CN102502820B - One-dimensional Sb203 micro-nanometer powder and composite-morphological Sb203 micro-nanometer powder prepared in one-step method - Google Patents
One-dimensional Sb203 micro-nanometer powder and composite-morphological Sb203 micro-nanometer powder prepared in one-step method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 title abstract 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 17
- 239000002159 nanocrystal Substances 0.000 claims description 16
- 239000011858 nanopowder Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000012670 alkaline solution Substances 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 11
- 239000008187 granular material Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000006460 hydrolysis reaction Methods 0.000 description 7
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000000643 oven drying Methods 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
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- 235000013339 cereals Nutrition 0.000 description 3
- 239000002127 nanobelt Substances 0.000 description 3
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical group Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
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- 238000003763 carbonization Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of preparation of micro-nanometer materials, and particularly relates to a one-step method for preparing one-dimensional Sb203 micro-nanometer powder and composite-morphological Sb203 micro-nanometer powder. Liquor with SbCl3 soluble in ethanol is added into alkali liquor to realize reaction, and one-dimensional Sb203 micro-nanometer powder and composite-morphological Sb203 micro-nanometer powder are obtained by means of filtering and drying. The method is simple, time-saving and labor-saving, is low in cost and environmental pollution, and saves energy, optional additives are omitted in a preparation procedure, and the one-step method has high industrial application potential.
Description
Technical field
The invention belongs to technical field of micro nano material preparation, particularly a kind of single stage method prepares one dimension and compound pattern Sb thereof
2o
3the method of micro-nano powder.
Background technology
Because one dimension and composite structure micro Nano material thereof have the character such as some unique mechanics, optics, electromagnetism, thereby become the focus that material supply section educational circles pays close attention to.The method for preparing at present one dimension and composite structure micro-nano powder thereof mainly comprises vapour deposition process, water/solvent-thermal method, template and ultrasonic method etc.But aforesaid method preparation technology comparatively complexity, long reaction time, energy dissipation is serious and need add a large amount of additives, and contaminate environment, seriously restricted the micro Nano material applied research.So far, liquid phase method especially prepares one dimension and composite structure micro-nano granules thereof and is acknowledged as the simplest, feasible and the preparation method of prospects for commercial application arranged in water in research.But the polarity of water is large, nucleation, the fast growth that hydrolysis reaction generates oxide compound or oxyhydroxide occurs in metal ion therein, have large quantity of moisture on the nano grain surface prepared, these water moleculess can combine by the hydroxide radical on hydrogen bond and nano grain surface.When grain spacing from close to the time, lip-deep water molecules can be used as " bridge " molecule, very easily causes that in drying process between particle, hard aggregation grows up to macrobead, thereby makes quantum effect, the surface effects of nano particle, tunnel drills effect etc. and can't bring into play.
Summary of the invention
The object of the present invention is to provide a kind of single stage method to prepare one dimension and compound pattern Sb thereof
2o
3the method of micro-nano powder, overcome the easy hard aggregation of product that existing method prepares, thereby affect quantum effect, the surface effects of nano particle, and tunnel drills the defect that effect etc. can't be brought into play.
The technical solution used in the present invention is as follows:
Single stage method prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, by SbCl under normal temperature
3ethanolic soln joins in alkaline solution and reacts, and filtration, drying obtain one dimension and compound pattern Sb thereof
2o
3micro-nano powder.
SbCl
3the concentration of ethanolic soln is 0.01-4.0 mol/L.
In described alkaline solution, the mass concentration of alkali is 0.02-30.0%.
The aqueous solution that described alkaline solution is sodium hydroxide, ammoniacal liquor, quadrol, diethanolamine.
SbCl
3the volume ratio of ethanolic soln and alkaline solution is that 1:1 is to 1:20.
SbCl
3ethanolic soln dropwise adds or disposable pouring in alkaline solution.
Temperature of reaction is 5-85 ℃, and the time is 0.1-0.5 h, in the time of reaction, is stirred.
Stir as electric stirring or magnetic agitation.
