CN1180912C - Gas-phase laser method and equipment for preparing silver nano-particles - Google Patents
Gas-phase laser method and equipment for preparing silver nano-particles Download PDFInfo
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- CN1180912C CN1180912C CNB001343483A CN00134348A CN1180912C CN 1180912 C CN1180912 C CN 1180912C CN B001343483 A CNB001343483 A CN B001343483A CN 00134348 A CN00134348 A CN 00134348A CN 1180912 C CN1180912 C CN 1180912C
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- 238000000034 method Methods 0.000 title claims abstract description 25
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 title description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 50
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 40
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000000889 atomisation Methods 0.000 claims abstract description 12
- 229910052709 silver Inorganic materials 0.000 claims abstract description 11
- 239000004332 silver Substances 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 63
- 238000006243 chemical reaction Methods 0.000 claims description 50
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 12
- 238000003860 storage Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000012495 reaction gas Substances 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 229910018503 SF6 Inorganic materials 0.000 claims 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 claims 1
- 229960000909 sulfur hexafluoride Drugs 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 16
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000010574 gas phase reaction Methods 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical group [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 150000003379 silver compounds Chemical class 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- BSWGGJHLVUUXTL-UHFFFAOYSA-N silver zinc Chemical compound [Zn].[Ag] BSWGGJHLVUUXTL-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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Abstract
The present invention discloses a method for preparing nanometer silver particles through a laser gas phase, and a device thereof. By changing a silver nitrate solution into a gas phase substance through ultrasonic atomization processing, by using SF6 as photoconductive gas, and by realizing preparing nanometer silver particles through a laser gas phase with the device disclosed by the present invention, the present invention can realize the continuous preparation of nanometer silver particles. The present invention has easy acquirement of raw materials, simple technology, high powder yield and practicability of industrialized production.
Description
Technical Field
The invention relates to a method and a device for preparing nano silver particles by adopting a laser-induced gas-phase pyrolysis method.
Background
The nanometer silver powder is used as a functional material in more applications in the electronic industry, and is mainly used for manufacturing silver-containing conductive paste, electrodes of certain electronic devices and high-grade alkaline zinc-silver storage batteries. In the rapid microelectronic industry at present, the market demand for high-purity nano silver powder is greatly increased; meanwhile, the nano silver particles are also excellent biological materials and environmental materials, have the characteristics of no toxicity to human bodies and high-efficiency sterilization, and can be used for manufacturing high-grade sanitary fabrics; the nano silver powder has application in catalysis and heat transfer.
Conventional methods for producing silver powder generally include: thermal decomposition of silver oxide, thermal decomposition of organic silver, reduction with a reducing agent, electrolytic cathode deposition, and the like. The granularity of the silver powder manufactured by the traditional method is basically more than 50 meshes.
In an improved chemical reduction method (such as the disclosed invention patent CN1227148A), a conventional dispersant is added into a silver nitrate solution, then ammonia water is added to form a silver-ammonia complex ion solution, a reducing agent is sprayed in through a special spray head, and meanwhile, high-speed stirring is adopted to match with PH value and temperature control, so that spherical ultrafine silver particles are prepared. Another invention patent (publication No. 1128188A) discloses a method for activating a silver nitrate solution with controlled concentration before chemical reduction reaction, and nano-silver particles with controllable particle size are obtained. The chemical method for preparing the nano silver powder has more complicated process procedures and longer period, and powder with uniform particle size is obtained in large-scale production, so that the process control difficulty is higher. Other physical methods such as vacuum evaporation, high-energy beam bombardment evaporation and the like are used for preparing the nano silver particles, and the yield of the silver powder is low.
