CN1669913A - Method for preparing elemental selenium nanotubes by liquid phase reduction without template - Google Patents
Method for preparing elemental selenium nanotubes by liquid phase reduction without template Download PDFInfo
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- CN1669913A CN1669913A CN 200510024071 CN200510024071A CN1669913A CN 1669913 A CN1669913 A CN 1669913A CN 200510024071 CN200510024071 CN 200510024071 CN 200510024071 A CN200510024071 A CN 200510024071A CN 1669913 A CN1669913 A CN 1669913A
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000002071 nanotube Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000007791 liquid phase Substances 0.000 title claims abstract description 10
- 239000011669 selenium Substances 0.000 claims abstract description 22
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 20
- 229940091258 selenium supplement Drugs 0.000 claims abstract description 20
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 12
- 239000008103 glucose Substances 0.000 claims abstract description 12
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229960001471 sodium selenite Drugs 0.000 claims abstract description 11
- 235000015921 sodium selenite Nutrition 0.000 claims abstract description 11
- 239000011781 sodium selenite Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 230000002829 reductive effect Effects 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 125000003748 selenium group Chemical group *[Se]* 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002070 nanowire Substances 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 1
- 239000002159 nanocrystal Substances 0.000 abstract 1
- 230000001988 toxicity Effects 0.000 abstract 1
- 231100000419 toxicity Toxicity 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 6
- 229960000935 dehydrated alcohol Drugs 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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Abstract
本发明提供了一种无模板液相还原合成单质硒纳米管的方法。主要特征是以亚硒酸钠为硒源，以葡萄糖为还原剂，通过水热反应一步获得结晶完好的单质硒纳米管。制备过程中不需任何模板，也不需添加表面活性剂，在水热环境下快速制备；在150－200℃下水热反应8－12h能获得外径200－300nm，内径150－200nm，长径比15－40的高质量纳米管。本方法选用更加环境友好的绿色还原剂葡萄糖作还原剂，降低废液排放毒性，比以往使用水合肼作还原剂更加安全实用；并且一步还原可以省略很多繁琐的步骤；水热环境更加适合晶体生长，可以快速生长高质量的纳米晶，较常用室温生长纳米线快得多。本方法具有工艺简单、操作方便、成本低廉和环境友好等特点。
The invention provides a method for synthesizing elemental selenium nanotubes by liquid phase reduction without template. The main feature is to use sodium selenite as a selenium source and glucose as a reducing agent to obtain well-crystallized elemental selenium nanotubes in one step through hydrothermal reaction. The preparation process does not require any templates, nor does it need to add surfactants, and can be rapidly prepared in a hydrothermal environment; hydrothermal reaction at 150-200°C for 8-12 hours can obtain an outer diameter of 200-300nm, an inner diameter of 150-200nm, and a long diameter High-quality nanotubes with a ratio of 15-40. This method uses the more environmentally friendly green reducing agent glucose as the reducing agent to reduce the toxicity of waste liquid discharge, which is safer and more practical than using hydrazine hydrate as the reducing agent in the past; and one-step reduction can omit many tedious steps; the hydrothermal environment is more suitable for crystal growth , can quickly grow high-quality nanocrystals, which is much faster than the usual room temperature growth of nanowires. The method has the characteristics of simple process, convenient operation, low cost and environmental friendliness.
Description
Technical field
The present invention relates to the preparation method of elemental selenium nanotube.Belong to field of nanometer material technology.
