CN102502820A - 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 29
- 239000000843 powder Substances 0.000 title abstract 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 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
- 239000011858 nanopowder Substances 0.000 claims description 17
- 239000002159 nanocrystal 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
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 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 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 3
- 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 12
- 239000008187 granular material Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 238000006460 hydrolysis reaction Methods 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
- 238000002389 environmental scanning electron microscopy Methods 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 230000002776 aggregation Effects 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
- 235000013339 cereals Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 239000008346 aqueous phase 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
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- 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
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007246 mechanism Effects 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
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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 character such as some unique mechanical, 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 method for preparing technology comparatively complicacy, long reaction time, energy dissipation is serious and need to add the heavy addition agent, and contaminate environment has seriously restricted the micro Nano material applied research.Research so far, liquid phase method especially prepares one dimension and composite structure micro-nano granules thereof at aqueous phase and is acknowledged as the simplest, feasible and the preparation method of prospects for commercial application is arranged.But the polarity of water is big; Metals ion hydrolytic reactions therein generates nucleation, the fast growth of oxide compound or oxyhydroxide; Have large quantity of moisture on the nano grain surface for preparing, these water moleculess can combine through the hydroxide radical on hydrogen bond and the nano grain surface.When spacing of particle when near, lip-deep water molecules can be used as " bridge " molecule, very easyly in drying process causes that hard aggregation grows up to macrobead between particle, thereby makes quantum effect, the surface effects of nano particle, the 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 overcomes the easy hard aggregation of product that existing method prepares, thereby influences quantum effect, the surface effects of nano particle, and the tunnel drills the defective that effect etc. can't be brought into play.
The technical scheme that the present invention adopts is following:
Single stage method prepares one dimension and compound pattern Sb thereof
2O
3Micro-nano powder is with SbCl under the normal temperature
3Ethanolic soln joins in the 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.
The mass concentration of alkali is 0.02-30.0% in the said alkaline solution.
Said alkaline solution is the aqueous solution of sodium hydroxide, ammoniacal liquor, quadrol, diethylolamine.
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 the alkaline solution.
Temperature of reaction is 5-85 ℃, and the time is 0.1-0.5 h, stirs in the time of reaction.
Stir and be electronic stirring or magnetic agitation.
Concrete, temperature of reaction is 50-60 ℃, is in the ammonia soln of 0.02-5% in mass concentration, obtains banded Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 40-70 ℃, is in the aqueous sodium hydroxide solution of 0.02-1% in mass concentration, obtains nearly flower-shaped Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 20-50 ℃, is in the ammonia soln of 0.02-10% in mass concentration, obtains being with pencil Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 50-85 ℃, is in the ammonia soln of 5-12% in mass concentration, obtains bowknot shape Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 10-20 ℃, is in the ammonia soln of 12-25% in mass concentration, obtains flower-shaped Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 40-80 ℃, is in the diethylolamine aqueous solution of 1-5% in mass concentration, obtains stratiform Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 30-70 ℃, is in the ethylenediamine solution of 2-5% in mass concentration, obtains stratiform Sb
2O
3Micro-nano crystal grain.
The object of the invention is to make reactant SbCl through the control different reaction conditions
3One step generated the Sb of different-shape
2O
3Micro-nano granules, and the particle that generates is difficult for reuniting.At first under normal temperature condition, use anhydrous alcohol solution SbCl
3, make inorganic metal salt SbCl
3Generate alcohol solvent compound therein, SbCl like this can slow down
3Hydrolysis generates the oxidiferous nucleation and the speed of growth, grows according to incomplete oriented adsorption and Ostwarld slaking mechanism; In addition, the small amount of ethanol molecule that exists in the system can be adsorbed onto particle surface, reaches sterically hindered effect, has reduced between particle and has taken the phenomenon that " bridge " grows up through water molecules.Through adjusting different reaction parameters, control the product pattern, prepare the Sb of one dimension and composite structure pattern thereof
2O
3Micro-nano powder is like different-shapes such as banded, band pencil, bowknot shape, flower-shaped and stratiforms.The micro-nano granules for preparing not only has comparatively regular pattern, and granule surface area is big, and what have also has a bigger length-to-diameter ratio, and output is big, will have good application prospects in fields such as fire-retardant, catalysis, electrochemistry.This method has that preparation is simple, cost is low, time saving and energy saving, save energy, environmental pollution are little, does not add additive such as the tensio-active agent of any control pattern etc. in the preparation process, is fit to the requirements of the times of current low carbonization, has industrial applications potential.Present method also is expected to be used for the preparation and the industriallization research of the micro Nano material of other kind.