Concrete, temperature of reaction is 50-60 ℃, in the ammonia soln that is 0.02-5% in mass concentration, obtains banded Sb
2o
3micro-nano crystal grain; Temperature of reaction is 40-70 ℃, in the aqueous sodium hydroxide solution that is 0.02-1% in mass concentration, obtains nearly flower-shaped Sb
2o
3micro-nano crystal grain; Temperature of reaction is 20-50 ℃, in the ammonia soln that is 0.02-10% in mass concentration, obtains being with pencil Sb
2o
3micro-nano crystal grain; Temperature of reaction is 50-85 ℃, in the ammonia soln that is 5-12% in mass concentration, obtains bowknot shape Sb
2o
3micro-nano crystal grain; Temperature of reaction is 10-20 ℃, in the ammonia soln that is 12-25% in mass concentration, obtains flower-shaped Sb
2o
3micro-nano crystal grain; Temperature of reaction is 40-80 ℃, in the diethanolamine aqueous solution that is 1-5% in mass concentration, obtains stratiform Sb
2o
3micro-nano crystal grain; Temperature of reaction is 30-70 ℃, in the ethylenediamine solution that is 2-5% in mass concentration, obtains stratiform Sb
2o
3micro-nano crystal grain.
The object of the invention is to make reactant SbCl by controlling different reaction conditionss
3one step generates the Sb of different-shape
2o
3micro-nano granules, and the particle generated is difficult for reuniting.At first use anhydrous alcohol solution SbCl under normal temperature condition
3, make inorganic metal salt SbCl
3generate therein alcohol solvent compound, SbCl like this can slow down
3hydrolysis generates oxidiferous nucleation and the speed of growth, according to incomplete oriented adsorption and Ostwarld slaking mechanism, is grown; In addition, a small amount of ethanol molecule existed in system can be adsorbed onto particle surface, reaches sterically hindered effect, has reduced between particle and has taken by water molecules the phenomenon that " bridge " grows up.By adjusting different reaction parameters, control the product pattern, prepare the Sb of one dimension and composite structure pattern thereof
2o
3micro-nano powder, as different-shapes such as banded, band pencil, bowknot shape, flower-shaped and stratiforms.The micro-nano granules prepared not only has comparatively regular pattern, and granule surface area is large, and what have also has a larger length-to-diameter ratio, and output is large, in fields such as fire-retardant, catalysis, electrochemistry, will have good application prospect.This method has that preparation is simple, cost is low, time saving and energy saving, save energy, environmental pollution are little, and the additive that does not add any control pattern in preparation process as tensio-active agent etc., is applicable to the requirements of the times of current low carbonization, has industrial applications potential.Present method also is expected to for the preparation of the micro Nano material of other kind and industrialization research.
The present invention, with respect to prior art, has following advantage:
Product particle that the present invention prepares is better dispersed, is not easy to occur hard aggregation, and method is simple, cost is low, time saving and energy saving, save energy, environmental pollution are little, does not add any additive in preparation process, has industrial applications potential.
The accompanying drawing explanation
The Sb that Fig. 1 is banded pattern
2o
3the SEM figure of micro-nano granules;
Fig. 2 is the Sb with the pencil pattern
2o
3the SEM figure of micro-nano granules;
The Sb that Fig. 3 is the bowknot shape pattern
2o
3the SEM figure of micro-nano granules;
The Sb that Fig. 4 is floriform appearance
2o
3the SEM figure of micro-nano granules;
The Sb that Fig. 5 is the stratiform pattern
2o
3the SEM figure of micron particle;
The Sb that Fig. 6 is banded pattern
2o
3the XRD figure of micro-nano granules.
Embodiment
Below with specific embodiment, technical scheme of the present invention is described, but protection scope of the present invention is not limited to this:
Embodiment 1
In the time of 60 ℃, the SbCl of 5 mL 0.5 mol/L
3ethanolic soln is added drop-wise in the ammonia soln of 45 mL 3% (wt %), and magnetic agitation is reacted 0.2 h, the Sb then hydrolysis generated
2o
3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2o
3powdered sample.
By the Sb prepared on a small quantity
2o
3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 1.Particle as we can see from the figure is banded pattern, and length reaches 10-20 μ m, and the thickness of single nano belt is in the 100nm left and right.
