CN113663624A - Equipment for preparing superfine cathode ray fluorescent powder - Google Patents
Equipment for preparing superfine cathode ray fluorescent powder Download PDFInfo
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- CN113663624A CN113663624A CN202110893574.6A CN202110893574A CN113663624A CN 113663624 A CN113663624 A CN 113663624A CN 202110893574 A CN202110893574 A CN 202110893574A CN 113663624 A CN113663624 A CN 113663624A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/121—Coherent waves, e.g. laser beams
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/288—Sulfides
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- C01F17/00—Compounds of rare earth metals
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- C01F17/288—Sulfides
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7701—Chalogenides
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Abstract
The invention discloses equipment for preparing superfine cathode ray fluorescent powder, belonging to the technical field of laser technology and materials. The equipment comprises a laser emitter, a photo-thermal reaction kettle and a displacement platform. The method comprises the steps of placing the prepared precursor solution in a photo-thermal reaction kettle through laser irradiation, controlling the pressure and the temperature in the reaction kettle, adjusting a displacement platform, centrifugally drying the irradiated solution, and vulcanizing and sintering to finally obtain the ultrafine cathode ray fluorescent powder particles. The invention has strong practicability and high controllability, the particle size of the fluorescent powder obtained by the equipment is within 5-80nm, and the invention can be widely applied to the preparation of the superfine cathode ray fluorescent powder.
Description
Technical Field
The invention belongs to the technical field of laser technology and materials, and relates to equipment for preparing superfine cathode ray fluorescent powder.
Background
Phosphor is a material that converts energy supplied from the outside into light, is widely used as a substance that converts to visible light that can be seen by the human eye, and is an important support material in the field of illumination and display. Since light incident on the eye is emitted from the phosphor, it can be said that the portions of brightness, color, and the like that are eventually perceived by humans depend on the phosphor. The fluorescent powder is called cathode ray fluorescent powder, and its main chemical composition includes rare earth metal elements of yttrium (Y), europium (Eu), cerium (Ce), terbium (Te) and so on. The preparation method of the cathode ray fluorescent powder mainly comprises a solid phase method, a solvothermal method and the like, and the cathode ray fluorescent powder is widely applied to various fields such as illumination, display, medical treatment, detection of radiation fields and the like.
Current research on cathode ray phosphors suggests that the smaller the particle size, the lower the luminous efficiency of the phosphor, and thus there is little research on the performance of nano-sized phosphors. On the other hand, the smaller the particle size, the higher the image definition, and the small particle size phosphor particles can form a dense and compact powder layer, which can significantly improve the aging problem of the device, thus providing a new idea for the application of nano-level phosphor. Therefore, the development of a device for efficiently preparing the superfine cathode ray fluorescent powder is the important point for realizing the industrial application of the nano-grade fluorescent powder.
Aiming at the problems, the invention provides a laser photo-thermal reaction kettle system, which utilizes a precursor solution in a laser irradiation reaction kettle to realize the regulation and control of the particle diameter of fluorescent powder, obtains nano-grade fluorescent powder with high brightness, small attenuation and uniform dispersion, and well solves the problem that the superfine fluorescent powder is difficult to prepare.
Disclosure of Invention
The invention aims to provide a device for preparing superfine fluorescent powder by utilizing laser irradiation, aiming at the defects of the prior nanometer-sized cathode ray fluorescent powder preparation technology. The device passes through laser instrument transmission laser, then through the precursor solution in the light and heat reation kettle of light path system irradiation, monitors simultaneously and controls the temperature and the pressure in the reation kettle, lets solution remain the rotation state throughout, controls displacement platform during and finds suitable radiation position, then carries out centrifugal drying, vulcanization sintering with the solution after the laser irradiation, finally can obtain the phosphor powder granule that dispersion is even, the particle size is tiny.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the device comprises a laser emitter, a light path system, a photo-thermal reaction kettle and a displacement platform, wherein a light outlet is formed in the laser emitter, and the light path system comprises an aperture, a first reflector, a second reflector, a third reflector, a lens, a first telescopic rod and a second telescopic rod;
the aperture, the first telescopic rod and the second telescopic rod are sequentially arranged in the light emitting direction of the light outlet, the first reflector and the second reflector are respectively arranged on the upper side and the lower side of the first telescopic rod, the third reflector and the lens are respectively arranged on the upper side and the lower side of the second telescopic rod, telescopic adjusting devices are fixedly connected to the bottom of the aperture, the bottom of the lens and the bottom of the third reflector, and angle adjusters are respectively arranged on the first reflector, the second reflector and the third reflector;
utilize the deflection angle of angle regulator adjustment first speculum, second reflector and third reflector, utilize flexible adjusting device adjustment light ring, flexible length on lens, the third reflector to make the laser that jets out from the light-emitting window pass light ring, first speculum, second reflector, third reflector and lens in proper order and jet into after light-thermal reaction cauldron's inside, light-thermal reaction cauldron sets up on displacement platform, utilizes displacement platform adjustment light-thermal reaction cauldron's position.
