CN113405995A - Preparation method of light conversion ultraviolet beam analyzer - Google Patents
Preparation method of light conversion ultraviolet beam analyzer Download PDFInfo
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- CN113405995A CN113405995A CN202110704623.7A CN202110704623A CN113405995A CN 113405995 A CN113405995 A CN 113405995A CN 202110704623 A CN202110704623 A CN 202110704623A CN 113405995 A CN113405995 A CN 113405995A
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- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 3
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- 229910052688 Gadolinium Inorganic materials 0.000 description 1
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- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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Abstract
A method for preparing a light conversion ultraviolet beam analyzer; it includes: the device comprises a light filter, an ultraviolet detection transparent ceramic chip and a CCD image processor; is characterized in that the ultraviolet detection transparent ceramic wafer after being processed is packaged on the surface of a CCD image processor, then the surface of the ultraviolet detection transparent ceramic wafer is covered with a visible light filter, and a sensitive glue is adopted to package a device; when ultraviolet light passes through the optical filter, the ultraviolet light is converted into visible light on the surface of the ultraviolet detection transparent ceramic wafer, then the visible light is received by the CCD photosensitive chip, visible light spots are recorded through the photoelectric conversion system, and the stability and the loss of the ultraviolet light in the transmission process can be calculated through processing the spots; the method can be used for manufacturing detection equipment such as an energy controller, a beam shape setter and the like in a photoetching machine, and can realize beam analysis of high-power DUV and EUV lasers; the technology has wider application scenes in the fields of laser communication, beam analysis, laser calibration and the like.
Description
Technical Field
The present invention belongs to the field of light exciting luminescent material preparing and applying technology.
Background
In the high and new technologies such as laser micromachining, medical laser source diagnosis and treatment, laser radar, inertial confinement nuclear fusion and the like which are newly developed in recent years, stricter requirements are provided for the beam quality such as the laser beam focusing degree and the beam mode, and higher requirements are provided for the accurate and effective measurement of laser airspace parameters for measuring the laser beam quality and representing the transmission characteristic of the laser beam. Conventional devices for analyzing laser beams include a rotating needle that reflects a small sample of the focused laser beam into a detector. When the needle rotates, it moves along the optical axis and measures the beam waist of the focused laser beam, a disadvantage of this method is that the device is bulky and requires many moving parts. Thus, not facilitating rapid and real-time analysis of the laser beam.
With the continuous development of the production and manufacturing industry, the application field of the laser is more and more extensive. For example, the stability of the laser marking head can be indirectly measured by measuring the stability of the coordinates of the light spots; in the optical field, the analysis of the focused light spot can be used for evaluating the effect of a lens or a designed optical system on a light beam, and guidance is provided for the quality improvement of a product; in the fields of laser marking, cutting and welding of various plastics, glass, metal and other materials such as mobile phone shells, toys and the like, the quality of laser spots needs to be analyzed in advance to improve the process or improve the yield and the like, and most of current light beam analysis adopts foreign systems and is high in price. In addition, during testing, a tester needs to manually capture a picture and write a test report by himself, and the test is tedious.
The invention discloses a preparation method of a light conversion ultraviolet beam analyzer; it includes: the device comprises a light filter, an ultraviolet detection transparent ceramic chip and a CCD image processor; is characterized in that the ultraviolet detection transparent ceramic wafer after being processed is packaged on the surface of a CCD image processor, then the surface of the ultraviolet detection transparent ceramic wafer is covered with a visible light filter, and a sensitive glue is adopted to package a device; when ultraviolet light passes through the optical filter, the ultraviolet light is converted into visible light on the surface of the ultraviolet detection transparent ceramic wafer, then the visible light is received by the CCD photosensitive chip, visible light spots are recorded through the photoelectric conversion system, the stability and the loss of the ultraviolet light in the transmission process can be calculated through processing the spots, and the shape and the size of the spots are adjusted; the method can be used for manufacturing detection equipment such as an energy controller, a beam shape setter and the like in a photoetching machine, and can realize beam analysis of high-power DUV and EUV lasers; the technology has wider application scenes in the fields of laser communication, beam analysis, laser calibration and the like.
