CN103991900B - A kind of preparation method of titanium disulfide nanometer sheet of high-purity and high-crystallinity - Google Patents
A kind of preparation method of titanium disulfide nanometer sheet of high-purity and high-crystallinity Download PDFInfo
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- CN103991900B CN103991900B CN201410232104.5A CN201410232104A CN103991900B CN 103991900 B CN103991900 B CN 103991900B CN 201410232104 A CN201410232104 A CN 201410232104A CN 103991900 B CN103991900 B CN 103991900B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000005864 Sulphur Substances 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 19
- 239000013543 active substance Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 13
- 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 12
- -1 octadecylene Chemical group 0.000 claims description 12
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000002513 implantation Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 abstract description 11
- 239000000084 colloidal system Substances 0.000 abstract description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 abstract description 2
- 238000009830 intercalation Methods 0.000 abstract description 2
- 230000002687 intercalation Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910004338 Ti-S Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000366 colloid method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention is a kind of preparation method of titanium disulfide nanometer sheet of high-purity and high-crystallinity.Stratiform TiS
2nanometer sheet has good electronic mobility and good intercalation, can be used for cathode material for lithium ion battery and ultracapacitor etc.The present invention adopts two-step approach liquid phase colloid synthetic technology, with the high-purity and high-crystallinity TiS of titanium source, sulphur source, tensio-active agent Reactive Synthesis hexagonal system
2nanometer sheet.First titanium source and tensio-active agent are mixed at a certain temperature; Then inject sulphur source, be warmed up to assigned temperature and be incubated for some time, thus generate the high-purity and high-crystallinity TiS of different thickness
2nanometer sheet.Reaction conditions of the present invention is gentle, and preparation technology is simple, easily control, reproducible.The TiS that the present invention obtains
2nanometer sheet size and pattern is homogeneous, size is controlled, good crystallinity, purity are high.
Description
Technical field
The present invention relates to nano material technology, particularly a kind of hexagonal system titanium disulfide (TiS that can be applicable to photodetector, lithium ion battery and ultracapacitor
2) preparation method of nanometer sheet.
Background technology
Titanium disulfide (TiS
2) be typical transition metal two chalkogenide, its rock steady structure is the octahedral coordination structure of 1T type, and this is a kind of six side close heap CdI
2structure, six side's basal planes are high anisotropy perpendicular to basal plane; Six the S atomic buildings octahedron closed in layer, Ti is positioned at octahedra center, forms a TiS
6octahedron, they are with covalent bonds; Form " sandwich " laminate structure of S-Ti-S in c-axis direction, connected by very weak Van der Waals force between layers.
The TiS of laminate structure
2owing to having the larger Van der Waals layer in gap, other molecular atoms is easy to just can be intercalation into wherein, due to Li
+can be easier to pass in and out TiS
2van der Waals layer, therefore TiS
2be widely studied as cathode material for lithium ion battery.Meanwhile, the TiS of nanoscale
2there is surface plasma resonance phenomenon, can be used for surface-enhanced Raman signals and detect, in biomedicine, have good application prospect as sensitive chemistry and biosensing device.
At present, TiS
2preparation method mainly comprise solid sintering technology and liquid phase colloid method.The titanium disulfide block materials that the main preparation scale of solid phase method is very large, and liquid phase colloid synthesis method can prepare titanium disulfide nano material.Document (Well-Defined Colloidal 2-D Layered Transition-Metal Chalcogenide Nanocrystals via Generalized Synthetic protocols, J. Am. Chem. Soc. 2012,134,18233-18236) adopt the method that liquid phase colloid synthesizes, with TiCl
4, oleyl amine and CS
2for reaction reagent has prepared undersized TiS
2nanocrystalline, and size range regulation and control are littlely only 40nm to 150nm, the TiS of preparation
2nanocrystalline crystallinity is bad, purity is not high, does not have obvious two-dimensional sheet material feature.Document (Synthetic Strategy and Structural and Optical Characterization of Thin Highly Crystalline Titanium Disulfide Nanosheets, J. Phys. Chem. Lett. 2012,3,1554 1558) liquid phase method is adopted, with sulphur powder, TiCl
4with oleyl amine be starting material reaction prepare the larger TiS of area
2nanometer sheet, but nanometer sheet size prepared by this method and pattern heterogeneity, size is uncontrollable, and purity is not high, containing obvious needle-like TiO
2impurity.At present, also do not exist in existing liquid phase synthesis techniques and can prepare size and pattern is homogeneous, good dispersity, size can regulate and control, the TiS of degree of crystallinity and very high purity on a large scale
2the technology of preparing of nanometer sheet.
