CN104328367A - Method for preparing ribbon amorphous alloy under mild condition - Google Patents
Method for preparing ribbon amorphous alloy under mild condition Download PDFInfo
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- CN104328367A CN104328367A CN201410564957.9A CN201410564957A CN104328367A CN 104328367 A CN104328367 A CN 104328367A CN 201410564957 A CN201410564957 A CN 201410564957A CN 104328367 A CN104328367 A CN 104328367A
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- amorphous alloy
- amorphous metal
- crystaline amorphous
- pet
- film
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- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title abstract description 12
- 229920000728 polyester Polymers 0.000 claims abstract description 23
- 229920002799 BoPET Polymers 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 239000005300 metallic glass Substances 0.000 claims description 37
- 238000002156 mixing Methods 0.000 claims description 20
- 229910020598 Co Fe Inorganic materials 0.000 claims description 10
- 229910002519 Co-Fe Inorganic materials 0.000 claims description 10
- 101150003085 Pdcl gene Proteins 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 241000080590 Niso Species 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 4
- 239000002585 base Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract 4
- 238000000576 coating method Methods 0.000 abstract 4
- 239000007788 liquid Substances 0.000 abstract 4
- 229910002666 PdCl2 Inorganic materials 0.000 abstract 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 abstract 1
- RITIIWBOOBSEFQ-UHFFFAOYSA-N [P].[Co].[Ni].[Fe] Chemical compound [P].[Co].[Ni].[Fe] RITIIWBOOBSEFQ-UHFFFAOYSA-N 0.000 abstract 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 abstract 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 abstract 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 abstract 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 abstract 1
- 238000007747 plating Methods 0.000 abstract 1
- 239000001509 sodium citrate Substances 0.000 abstract 1
- 235000011150 stannous chloride Nutrition 0.000 abstract 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 abstract 1
- 235000019263 trisodium citrate Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 35
- 238000004458 analytical method Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910001020 Au alloy Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a method for preparing a ribbon amorphous alloy under a mild condition. A ribbon polyester (PET) film is used as a base material, and a nickel-cobalt-iron-phosphorus amorphous alloy coating is plated on the surface of the PET film; the method comprises the steps of coating and plating the amorphous alloy and removing the film; particularly, the method comprises the steps of soaking the PET film with alkali weigh reduction on one side in SnCl2 and PdCl2 liquids with set concentrations sequentially for a certain time, then soaking in a mixed liquid of Na3C6H5O7, H3BO3, Na2H2PO2, NiSO4, CoSO4, and FeSO4, wherein the mixed liquid with certain concentration and certain pH value is at certain temperature, coating the amorphous alloy coating on the PET film, and carrying out accelerant-containing alkaline liquid treatment, superheated steam treatment and 350-450 DEG C heat treatment to obtain the ribbon amorphous alloy. The process is simple and effective, the preparation condition is mild, and the ribbon amorphous alloy can be effectively prepared.
Description
Technical field
The present invention relates to the preparation method of non-crystaline amorphous metal, particularly relate to a kind of method preparing banded non-crystaline amorphous metal in a mild condition.
Background technology
Non-crystaline amorphous metal refers to using metallic bond as its constitutional features, is topological disorder shape in three-dimensional atomic arrangement, does not have the crystal grain of crystal alloy, crystal boundary.Compared with the crystal alloy of routine, non-crystaline amorphous metal has excellent mechanical property (high strength, high rigidity etc.), magnetic, solidity to corrosion, wear resistance, high resistivity and the advantage such as electromechanical coupling performance and hydrogen storage property, machinery, communication, electric power, aerospace, automotive industry and even national defense and military all have a wide range of applications potentiality.What the preparation of non-crystaline amorphous metal adopted usually is super quench solidification, and namely usually require high temperature and high speed of cooling, the setting time of alloy is extremely short, is difficult to control.Harsh owing to preparing required condition, need to cool rapidly with the speed of 1,000,000 degree per second, make production cost higher, and due to the impact by cooling rate, be difficult to produce the amorphous alloy strips of thickness more than 50 microns, affect large-scale commercial applications.Therefore, utilize the method for simple possible to produce thickness in a mild condition and the method for amorphous alloy strips more than 50 microns can have great realistic meaning.
Summary of the invention
The object of the invention is for condition required in conventional non-crystaline amorphous metal preparation process harsh, and be difficult to prepare thickness amorphous alloy strips problem more than 50 microns, provide a kind of method preparing banded non-crystaline amorphous metal in a mild condition.