The invention can realize visual ultraviolet laser detection, the absorption waveband range is 10nm-200nm, the emission waveband is 530nm-660nm, different ultraviolet detection transparent ceramic plates can be matched according to the photosensitive peak value of the CCD, the ceramic density can reach 90% -100%, the ultraviolet detection transparent ceramic plates have higher conversion efficiency in the light conversion process, high-precision display is easier to form in the light spot imaging process, and the invention has higher advantage application to laser imaging and light beam analysis. Meanwhile, laser detection with different powers of 10Mw-30W can be realized, and the method has the advantages of simplicity in operation, low cost and visualization.
Disclosure of Invention
A method for preparing a light conversion ultraviolet beam analyzer; it includes: the device comprises a light filter, an ultraviolet detection transparent ceramic chip and a CCD image processor; is characterized in that the ultraviolet detection transparent ceramic wafer after being processed is packaged on the surface of a CCD image processor, then the surface of the ultraviolet detection transparent ceramic wafer is covered with a visible light filter, and a sensitive glue is adopted to package a device; when ultraviolet light passes through the optical filter, the ultraviolet light is converted into visible light on the surface of the ultraviolet detection transparent ceramic wafer, then the visible light is received by the CCD photosensitive chip, visible light spots are recorded through the photoelectric conversion system, and the stability and the loss of the ultraviolet light in the transmission process can be calculated through processing the spots; the method can be used for manufacturing detection equipment such as an energy controller, a beam shape setter and the like in a photoetching machine, and can realize beam analysis of high-power DUV and EUV lasers; the technology has wider application scenes in the fields of laser communication, beam analysis, laser calibration and the like.
A method for preparing a light conversion ultraviolet beam analyzer; the filter is characterized in that the effective range of the wave band of the filter is 300-700 nm, the absorption rate is more than 99%, and the influence of external visible light on the detection result is effectively isolated; the ultraviolet detection transparent ceramic sheet is a material capable of converting ultraviolet invisible laser into visible light, the absorption waveband range of the ultraviolet detection transparent ceramic sheet is 10nm-200nm, the emission waveband of the ultraviolet detection transparent ceramic sheet is 530nm-660nm, and different ultraviolet detection transparent ceramic sheets can be matched according to the photosensitive peak value of a CCD; a CCD image processor is a processor that converts visible light into an electric signal and then outputs it as an image through a photoelectric conversion system.
A method for preparing a light conversion ultraviolet beam analyzer; the ultraviolet detection transparent ceramic plate is LuAG, Ce, YAG; ce. One or more of GOS and Eu; wherein the characteristic absorption wave band of the Ce system is 100-200nm, the emission wave band is 530-550 nm, and the effective power detection range is 10 mW-10W; wherein YAG; the absorption wavelength band of the Ce system is 150nm-200nm, the emission wavelength band is 560nm-610nm, and the power effective detection range is 100 mW-10W, wherein the absorption wavelength band of the Eu system is 100nm-200nm, the emission wavelength band is 610nm-660nm, and the power effective detection range is 100 mW-30W.
A method for preparing a light conversion ultraviolet beam analyzer; it is characterized in that the LuAG, the Ce and the YAG; the preparation method of the Ce ultraviolet detection transparent ceramic wafer comprises the steps of firstly preparing a nano precursor material by a hydrothermal method, wherein the particle size distribution range of the precursor is 30-100 nm; then the precursor is sintered for 1-3h by discharge plasma under the conditions of 1200-1550 ℃ and 60-200MPa to obtain LuAG, Ce and YAG; the Ce block is then doped with the lost doping ions Ce in the sintering process in an ion implantation mode, and then LuAG, Ce and YAG are added; annealing the Ce block in a muffle furnace for 30min at 500 ℃, wherein nitrogen protective gas is used in the annealing process; then, annealing the LuAG, Ce and YAG; carrying out hot isostatic pressing secondary sintering on the Ce block body at 1300-1500 ℃ in an inert gas environment of 150-250MPa for 3-6 hours to obtain LuAG, Ce and YAG; polishing and cutting the Ce ceramic wafer to obtain required LuAG, Ce and YAG; the Ce ultraviolet detection transparent ceramic sheet has the ceramic density of 90-100%.