Background technology
Simple substance selenium is a kind of important elemental semiconductor, has numerous tempting performances in many aspects, as lower fusing point (～490K), high optical conductivity (～8 * 10
4Scm
-1), nonlinear optical response performance and high chemically reactive etc., on photocell, rectifier, mechanical sensing device, photosensor and reprography, have application market widely.Since S.Iijima discovery carbon nanotube in 1991, the tubular nanometer structure was because its unique feature and performance become the focus that the investigation of materials scholar pays close attention at once.Because Se self crystalline structure is a kind of chain-like structure, have unique unsymmetric structure, make it to possess spontaneous one-dimensional growth habit.Therefore, the research of simple substance selenium one-dimentional structure is carried out in a large number, as one-dimensional nano line, nanometer rod and nano belt etc.Prior preparation method has physical methods such as laser splash and gas-solid deposition, and wet chemical method such as solvent thermal.Wherein the typical case of wet chemistry method representative is the research of the nano wire carried out of Xia Younan and group member thereof, and they are with H
2SeO
3Be selenium source, hydrazine hydrate is a reductive agent, by forming the red selenium of amorphous behind the room temperature reaction, in ethanol medium, and room temperature is grown (week) for a long time under the lucifuge, perhaps the assisting ultrasonic technology growth goes out tripartite selenium nano wire (B.Gates, B.Mayers, the A.Grossman of high length-diameter ratio, Y.Xia, Advanced Materials, 2002,14 (23): 1749-1752).Other selenium sources commonly used have Na
2SeSO
3, Na
2SeO
3With Se etc., also applied to prepare elemental selenium nano line or nanometer rod in a large number, big quantity research with simple substance Te of similar structures has also prepared corresponding nano wire, nanometer rod even nanotube (B.Mayers, Y.Xia, Advanced Materials, 2002,14 (4): 279-282), but but there is very big difficulty in the preparation of elemental selenium nanotube always, and it is less to be seen in report.Lu Jun etc. are by the solvent-thermal method growth, and in ethanol medium, 200 ℃ of growth 12h obtain the micron single-transistor of diameter 30 μ m with simple substance selenium, big (the Jun Lu of size, Yi Xie, Fen Xu, Liying Zhu, J.Mater.Chem., 2002,12,2755-2761).Nearest Ma Yurong etc. are with Na
2SeSO
3Disproportionation reaction in the acidic medium of micellar solution successfully prepare external diameter 80-300nm length from several μ m to the above elemental selenium nanotube of 100 μ m, wherein use surfactant B rij-35 to form micella and make soft template, assisting ultrasonic means room temperature growth (Yurong Ma, Limin Qi, Jiming Ma, Humin Cheng, Advanced Materials, 2004,16 (12): 1023-1026).Zhang Hui etc. are selenium source with simple substance selenium, prepare precursor aqueous solution (NH earlier in 200 ℃ of thermal and hydric environments
4)
2SeO
3, with the hydrazine hydrate reductive agent again, the assisting ultrasonic technology growth goes out the nanotube of external diameter 200-500nm, thickness of pipe 50nm, but the curtailment of nanotube (Hui Zhang, Deren Yang, Yujie Ji, Xiangyang Ma, Jin Xu, DuanlingQue, J.Phys.Chem.B, 108,1179-1182).Also there are many potential safety hazards in the reductive agent hydrazine hydrate that uses, and experimental implementation is closed liquid waste disposal all must be very careful.This shows that existing wet-chemical prepares the means major part grows based on ultrasonic technique, perhaps use surfactant modified or the limit threshold.Carry out the research of elemental selenium nanotube preparation, demand developing safe and practical easy synthesizing mean urgently.
Summary of the invention
The object of the invention is to provide a kind of non-template liquid phase reduction legal system to be equipped with elemental selenium nanotube, it is a kind of method for preparing the elemental selenium nanotube of complete crystallization by a stage reduction method, simplify the experimental technique route, and use safer reductive agent, need not the promptly synthetic elemental selenium nanotube of template, make it more easy to use, environmental friendliness.
The present invention implements like this: with the Sodium Selenite is selenium source, is reductive agent with glucose, passes through hydro-thermal reaction 10h one-step synthesis elemental selenium nanotube at 180 ℃.
(1) mol ratio with Sodium Selenite and glucose is set in 1: 2-1: 4 scopes, in the teflon-lined stainless steel cauldron of packing into, adding distil water to 80% volume is stirred to dissolving with glass stick, forms water white mixing solutions.