The early 1980 s, the American college of labor science in Massachusetts, reported the work of laser gas-phase synthesis of nano-ceramic powder, and the main prepared nano-powder has Si3N4、SiC、Si、B4C and the like. The principle of laser gas phase synthesis of nano particles is as follows: the gas phase material is used as raw material, when the absorption line of the gasphase material is coincident with a certain laser wavelength, the gas molecules absorb photon energy due to resonance to open the chemical bonds of the gas molecules, and the gas molecules are recombined to form the solid phase material. Because the laser reaction area is very small, the solid-phase substance which just forms nucleus instantly departs from the high-temperature reaction area and enters the room temperature, and the rapid cooling rate reaches 10-6At a temperature of DEG C/sec, the particles cannot grow any longerLarge, and can only remain in a nanoscale state, thereby forming nanoparticles. According to the characteristics of the laser gas phase method, the raw material for carrying out laser gas phase synthesis should be gas phase substances (gas, steam and the like), and the raw material should have strong absorption to laser with a certain specific wavelength. Such as laser gas phase synthesis of nano Si3N4Powder of SiH4And NH3Gases as raw materials, they are for CO with wavelength of 10.6 mu2Laser absorption of SiH4It is strongly absorbed. The laser gas-phase synthesis of the iron-based nano-particles is Fe (CO)5As a source of iron. Because most of common silver compounds are solid and difficult to vaporize, no report on preparing nano silver particles by using laser gas phase exists.
Disclosure of Invention
The invention aims to provide a method and a device for preparing nano silver particles by laser gas phase, which have simple process, continuous production, high yield and uniform powder granularity.
The object of the invention is achieved by the following method and device.
The method for preparing the nano silver particles by laser gas phase comprises the following steps: preparing silver nitrate (AgNO) with a certain molar ratio3) 5-50% solution is put in a storage tank and atomized by an ultrasonic nozzleSilver nitrate solution and photosensitive gas SF6Mixing with carrier gas (selected from argon, nitrogen and clean air) to form reaction gas, entering a reaction chamber, wherein the molar ratio of silver nitrate to photosensitive gas is 20-30: 1, the molar ratio of photosensitive gas to carrier gas is 1: 30-80, the flow rate of the mixed gas is 200-300 cm/S, the mixed gas meets a continuous carbon dioxide laser beam in an orthogonal mode, the air pressure of the reaction chamber is lower than normal pressure and is dynamically maintained at a set value, and the set value is SF6Under the action of light energy absorption and transmission with gas as photosensitive gas, maintaining the reaction to be carried out, wherein the temperature in a reaction area exceeds the thermal decomposition temperature of silver nitrate, so that the silver nitrate is completely decomposed to form a silver particle core, nano silver particles are formed in the subsequent quenching process, laser gas phase pyrolysis reaction is carried out under the action of the photosensitive gas, the pressure is 40-80 Kpa, the reaction temperature reaches 450-600 ℃ of the thermal decomposition temperature of the silver nitrate, and the laser power is 1000-2000W/cm2The silver nitrate decomposes to produce silver nanoparticles and gases such as nitrogen, oxygen, and nitrogen oxides. The chemical reaction process is expressed as
*(N, O) ×: and pumping gases such as nitrogen, oxygen and nitrogen oxide by a suction pump, and conveying the generated silver particles with carrier gas to a powder collector for collection. The laser energy remaining from the reaction is absorbed by a water-cooled light absorber.
The preparation device for realizing the method comprises the following steps: the device comprises a storage tank, an ultrasonic atomizing nozzle, a gas mixing chamber, a reaction chamber, a gas pressure control unit, a powder collector and an air pump. The ultrasonic atomization feeding system (comprising a storage tank, an ultrasonic atomization nozzle and a gas mixing chamber) is connected with the reaction chamber through a pipeline, and the silver nitrate solution in the storage tank is atomized by the ultrasonic atomization nozzle and then mixed with the photosensitive gas and the carrier gas to form reaction gas. The nano particles produced by the gas-phase reaction of the gas-phase reaction substance meeting the laser beam in the reaction chamber are conveyed to the powder collector by the air pump to be collected, and the reaction chamber is connected with an air pressure control unit for controlling the reaction air pressure.
The invention has the advantages that:
1. the silver nitrate is converted into an atomized raw material capable of carrying out gas phase reaction by using the ultrasonic atomization device, and the silver nitrate solution can be continuously added into the ultrasonic atomization device, so that the continuous preparation of nano silver particles can be realized, and the method has the feasibility of industrial production;
2. the preparation process of the powder is simplified, and the nano silver particles are obtained by a one-step method;
3. because the time-temperature process of the reaction of the gas phase raw materials through the laser beam is basically consistent under a certain flow velocity, the prepared nano silver particles have uniform particle size.