A method for preparing a light conversion ultraviolet beam analyzer; the preparation method of the Eu ultraviolet detection transparent ceramic wafer is characterized in that firstly, a nano precursor material is prepared by a hydrothermal method, and the particle size distribution range of the precursor is 20-70 nm; then placing the precursor in the conditions of 1000-1150 ℃ and 30-150MPa, sintering for 3-5h by discharge plasma to obtain GOS and a Eu block, supplementing lost doped ions Eu in the sintering process by adopting an ion implantation mode, and then annealing the GOS and the Eu block in a muffle furnace for 30min at 500 ℃; the annealing process is carried out in a sulfur atmosphere, then the annealed GOS and the Eu block are subjected to hot isostatic pressing secondary sintering in an inert gas environment with the temperature of 1200-1300 ℃ and the pressure of 100-200MPa, the sintering time is 6-8 hours, the obtained GOS is obtained after the sintering, the Eu ceramic chip is subjected to polishing, cutting and other treatment modes to obtain the required GOS, and the density of the ceramic can reach 80-97% by virtue of the Eu ultraviolet detection transparent ceramic chip.
A method for preparing a light conversion ultraviolet beam analyzer; the specification of the ultraviolet detection transparent ceramic wafer required by cutting according to the size of the CCD chip is cut, the ceramic wafer is packaged on the surface of the CCD chip by utilizing an ultraviolet curing process, then the optical filter is attached to the surface of the ceramic wafer and is placed in a vacuum ultraviolet curing box, the vacuum standing is carried out for 30min, then ultraviolet packaging is carried out, the ultraviolet light beam visual detector is obtained after the ultraviolet light beam visual detector is completed, ultraviolet invisible light can be directly converted into visible light, meanwhile, the stability of the laser transmission process can be analyzed, the power loss in the laser transmission process is calculated, and the shape and the size of a light spot are adjusted.
Drawings
FIG. 1 is a cross-sectional view of a light-converting UV beam analyzer
Description of the drawings: 1 CCD image processor, 2 ultraviolet detecting transparent ceramic plate, 3 optical filter and 4 packaging photosensitive glue
Fig. 2 is a working schematic diagram of a light conversion ultraviolet beam analyzer.
Detailed Description
A method for preparing a light conversion ultraviolet beam analyzer; it includes: the device comprises a light filter, an ultraviolet detection transparent ceramic chip and a CCD image processor; is characterized in that the ultraviolet detection transparent ceramic wafer after being processed is packaged on the surface of a CCD image processor, then the surface of the ultraviolet detection transparent ceramic wafer is covered with a visible light filter, and a sensitive glue is adopted to package a device; when ultraviolet light passes through the optical filter, the ultraviolet light is converted into visible light on the surface of the ultraviolet detection transparent ceramic wafer, then the visible light is received by the CCD photosensitive chip, visible light spots are recorded through the photoelectric conversion system, and the stability and the loss of the ultraviolet light in the transmission process can be calculated through processing the spots; the method can be used for manufacturing detection equipment such as an energy controller, a beam shape setter and the like in a photoetching machine, and can realize beam analysis of high-power DUV and EUV lasers; the technology has wider application scenes in the fields of laser communication, beam analysis, laser calibration and the like.
A method for preparing a light conversion ultraviolet beam analyzer; the filter is characterized in that the effective range of the wave band of the filter is 300-700 nm, the absorption rate is more than 99%, and the influence of external visible light on the detection result is effectively isolated; the ultraviolet detection transparent ceramic sheet is a material capable of converting ultraviolet invisible laser into visible light, the absorption waveband range of the ultraviolet detection transparent ceramic sheet is 10nm-200nm, the emission waveband of the ultraviolet detection transparent ceramic sheet is 530nm-660nm, and different ultraviolet detection transparent ceramic sheets can be matched according to the photosensitive peak value of a CCD; a CCD image processor is a processor that converts visible light into an electric signal and then outputs it as an image through a photoelectric conversion system.
