CN100593019C - A kind of antimony-doped tin dioxide nanopowder and preparation method thereof - Google Patents
A kind of antimony-doped tin dioxide nanopowder and preparation method thereof Download PDFInfo
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- CN100593019C CN100593019C CN200810229400A CN200810229400A CN100593019C CN 100593019 C CN100593019 C CN 100593019C CN 200810229400 A CN200810229400 A CN 200810229400A CN 200810229400 A CN200810229400 A CN 200810229400A CN 100593019 C CN100593019 C CN 100593019C
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000011858 nanopowder Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 32
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 27
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 27
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 5
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 3
- 239000003795 chemical substances by application Substances 0.000 claims abstract 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract 4
- 150000001462 antimony Chemical class 0.000 claims abstract 4
- 238000013329 compounding Methods 0.000 claims abstract 4
- 239000002243 precursor Substances 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 239000004584 polyacrylic acid Substances 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims 1
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims 1
- 239000011975 tartaric acid Substances 0.000 claims 1
- 235000002906 tartaric acid Nutrition 0.000 claims 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims 1
- 239000008096 xylene Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000012266 salt solution Substances 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 238000007796 conventional method Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 description 12
- 238000006460 hydrolysis reaction Methods 0.000 description 7
- 238000000975 co-precipitation Methods 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 4
- 230000001476 alcoholic effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229940095064 tartrate Drugs 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000009841 combustion method Methods 0.000 description 3
- 210000003608 fece Anatomy 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OPFSQGIWBZCDEP-UHFFFAOYSA-N O(O)O.[Sb] Chemical compound O(O)O.[Sb] OPFSQGIWBZCDEP-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
本发明涉及纳米材料。一种锑均匀掺杂的二氧化锡纳米粉体的制备方法，搅拌下，将锑的醇溶液和氨水同时加入锡溶液中，15-60min内加入完毕，反应液的pH值位于3-4之间，然后将反应溶液在50-70℃的条件下陈化2-5h，过滤、水洗以去除其中的水溶性无机盐，分散于有机溶剂，干燥除去有机溶剂；煅烧0.5-3h，即可得到深蓝色的ATO纳米粉体。本发明将锑盐的醇溶液和沉淀剂氨水溶液以双滴加的方式同步滴入锡盐水溶液中，在配合剂的作用下，锡、锑同步水解，实现锑的均匀掺杂。本发明克服了常规方法制备ATO粉体锑掺杂不均匀、颗粒易团聚等缺点，扩大了ATO纳米粉体的应用范围。The present invention relates to nanomaterials. A preparation method of tin dioxide nano-powder evenly doped with antimony. Under stirring, the alcohol solution of antimony and ammonia water are added to the tin solution at the same time, the addition is completed within 15-60 minutes, and the pH value of the reaction solution is between 3-4 Then, the reaction solution is aged at 50-70°C for 2-5h, filtered and washed with water to remove the water-soluble inorganic salt, dispersed in an organic solvent, dried to remove the organic solvent; calcined for 0.5-3h to obtain Dark blue ATO nanopowder. In the present invention, the alcohol solution of the antimony salt and the ammonia solution of the precipitating agent are dropped into the tin salt solution synchronously in the manner of double dropping, and under the action of the compounding agent, the tin and the antimony are synchronously hydrolyzed to realize the uniform doping of the antimony. The invention overcomes the disadvantages of non-uniform doping of antimony and easy agglomeration of particles in the ATO powder prepared by the conventional method, and expands the application range of the ATO nanometer powder.
Description
One, technical field
The present invention relates to nano material, antimony doped stannic oxide nanometer material particularly also relates to the preparation method of its powder in addition.
