of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in this embodiment were tested using a fluorescence spectrometer. The test results are shown in Figure 2. Figure 4 As shown, A is the luminous intensity curve of the quantum dot glass film quartz plate, and B is the luminous intensity curve of the optical fiber imaging element for high-resolution ultraviolet detection. The peak position of the quantum dot glass film quartz plate is at 530nm and the peak shape is sharp, and the relative luminous intensity is 100%. The peak position of the optical fiber imaging element for high-resolution ultraviolet detection is at 530nm and the peak shape is sharp, indicating that the luminous purity of the sample is high; the relative luminous intensity is 80%, and the luminous intensity is only lost by 20%, indicating that the luminous intensity of the sample is high. Using ultraviolet light as the light source to test the resolution of the optical fiber panel in this embodiment is 50.8lp / mm, and the resolution of the optical fiber imaging element for high-resolution ultraviolet detection is 50.8lp / mm, indicating that there is no loss of resolution when filling the quantum dot glass powder in the microporous structure.
[0093] Example 2:
[0094] This embodiment provides a high-resolution ultraviolet detection optical fiber image transmission element, the structural diagram of which is shown in FIG. Figure 2 .
[0095] This embodiment differs from Example 1 in that the optical fiber imaging element utilizes an optical fiber taper with a core diameter of 10 μm and a thickness of 10 mm. Furthermore, the pickled optical fiber panel 4 in Example 1 is replaced by a pickled optical fiber taper 5 in this embodiment; the filled optical fiber panel in Example 1 is replaced by a filled optical fiber taper in this embodiment.
[0096] The fluorescence spectra of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in this embodiment were tested using a fluorescence spectrometer. The test results are shown in Figure 2. Figure 5As shown, A is the luminous intensity curve of the quantum dot glass film quartz plate, and B is the luminous intensity curve of the optical fiber imaging element for high-resolution ultraviolet detection. The peak position of the quantum dot glass film quartz plate is at 530nm and the peak shape is sharp, and the relative luminous intensity is 100%. The peak position of the optical fiber imaging element for high-resolution ultraviolet detection is at 530nm and the peak shape is sharp, indicating that the luminous purity of the sample is high; the relative luminous intensity is 75%, and the luminous intensity is only lost by 25%, indicating that the luminous intensity of the sample is high. Using ultraviolet light as the light source to test the resolution of the optical fiber light cone in this embodiment is 50.8lp / mm, and the resolution of the optical fiber imaging element for high-resolution ultraviolet detection is 50.8lp / mm, indicating that there is no loss of resolution when filling the quantum dot glass powder in the microporous structure.
[0097] Example 3:
[0098] This embodiment provides a high-resolution ultraviolet detection optical fiber image transmission element, the structural diagram of which is shown in FIG. Figure 3 .
[0099] This embodiment differs from Embodiment 1 in that the optical fiber image transmission element utilizes an optical fiber image inverter with a core diameter of 10 μm and a thickness of 10 mm. Furthermore, the pickled optical fiber panel 4 in Embodiment 1 is replaced by the pickled optical fiber image inverter 6 in this embodiment; the filled optical fiber panel in Embodiment 1 is replaced by the filled optical fiber image inverter in this embodiment.
[0100] The fluorescence spectra of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in this embodiment were tested using a fluorescence spectrometer. The test results are shown in Figure 2. Figure 6 As shown, A is the luminous intensity curve of the quantum dot glass film quartz plate, and B is the luminous intensity curve of the optical fiber imaging element for high-resolution ultraviolet detection. The peak position of the quantum dot glass film quartz plate is at 530nm and the peak shape is sharp, and the relative luminous intensity is 100%. The peak position of the optical fiber imaging element for high-resolution ultraviolet detection is at 530nm and the peak shape is sharp, indicating that the luminous purity of the sample is high; the relative luminous intensity is 62%, and the luminous intensity is only lost by 38%, indicating that the luminous intensity of the sample is high. Using ultraviolet light as the light source to test the resolution of the optical fiber image inverter in this embodiment is 50.8lp / mm, and the resolution of the optical fiber imaging element for high-resolution ultraviolet detection is 50.8lp / mm, indicating that there is no loss of resolution when filling the quantum dot glass powder in the microporous structure.