(2) the reactor sealing is tightened, put into baking oven, temperature is set in 150-200 ℃, take out reactor behind the reaction 8-12h, make its naturally cooling.
(3) subsequently the reaction precipitation thing is poured out, it is inferior to give a baby a bath on the third day after its birth with distilled water, washes twice with dehydrated alcohol again.50-70 ℃ of following dry 3-6h in vacuum drying oven collects sample retention in moisture eliminator at last.
The method of the synthetic elemental selenium nanotube of a kind of non-template liquid phase reduction provided by the invention is characterized in:
(1) is water-soluble selenium source with Sodium Selenite, can obtains uniform reaction system;
(2) with glucose be reductive agent, toxicological harmless is a kind of green environment close friend's a weak reductant, avoids using dangerous big reductive agent, for example uses hydrazine hydrate as reductive agent than in the past, not only reduces toxin expelling, and safety;
(3) reaction need not any template limit threshold or adds any surfactant modifiedly, and next step can obtain elemental selenium nanotube at thermal and hydric environment;
(4) the experimental technique route is simple, and operation is convenient.
(5) preparation elemental selenium nano external diameter of pipe 200-300nm, internal diameter 150-200nm, length-to-diameter ratio is up to 15-40, the complete crystallization monocrystalline.
Description of drawings
Fig. 1 elemental selenium nano powder X ray diffracting spectrum
Fig. 2 nanotube transmission electron microscope photo and electron diffraction spot: (a) (b) embodiment 1, (c) (d) embodiment 2
The single nanotube EDS of Fig. 3 power spectrum collection of illustrative plates
Embodiment
Further specify embodiment and effect with following indefiniteness embodiment:
The mol ratio of Sodium Selenite and glucose was set in 1: 2, get 0.0025mol Sodium Selenite and 0.005mol glucose, the volume 80mL that packs into gets in the teflon-lined stainless steel cauldron, adding distil water to 80% volume, be stirred to dissolving with glass stick, form water white mixing solutions.The reactor sealing is tightened, put into baking oven, temperature is set in 180 ℃, take out reactor behind the reaction 10h, make its naturally cooling.Subsequently the reaction precipitation thing is poured out, it is inferior to give a baby a bath on the third day after its birth with distilled water, washes twice with dehydrated alcohol again.60 ℃ of following dry 4h in vacuum drying oven collect sample retention in moisture eliminator at last.Fig. 1 is the X-ray diffraction spectrogram of the nanometer selenium powder of present embodiment preparation, as seen the gained powder is tripartite phase simple substance selenium, and diffraction peak is successively corresponding to the crystal face diffraction peak of (100), (101), (111), (102), (111), (200), (201), (003), (112), (103), (202), (210), (211) and (113) in the spectrogram; Do not find the diffraction peak of any impurity in the spectrogram, diffraction peak intensity is high and sharp-pointed, has as seen obtained the intact tripartite phase simple substance selenium of purity higher crystalline.Fig. 2 a-b is the transmission electron microscope photo of prepared sample, and visible simple substance selenium presents the tubulose pattern, nanotube external diameter 200-300nm, and internal diameter 150-200nm, length-to-diameter ratio has exceeded field range up to more than 15 in transmission electron microscope photo.The electron diffraction spot explanation nanotube that is inserted in Fig. 2 (a) is the monocrystalline of complete crystallization.Fig. 3 is the single nanotube EDS energy of a sample spectrogram, and product purity is higher, except the peak from copper mesh back of the body end C and Cu occurring, all is the power spectrum peak of simple substance selenium.