Summary of the invention
The object of this invention is to provide a kind of preparation method of titanium disulfide nanometer sheet of high-purity and high-crystallinity.
The technical solution realizing the object of the invention is: a kind of preparation method of titanium disulfide nanometer sheet of high-purity and high-crystallinity, adopt the liquid phase colloid synthetic technology of two-step approach, the first step adds titanium source and tensio-active agent in container, is heated to certain temperature and is uniformly mixed; Second step injects sulphur source, is warmed up to temperature of reaction and is incubated for some time.By changing reaction times, temperature of reaction, reactant concn, obtain the TiS of different size thickness
2nanometer sheet, specifically comprises the following steps:
Step 1, in reaction vessel, add titanium source and tensio-active agent, mix and blend; The titanium source added is TiCl
4, tensio-active agent is the mixture of oleyl amine and octadecylene, and the ratio of the amount of substance of oleyl amine and octadecylene is 1:1 ~ 1:6, and the amount of substance of titanium source and tensio-active agent is than being 1:5 ~ 1:20.
Step 2, be warming up to design temperature, bleed with mechanical pump, then pass into protective gas, then bleed, so move in circles, to remove impurity, finally pass into protective gas thus ensure that reaction system is inert environments; Described design temperature is 100 ~ 140 DEG C, and protective gas is Ar gas, N
2gas or the mixed gas of the two, the number of times moved in circles is 10 ~ 15 times.
Step 3, reaction system is continued to be warmed up to assigned temperature, stir afterwards, reactant is mixed; Assigned temperature is 180 ~ 300 DEG C, and churning time is 20 ~ 30min.
Step 4, in reaction vessel, inject sulphur source, be then warmed up to temperature of reaction, and be incubated; Sulphur source is CS
2or sulphur powder, implantation temperature is 180 ~ 300 DEG C, and the amount of substance in titanium source and sulphur source is than being 1:2 ~ 1:15, and temperature of reaction is 260 ~ 320 DEG C, and soaking time is 60min ~ 180min.
After step 5, reaction terminate, remove thermal source, cool to room temperature;
Step 6, add organic solvent in the product, by centrifugal, give up supernatant liquor, be precipitated, described precipitation is TiS
2nanometer sheet.The organic solvent added is the mixture of normal hexane and ethanol or the mixture of toluene and methyl alcohol, and centrifugal rotational speed is 8000 ~ 10000r/min, and centrifugation time is 2 ~ 4min, and centrifugal number of times is 2 ~ 4 times.
Compared with prior art, its remarkable advantage is in the present invention: 1) reaction temperature of the present invention and, temperature of reaction can be low to moderate 260 DEG C, and preparation technology is simple, easily control, reproducible; 2) present invention adds new tensio-active agent octadecylene, increase reaction system total amount, temperature fluctuation is little, be heated evenly; Reactant dispersion evenly, do not reunite; Octadecylene, as protectiveness liquid, makes reaction environment in reaction system purer; 3) TiS that obtains of the present invention
2nanometer sheet size and pattern is homogeneous, size can regulate and control on a large scale, good crystallinity, purity are high.
Accompanying drawing explanation
Fig. 1 is product TiS prepared by the embodiment of the present invention 1
2the SEM figure of nanometer sheet.
Fig. 2 is product TiS prepared by the embodiment of the present invention 1
2the TEM figure of nanometer sheet.