[0101] Example 4:
[0102] This embodiment provides a fiber optic imaging element for high-resolution ultraviolet detection and a method for preparing the same.
[0103] This example differs from Example 1 in that the perovskite quantum dot glass in this example is a CsPbCl3 perovskite quantum dot glass that fluoresces blue. The CsPbCl3 perovskite quantum dot glass composition, calculated by oxide mass percentage, is 30% SiO2; 30% H3BO3; 20% ZnO; 10% Cs2CO3; 5% PbCl2; and 5% NaCl. 10g of high-purity raw materials were thoroughly mixed and melted in air at 1050°C for 12 minutes to produce a uniform glass melt. The glass melt was then poured into a brass mold to produce a precursor glass. Finally, the precursor glass was annealed by heating at 400°C for 2 hours to induce in-situ growth of CsPbCl3 within the glass matrix, yielding the CsPbCl3 perovskite quantum dot glass.
[0104] The fluorescence spectra of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in this embodiment were tested using a fluorescence spectrometer. The test results are shown in Figure 2. Figure 7 As shown, A is the luminous intensity curve of the quantum dot glass film quartz plate, and B is the luminous intensity curve of the optical fiber imaging element for high-resolution ultraviolet detection. The peak position of the quantum dot glass film quartz plate is at 450nm and the peak shape is sharp, and the relative luminous intensity is 100%. The peak position of the optical fiber imaging element for high-resolution ultraviolet detection is at 450nm and the peak shape is sharp, indicating that the luminous purity of the sample is high; the relative luminous intensity is 80.2%, and the luminous intensity is only lost by 19.8%, indicating that the luminous intensity of the sample is high. Using ultraviolet light as the light source to test the resolution of the optical fiber image inverter in this embodiment is 50.8lp / mm, and the resolution of the optical fiber imaging element for high-resolution ultraviolet detection is 50.8lp / mm, indicating that there is no loss of resolution when filling the quantum dot glass powder in the microporous structure.
[0105] Example 5:
[0106] This embodiment provides a fiber optic imaging element for high-resolution ultraviolet detection and a method for preparing the same.
[0107] This example differs from Example 1 in that the perovskite quantum dot glass in this example is CsPbI3 perovskite quantum dot glass that fluoresces red. The composition of the CsPbI3 perovskite quantum dot glass, calculated by oxide mass percentage, is 30% SiO2; 30% H3BO3; 20% ZnO; 10% Cs2CO3; 5% PbI2; and 5% NaI. 10g of high-purity raw materials were thoroughly mixed and melted in air at 1050°C for 12 minutes to produce a uniform glass melt. The glass melt was then poured into a brass mold to produce a precursor glass. Finally, the precursor glass was annealed at 400°C for 2 hours to induce in-situ growth of CsPbI3 within the glass matrix, resulting in the CsPbI3 perovskite quantum dot glass.
[0108] The fluorescence spectra of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in this embodiment were tested using a fluorescence spectrometer. The test results are shown in Figure 2. Figure 8 As shown, A is the luminous intensity curve of the quantum dot glass film quartz plate, and B is the luminous intensity curve of the optical fiber imaging element for high-resolution ultraviolet detection. The peak position of the quantum dot glass film quartz plate is at 630nm and the peak shape is sharp, and the relative luminous intensity is 100%. The peak position of the optical fiber imaging element for high-resolution ultraviolet detection is at 630nm and the peak shape is sharp, indicating that the luminous purity of the sample is high; the relative luminous intensity is 79.7%, and the luminous intensity is only lost by 20.3%, indicating that the luminous intensity of the sample is high. Using ultraviolet light as the light source to test the resolution of the optical fiber image inverter in this embodiment is 50.8lp / mm, and the resolution of the optical fiber imaging element for high-resolution ultraviolet detection is 50.8lp / mm, indicating that there is no loss of resolution when filling the quantum dot glass powder in the microporous structure.