Further, the laser emitter is Nd: YAG solid laser can output laser with 1064, 532 and 355nm wavelength.
Further, the retractable adjustment device comprises a fixing rod, a sleeve rod and a fastening screw, wherein one end of the fixing rod is fixedly connected to the aperture or the lens, the other end of the fixing rod is slidably arranged in the sleeve rod, the sleeve rod is provided with a threaded hole, and the fastening screw is in threaded connection with the interior of the threaded hole.
Furthermore, the adjusting range of the telescopic rod is 20-60cm, and the adjusting range of the telescopic adjusting device is 10-30 cm.
Further, a magneton is placed in the photo-thermal reaction kettle, so that the solution is always in a rotating state in the experimental process.
Furthermore, the temperature of the photo-thermal reaction kettle can be adjusted within the range of 25-250 ℃, the rotating speed of the photo-thermal reaction kettle is 0-1200 r/min, and the working pressure of the photo-thermal reaction kettle is 0-20 Mpa.
Furthermore, the charging coefficient of the photo-thermal reaction kettle body is two thirds of the full volume, and the photo-thermal reaction kettle body is only suitable for charging liquid media.
Furthermore, the displacement platform is respectively provided with a motor and a screw rod for driving in X, Y, Z three directions, and is provided with a slide rail and a slide groove which are matched with each other for guiding.
Furthermore, the displacement platform is made of aluminum alloy, and the movement speed in the X, Y, Z three directions is 0-50 mm/s.
Compared with the prior art, the invention has the following beneficial effects:
1. aiming at the shortage of the prior art for preparing the superfine cathode ray fluorescent powder, a laser irradiation system is introduced to control the size of the fluorescent powder particles. In the irradiation process, the particle size is well controlled, new defects are introduced to suspended precursor particles in the irradiation process by laser, and the performance of the finally synthesized cathode ray fluorescent powder is well influenced.
2. The photo-thermal reaction kettle is introduced for controlling temperature and pressure and simultaneously providing a function of stirring solution, so that laser can uniformly irradiate the precursor solution in the experimental process, and finally fluorescent powder particles with uniform dispersion and fine particle size can be obtained after centrifugal drying and vulcanization sintering treatment.
3. The displacement platform is introduced, so that the position and the height of the photo-thermal reaction kettle can be changed in the laser irradiation process, and the laser irradiation efficiency is further improved. A plurality of groups of contrast tests can be set, and the most suitable laser irradiation position and height can be selected by adjusting the displacement platform, so that the foundation is laid for the mass production of the superfine cathode ray fluorescent powder.
4. The device has high applicability and strong controllability, and can realize the preparation of the nano-scale cathode ray fluorescent powder. The cathode ray fluorescent powder prepared by the equipment has the advantages of controllable central particle size in the range of 5-80nm, high brightness, small attenuation, small dispersion and high luminous efficiency.
Drawings
FIG. 1 is a schematic view of an apparatus for preparing ultra-fine cathode ray phosphor powder in a laser photo-thermal reactor;
in the figure: 1. a laser transmitter; 2. a light outlet; 3. an aperture; 4. a first telescopic adjusting device knob; 5. a first telescopic adjusting device; 6. an adjusting knob of the telescopic rod; 7. a first telescopic rod; 8. a second reflecting mirror; 9. a second screw of the reflector; 10. a mirror two carrier; 11. a second angle adjuster of the reflector; 12. a carrier fixing bracket; 13. a screw of the reflector; 14. a first reflecting mirror; 15. a reflector-carrier; 16. a mirror angle adjuster; 17. a second telescopic rod; 18. a second adjusting knob of the telescopic rod; 19. a second telescopic adjusting device knob; 20. a mirror triangle adjuster; 21. a reflector three-carrier; 22. a reflector triple screw; 23. a third reflector; 24. a second telescopic adjusting device; 25. a third telescopic adjusting device knob; 26. a lens carrier; 27. a lens; 28. a pressure gauge and a burst valve; 29. a needle valve; 30. a main machine box body of the photothermal reaction kettle; 31. a photo-thermal reaction kettle body; 32. a control panel; 33. a magneton; 34. a Z-direction sliding device; 35. an X-direction slide rail; 36. a Y-direction slide rail; 37. a displacement platform; 38. and a third telescopic adjusting device.