The object of the invention is to be achieved through the following technical solutions, a kind of method preparing banded non-crystaline amorphous metal in a mild condition, comprises the following steps:
(1) by one side alkali mass loss rate be banded polyester (PET) film of 5%-15%, successively at the SnCl of 10-15g/L
2the PdCl of 5-10 min, 0.15-0.30g/L is soaked in solution (room temperature)
2solution (room temperature) middle immersion 5-10 min, temperature are 50-60 DEG C, pH value is soak 2.5-3.5 hour in the Ni-Co-Fe mixing solutions of 8.0-8.5, then use the heat water-spraying 5-10 min of 60 DEG C, at 80 DEG C, after dry 30-60 min, obtain band shape (PET) film being coated with non-crystaline amorphous metal; Described SnCl
2solution and PdCl
2the solvent of solution is deionized water; The each component of described Ni-Co-Fe mixing solutions is as follows: 50-70g/L Na
3c
6h
5o
7, 0.5 mol/L H
3bO
3, 20-30g/L Na
2h
2pO
2, 0.04 mol/L NiSO
4, 0.015 mol/L CoSO
4, 0.01-0.02 mol/L FeSO
4, solvent is deionized water;
(2) PET film being coated with non-crystaline amorphous metal is soaked 20-30 min in NaOH and TF1181 mixed aqueous solution, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 5-10g/L, TF1181 is 0.5-1.0 g/L; Then 5 min are sprayed by the hot steam of 120 DEG C, after washing, thermal treatment 5min under the condition of 350-450 DEG C, obtained banded non-crystaline amorphous metal.
The invention has the beneficial effects as follows, banded non-crystaline amorphous metal method prepared by the present invention is simple, processing condition are gentle, and the banded non-crystaline amorphous metal thickness obtained can more than 50 microns, and can regulate and control the thickness of banded amorphous alloy layer by the concentration of each solution and soak time in the solution; And can according to the ratio of mixing solutions, the atomic ratio in regulation and control non-crystaline amorphous metal;
PET is adopted to be base film material in the present invention, after being partly dissolved in containing the NaOH solution of base reduction promoter, under the effect of superheated vapour, pierceability can be formed dissolve, avoid PET makes top layer banded non-crystaline amorphous metal fracture because of high-temperature shrinkage, and thermal treatment certain hour can remove film completely at 350-450 DEG C, obtain the non-au-alloy of pure band shape.
Accompanying drawing explanation
Fig. 1 is the non-crystaline amorphous metal schematic diagram that the present invention obtains on PET film surface;
Fig. 2 is ultimate analysis (EDS) spectrogram of the non-crystaline amorphous metal that embodiment 1 obtains;
Fig. 3 is the X-ray diffractogram of the non-crystaline amorphous metal that embodiment 1 obtains;
Fig. 4 is ultimate analysis (EDS) spectrogram of the non-crystaline amorphous metal that embodiment 2 obtains;
Fig. 5 is the X-ray diffractogram of the non-crystaline amorphous metal that embodiment 2 obtains.
Embodiment
Prepare a method for banded non-crystaline amorphous metal in a mild condition, comprise the following steps:
(1) by one side alkali mass loss rate be banded polyester (PET) film of 5%-15%, successively at the SnCl of 10-15g/L
2the PdCl of 5-10 min, 0.15-0.30g/L is soaked in solution (room temperature, 25 DEG C)
2solution (room temperature, 25 DEG C) in soak 5-10 min, temperature is 50-60 DEG C, pH value is soak 2.5-3.5 hour in the Ni-Co-Fe mixing solutions of 8.0-8.5, then use the heat water-spraying 5-10 min of 60 DEG C, at 80 DEG C, after dry 30-60 min, obtain band shape (PET) film being coated with non-crystaline amorphous metal; Described SnCl
2solution and PdCl
2the solvent of solution is deionized water; The each component of described Ni-Co-Fe mixing solutions is as follows: 50-70g/L Na
3c
6h
5o
7, 0.5 mol/L H
3bO
3, 20-30g/L Na
2h
2pO
2, 0.04 mol/L NiSO
4, 0.015 mol/L CoSO
4, 0.01-0.02 mol/L FeSO
4, solvent is deionized water; This step completes in a mild condition, regulates and controls the thickness of banded amorphous alloy layer by the concentration of each solution and soak time in the solution, and can according to the ratio of mixing solutions, the atomic ratio in regulation and control non-crystaline amorphous metal.