Embodiment 2
In the time of 40 ℃, the SbCl of 20 mL 0.1 mol/L
3ethanolic soln splashes in the ammonia soln of 50 mL 5% (wt %), and magnetic agitation is reacted 0.5 h, the Sb then hydrolysis generated
2o
3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2o
3powdered sample.
By the Sb prepared on a small quantity
2o
3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 2.Particle as we can see from the figure is band pencil pattern, and length is in 20 μ m left and right, and the thickness of single nano belt is in 100 nm left and right, and the length of band bundle one side can reach 10 μ m.
Embodiment 3
In the time of 60 ℃, the SbCl of 5 mL 0.5 mol/L
3ethanolic soln is poured in the ammonia soln of 45 mL 6% (wt %), and electric stirring reacts 0.1 h, the Sb then hydrolysis generated
2o
3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2o
3powdered sample.
By the Sb prepared on a small quantity
2o
3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 3.Particle as we can see from the figure is the bowknot shape pattern, and length is in 20 μ m left and right, and the thickness of the nano belt of composition bow-knot-double is in 100 nm left and right, and the length of bow-knot-double one side can reach 10 μ m.
Embodiment 4
In the time of 10 ℃, the SbCl of 5 mL 1.5 mol/L
3ethanolic soln is added drop-wise in the ammonia soln of 45 mL 14% (wt %), and magnetic agitation is reacted 0.5 h, the Sb then hydrolysis generated
2o
3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2o
3powdered sample.
By the Sb prepared on a small quantity
2o
3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 4.The absolutely large number of particle as we can see from the figure is floriform appearance, and the diameter of flower is about 5 μ m left and right, and the micro-nano popped rice is by from center, longer length is 2-3 μ m one by one, and thickness forms at the sheet of 100 nm left and right.
Embodiment 5
In the time of 60 ℃, the SbCl of 5 mL 0.5 mol/L
3ethanolic soln is added drop-wise in the ethylenediamine solution of 45 mL 2% (wt %), and electric stirring reacts 0.5 h, the Sb then hydrolysis generated
2o
3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2o
3powdered sample.
By the Sb prepared on a small quantity
2o
3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 5.Particle as we can see from the figure is the laminate structure pattern, and the thickness of every one deck is also nanometer scale, and the mutual cross of some laminate structures is similar to flower-shaped.
Embodiment 6
Changing temperature is 50 ℃, the aqueous sodium hydroxide solution that alkaline solution is 0.5% (wt %), and other obtain nearly flower-shaped Sb with embodiment 4
2o
3micro-nano crystal grain.
Embodiment 7
Changing temperature of reaction is 75 ℃, and alkaline solution is 1.5% (wt %) diethanolamine aqueous solution, and other obtain stratiform Sb with embodiment 5
2o
3micro-nano crystal grain.
Fig. 6 is the banded pattern Sb of embodiment 1
2o
3the X-ray powder diffraction of powdered sample.Can see multiple diffraction absorption peak from collection of illustrative plates, the peak position of absorption peak well with rhombic form Sb
2o
3(JCPDS, 71-0383) matches, and is illustrated as rhombic form Sb
2o
3, the stronger interpret sample of absorption peak strength has comparatively perfect crystalline structure.With Sb
2o
3standard diagram compare, the Sb obtained
2o
3the intensity of (110) of powdered sample and (200) face diffraction peak improves, and the strength decreased of (111) face diffraction peak (012), this just illustrates that the crystal growth for preparing sample has certain orientation, and this is corresponding with banded pattern well.Do not find other diffraction peak yet from diffracting spectrum, illustrate that to obtain sample purity fine.
Above-described embodiment is the preferred embodiment of the present invention, but embodiments of the present invention are not restricted to the described embodiments, and the change that other any the present invention of not deviating from does all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (8)
1. single stage method prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, by SbCl
3ethanolic soln joins in alkaline solution and reacts, SbCl
3the volume ratio of ethanolic soln and alkaline solution is 1:1-20, and filtration, drying obtain one dimension and compound pattern Sb thereof
2o
3micro-nano powder, one dimension and compound pattern thereof are band shape, band pencil, bowknot shape, flower-shaped, stratiform.