A method for preparing a light conversion ultraviolet beam analyzer; the ultraviolet detection transparent ceramic plate is LuAG, Ce, YAG; ce. One or more of GOS and Eu; wherein the characteristic absorption wave band of the Ce system is 100-200nm, the emission wave band is 530-550 nm, and the effective power detection range is 10 mW-10W; wherein YAG; the absorption wavelength band of the Ce system is 150nm-200nm, the emission wavelength band is 560nm-610nm, and the power effective detection range is 100 mW-10W, wherein the absorption wavelength band of the Eu system is 100nm-200nm, the emission wavelength band is 610nm-660nm, and the power effective detection range is 100 mW-30W.
The preparation method of the LuAG and Ce system comprises the following steps: firstly weighing lutetium oxide, aluminum oxide and gallium oxide according to a proportion, placing the materials into a beaker, adding dilute nitric acid to dissolve the materials, then preparing the materials into a solution with the mass fraction of 3% by using deionized water for standby, taking another beaker, weighing activators such as cerium oxide and neodymium oxide according to the weight ratio of 2-2.5%, adding nitric acid to dissolve the materials, then preparing the solution with the mass fraction of 1% by using the deionized water, and then preparing the solution according to the volume ratio of 80; 20, measuring the solution, mixing, adding 3% by weight of oxalic acid complexing agent, performing centrifugal washing to be neutral after precipitation is finished, and drying in a 120-DEG C vacuum drying oven for 3 hours to obtain a precursor material with the particle size distribution range of 30-100nm, wherein the nano precursor material can more easily form a high-density material in the process of sintering ceramics; the parameters of the discharge plasma are set in the primary sintering as follows: sintering at 1200-1550 ℃, under 60-200MPa for 1-3h in the presence of hydrogen in the reaction atmosphere, and obtaining LuAG and Ce block, supplementing lost doped ions Ce in the sintering process by ion implantation, and annealing the LuAG and Ce block in a vacuum furnace at 500 ℃ for 30min by using nitrogen protective gas in the annealing process; and then carrying out hot isostatic pressing on the annealed LuAG and Ce block for the third sintering, wherein the set parameters are as follows: the sintering temperature is 1300-1500 ℃, the sintering pressure is 150-250MPa, the sintering time is 3-6 hours, hot isostatic pressing sintering is carried out under the nitrogen protection environment, the obtained LuAG is obtained after the hot isostatic pressing sintering, the required LuAG is obtained by carrying out processing modes such as polishing, cutting and the like on the Ce ceramic wafer, the ceramic density of the Ce ultraviolet detection transparent ceramic wafer can reach 90-100%, so that the ultraviolet detection transparent ceramic wafer has higher conversion efficiency in the light conversion process, high-precision display is more easily formed in the light spot imaging process, and the method has higher advantage application to laser imaging and light beam analysis.