(2) PET film being coated with non-crystaline amorphous metal is soaked 20-30 min in NaOH and TF1181 mixed aqueous solution, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 5-10g/L, TF1181 is 0.5-1.0 g/L; Then spray 5 min by the hot steam of 120 DEG C, PET pierceability is partly dissolved, after washing, at the thermal treatment 5-20 min of 350-450 DEG C, after removing PET film completely, obtained banded non-crystaline amorphous metal.PET is adopted to be base film material in the present invention, after being partly dissolved in containing the NaOH solution of base reduction promoter, under the effect of superheated vapour, pierceability can be formed dissolve, avoid PET makes top layer banded non-crystaline amorphous metal fracture because of high-temperature shrinkage, and thermal treatment certain hour can remove film completely at 350-450 DEG C, obtain the non-au-alloy of pure band shape.
Below in conjunction with embodiment, the invention will be further described.
embodiment 1:
(1) by one side alkali mass loss rate be 5% banded polyester (PET) film, successively at the SnCl of 10g/L
2the PdCl of 10 min, 0.30g/L is soaked in solution (room temperature, 25 DEG C)
2solution (room temperature, 25 DEG C) middle immersion 5 min, temperature is 50 DEG C, pH value is soak 2.5 hours in the Ni-Co-Fe mixing solutions of 8.5, then uses heat water-spraying 5 min of 60 DEG C, obtains band shape (PET) film being coated with non-crystaline amorphous metal at 80 DEG C after dry 30 min; The each component of described Ni-Co-Fe mixing solutions is as follows: 50g/L Na
3c
6h
5o
7, 0.5 mol/L H
3bO
3, 20g/L Na
2h
2pO
2, 0.04 mol/L NiSO
4, 0.015 mol/L CoSO
4, 0.01 mol/L FeSO
4, solvent is deionized water.
(2) PET film being coated with non-crystaline amorphous metal is soaked 20 min in NaOH and TF1181 mixing solutions, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 10g/L, TF1181 is 0.5 g/L; Then spray 5 min by the hot steam of 120 DEG C, PET pierceability is partly dissolved, after washing, enter the tube furnace process 20min of 350 DEG C, after removing PET film completely, obtained thickness is the banded non-crystaline amorphous metal of 50 microns.
The ultimate analysis of products therefrom is as shown in Figure 2, as can be seen from the figure, main containing metallic elements such as Fe, Co, Ni in the product prepared under this condition, and proportionlity is: Fe:Co:Ni=2.02:6.71:69.53.
As shown in Figure 3, as seen from Figure 3, product does not produce diffraction peak to the XRD of products therefrom, illustrates that this product is amorphous.
embodiment 2:
(1) by one side alkali mass loss rate be 15% banded polyester (PET) film, successively at the SnCl of 15g/L
2the PdCl of 5min, 0.15g/L is soaked in solution (room temperature, 25 DEG C)
2solution (room temperature, 25 DEG C) in soak that 10min, temperature are 60 DEG C, pH value is soak 3.5 hours in the Ni-Co-Fe mixing solutions of 8.0, then use the heat water-spraying 10min of 60 DEG C, at 80 DEG C, after dry 60min, obtain band shape (PET) film being coated with non-crystaline amorphous metal; The each component of described Ni-Co-Fe mixing solutions is as follows: 70g/L Na
3c
6h
5o
7, 0.5 mol/L H
3bO
3, 30g/L Na
2h
2pO
2, 0.04 mol/L NiSO
4, 0.015 mol/L CoSO
4, 0.02 mol/L FeSO
4, solvent is deionized water.
(2) PET film being coated with non-crystaline amorphous metal is soaked 30min in NaOH and TF1181 mixing solutions, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 5g/L, TF1181 is 1.0 g/L; Then with the hot steam spray 5min of 120 DEG C, PET pierceability is partly dissolved, after washing, enters the tube furnace process 5min of 450 DEG C, after removing PET film completely, obtained thickness is the banded non-crystaline amorphous metal of 85 microns.
The ultimate analysis of products therefrom is as shown in Figure 4, as can be seen from the figure, main containing metallic elements such as Fe, Co, Ni in the product prepared under this condition, and proportionlity is: 2.34:6.77:71.51.
The XRD of products therefrom as shown in Figure 5, as seen from Figure 5, the XRD diffracting spectrum of product and the diffracting spectrum of embodiment 1 products therefrom basically identical, all do not produce diffraction peak, illustrate that this product is amorphous.
Above-described embodiment is used for explaining and the present invention is described, instead of limitation of the present invention, in the protection domain of spirit of the present invention and claim, to any amendment of the present invention and change, all falls into protection scope of the present invention.