4. The silver nitrate as silver-containing raw material is a widely used chemical raw material and is easy to obtain.
5. The high yield of the nano silver particles is up to 250-340 g/h.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing nano silver particles by laser gas phase;
FIG. 2 shows the X-ray results of the silver nanoparticles of example 1;
FIG. 3 is a TEM result of nano-silver particles of example 1;
FIG. 4 shows the X-ray results of the silver nanoparticles of example 2;
FIG. 5 shows TEM results of silver nanoparticles of example 2.
Detailed Description
Embodiments of the invention are described below with reference to the drawings. The air suction pump 12 is operated and the air pressure control unit 13 dynamically maintains the air pressure in the reaction chamber 7 at the predetermined value again by feedback-controlling the air discharge regulating valve 11. The reaction raw material silver nitrate solution is filled into an ultrasonic atomization storage tank 1, and silver nitrate vapor is formed in a gas mixing chamber 4 through an ultrasonic atomization nozzle 3 under the control of a liquid flowmeter 2. The photosensitive gas and the carrier gas (argon, nitrogen and clean air) enter the gas mixing chamber 4 under the control of the gas flowmeter 5, and carry silver nitrate vapor to enter the reaction chamber 7 through the reaction nozzle 6. A gas mixing chamber 4 connected with a gas inlet nozzle 6 of a reaction chamber 7An ultrasonic atomizing nozzle 3 is fixed, the ultrasonic atomizing nozzle 3 is connected to a material storage tank 1 through a liquid flowmeter 2, two paths of air inlets on a gas mixing chamber are connected with aphotosensitive air source and a carrier gas source through a pipeline and a gas flowmeter 5, an air inlet nozzle 6 and a powder conveying pipe 9 of reaction gas are fixed at positions corresponding to the upper part and the lower part of a reaction chamber 7, a focusing mirror 8 and a light absorber 14 are fixed at positions corresponding to the horizontal part of the reaction chamber 7, and the reaction chamber 7 is connected with a powder collector 10 through the powder conveying pipe 9. The gas pressure in the reaction chamber 7 is measured in real time, and the opening of the exhaust control valve 11 is feedback-controlled to limit the amount of exhaust gas from the air pump 12 and keep the gas pressure in the reaction chamber 7 constant. The concentration of silver nitrate vapor and photosensitive gas can be controlled by the control of a flow meter. CO with power of 300-400W2The laser beam enters the reaction chamber through the focusing mirror 8, the reaction gas orthogonally enters the laser beam at the focus of the laser beam, the reaction gas absorbs the light energy and is rapidly heated to form a reaction zone due to the energy transfer effect of the photosensitive gas, the temperature of the reaction zone exceeds the pyrolysis temperature of the silver nitrate and reaches 450-600 ℃, and the silver nitrateDecomposing to generate nano silver particles. The nano silver particles are pumped by an air pump 12 through a powder conveying pipe 9 and conveyed into a collector 10 to be collected. The remaining laser energy is absorbed by a water-cooled light absorber 14.
Example 1:
first, the suction pump was started and the dynamic equilibrium pressure in the reaction chamber was adjusted to 80 Kpa. Charging a certain amount of 30% silver nitrate solution (which can be continuously added with consumption) into a storage tank, performing ultrasonic atomization at a liquid flow rate of 13.5 ml/min, and performing ultrasonic atomization with SF6The photosensitive gas and the nitrogen gas are used as carrier gases, and the flow rates are respectively 20ml per minute and 800ml per minute. CO at power of 300W2The power density of the focused laser beam is 1500W/m2And the light beam meets the reaction airflow to form a reaction zone, the temperature of the reaction zone is 450-500 ℃, and the generated nano silver particles are collected in a powder collector along with the carrier airflow. The nano silver particles are white spherical powder with the average particle size of 15nm, and the yield of the powder is 250 g/h. The X-ray result of the nano silver particles is shown in figure 2, and the TEM result is shown in figure 3.