Embodiment 2
The mol ratio of preparation Sodium Selenite and glucose is 1: 4, and the volume 80mL that packs into gets in the teflon-lined stainless steel cauldron, and adding distil water to 80% volume is stirred to dissolving with glass stick, forms water white mixing solutions.The reactor sealing is tightened, put into baking oven, temperature is set in 180 ℃, take out reactor behind the reaction 10h, make its naturally cooling.Subsequently the reaction precipitation thing is poured out, it is inferior to give a baby a bath on the third day after its birth with distilled water, washes twice with dehydrated alcohol again.70 ℃ of oven dry down in vacuum drying oven are at last collected sample retention in moisture eliminator.Preparation selenium nanotube diameter 250-300nm, internal diameter 150-200nm, length-to-diameter ratio is up to 40.Fig. 2 c-d is the transmission electron microscope photo of prepared sample.
Embodiment 3
The mol ratio of preparation Sodium Selenite and glucose is 1: 2, and in the teflon-lined stainless steel cauldron of the volume 80mL that packs into, adding distil water to 80% volume is stirred to dissolving with glass stick, forms water white mixing solutions.The reactor sealing is tightened, put into baking oven, temperature is set in 150 ℃, take out reactor behind the reaction 12h, make its naturally cooling.Subsequently the reaction precipitation thing is poured out, it is inferior to give a baby a bath on the third day after its birth with distilled water, washes twice with dehydrated alcohol again.50 ℃ of oven dry down in vacuum drying oven are at last collected sample retention in moisture eliminator.Preparation selenium nanotube diameter 200-300nm, internal diameter 150-200nm, length-to-diameter ratio reaches 15.
Embodiment 4
The mol ratio of preparation Sodium Selenite and glucose is 1: 2, and the volume 80mL that packs into gets in the teflon-lined stainless steel cauldron, and adding distil water to 80% volume is stirred to dissolving with glass stick, forms water white mixing solutions.The reactor sealing is tightened, put into baking oven, temperature is set in 200 ℃, take out reactor behind the reaction 8h, make its naturally cooling.Subsequently the reaction precipitation thing is poured out, it is inferior to give a baby a bath on the third day after its birth with distilled water, washes twice with dehydrated alcohol again.50 ℃ of oven dry down in vacuum drying oven are at last collected sample retention in moisture eliminator.Prepared selenium nanotube length-to-diameter ratio reaches 20.All the other are with embodiment 1.
Claims (5)
1, a kind ofly need not the method that template liquid phase reduction prepares elemental selenium nanotube, it is characterized in that: with inorganic Sodium Selenite is selenium source, with glucose is reductive agent, reaction one-step synthesis tubulose elemental selenium nano crystalline substance under hydrothermal condition, the mol ratio that concrete processing condition are Sodium Selenite and glucose 1: 2～1: 4, pack in the teflon-lined stainless steel cauldron, add distilled water and form colourless transparent solution, reactor is tightened in sealing, under 150-200 ℃ of condition, react 8-12h, naturally cooling.Throw out takes out after washing in vacuum drying oven in 50-70 ℃ of dry 3-6h.
2, need not the method that template liquid phase reduction prepares elemental selenium nanotube by claim 1 is described, it is characterized in that adding and form colourless transparent solution behind the distilled water and account for stainless steel cauldron volume 80%.
3, describedly need not the method that template liquid phase reduction prepares elemental selenium nanotube by claim 1 or 2, it is characterized in that stainless steel cauldron is is liner with tetrafluoroethylene.
4, need not the method that template liquid phase reduction prepares elemental selenium nanotube by claim 1 is described, it is characterized in that it is to use earlier distilled water that throw out takes out washing, after use ethanol.
5, describedly need not the method that the template liquid phase reduction legal system is equipped with elemental selenium nanotube by claim 1,2 or 4, it is characterized in that elemental selenium nano external diameter of pipe 200-300nm, internal diameter 150-200nm, length-to-diameter ratio can reach 15-40.