Detailed Description
The device comprises a laser emitter, a light path system, a photo-thermal reaction kettle and a displacement platform, wherein a light outlet is formed in the laser emitter, and the light path system comprises an aperture, a first reflector, a second reflector, a third reflector, a lens, a first telescopic rod and a second telescopic rod;
the aperture, the first telescopic rod and the second telescopic rod are sequentially arranged in the light emitting direction of the light outlet, the first reflector and the second reflector are respectively arranged on the upper side and the lower side of the first telescopic rod, the third reflector and the lens are respectively arranged on the upper side and the lower side of the second telescopic rod, telescopic adjusting devices are fixedly connected to the bottom of the aperture, the bottom of the lens and the bottom of the third reflector, and angle adjusters are respectively arranged on the first reflector, the second reflector and the third reflector;
utilize the deflection angle of angle regulator adjustment first speculum, second reflector and third reflector, utilize flexible adjusting device adjustment light ring, flexible length on lens, the third reflector to make the laser that jets out from the light-emitting window pass light ring, first speculum, second reflector, third reflector and lens in proper order and jet into after light-thermal reaction cauldron's inside, light-thermal reaction cauldron sets up on displacement platform, utilizes displacement platform adjustment light-thermal reaction cauldron's position.
Further, the laser emitter is Nd: YAG solid laser can output laser with 1064, 532 and 355nm wavelength.
Further, scalable adjusting device includes dead lever, loop bar and fastening screw, dead lever one end fixed connection is in light ring or lens, and the other end slides and sets up inside the loop bar, be provided with the screw hole on the loop bar, fastening screw threaded connection is inside the screw hole.
Furthermore, the adjusting range of the telescopic rod is 20-60cm, and the adjusting range of the telescopic adjusting device is 10-30 cm.
Furthermore, a magneton is placed in the reaction kettle, so that the solution is always in a rotating state in the experimental process.
Furthermore, the temperature adjustable range of the photo-thermal reaction kettle is 25-250 ℃, the rotating speed range is 0-1200 r/min, and the working pressure is 0-20 Mpa.
Furthermore, the charging coefficient of the photo-thermal reaction kettle body is two thirds of the full volume, and the photo-thermal reaction kettle body is only suitable for charging liquid media.
Furthermore, the displacement platform is provided with a motor and a screw rod for driving, and a sliding rail and a sliding groove which are matched with each other for guiding in X, Y, Z three directions respectively.
Furthermore, the displacement platform is made of aluminum alloy, and the movement speed in the X, Y, Z three directions is 0-50 mm/s.
The invention is further illustrated with reference to the figures and examples.
As shown in the figures, the overall embodiment of the present invention is: the aperture 3 and the reflectors 14,8 and 23 are used for transmitting light paths, the lens 27 is used for focusing light beams, the photothermal reaction kettle 30 is used for adjusting the temperature of the precursor solution and providing a stirring function, and the displacement platform 37 is used for adjusting the position and the height of the photothermal reaction kettle. The screws 13,9,22 on the lens carrier 26 and the carriers 15,10,21 of the mirrors one, two, three, respectively, are first unscrewed with a tool, and then the mirrors 14,8,23 and the lenses 27 are mounted on the corresponding carriers 15,10,21,26, respectively. And the first telescopic adjusting device knob 4 is rotated to enable the light outlet 2 and the diaphragm 3 to be in the same horizontal plane, so that the light path can smoothly enter the diaphragm 3. Then, adjusting knobs 6 and 18 of the first telescopic rod and the second telescopic rod 7 and 17 are rotated to enable the telescopic rods to reach proper heights, angle adjusters 16,11 and 20 on the first reflecting mirror, the second reflecting mirror and the third reflecting mirror 14,8 and 23 are respectively adjusted, so that the aperture 3 and the first reflecting mirror 14 form a proper angle, the first reflecting mirror 14 and the second reflecting mirror 8 form a proper angle, and the second reflecting mirror 8 and the third reflecting mirror 23 form a proper angle, and smooth transmission of a light path is guaranteed. And meanwhile, the first telescopic adjusting device knob, the second telescopic adjusting device knob 19 and the second telescopic adjusting device knob 25 on the second telescopic rod 17 are adjusted to ensure that the light path penetrates through the aperture 3, the first reflector 14, the second reflector 8, the third reflector 23 and the lens 27 in sequence and then is injected into the photo-thermal reaction kettle. Dry and clean magnets 33 are put into the photo-thermal reaction vessel body 31, and then the needle valve 29 is rotated counterclockwise to ventilate, and the needle valve is closed clockwise at the beginning of the experiment. The displacement platform 37 is connected to a computer and the platform is controlled using corresponding computer software.