[0109] Example 6
[0110] This embodiment provides a fiber optic imaging element for high-resolution ultraviolet detection and a method for preparing the same.
[0111] The difference between this embodiment and embodiment 1 is that in the high-resolution ultraviolet detection optical fiber imaging element of this embodiment, the aluminum oxide and hafnium oxide composite film 2 is not plated on the filling surface of the filling optical fiber faceplate.
[0112] The fluorescence spectra of the quantum dot glass film quartz plate and the high-resolution ultraviolet detection optical fiber imaging element in this embodiment were tested using a fluorescence spectrometer. The peak position of the quantum dot glass film quartz plate is at 530nm and the peak shape is sharp, and the relative luminous intensity is 100%. The peak position of the high-resolution ultraviolet detection optical fiber imaging element is at 530nm and the peak shape is sharp, indicating that the luminous purity of the sample is high; the relative luminous intensity is 70%, and the luminous intensity is only lost by 30%, indicating that the luminous intensity of the sample is high. Using ultraviolet light as the light source to test the resolution of the optical fiber panel in this embodiment is 50.8lp / mm, and the resolution of the high-resolution ultraviolet detection optical fiber imaging element is 50.8lp / mm, indicating that there is no loss of resolution when filling the quantum dot glass powder in the microporous structure.
[0113] Example 7
[0114] The difference between this embodiment and embodiment 1 is that when preparing the quantum dot glass film quartz plate and the optical fiber imaging element for high-resolution ultraviolet detection, the CsPbBr3 perovskite quantum dot glass powder is replaced with CdSe perovskite quantum dot glass powder.
[0115] Fluorescence spectra of the high-resolution ultraviolet detection fiber optic imaging element in Example 1 and the high-resolution ultraviolet detection fiber optic imaging element in this example were measured using a fluorescence spectrometer. The high-resolution ultraviolet detection fiber optic imaging element in Example 1 exhibited a peak at 530 nm, with a sharp peak shape and a relative luminous intensity of 100%. The high-resolution ultraviolet detection fiber optic imaging element in this example exhibited a peak at 530 nm, but with a larger full width at half maximum (FWHM) and a relative luminous intensity of 85%.
[0116] Comparative Example 1:
[0117] The optical fiber panel in Example 1 was used as a substrate, and a 10 μm thick perovskite quantum dot glass film was prepared on its surface to obtain a quantum dot glass film optical fiber imaging element. The specific method was as follows: the perovskite quantum dot glass powder in Example 1 was dispersed in anhydrous ethanol to prepare a quantum dot dispersion liquid. 0.2 ml of the quantum dot dispersion liquid was dripped onto the surface of the optical fiber panel. The spin coating method was controlled at a speed of 800 rpm for 60 seconds. After spin coating, the substrate was heated in an oven at 60°C for 30 minutes to form a 10 μm thick quantum dot glass film on the substrate surface.
[0118] The resolution of the quantum dot glass film fiber-optic imaging element was tested using ultraviolet light as a light source, resulting in a resolution of 45.3 lp / mm. This is lower than the high-resolution ultraviolet detection fiber-optic imaging element described in Example 1, demonstrating that the perovskite quantum dot glass powder filled into the microporous structure of the fiber faceplate effectively improves resolution.
[0119] Comparative Example 2:
[0120] The difference between Comparative Example 2 and Example 1 is that the perovskite quantum dot glass powder is replaced with P20 phosphor to obtain a P20 phosphor optical fiber imaging element.
[0121] The fluorescence spectra of the high-resolution ultraviolet detection optical fiber imaging element in Example 1 and the above-mentioned P20 phosphor optical fiber imaging element were tested using a fluorescence spectrometer. The test results are as follows: Figure 9 As shown in Figure 1, B is the luminous intensity curve of the high-resolution ultraviolet detection fiber optic imaging element in Example 1, and C is the luminous intensity curve of the P20 phosphor fiber optic imaging element. Taking the luminous intensity of the high-resolution ultraviolet detection fiber optic imaging element in Example 1 as 100%, the luminous intensity of the P20 phosphor fiber optic imaging element is only 47%, indicating that its luminous intensity is low. Its half-maximum width is large, indicating that its luminous purity is poor. The fiber optic imaging element provided by the present invention exhibits high luminous intensity and purity, effectively improving detection efficiency.