Example 2:
a certain amount of silver nitrate solution with the concentration of 40 percent is filled in the storage tank. The dynamic equilibrium pressure of the reaction chamber was adjusted to 40Kpa and ultrasonic atomization was performed at a liquid flow rate of 13.5ml per minute. With SF6The photosensitive gas and the nitrogen gas are used as carrier gases, and the flow rates are respectively 20ml per minute and 1200ml per minute. CO of 400W power2The power density of the focused laser beam is 2000W/m2The light beam meets the reaction gas flow to form a reaction zone, and the temperature of the reaction zone is 550-600 ℃. The yield of the produced white spherical nano silver particles with the average particle diameter of 15nm was 340 g/h. The detection result of the nano silver particles is basically consistent with that of the embodiment 1, the X-ray result is shown in figure 4, and the TEM result is shown in figure 5.
Claims (4)
1. A method for preparing nano silver particles by laser gas phase is characterized in that:carrying out ultrasonic atomization treatment on silver nitrate solution, mixing the silver nitrate solution with photosensitive gas and carrier gas to form reaction gas, enabling the reaction gas to enter a reaction chamber to orthogonally meet a laser beam, enabling the air pressure of the reaction chamber to be lower than normal pressure, dynamically maintaining the pressure at a set value, and carrying out SF (sulfur hexafluoride) treatment6Under the action of light energy absorption and transmission of photosensitive gas, the reaction is maintained to be carried out, the temperature of a reaction zone exceeds the thermal decomposition temperature of silver nitrate, so that the silver nitrate is completely decomposed to form a silver particle core, and nano silver particles are formed in the subsequent quenching process and pumped into a powder collector to be collected.
2. The method for preparing nano silver particles by laser gas phase according to claim 1, wherein: the carrier gas is selected from any one of argon, nitrogen and clean air.
3. The method for preparing nano silver particles by laser gas phase according to claim 1, wherein: the pressure of the reaction chamber is 40-80 Kpa, and the temperature of the reaction zone is 450-600 ℃.
4. A device for preparing nano silver particles by laser gas phase is characterized by comprising a storage tank (1), an ultrasonic atomizing nozzle (3), a gas mixing chamber (4), a reaction chamber (7), a gas pressure control unit (13), a powder collector (10) and an air extracting pump (12), wherein the ultrasonic atomizing nozzle (3) is fixed on the gas mixing chamber (4) connected with a gas inlet nozzle (6) of the reaction chamber (7), the ultrasonic atomizing nozzle (3) is connected to the storage tank (1) through a liquid flowmeter (2), two gas inlets on the gas mixing chamber are connected with a photosensitive gas source and a carrier gas source through a pipeline and a gas flowmeter (5), a silver nitrate solution in the storage tank is atomized by the ultrasonic atomizing nozzle (3) and then mixed with the photosensitive gas and the carrier gas to form reaction gas, the gas inlet nozzle (6) and a powder conveying pipe (9) of the reaction gas are fixed at positions corresponding to the upper part and the lower part of the reaction chamber (7), the focusing mirror (8) and the light absorber (14) are fixed on the position corresponding to the horizontal position of the reaction chamber (7), the reaction chamber (7) is connected with the powder collector (10) through the powder conveying pipe (9), and the reaction chamber (7) is connected with the air pressure control unit (13) used for controlling the reaction air pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB001343483A CN1180912C (en) | 2000-12-22 | 2000-12-22 | Gas-phase laser method and equipment for preparing silver nano-particles |
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| CNB001343483A CN1180912C (en) | 2000-12-22 | 2000-12-22 | Gas-phase laser method and equipment for preparing silver nano-particles |
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| CN1359775A CN1359775A (en) | 2002-07-24 |
| CN1180912C true CN1180912C (en) | 2004-12-22 |
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| JP4293586B2 (en) * | 2002-08-30 | 2009-07-08 | 浜松ホトニクス株式会社 | Nanoparticle production method and production apparatus |
| US8895962B2 (en) * | 2010-06-29 | 2014-11-25 | Nanogram Corporation | Silicon/germanium nanoparticle inks, laser pyrolysis reactors for the synthesis of nanoparticles and associated methods |
| CN104174858A (en) * | 2013-05-27 | 2014-12-03 | 刘建 | Preparation method of silver powder or doped silver powder |
| CN105218689A (en) * | 2015-11-06 | 2016-01-06 | 河南工业大学 | A kind of laser treatment prepares the device of modified starch |
| CN115955893B (en) * | 2023-03-15 | 2023-05-30 | 南京迪视泰光电科技有限公司 | Preparation method of OLED device containing Ag electrode |
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