Two, background technology
Stibium doping stannic oxide (Antimony Doped Tin Oxide, be called for short ATO) is a kind of novel multifunctional semiconductor material, has characteristics such as high temperature resistant, corrosion-resistant, good dispersity.In the environmental protection and energy saving field, because nano ATO has this special performances of very strong reflex action to the infrared rays in the sunlight, can be applicable to thermal insulating coating,, also can be used for fiber, polymeric membrane or the like as building energy-saving glass door and window, vehicles windshield; As antistatic and electro-conductive material, nano ATO can be applicable to various low-cost conductive glass again, as display device, solar cell etc. and various high-grade transparent antistatic coating; Utilize the decay of nano ATO, can be used on the field that computer house, radar shielding protective belt etc. need shielding electromagnetic wave microwave, or the like.Make the nano ATO material become one of material area research focus just because of these application prospects and marketable value.
The ATO preparation methods mainly contains solid phase method, hydrothermal method, combustion method and coprecipitation method etc. at present.
Solid phase method is with SnO
2, Sb
2O
3Mix Deng powder, add certain amount of organic solvent again, can obtain the ATO powder through ball milling, oven dry, high-temperature calcination.Solid phase method has advantages such as technology is simple, preparation flow is short, but owing to be solid state reaction, needs high temperature to transform fully, and it is serious and very irregular to obtain powder reuniting, and poor performance is difficult to reach the requirement of practicability.
Hydrothermal method is reaction raw materials to be dissolved in obtain precursor liquid in the distilled water, transfers in the autoclave hydro-thermal reaction 2 ~ 4h under the temperature more than 200 ℃, cooling after washing, dry, grind and promptly obtain final product.Hydrothermal Preparation ATO powder has improved reactive behavior, has reduced granularity, has improved specific surface area, but has a basic problem, because the Cl in the precursor
-, SO
4 2-, NO
3 -Or Na
+Isoionic existence has influence on electricity, the optical property of ATO powder widely, and hydrothermal method requires highly to device ', and there is potential safety hazard in large-scale industrial production.
Combustion method has technology simply, does not need complex apparatus, plurality of advantages such as synthetic polycompound easily, but up to the present, because combustion synthesis method is the problem from also existing some to be difficult to overcome on technological development still is theoretical investigation no matter, produce shortcomings such as the control of a large amount of smog, particle is inhomogeneous, the industrial combustion method synthesis of nano powder that do not adopt as yet as preparation process.
Liquid-phase coprecipitation is the most frequently used and the most sophisticated method of preparation ATO powder, and conventional preparation method is with SnCl
4Or SnCl
45H
2O and SbCl
3Be raw material, carry out co-precipitation and make the ATO precursor, carry out the high-temperature calcination processing again and can obtain the ATO powder.Coprecipitation method has advantages such as preparation technology is simple, cost is low, be easy to control, synthesis cycle is short, but when preparation ATO powder following shortcoming is arranged: (1) pink salt and antimonic salt be very easily hydrolysis all, in order to guarantee that tin antimony exists with the ionic form, need to add a large amount of strong acid and suppress its hydrolysis, and then make it hydrolytic precipitation with alkali, caused production cost height, seriously polluted like this; (2) Sb
3+And Sn
4+The ion hydrolysis is asynchronous, the truly even doping of Sb of being unrealized; (3) because " the key bridge " of water effect makes powder reuniting serious, can't obtain the uniform nano-powder of particle diameter, influenced its use value.
Three, summary of the invention
The objective of the invention is in order to overcome above-mentioned not enough problem, even adulterated stannic oxide nano powder of a kind of antimony and preparation method thereof is provided, coprecipitation method after the improvement, this method is simple, technical process short, it is little and be evenly distributed that the ATO nano-powder that makes has a particle diameter, has good electricity and optical characteristics.