YAG in the invention; the preparation method of the Ce system comprises the following steps: firstly weighing yttrium oxide, aluminum oxide and gallium oxide according to a proportion, placing the yttrium oxide, the aluminum oxide and the gallium oxide into a beaker, adding dilute nitric acid to dissolve the yttrium oxide, the aluminum oxide and the gallium oxide, and then preparing the solution with the mass fraction of 3% by deionized water for later use, taking another beaker, weighing activators such as cerium oxide and neodymium oxide according to the weight ratio of 2-2.5%, adding nitric acid to dissolve the activators, and then preparing the solution with the mass fraction of 1% by deionized water, and then preparing the solution with the volume ratio of 80; 20, measuring the solution, mixing, adding 3% by weight of oxalic acid complexing agent, performing centrifugal washing to be neutral after precipitation is finished, and drying in a 120-DEG C vacuum drying oven for 3 hours to obtain a precursor material with the particle size distribution range of 20-70nm, wherein the nano precursor material can more easily form a high-density material in the process of sintering ceramics; the parameters of the discharge plasma are set in the primary sintering as follows: sintering at 1200-1550 ℃, under 60-200MPa for 1-3h in hydrogen atmosphere, and obtaining YAG; ce block, then doping ion Ce lost in the sintering process is supplemented by adopting an ion implantation mode, and then YAG is added; annealing the Ce block in a vacuum furnace at 500 ℃ for 30min, wherein nitrogen is used as a protective gas in the annealing process; then annealing the YAG; carrying out hot isostatic pressing for the third sintering on the Ce block, and setting parameters as follows: sintering at 1300-1500 ℃ under the sintering pressure of 150-250MPa for 3-6 hours, and carrying out hot isostatic pressing sintering under the nitrogen protection environment to obtain YAG; polishing, cutting and other treatment modes are carried out on the Ce ceramic wafer to obtain the needed YAG; the ceramic density of the Ce ultraviolet detection transparent ceramic sheet can reach 90-100%, so that the ultraviolet detection transparent ceramic sheet has higher conversion efficiency in the light conversion process, high-precision display is easier to form in the light spot imaging process, and the Ce ultraviolet detection transparent ceramic sheet has higher advantage application to laser imaging and beam analysis.
The preparation method of the Eu system comprises the following steps: weighing gadolinium oxide according to a certain proportion, placing the gadolinium oxide into a beaker, adding dilute nitric acid to dissolve the gadolinium oxide, and then preparing the gadolinium oxide into a solution with the mass fraction of 5% by using deionized water for later use, taking another beaker, weighing 1-1.5% by weight of europium oxide, cerium oxide, neodymium oxide, samarium oxide and other activators, adding nitric acid to dissolve the europium oxide, cerium oxide, neodymium oxide, samarium oxide and the like, and preparing the europium oxide, cerium oxide, samarium oxide and the like into a solution with the mass fraction of 5%, and then preparing the gadolinium; 15, measuring the solution, mixing, adding 5% by weight of oxalic acid complexing agent, performing centrifugal water washing to be neutral after precipitation is finished, drying for 3 hours in a 120-DEG C vacuum drying oven to obtain a precursor material, adding 3% of high-purity sulfur into the precursor material, placing the precursor material in a ball milling tank for ball milling for 4 hours, and obtaining the precursor material with the particle size distribution range of 30-80nm after ball milling is finished; parameters of the discharge plasma furnace were set as follows: sintering temperature is 1000-1150 ℃, vacuum pressure is 30-150MPa, sintering time is 3-5 hours, and GOS and Eu blocks are obtained after sintering is finished; then, supplementing lost doping ions Eu in the sintering process by adopting an ion implantation mode, and then annealing the Eu block in a muffle furnace for 30min at the temperature of 500 ℃; the annealing process is carried out in a sulfur atmosphere, and then the annealed GOS and Eu blocks are sintered for the third time by hot isostatic pressing, and the set parameters are as follows: the sintering temperature is 1200-1300 ℃, the vacuum pressure is 100-200MPa, the sintering time is 6-8 hours, the sintering process is completed in the inert gas environment of nitrogen, then the obtained GOS is obtained, the processing modes of polishing, cutting and the like are carried out on the Eu ceramic chip to obtain the GOS with the required specification, the ceramic density of the Eu ultraviolet detection transparent ceramic chip can reach 80-97 percent, so that the ultraviolet detection transparent ceramic chip has higher conversion efficiency in the light conversion process, high-precision display is more easily formed in the light spot imaging process, and the Eu ultraviolet detection transparent ceramic chip has higher advantage application for laser imaging and light beam analysis.