Claims (1)
1. prepare a method for banded non-crystaline amorphous metal in a mild condition, it is characterized in that, it comprises the following steps:
(1) by one side alkali mass loss rate be banded polyester (PET) film of 5%-15%, successively at the SnCl of 10-15g/L
2the PdCl of solution soaking 5-10 min, 0.15-0.30g/L
2solution soaking 5-10 min, 2.5-3.5 hour is soaked in the Ni-Co-Fe mixing solutions that temperature is 50-60 DEG C, pH value is 8.0-8.5, then use the heat water-spraying 5-10 min of 60 DEG C, at 80 DEG C, obtain the banded PET film being coated with non-crystaline amorphous metal after dry 30-60 min; The each component of described Ni-Co-Fe mixing solutions is as follows: 50-70g/L Na
3c
6h
5o
7, 0.5 mol/L H
3bO
3, 20-30g/L Na
2h
2pO
2, 0.04 mol/L NiSO
4, 0.015 mol/L CoSO
4, 0.01-0.02 mol/L FeSO
4, solvent is deionized water;
(2) PET film being coated with non-crystaline amorphous metal that step (1) obtains is soaked 20-30 min in NaOH and TF1181 mixing solutions, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, the concentration of NaOH solution is the concentration of 5-10g/L, TF1181 is 0.5-1.0 g/L; Then spray 5 min by the hot steam of 120 DEG C, after washing, under the condition of 350-450 DEG C, process 5-20 min, obtained banded non-crystaline amorphous metal.
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CN201410564957.9A CN104328367B (en) | 2014-10-22 | 2014-10-22 | A kind of method of preparing banded non-crystaline amorphous metal under temperate condition |
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CN201410564957.9A CN104328367B (en) | 2014-10-22 | 2014-10-22 | A kind of method of preparing banded non-crystaline amorphous metal under temperate condition |
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CN104328367A true CN104328367A (en) | 2015-02-04 |
CN104328367B CN104328367B (en) | 2016-05-18 |
Family
ID=52403172
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112250227A (en) * | 2020-09-11 | 2021-01-22 | 杭州娃哈哈科技有限公司 | Zero-emission alkaline electrolyzed water production device |
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US4368221A (en) * | 1980-07-04 | 1983-01-11 | Bacs Megyei Allami Epitoipari Vallalat | Process for coating fibrous glass with amorphous nickel phosphorous glass metal |
CN1710137A (en) * | 2005-06-23 | 2005-12-21 | 复旦大学 | Amorphous nickel-boron nuclear-shell, ghost structural material and its preparing material |
CN1737183A (en) * | 2005-07-28 | 2006-02-22 | 复旦大学 | Process for preparing noncrystalline nickel-phosphor-core - shell, hollow shell structure material |
CN1843997A (en) * | 2005-04-08 | 2006-10-11 | 富士电机电子设备技术株式会社 | Method of plating on a glass base plate, a disk substrate, method for manufacturing the same and a perpendicular magnetic recording medium |
RU2501888C1 (en) * | 2012-07-20 | 2013-12-20 | Федеральное государственное бюджетное учреждение науки институт физики им. Л.В. Киренского Сибирского отделения Российской академии наук | METHOD OF PRODUCING AMORPHOUS MAGNETIC Co-P FILMS |
CN103632794A (en) * | 2012-08-28 | 2014-03-12 | 有研稀土新材料股份有限公司 | Composite soft magnetic material and method for preparing material |
-
2014
- 2014-10-22 CN CN201410564957.9A patent/CN104328367B/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4368221A (en) * | 1980-07-04 | 1983-01-11 | Bacs Megyei Allami Epitoipari Vallalat | Process for coating fibrous glass with amorphous nickel phosphorous glass metal |
CN1843997A (en) * | 2005-04-08 | 2006-10-11 | 富士电机电子设备技术株式会社 | Method of plating on a glass base plate, a disk substrate, method for manufacturing the same and a perpendicular magnetic recording medium |
CN1710137A (en) * | 2005-06-23 | 2005-12-21 | 复旦大学 | Amorphous nickel-boron nuclear-shell, ghost structural material and its preparing material |
CN1737183A (en) * | 2005-07-28 | 2006-02-22 | 复旦大学 | Process for preparing noncrystalline nickel-phosphor-core - shell, hollow shell structure material |
RU2501888C1 (en) * | 2012-07-20 | 2013-12-20 | Федеральное государственное бюджетное учреждение науки институт физики им. Л.В. Киренского Сибирского отделения Российской академии наук | METHOD OF PRODUCING AMORPHOUS MAGNETIC Co-P FILMS |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112250227A (en) * | 2020-09-11 | 2021-01-22 | 杭州娃哈哈科技有限公司 | Zero-emission alkaline electrolyzed water production device |
CN112250227B (en) * | 2020-09-11 | 2022-05-27 | 杭州娃哈哈科技有限公司 | Zero-emission alkaline electrolyzed water production device |
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