The present invention has following advantage with respect to prior art:
Product particle that the present invention prepares is better dispersed, is not easy to take place hard aggregation, and method is simple, cost is low, time saving and energy saving, save energy, environmental pollution are little, does not add any additives in the preparation process, has industrial applications potential.
Description of drawings
Fig. 1 is the Sb of banded pattern
2O
3The SEM figure of micro-nano granules;
Fig. 2 is the Sb of band pencil pattern
2O
3The SEM figure of micro-nano granules;
Fig. 3 is the Sb of bowknot shape pattern
2O
3The SEM figure of micro-nano granules;
Fig. 4 is the Sb of floriform appearance
2O
3The SEM figure of micro-nano granules;
Fig. 5 is the Sb of stratiform pattern
2O
3The SEM figure of micron particle;
Fig. 6 is the Sb of 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 thereto:
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 that generates hydrolysis then
2O
3Suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2O
3Powdered sample.
With the Sb for preparing on a small quantity
2O
3Powdered sample directly adheres on the copper platform of conductive resin, it is carried out metal spraying after, under ESEM, observe, the result is as shown in Figure 1.The particle that from figure, can see is banded pattern, and length reaches 10-20 μ m, and the thickness of single nano belt is about 100nm.
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 that generates hydrolysis then
2O
3Suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2O
3Powdered sample.
With the Sb for preparing on a small quantity
2O
3Powdered sample directly adheres on the copper platform of conductive resin, it is carried out metal spraying after, under ESEM, observe, the result is as shown in Figure 2.The particle that from figure, can see is a band pencil pattern, and length is about 20 μ m, and the thickness of single nano belt is about 100 nm, 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 %), electronic stirring reaction 0.1 h, the Sb that generates hydrolysis then
2O
3Suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2O
3Powdered sample.
With the Sb for preparing on a small quantity
2O
3Powdered sample directly adheres on the copper platform of conductive resin, it is carried out metal spraying after, under ESEM, observe, the result is as shown in Figure 3.The particle that from figure, can see is the bowknot shape pattern, and length is about 20 μ m, and the thickness of the nano belt of composition bow-knot-double is about 100 nm, 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 that generates hydrolysis then
2O
3Suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2O
3Powdered sample.
With the Sb for preparing on a small quantity
2O
3Powdered sample directly adheres on the copper platform of conductive resin, it is carried out metal spraying after, under ESEM, observe, the result is as shown in Figure 4.The particle that from figure, can see number extremely greatly is a floriform appearance, and the diameter of flower is about about 5 μ m, and the micro-nano popped rice is that the sheet of thickness about 100 nm formed by longer length is 2-3 μ m from the center one by one.
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 %), electronic stirring reaction 0.5 h, the Sb that generates hydrolysis then
2O
3Suspension filtered, washing, 60 ℃ of oven dryings obtain Sb
2O
3Powdered sample.
With the Sb for preparing on a small quantity
2O
3Powdered sample directly adheres on the copper platform of conductive resin, it is carried out metal spraying after, under ESEM, observe, the result is as shown in Figure 5.The particle that can see is the laminate structure pattern from figure, and the thickness of each layer also is nanometer scale, some laminate structures intersect each other be similar to flower-shaped.