The technical scheme that the present invention is adopted for achieving the above object is: the preparation method of the even adulterated stannic oxide nano powder of a kind of antimony, and concrete preparation process is as follows:
(1) pink salt is mixed with the aqueous solution that concentration is 0.3-0.8mol/L, adds the Synergist S-421 95 that accounts for pink salt quality 2-6% again, it is stand-by to make solution of tin after Synergist S-421 95 dissolves fully, and wherein Synergist S-421 95 adopts one or more in tartrate, citric acid, the polyacrylic acid;
(2) antimonic salt is adopted pure liquid dissolving, be mixed with the alcoholic solution that concentration is 0.1-0.5mol/L antimony;
(3) stir down, the alcoholic solution and the ammoniacal liquor of antimony is added in the solution of tin simultaneously, add in the 15-60min and finish, the pH value of reaction solution then with reaction soln ageing 2-5h under 50-70 ℃ condition, promptly obtains the precursor suspension liquid of milk yellow between 3-4;
(4) the precursor suspension liquid that then (3) is obtained filters, washes to remove water-soluble inorganic salt wherein;
(5) precursor that again (4) is obtained is scattered in organic solvent, and drying is removed organic solvent then;
(6) precursor that at last (5) is obtained is calcined 0.5-3h in 600-900 ℃ air, can obtain navy blue ATO nano-powder.
Described pink salt is one or more in the muriate, nitrate, Citrate trianion of tin.Antimonic salt is one or more in the muriate, nitrate, Citrate trianion of antimony.
The alcohol of described dissolving antimonic salt adopts one or more in methyl alcohol, ethanol, the propyl alcohol.
Described antimony is 1 with the ratio of tin mole: 10-20.
Described step (3) under agitation adopts simultaneously two dropping modes to add in the solution of tin alcoholic solution and the ammoniacal liquor of antimony, dropwises in the 15-60min.
Organic solvent in the described step (5) is one or more in toluene, dimethylbenzene, the propyl carbinol.
The present invention with compare with product preparation method, have outstanding advantage and beneficial effect:
(1) the present invention adds Synergist S-421 95s such as tartrate, citric acid, polyacrylic acid in the aqueous solution of tin, these Synergist S-421 95s form title complex with tin, antimony in coprecipitation process, reduce the settling rate of tin, antimony oxyhydroxide, helped the even growth of nano particle;
(2) antimonic salt adopts pure liquid dissolving among the present invention, because antimonic salt hydrolysis rate in water is fast, needs to add a large amount of strong acid and suppresses its hydrolysis, and antimonic salt hydrolysis rate in alcoholic solution slows down greatly, avoid introducing strong acid, provide cost savings and also reduced pollution, improved processing safety;
(3) antimonic salt alcohol liquid and ammoniacal liquor add in the tin-salt solution simultaneously continuously, impel antimony, the synchronous hydrolysis reaction of tin, have realized really evenly mixing of antimony;
(4) the nano-powder precursor is scattered in organic solvent, has not only removed residual moisture content in the exsiccant process, has also guaranteed the dispersiveness of powder, suppresses the reunion of powder effectively, makes little, the narrowly distributing of the particle diameter of nanometer powder that makes.
Four, description of drawings
Fig. 1 is the preparation flow figure of nano ATO powder of the present invention.
Five, embodiment
Embodiment 1
(1) with 26.1gSnCl
45H
2O is mixed with the aqueous solution that concentration is 0.3mol/L, adds 1.57g tartrate again, and it is stand-by that tartrate dissolves the back fully; (2) with 2.28gSbCl
3Be mixed with the ethanolic soln that concentration is 0.1mol/L; (3) under stirring condition, the ethanolic soln of antimony and the ammoniacal liquor mode by two droppings was splashed in the solution of tin in the time of 30min, wherein the ratio of the amount of substance of antimony and tin is 1: 10, dropwises the pH=3 of back solution, with reaction soln ageing 2h under 70 ℃ condition; (4) then the precursor that obtains is filtered, washes 3 times, remove NH wherein
4Cl; (5) the no NH that will obtain again
4The precursor of Cl is scattered in toluene, the dry then solvent of removing wherein; (6) at last the precursor that obtains is calcined 3h in 600 ℃ air, can obtain navy blue ATO nano-powder, its particle diameter is 10-25nm, is uniformly dispersed.