[0122] The technical features in the claims and / or the specification of the present invention may be combined, and the manner of combination is not limited to the combination obtained by reference in the claims. The technical solutions obtained by combining the technical features in the claims and / or the specification are also within the scope of protection of the present invention.
[0123] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.
Claims
1. A method for preparing a fiber optic imaging element for high-resolution ultraviolet detection, characterized in that: The steps include: Acid-washing the cross section of one end of the optical fiber imaging element to form a microporous structure at the cross section, wherein the depth of the microporous structure is 10 to 50 μm, thereby obtaining an acid-washed optical fiber imaging element; wherein the core of the optical fiber imaging element is made of an acid-resistant material and the cladding is made of an acid-resistant material; Filling the microporous structure with perovskite quantum dot glass powder to obtain a filled optical fiber imaging element; and A protective layer is provided on the filling surface of the filled optical fiber imaging element to obtain a high-resolution optical fiber imaging element for ultraviolet detection; The perovskite quantum dot glass powder is CsPbX3 perovskite quantum dot glass powder; wherein X is at least one of Cl, Br and I.
2. The preparation method according to claim 1, characterized in that Calculated in terms of oxide mass percentage, the components of the CsPbX3 perovskite quantum dot glass powder include: SiO2: 30-40%; H3BO3: 20-30%; ZnO: 15-20%; Cs2CO3: 10-15%; PbX2: 5-10%; and NaX: 5-10%.
3. The preparation method according to claim 2, characterized in that The preparation method of the CsPbX3 perovskite quantum dot glass powder comprises the following steps: preparing glass raw materials, and melting the glass raw materials at 1000-1100° C. to obtain a glass melt; pouring the glass melt into a mold to obtain a precursor glass; The precursor glass is annealed at 350-450° C. for 2-3 hours to obtain CsPbX3 perovskite quantum dot glass; and The CsPbX3 perovskite quantum dot glass is ground into powder to obtain the CsPbX3 perovskite quantum dot glass powder.
4. The preparation method according to claim 1, characterized in that The method of filling the perovskite quantum dot glass powder into the microporous structure comprises the following steps: a. The perovskite quantum dot glass powder is dispersed in an organic solvent to obtain a quantum dot dispersion; b. The microporous structure of the pickled optical fiber imaging element is immersed in the quantum dot dispersion, ultrasonically treated, and then the pickled optical fiber imaging element is removed, the surface of the quantum dot dispersion is scraped off without pores, and dried; Repeat step b multiple times until the perovskite quantum dot glass powder completely fills the microporous structure to obtain the filled optical fiber imaging element.
5. The preparation method according to claim 1, characterized in that The size of the perovskite quantum dot glass powder is 100-200 nm.
6. The preparation method according to claim 1, characterized in that The protective layer includes an anti-reflection film.
7. The preparation method according to claim 1, characterized in that The protective layer includes a quartz window, and the thickness of the quartz window is 2-3 mm.
8. A high-resolution ultraviolet detection optical fiber imaging element, characterized in that: It includes: An optical fiber imaging element, wherein the core of the optical fiber imaging element is made of an acid-etchable material, the cladding is made of an acid-resistant material, and the core is recessed at a cross section of one end of the optical fiber imaging element, forming a microporous structure with a depth of 10 to 50 μm at the cross section; Perovskite quantum dot glass powder, wherein the perovskite quantum dot glass powder is filled in the microporous structure; the perovskite quantum dot glass powder is CsPbX3 perovskite quantum dot glass powder; wherein X is at least one of Cl, Br and I; and A protective layer is provided on the cross section of the optical fiber imaging element filled with the perovskite quantum dot glass powder.
9. Use of the high-resolution ultraviolet detection optical fiber imaging element according to claim 8 in the field of ultraviolet detection.
Citation Information
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