Fig. 3 is product TiS prepared by the embodiment of the present invention 1
2the XRD figure of nanometer sheet.
Fig. 4 is product TiS prepared by the embodiment of the present invention 2
2the TEM figure of nanometer sheet.
Fig. 5 is product TiS prepared by the embodiment of the present invention 2
2the XRD figure of nanometer sheet.
Fig. 6 is product TiS prepared by the embodiment of the present invention 3
2the TEM figure of nanometer sheet.
Fig. 7 is product TiS prepared by the embodiment of the present invention 3
2the XRD figure of nanometer sheet.
concrete real mode
The preparation method of the titanium disulfide nanometer sheet of a kind of high-purity and high-crystallinity of the present invention, adopt the liquid phase colloid synthetic technology of two-step approach, the method utilizing colloid to synthesize prepares size and pattern is homogeneous, good dispersity, size can regulate and control on a large scale, the TiS of degree of crystallinity and very high purity
2nanometer sheet; The first step adds titanium source and tensio-active agent in container, is heated to certain temperature and is uniformly mixed.Second step injects sulphur source, is warmed up to temperature of reaction and is incubated for some time.By changing reaction times, temperature of reaction, reactant concn, obtain the TiS of different size thickness
2nanometer sheet, specifically comprises the following steps:
Step 1, in reaction vessel, add titanium source and tensio-active agent, mix and blend; The described titanium source added is TiCl
4, tensio-active agent is the mixture of oleyl amine and octadecylene, and the ratio of the amount of substance of oleyl amine and octadecylene is 1:1 ~ 1:6, and the amount of substance of titanium source and tensio-active agent is than being 1:5 ~ 1:20.
Step 2, be warming up to design temperature, bleed with mechanical pump, then pass into protective gas, then bleed, so move in circles, to remove impurity, finally pass into protective gas thus ensure that reaction system is inert environments; Described design temperature is 100 ~ 140 DEG C, and protective gas is Ar gas, N
2gas or the mixed gas of the two, the number of times moved in circles is 10 ~ 15 times.
Step 3, reaction system is continued to be warmed up to assigned temperature, stir afterwards, reactant is mixed; Described assigned temperature is 180 ~ 300 DEG C, and churning time is 20 ~ 30min.
Step 4, in reaction vessel, inject sulphur source, be then warmed up to temperature of reaction, and be incubated; Described sulphur source is CS
2or sulphur powder, implantation temperature is 180 ~ 300 DEG C, and the amount of substance in titanium source and sulphur source is than being 1:2 ~ 1:15, and temperature of reaction is 260 ~ 320 DEG C, and soaking time is 60min ~ 180min.
After step 5, reaction terminate, remove thermal source, cool to room temperature;
Step 6, add organic solvent in the product, by centrifugal, give up supernatant liquor, be precipitated, described precipitation is TiS
2nanometer sheet.The described organic solvent added is the mixture of normal hexane and ethanol or the mixture of toluene and methyl alcohol, and centrifugal rotational speed is 8000 ~ 10000r/min, and centrifugation time is 2 ~ 4min, and centrifugal number of times is 2 ~ 4 times.
embodiment 1
Adopt the liquid phase colloid synthetic method of two-step approach, the first step adds titanium source and tensio-active agent in container, is heated to certain temperature and is uniformly mixed.Second step injects sulphur source, is warmed up to temperature of reaction and is incubated for some time, prepared size and homogeneous, the highly purified TiS of pattern
2nanometer sheet, concrete steps are as follows:
Step 1, in 100ml four-hole boiling flask, add 0.11ml TiCl
4, 3.7ml oleyl amine, 15ml octadecylene, mix and blend.
Step 2, be warming up to 100 DEG C, bleed 40s with mechanical pump, pass into Ar gas, 10 times so repeatedly, to remove impurity.
Step 3, continue to be warmed up to 180 DEG C, stir 30min, reactant is mixed.