A method for preparing a light conversion ultraviolet beam analyzer; the specification of the ultraviolet detection transparent ceramic wafer required by cutting according to the size of the CCD chip is cut, the ceramic wafer is packaged on the surface of the CCD chip by utilizing an ultraviolet curing process, then the optical filter is attached to the surface of the ceramic wafer and is placed in a vacuum ultraviolet curing box, the vacuum standing is carried out for 30min, then ultraviolet packaging is carried out, the ultraviolet light beam visual detector is obtained after the ultraviolet light beam visual detector is completed, ultraviolet invisible light can be directly converted into visible light, meanwhile, the stability of the laser transmission process can be analyzed, the power loss in the laser transmission process is calculated, and the shape and the size of a light spot are adjusted.
The invention has the advantages that
1) The preparation method of the light conversion ultraviolet beam analyzer is simple in production process, easy to control in process, suitable for mass production, low in cost and convenient to use.
2) The preparation method of the light conversion ultraviolet beam analyzer is non-toxic, harmless, low in cost and high in efficiency.
) The invention records visible light spots through a photoelectric conversion system, and the stability and the loss of ultraviolet laser in the transmission process can be calculated through processing the spots; the technology has wider application scenes in the fields of laser communication, beam analysis, laser calibration and the like.
Examples
Example 1
Respectively weighing 5.5 g of Lu2O3, 4.2 g of Ga2O3 and 6.8 g of Al2O3, placing the materials in a beaker, then adding 100mL of 18% dilute nitric acid solution, stirring and dissolving the materials at room temperature, respectively placing the solutions on an electric furnace for heating crystallization after the dissolution is finished, evaporating the redundant nitric acid solution, and then respectively adding 2000mL of deionized water to dilute the solution into a neutral solution A for later use.
And (3) taking another beaker, weighing 1.5g of CeO2, placing the weighed beaker into the beaker, adding 20mL of 18% dilute nitric acid solution, stirring and dissolving the solution at room temperature, placing the solution on an electric furnace respectively after the solution is dissolved, heating and crystallizing the solution, evaporating the redundant nitric acid solution, and then adding 2000mL of deionized water respectively to dilute the solution into a neutral solution B for later use.
And finally, taking 10 g of oxalic acid, adding deionized water for dissolving and filtering, and then fixing the volume of the solution to 300ml to prepare a complexing agent solution C for later use.
Firstly, evenly mixing A, B solution, stirring at room temperature, then adding the solution C into the mixed solution at the speed of 5ml/min through a peristaltic pump, continuously stirring, reacting for 1 hour, centrifuging the solution to obtain a precursor material, and drying for 3 hours in a 120 ℃ vacuum drying oven to obtain the precursor material with the average particle size of 50 nm.
The parameters of the discharge plasma are set in the primary sintering as follows: the method comprises the steps of (1) carrying out sintering at 1350 ℃, sintering at 150MPa for 1.5 hours in hydrogen atmosphere, obtaining LuAG after the reaction is finished, carrying out surface pretreatment on a Ce block, removing surface sintering damaged materials, supplementing lost doped ion Ce in the sintering process by adopting an ion injection mode, then wrapping the LuAG and Ce block in an aluminum foil, annealing for 30min in a vacuum furnace at 500 ℃, and using nitrogen protection gas in the annealing process; and (3) sintering for the third time: and placing the annealed LuAG and Ce block body into a hot isostatic pressing furnace, and setting the parameters as follows: the sintering temperature is 1500 ℃, the sintering pressure is 250MPa, the sintering time is 3 hours, hot isostatic pressing sintering is carried out under the nitrogen protection environment, the obtained LuAG is obtained after the hot isostatic pressing sintering, the Ce ceramic wafer is subjected to processing modes such as polishing, cutting and the like to obtain the required LuAG, the Ce ultraviolet detection transparent ceramic wafer can reach 99% of ceramic density through testing, the transmittance is higher than 80%, and the relative conversion efficiency is 95%.
Example 2
10.5 g of Gd2O3 is respectively weighed and placed in a beaker, then 60mL of 18% dilute nitric acid solution is added, the mixture is stirred and dissolved at room temperature, after the dissolution is finished, the solutions are respectively placed on an electric furnace to be heated and crystallized, redundant nitric acid solution is evaporated, and then 2000mL of deionized water is respectively added to dilute the solution into neutral solution D for standby.