Embodiment 6
Changing temperature is 50 ℃, and alkaline solution is the aqueous sodium hydroxide solution of 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 %) diethylolamine aqueous solution, and other obtain stratiform Sb with embodiment 5
2O
3Micro-nano crystal grain.
Fig. 6 is embodiment 1 banded pattern Sb
2O
3The X-ray powder diffraction of powdered sample.From collection of illustrative plates, can see multiple diffraction absorption peak, 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 strong interpret sample of absorption peak strength has comparatively perfect crystalline structure.With Sb
2O
3Standard diagram compare the Sb that obtains
2O
3The intensity of (110) of powdered sample and (200) face diffraction peak improves, and the intensity of (012) and (111) face diffraction peak reduces, and this has certain orientation with regard to the crystal growth that explanation prepares sample, and this is corresponding with zonal pattern well.From diffracting spectrum, do not find other diffraction peak yet, explain that to obtain sample purity fine.
The foregoing description is the preferred embodiment of the present invention, but embodiment of the present invention is not restricted to the described embodiments, and other the change that any the present invention of not deviating from did all should be the substitute mode of equivalence, is included within protection scope of the present invention.
Claims (9)
1. single stage method prepares one dimension and compound pattern Sb thereof
2O
3Micro-nano powder is characterized in that, with SbCl
3Ethanolic soln joins in the alkaline solution and reacts, and filtration, drying obtain one dimension and compound pattern Sb thereof
2O
3Micro-nano powder.
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, stirs in the time of reaction.
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, the mass concentration of alkali is 0.02-30.0% in the said alkaline solution.
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, said alkaline solution is the aqueous solution of sodium hydroxide, ammoniacal liquor, quadrol, diethylolamine.
6. single stage method as claimed in claim 4 prepares one dimension and compound pattern Sb thereof
2O
3Micro-nano powder is characterized in that, SbCl
3The volume ratio of ethanolic soln and alkaline solution is 1:1-20.
7. 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 the alkaline solution.
8. 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 to be electronic stirring or magnetic agitation.
9. prepare one dimension and compound pattern Sb thereof like the described single stage method of one of claim 1-8
2O
3Micro-nano powder is characterized in that, temperature of reaction is 50-60 ℃, is in the ammonia soln of 0.02-5% in mass concentration, obtains banded Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 40-70 ℃, is in the aqueous sodium hydroxide solution of 0.02-1% in mass concentration, obtains nearly flower-shaped Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 20-50 ℃, is in the ammonia soln of 0.02-10% in mass concentration, obtains being with pencil Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 50-85 ℃, is in the ammonia soln of 5-12% in mass concentration, obtains bowknot shape Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 10-20 ℃, is in the ammonia soln of 12-25% in mass concentration, obtains flower-shaped Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 40-80 ℃, is in the diethylolamine aqueous solution of 1-5% in mass concentration, obtains stratiform Sb
2O
3Micro-nano crystal grain; Temperature of reaction is 30-70 ℃, is in the ethylenediamine solution of 2-5% in mass concentration, obtains stratiform Sb
2O
3Micro-nano crystal grain.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106006575A (en) * | 2016-05-12 | 2016-10-12 | 武汉光电工业技术研究院有限公司 | One-dimensional inorganic polymer and universal preparing method thereof |
| 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 |
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| 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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Patent 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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| Title |
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| DEBAO WANG, ET AL.: "Phase and morphology controllable synthesis of Sb2O3 microcrystals", 《JOURNAL OF CRYSTAL GROWTH》 * |
| 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》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006575A (en) * | 2016-05-12 | 2016-10-12 | 武汉光电工业技术研究院有限公司 | One-dimensional inorganic polymer and universal preparing method thereof |
| CN106006575B (en) * | 2016-05-12 | 2017-11-14 | 武汉光电工业技术研究院有限公司 | A kind of one-dimensional inorganic macromolecule and its general preparative methods |
| 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 |
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