Step 4, in container, inject CS
2, be raised to 300 DEG C, insulation 3h.
After step 5, reaction terminate, take away thermal source, be cooled fast to room temperature.
Step 6, add excessive propyl carbinol, to be centrifugally precipitated.The mixed solution of precipitation normal hexane and ethanol is washed 2 times, centrifugal rotational speed 9000r/min, time 3min.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 1, Figure 2, Figure 3 shows.Result shows the processing parameter according to embodiment 1, can obtain the hexagonal system TiS that pattern is even, size is homogeneous, size is about 250nm
2nanometer sheet; As can be seen from XRD, all diffraction peaks are TiS
2characteristic peak, have no any dephasign, the nanometer sheet prepared has high crystallinity and purity.
embodiment 2
Adopt the liquid phase colloid synthetic method of two-step approach, the first step adds titanium source and tensio-active agent in container, is heated to certain temperature and is uniformly mixed.Second step injects sulphur source, is warmed up to temperature of reaction and is incubated for some time, prepared highly purified TiS
2nanometer sheet, concrete steps are as follows:
Step 1, in 100ml four-hole boiling flask, add 0.11ml TiCl
4, 3.7ml oleyl amine, 10ml octadecylene, mix and blend.
Step 2, be warming up to 120 DEG C, bleed 40s with mechanical pump, pass into Ar gas, 15 times so repeatedly, to remove impurity.
Step 3, continue to be warmed up to 260 DEG C, stir 20min, reactant is mixed.
Step 4, in container, inject CS
2, be raised to 270 DEG C, insulation 1h.
After step 5, reaction terminate, take away thermal source, be cooled fast to room temperature.
Step 6, add excessive propyl carbinol, to be centrifugally precipitated.The mixed solution of precipitation toluene and methyl alcohol is washed 2 times, centrifugal rotational speed 8000r/min, time 4min.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 4, Figure 5.Result shows the processing parameter according to embodiment 2, can obtain the hexagonal system TiS that pattern is even, size is homogeneous, size is about 800nm
2nanometer sheet; As can be seen from XRD, all diffraction peaks are TiS
2characteristic peak, have no any dephasign, the nanometer sheet prepared has high crystallinity and purity.
embodiment 3
Adopt the liquid phase colloid synthetic method of two-step approach, the first step adds titanium source and tensio-active agent in container, is heated to certain temperature and is uniformly mixed.Second step injects sulphur source, is warmed up to temperature of reaction and is incubated for some time, prepared highly purified TiS
2nanometer sheet, concrete steps are as follows:
Step 1, in 100ml four-hole boiling flask, add 0.11ml TiCl
4, 3.7ml oleyl amine, 20ml octadecylene, mix and blend.
Step 2, be warming up to 140 DEG C, bleed 40s with mechanical pump, pass into Ar gas, 12 times so repeatedly, to remove impurity.
Step 3, continue to be warmed up to 300 DEG C, stir 20min, reactant is mixed.
Step 4, in container, inject CS
2, be raised to 310 DEG C, insulation 3h.
After step 5, reaction terminate, take away thermal source, be cooled fast to room temperature.
Step 6, add excessive propyl carbinol, to be centrifugally precipitated.The mixed solution of precipitation normal hexane and ethanol is washed 2 times, centrifugal rotational speed 10000r/min, time 2min.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 6, Figure 7.Result shows the processing parameter according to embodiment 3, can obtain the hexagonal system TiS that pattern is even, size is homogeneous, size is about 20nm
2nanometer sheet; As can be seen from XRD, all diffraction peaks are TiS
2characteristic peak, have no any dephasign, the nanometer sheet prepared has high crystallinity and purity.