And (3) taking another beaker, weighing 0.5gEu2O3, placing the beaker into the beaker, adding 10mL of 18% dilute nitric acid solution, stirring and dissolving the solution at room temperature, placing the solution on an electric furnace respectively for heating crystallization after the solution is dissolved, evaporating the redundant nitric acid solution, and then adding 100mL of deionized water respectively to dilute the solution into a neutral solution E for later use.
And finally, taking 5g of oxalic acid, adding deionized water for dissolving and filtering, and then fixing the volume of the solution to 200ml to prepare a complexing agent solution F for later use.
Firstly, evenly mixing D, E solution, stirring at room temperature, then adding the solution C into the mixed solution at the speed of 5ml/min through a peristaltic pump, continuously stirring, reacting for 1 hour, centrifuging the solution to obtain a precursor material, drying for 3 hours in a 120 ℃ vacuum drying oven to obtain the precursor material with the average particle size of 30nm, then weighing 0.3 g of high-purity sulfur, adding the high-purity sulfur into the precursor, performing ball milling treatment to obtain GOS, and keeping the Eu precursor for later use.
The parameters of the discharge plasma are set in the primary sintering as follows: the method comprises the steps of sintering at 1000 ℃, sintering at 100MPa for 4 hours to obtain GOS, pretreating the surface of a Eu block to remove surface sintering blanks, supplementing lost doped Eu in the sintering process by adopting an ion implantation mode, and annealing the Eu block in a muffle furnace at 500 ℃ for 30min by using sulfur gas protective gas in the annealing process; and (3) sintering for the third time: placing the annealed GOS and Eu blocks into a hot isostatic pressing furnace, and setting the parameters as follows: the sintering temperature is 1100 ℃, the sintering pressure is 120MPa, the sintering time is 8 hours, hot isostatic pressing sintering is carried out under the nitrogen protection environment, the obtained GOS is obtained after the hot isostatic pressing sintering, the required GOS is obtained by carrying out processing modes such as polishing, cutting and the like on the Eu ceramic wafer, the density of the Eu ultraviolet detection transparent ceramic wafer can reach 95% through testing, the transmittance is higher than 82%, and the relative conversion efficiency is 98%.
While the foregoing is directed to the preferred embodiment of the present invention, it will be apparent to those skilled in the art that various changes and modifications can be made herein without departing from the spirit and scope of the invention.
Claims (8)
1. A method for preparing a light conversion ultraviolet beam analyzer; it includes: the device comprises a light filter, an ultraviolet detection transparent ceramic chip and a CCD image processor; is characterized in that the ultraviolet detection transparent ceramic wafer after being processed is packaged on the surface of a CCD image processor, then the surface of the ultraviolet detection transparent ceramic wafer is covered with a visible light filter, and a sensitive glue is adopted to package a device; when ultraviolet light passes through the optical filter, the ultraviolet light is converted into visible light on the surface of the ultraviolet detection transparent ceramic wafer, then the visible light is received by the CCD photosensitive chip, visible light spots are recorded through the photoelectric conversion system, and the stability and the loss of the ultraviolet light in the transmission process can be calculated through processing the spots; the method can be used for manufacturing detection equipment such as an energy controller, a beam shape setter and the like in a photoetching machine, and can realize beam analysis of high-power DUV and EUV lasers; the technology has wider application scenes in the fields of laser communication, beam analysis, laser calibration and the like.
2. A method of making a light-converting ultraviolet beam analyzer according to claim 1; the filter is characterized in that the effective over-rate wave band range of the filter is 300-700 nm, the absorption rate reaches more than 99%, and the influence of external visible light on the detection result is effectively isolated.
3. A method of making a light-converting ultraviolet beam analyzer according to claim 1; the ultraviolet detection transparent ceramic sheet is a material capable of converting ultraviolet invisible laser into visible light, the absorption waveband range of the ultraviolet detection transparent ceramic sheet is 10nm-200nm, the emission waveband of the ultraviolet detection transparent ceramic sheet is 530nm-660nm, and different ultraviolet detection transparent ceramic sheets can be matched according to the photosensitive peak value of a CCD.