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|---|---|---|---|
| CN 200510024071 CN1289387C (en) | 2005-02-25 | 2005-02-25 | Non-template liquid phase reduction method for preparing elemental selenium nanotube |
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| CN1289387C CN1289387C (en) | 2006-12-13 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885475A (en) * | 2010-07-26 | 2010-11-17 | 南京理工大学 | A kind of synthetic method of elemental selenium nanoribbon |
| WO2011001246A3 (en) * | 2009-06-29 | 2011-05-19 | Pacific Rare Specialty Metals & Chemicals, Inc. | A process for the recovery of selenium from minerals and/or acidic solutions |
| US8268285B2 (en) | 2009-06-29 | 2012-09-18 | Pacific Rare Specialty Metals and Chemicals, Inc. | Process for the recovery of tellurium from minerals and/or acidic solutions |
| CN102730651A (en) * | 2012-07-08 | 2012-10-17 | 桂林理工大学 | Solvothermal method for regulating morphology of elemental nano-selenium |
| CN103302304A (en) * | 2013-06-07 | 2013-09-18 | 上海交通大学 | Preparation method of nickel or nickel alloy nanotube |
| CN103420344A (en) * | 2012-05-14 | 2013-12-04 | 武汉理工大学 | Preparation method for nano-selenium |
| CN108793099A (en) * | 2018-07-17 | 2018-11-13 | 武汉理工大学 | A kind of radial selenium nanotube and preparation method thereof |
| CN109911869A (en) * | 2019-03-12 | 2019-06-21 | 湖南工业大学 | A method for reducing, decomposing, cleaning and extracting selenium from iron selenate slag |
-
2005
- 2005-02-25 CN CN 200510024071 patent/CN1289387C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8268285B2 (en) | 2009-06-29 | 2012-09-18 | Pacific Rare Specialty Metals and Chemicals, Inc. | Process for the recovery of tellurium from minerals and/or acidic solutions |
| WO2011001246A3 (en) * | 2009-06-29 | 2011-05-19 | Pacific Rare Specialty Metals & Chemicals, Inc. | A process for the recovery of selenium from minerals and/or acidic solutions |
| US8092776B2 (en) | 2009-06-29 | 2012-01-10 | Pacific Rare Specialty Metals and Chemicals, Inc. | Process for the recovery of selenium from minerals and/or acidic solutions |
| US8361431B2 (en) | 2009-06-29 | 2013-01-29 | Pacific Rare Specialty Metals & Chemicals, Inc. | Process for the recovery of selenium from minerals and/or acidic solutions |
| CN101885475B (en) * | 2010-07-26 | 2012-05-16 | 南京理工大学 | Method for synthesizing elemental selenium nano belt |
| CN101885475A (en) * | 2010-07-26 | 2010-11-17 | 南京理工大学 | A kind of synthetic method of elemental selenium nanoribbon |
| CN103420344A (en) * | 2012-05-14 | 2013-12-04 | 武汉理工大学 | Preparation method for nano-selenium |
| CN103420344B (en) * | 2012-05-14 | 2015-07-22 | 武汉理工大学 | Preparation method for nano-selenium |
| CN102730651A (en) * | 2012-07-08 | 2012-10-17 | 桂林理工大学 | Solvothermal method for regulating morphology of elemental nano-selenium |
| CN103302304A (en) * | 2013-06-07 | 2013-09-18 | 上海交通大学 | Preparation method of nickel or nickel alloy nanotube |
| CN103302304B (en) * | 2013-06-07 | 2015-07-08 | 上海交通大学 | Preparation method of nickel or nickel alloy nanotube |
| CN108793099A (en) * | 2018-07-17 | 2018-11-13 | 武汉理工大学 | A kind of radial selenium nanotube and preparation method thereof |
| CN108793099B (en) * | 2018-07-17 | 2021-12-07 | 武汉理工大学 | Radial selenium nanotube and preparation method thereof |
| CN109911869A (en) * | 2019-03-12 | 2019-06-21 | 湖南工业大学 | A method for reducing, decomposing, cleaning and extracting selenium from iron selenate slag |
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| CN1289387C (en) | 2006-12-13 |
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