Claims (2)
1. a preparation method for the titanium disulfide nanometer sheet of high-purity and high-crystallinity, is characterized in that, specifically comprise the following steps:
Step 1, in reaction vessel, add titanium source and tensio-active agent, mix and blend, titanium source is TiCl
4, tensio-active agent is the mixture of oleyl amine and octadecylene, and the ratio of the amount of substance of oleyl amine and octadecylene is 1:1 ~ 1:6, and the amount of substance of titanium source and tensio-active agent is than being 1:5 ~ 1:20;
Step 2, be warming up to design temperature, bleed with mechanical pump, then pass into protective gas; bleed again, so move in circles, to remove impurity; finally pass into protective gas thus ensure that reaction system is inert environments, design temperature is 100 ~ 140 DEG C, and protective gas is Ar gas, N
2gas or the mixed gas of the two, the number of times moved in circles is 10 ~ 15 times;
Step 3, reaction system continued to be warmed up to assigned temperature, stir afterwards, reactant is mixed, assigned temperature is 180 ~ 300 DEG C, and churning time is 20 ~ 30min;
Step 4, in reaction vessel, inject sulphur source, be then warmed up to temperature of reaction, and be incubated, sulphur source is CS
2or sulphur powder, implantation temperature is 180 ~ 300 DEG C, and the amount of substance in titanium source and sulphur source is than being 1:2 ~ 1:15, and temperature of reaction is 260 ~ 320 DEG C, and soaking time is 60min ~ 180min;
After step 5, reaction terminate, remove thermal source, cool to room temperature;
Step 6, add organic solvent in the product, by centrifugal, give up supernatant liquor, be precipitated, described precipitation is TiS
2nanometer sheet.
2. the preparation method of the titanium disulfide nanometer sheet of high-purity and high-crystallinity according to claim 1, it is characterized in that, the organic solvent that step 6 adds is the mixture of normal hexane and ethanol or the mixture of toluene and methyl alcohol, centrifugal rotational speed is 8000 ~ 10000r/min, centrifugation time is 2 ~ 4min, and centrifugal number of times is 2 ~ 4 times.
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| CN108573813B (en) * | 2018-05-18 | 2019-08-27 | 河南大学 | A kind of preparation method of two-dimensional nano titanium disulfide and its membrane electrode |
| CN112023869B (en) * | 2020-07-31 | 2022-09-02 | 盐城工学院 | Method for preparing mesoporous titanium disulfide adsorbent and application |
| CN114259560B (en) * | 2020-09-25 | 2023-05-02 | 苏州大学 | Doped metal sulfide and preparation and application thereof |
| CN115624979B (en) * | 2022-10-19 | 2024-05-03 | 南京大学 | Application of modified black titanium dioxide in degradation of antibiotic wastewater |
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|---|---|---|---|---|
| US4137297A (en) * | 1977-12-01 | 1979-01-30 | Laporte Industries Limited | Process for the production of titanium disulphide |
| JPH0283215A (en) * | 1988-09-19 | 1990-03-23 | Furukawa Co Ltd | Production of titanium disulfide |
| CN101468793A (en) * | 2007-12-26 | 2009-07-01 | 三星电机株式会社 | Method for producing nano particle with lamination structure |
| CN102181495A (en) * | 2011-02-28 | 2011-09-14 | 北京理工大学 | Preparation method of nano-metal sulfide |
-
2014
- 2014-05-28 CN CN201410232104.5A patent/CN103991900B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4137297A (en) * | 1977-12-01 | 1979-01-30 | Laporte Industries Limited | Process for the production of titanium disulphide |
| JPH0283215A (en) * | 1988-09-19 | 1990-03-23 | Furukawa Co Ltd | Production of titanium disulfide |
| CN101468793A (en) * | 2007-12-26 | 2009-07-01 | 三星电机株式会社 | Method for producing nano particle with lamination structure |
| CN102181495A (en) * | 2011-02-28 | 2011-09-14 | 北京理工大学 | Preparation method of nano-metal sulfide |
Non-Patent Citations (1)
| Title |
|---|
| Liquid-Phase Synthesis of Flower-like and Flake-like Titanium Disulfide Nanostructures;Sujay Prabakar et al.;《Chemistry of Materials》;20090428;第21卷(第8期);第1725-1726页实验部分 * |
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