4. A method of making a light-converting ultraviolet beam analyzer according to claim 1; the CCD image processor is a processor which can convert visible light into electric signals and then output the electric signals as images through a photoelectric conversion system.
5. A method of making a light-converting ultraviolet beam analyzer according to claim 1; the ultraviolet detection transparent ceramic plate is LuAG, Ce, YAG; ce. One or more of GOS and Eu; wherein the characteristic absorption wave band of the Ce system is 100-200nm, the emission wave band is 530-550 nm, and the effective power detection range is 10 mW-10W; wherein YAG; the absorption wavelength band of the Ce system is 150nm-200nm, the emission wavelength band is 560nm-610nm, and the power effective detection range is 100 mW-10W, wherein the absorption wavelength band of the Eu system is 100nm-200nm, the emission wavelength band is 610nm-660nm, and the power effective detection range is 100 mW-30W.
6. A method of making a light-converting ultraviolet beam analyzer according to claim 1; it is characterized in that the LuAG, the Ce and the YAG; the preparation method of the Ce ultraviolet detection transparent ceramic wafer comprises the steps of firstly preparing a nano precursor material by a hydrothermal method, wherein the particle size distribution range of the precursor is 30-100 nm; then the precursor is sintered for 1-3h by discharge plasma under the conditions of 1200-1550 ℃ and 60-200MPa to obtain LuAG, Ce and YAG; the Ce block is then doped with the lost doping ions Ce in the sintering process in an ion implantation mode, and then LuAG, Ce and YAG are added; annealing the Ce block in a muffle furnace for 30min at 500 ℃, wherein nitrogen protective gas is used in the annealing process; then, annealing the LuAG, Ce and YAG; carrying out hot isostatic pressing secondary sintering on the Ce block body at 1300-1500 ℃ in an inert gas environment of 150-250MPa for 3-6 hours to obtain LuAG, Ce and YAG; polishing and cutting the Ce ceramic wafer to obtain 90-100% dense LuAG, Ce and YAG; the Ce ultraviolet detects the transparent ceramic plate.
7. A method of making a light-converting ultraviolet beam analyzer according to claim 1; the preparation method of the Eu ultraviolet detection transparent ceramic wafer is characterized in that firstly, a nano precursor material is prepared by a hydrothermal method, and the particle size distribution range of the precursor is 20-70 nm; then placing the precursor in the conditions of 1000-1150 ℃ and 30-150MPa, sintering for 3-5h by discharge plasma to obtain GOS and a Eu block, supplementing lost doped ions Eu in the sintering process by adopting an ion implantation mode, and then annealing the GOS and the Eu block in a muffle furnace for 30min at 500 ℃; annealing in sulfur atmosphere, hot isostatic pressing secondary sintering the annealed GOS and Eu block in an inert gas environment of 1200-1300 ℃ and 100-200MPa for 6-8 hours to obtain GOS, polishing and cutting the Eu ceramic chip to obtain 80-97% compact GOS, and detecting the Eu ultraviolet transparent ceramic chip.
8. A method of making a light-converting ultraviolet beam analyzer according to claim 1; the specification of the ultraviolet detection transparent ceramic wafer required by cutting according to the size of the CCD chip is cut, the ceramic wafer is packaged on the surface of the CCD chip by utilizing an ultraviolet curing process, then the optical filter is attached to the surface of the ceramic wafer and is placed in a vacuum ultraviolet curing box, the vacuum standing is carried out for 30min, then ultraviolet packaging is carried out, the ultraviolet light beam visual detector is obtained after the ultraviolet light beam visual detector is completed, ultraviolet invisible light can be directly converted into visible light, meanwhile, the stability of the laser transmission process can be analyzed, the power loss in the laser transmission process is calculated, and the shape and the size of a light spot are adjusted.
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