Embodiment 2
(1) with 36.7gSn (NO
3)
4Be mixed with the aqueous solution that concentration is 0.8mol/L, add the 1.45g citric acid again, it is stand-by that citric acid dissolves the back fully; (2) with 1.54gSb (NO
3)
3Be mixed with the methanol solution that concentration is 0.5mol/L; (3) under stirring condition, the methanol solution of antimony and the ammoniacal liquor mode by two droppings is splashed into Sn (NO in the inter-sync of the time of 15min
3)
4In the solution, wherein the ratio of the amount of substance of antimony and tin is 1: 20, dropwises the pH=4 of back solution, then with reaction soln ageing 5h under 50 ℃ condition; (4) then the precursor that obtains is filtered, washes 5 times, remove NH wherein
4NO
3What (5) will obtain removes NH again
4NO
3After precursor be scattered in dimethylbenzene, remove solvent wherein then; (6) will obtain precursor at last and calcine 0.5h in 900 ℃ air, and can obtain navy blue ATO nano-powder, its particle diameter is 10-20nm, is uniformly dispersed.
Embodiment 3
(1) with 31.1gSn (SO
4)
2Be mixed with the aqueous solution that concentration is 0.5mol/L, add the 1.56g polyacrylic acid again, it is stand-by that polyacrylic acid dissolves the back fully; (2) with 1.77gSb
2(SO
4)
3Being mixed with concentration is the n-propyl alcohol solution of 0.3mol/L; (3) under intensively stirred condition, with Sn (SO
4)
2N-propyl alcohol solution and the mode of ammoniacal liquor by two droppings splash into Sn (SO in the inter-sync of the time of 60min
4)
2In the solution, wherein the ratio of the amount of substance of antimony and tin is 1: 15, dropwises the pH=3.5 of back solution, then with reaction soln ageing 3h under 60 ℃ condition; (4) then the precursor that obtains is filtered, washes 4 times, remove (NH wherein
4)
2SO
4What (5) will obtain removes (NH again
4)
2SO
4After precursor be scattered in propyl carbinol, remove solvent wherein then; (6) will obtain precursor at last and calcine 1h in 700 ℃ air, and can obtain navy blue ATO nano-powder, its particle diameter is 15-25nm, is uniformly dispersed.
Claims (7)
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643200B (en) * | 2009-08-31 | 2012-02-08 | 石家庄铁道学院 | Preparation method of antimony-doped tin oxide nanopowder |
| CN103011263B (en) * | 2011-09-21 | 2015-04-01 | 中国科学院宁波材料技术与工程研究所 | Method for preparing sheet antimony tin oxide (ATO) powder body |
| CN103011262B (en) * | 2011-09-21 | 2015-08-12 | 中国科学院宁波材料技术与工程研究所 | The preparation method of tin ash base conductive material |
| CN102491408B (en) * | 2011-12-07 | 2014-03-12 | 富思特新材料科技发展股份有限公司 | Preparation method of antimony-doped tin dioxide nano-slurry |
| CN103508483B (en) * | 2013-09-11 | 2016-03-09 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of nano tin oxide powder |
| CN106315666A (en) * | 2016-07-29 | 2017-01-11 | 深圳大学 | ATO nanocrystal, ATO nanometer slurry, ATO/macromolecular polymer compound and preparation methods |
| CN106986382B (en) * | 2016-08-16 | 2018-06-29 | 郑雅 | The preparation method of improved nano antimony tin oxide powder |
| CN112591787B (en) * | 2021-02-03 | 2022-01-21 | 河南大学 | Method for preparing nano antimony doped tin oxide powder by microexplosion method |
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Non-Patent Citations (2)
| Title |
|---|
| 共沉淀法制备掺锑SnO2纳米级粉体. 李青山等.山东轻工业学院学报，第16卷第2期. 2002 * |
| 配合－共沉淀法制备锑掺杂二氧化锡(ATO)粉. 杨建广等.中国有色金属学报，第15卷第6期. 2005 * |
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