Dissolving a certain amount of matrix rare earth oxide and activator rare earth oxide in concentrated nitric acid, adding into a certain amount of glycol solution, and sequentially adding polyvinylpyrrolidone and ethanol solution dissolved with thiourea into the solution. Then, NaOH solution is dripped to adjust the pH value of the solution, and the obtained solution is poured into a photo-thermal chemical reaction kettle. Then, a nanosecond laser 1 is started, laser parameters are adjusted, laser with a wavelength of 1064nm is adopted, the energy is adjusted to be 0.4J, the frequency is adjusted to be 5HZ, then laser beams are emitted from a light outlet 2, the emitted laser beams are parallel to an aperture 3, then the laser beams are reflected by a first reflecting mirror, a second reflecting mirror, a third reflecting mirror 14, a third reflecting mirror 8 and a third reflecting mirror 23 in sequence and reach a lens 27, and the laser beams are focused by the lens 27 and then enter a reaction kettle body 31.
The reaction temperature is set by the control panel 32, and the stirring speed is set at the same time, so that the precursor solution is rotated by the magnetons 33. A pressure gauge and burst valve 28 may be used to monitor the pressure during the reaction, but care should be taken to prevent it.
During the reaction, the laser irradiation is observed, if the irradiation position of the solution is required to be changed, the displacement platform 37 is controlled by computer software to be adjusted in the X, Y and Z directions until the proper irradiation height and position are found.
And respectively cleaning the precursor solution subjected to laser irradiation for 3 times by using ethanol and deionized water, pouring into a centrifugal tube, and putting into a centrifugal machine for centrifugal operation. And after the centrifugation is finished, pouring out the waste liquid, then washing, and drying in a forced air drying oven after the washing is finished to obtain the precursor. The precursor is put into a crucible, and another crucible filled with sublimed sulfur is put at the air inlet of the tube furnace. And calcining the precursor by a double-crucible method to finally obtain the superfine cathode ray fluorescent powder.
Claims (9)
1. The utility model provides an equipment of preparation superfine cathode ray phosphor powder, includes laser emitter, optical path system, light and heat reation kettle and displacement platform, its characterized in that:
the laser emitter is provided with a light outlet, and the optical path system comprises an aperture, a first reflector, a second reflector, a third reflector, a lens, a first telescopic rod and a second telescopic rod; the aperture, the first telescopic rod and the second telescopic rod are sequentially arranged in the light emitting direction of the light outlet; the first reflector and the second reflector are respectively arranged on the upper side and the lower side of the first telescopic rod; the third reflector and the lens are respectively arranged at the upper side and the lower side of the second telescopic rod; the bottom parts of the aperture, the lens and the third reflector are fixedly connected with a telescopic adjusting device; the first reflector, the second reflector and the third reflector are respectively provided with an angle adjuster, the angle adjusters are used for adjusting the deflection angles of the first reflector, the second reflector and the third reflector, and the telescopic length of the aperture, the lens and the third reflector is adjusted by a telescopic adjusting device, so that the laser emitted from the light outlet sequentially penetrates through the aperture, the first reflector, the second reflector, the third reflector and the lens and then is emitted into the photo-thermal reaction kettle; the photo-thermal reaction kettle is arranged on the displacement platform, and the position of the photo-thermal reaction kettle is adjusted by the displacement platform.
2. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1, wherein: the laser emitter is Nd: YAG solid laser can output laser with 1064, 532 and 355nm wavelength.
3. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1, wherein: the telescopic adjusting device comprises a fixed rod, a sleeve rod and a fastening screw; one end of the fixed rod is fixedly connected with the aperture, the lens or the reflector, and the other end of the fixed rod is arranged in the loop bar in a sliding manner; the sleeve rod is provided with a threaded hole, and the fastening screw is in threaded connection with the inside of the threaded hole.
4. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1, wherein: the adjusting range of the telescopic rod is 20-60cm, and the adjusting range of the telescopic adjusting device is 10-30 cm.
5. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1, wherein: a magneton is placed in the photo-thermal reaction kettle, and the solution is guaranteed to be in a rotating state all the time in the experimental process.
6. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1, wherein: the temperature adjustable range of the photo-thermal reaction kettle is 25-250 ℃, the rotating speed range is 0-1200 r/min, and the working pressure is 0-20 Mpa.
7. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1, wherein: the material loading coefficient of the photo-thermal reaction kettle body is two thirds of the total volume, and the photo-thermal reaction kettle is only suitable for loading liquid media.
8. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1, wherein: the displacement platform is respectively provided with a motor and a screw rod for driving, and a sliding rail and a sliding groove which are matched with each other for guiding in X, Y, Z three directions.
9. The apparatus for preparing an ultrafine cathode ray phosphor according to claim 1 or 8, wherein: the displacement platform is made of aluminum alloy, and the motion speed in the X, Y, Z three directions is 0-50 mm/s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110893574.6A CN113663624A (en) | 2021-08-04 | 2021-08-04 | Equipment for preparing superfine cathode ray fluorescent powder |
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| CN115368894A (en) * | 2022-08-18 | 2022-11-22 | 北京科技大学 | Method for preparing sulfur oxide fluorescent powder by laser |
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