2. single stage method as claimed in claim 1 prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, temperature of reaction is 5-85 ℃, and the time is 0.1-0.5 h, in the time of reaction, is stirred.
3. single stage method as claimed in claim 1 prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, SbCl
3the concentration of ethanolic soln is 0.01-4.0 mol/L.
4. single stage method as claimed in claim 3 prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, in described alkaline solution, the mass concentration of alkali is 0.02-30.0%.
5. single stage method as claimed in claim 4 prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, the aqueous solution that described alkaline solution is sodium hydroxide, ammoniacal liquor, quadrol, diethanolamine.
6. single stage method as claimed in claim 1 prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, SbCl
3ethanolic soln dropwise adds or disposable pouring in alkaline solution.
7. single stage method as claimed in claim 2 prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, stirs as electric stirring or magnetic agitation.
8. single stage method as described as one of claim 1-7 prepares one dimension and compound pattern Sb thereof
2o
3micro-nano powder, is characterized in that, temperature of reaction is 50-60 ℃, in the ammonia soln that is 0.02-5% in mass concentration, obtains banded Sb
2o
3micro-nano crystal grain; Temperature of reaction is 40-70 ℃, in the aqueous sodium hydroxide solution that is 0.02-1% in mass concentration, obtains nearly flower-shaped Sb
2o
3micro-nano crystal grain; Temperature of reaction is 20-50 ℃, in the ammonia soln that is 0.02-10% in mass concentration, obtains being with pencil Sb
2o
3micro-nano crystal grain; Temperature of reaction is 50-85 ℃, in the ammonia soln that is 5-12% in mass concentration, obtains bowknot shape Sb
2o
3micro-nano crystal grain; Temperature of reaction is 10-20 ℃, in the ammonia soln that is 12-25% in mass concentration, obtains flower-shaped Sb
2o
3micro-nano crystal grain; Temperature of reaction is 40-80 ℃, in the diethanolamine aqueous solution that is 1-5% in mass concentration, obtains stratiform Sb
2o
3micro-nano crystal grain; Temperature of reaction is 30-70 ℃, in the ethylenediamine solution that is 2-5% in mass concentration, obtains stratiform Sb
2o
3micro-nano crystal grain.
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| CN106517324A (en) * | 2016-10-28 | 2017-03-22 | 乐山凯亚达光电科技有限公司 | Method for preparing antimonous oxide from antimony sulfide ore |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040192791A1 (en) * | 2003-03-27 | 2004-09-30 | Nissan Chemical Industries, Ltd. | Diantimony pentoxide sol and method for its preparation |
| CN101817557A (en) * | 2010-03-23 | 2010-09-01 | 河南大学 | Method for preparing antimony oxide or antimony oxychloride micro-nanometer particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040192791A1 (en) * | 2003-03-27 | 2004-09-30 | Nissan Chemical Industries, Ltd. | Diantimony pentoxide sol and method for its preparation |
| CN101817557A (en) * | 2010-03-23 | 2010-09-01 | 河南大学 | Method for preparing antimony oxide or antimony oxychloride micro-nanometer particles |
Non-Patent Citations (6)
| Title |
|---|
| Debao Wang, et al..Phase and morphology controllable synthesis of Sb2O3 microcrystals.《Journal of Crystal Growth》.2009,第311卷全文. |
| Phase and morphology controllable synthesis of Sb2O3 microcrystals;Debao Wang, et al.;《Journal of Crystal Growth》;20090618;第311卷;第3948-3953页 * |
| 室温制备晶体结构和形貌可控的三氧化二锑纳米材料;郑荣波等;《曲阜师范大学学报》;20110731;第37卷(第3期);第62-64页 * |
| 李宾杰.特殊结构含锑、镁化合物纳米材料的制备和阻燃性能研究.《中国博士学位论文全文数据库 工程科技Ⅰ辑》.2007,(第6期),第36-41页. |
| 特殊结构含锑、镁化合物纳米材料的制备和阻燃性能研究;李宾杰;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20071215(第6期);第36-41页 * |
| 郑荣波等.室温制备晶体结构和形貌可控的三氧化二锑纳米材料.《曲阜师范大学学报》.2011,第37卷(第3期),第62-64页. |
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