CN102945960B - Template induction method for preparing lithium iron phosphate nano particles - Google Patents
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- CN102945960B CN102945960B CN201210479256.6A CN201210479256A CN102945960B CN 102945960 B CN102945960 B CN 102945960B CN 201210479256 A CN201210479256 A CN 201210479256A CN 102945960 B CN102945960 B CN 102945960B
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Abstract
The invention discloses a template induction method for preparing lithium iron phosphate nano particles. The method comprises the steps of preprocessing silicon wafers to obtain hydroxylation silicon substrates; preparing 3-aminopropyl-trimethoxy silane (APTMS) membrane templates; subjecting the APTMS membrane template surfaces to amino in situ phosphorylation; and preparing the lithium iron phosphate nano particles. According to the template induction method for preparing lithium iron phosphate nano particles, the prepared lithium iron phosphate nano particles are high in purity and uniform in particle diameter. The method has the advantages of being abundant in material source, low in preparation process energy consumption, small in prepared nano particle size, non-toxic and the like.
Description
Technical field
The present invention relates to a kind of masterplate revulsion and prepare the method for LiFePO 4 nano particle, belong to battery material field.
Background technology
Along with becoming increasingly conspicuous of the energy and environmental problem, clean energy resource receives much attention, and this has higher requirement to secondary power supply.Lithium ion battery, as the high performance secondary green battery of one, is widely used in various portable type electronic products and communication tool.Olivine-type anode material for lithium-ion batteries LiFePO
4have that raw material resources are abundant, inexpensive, nontoxic, the advantage such as environmental friendliness, theoretical capacity are high, thermal stability and good cycle, be the first-selected positive electrode of lithium ion battery.
But the diffusion velocity of lithium ion in this electrode material is slow, LiFePO
4poor electric conductivity, the utilance of material is low, the rate charge-discharge poor performance of electrode has restricted the output of the large multiplying power of ferrousphosphate lithium material.At LiFePO
4charge and discharge process in, due to PO in crystal
4 3-limit Li
+mobile space, make Li
+embedding, de-process in material only have two-dimentional mobility, therefore LiFePO
4electronics, ionic conductivity all lower, under the condition of heavy-current discharge, have larger capacitance loss.For Li
+at LiFePO
4in embedding, off line reason, A. S. Andersson has proposed two kinds of possible charging and recharging model-radiation models (Radial Model) and mosaic model (Mosaic Model).Most of scientific research personnel think that two kinds of models exist simultaneously.From Li
+embedding off line reason set out, at present to LiFePO
4research work mainly launch from two aspects: on the one hand, control grain growth by different approaches, prepare uniform particle diameter, tiny material, the ionic conduction performance of strengthening material; On the other hand, on the basis of Optimization Technology by crystalline phase is adulterated, the means such as amorphous phase doping improve material electronics, ionic conductivity simultaneously.
Therefore, LiFePO
4the nanometer of material makes its particle size reduce to a great extent, shortens the evolving path of lithium ion, improves LiFePO
4the chemical property of electrode.By preparing the LiFePO 4 of nano-scale, reducing its particle agglomeration is to improve LIB entirety chemical property, improves one of effective ways of the large high rate performance of ferrousphosphate lithium material.
Recent domestic has been reported in a large number about distinct methods and has been synthesized, improved LiFePO
4material.The less 1-100 μ m that is distributed in of particle size that sol-gel process and emulsification seasoning are synthetic, but due to calcination process make particle agglomeration or sintering degree larger, increased lithium ion in intragranular diffusion length, the conductivity of material and large multiplying power output performance do not have substantial improvement; Hydro thermal method is with FeSO
4, H
3pO
4, LiOH is in molar ratio for 1:1:3 synthesizes the LiFePO of granularity at 50-100nm
4particle, when adding its size after surfactant softex kw (CTAB) can drop to 50nm, but hydro thermal method needs high temperature high voltage resistant equipment, and industrialization difficulty is larger.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for a kind of template-mediated legal system for LiFePO 4 nano particle for above-mentioned prior art, and dimensional controllability is high, prepared LiFePO 4 nano particle diameter homogeneous, and size is little.
The present invention solves the problems of the technologies described above adopted technical scheme:
Template-mediated legal system is for the method for LiFePO 4 nano particle, and it comprises the following steps:
1) preliminary treatment of silicon chip: by silicon chip successively Ultrasonic Cleaning 5 ~ 15min in acetone, ultra-pure water, then put into Piranha solution and soak 30-60min in 60 ~ 100 DEG C, take out silicon chip and rinse with ultra-pure water, then dry up and obtain hydroxylated silicon-based substrates with nitrogen;
2) preparation of 3-aminopropyl-trimethoxy silane (APTMS) thin-film template: the ethanolic solution that the hydroxylated silicon-based substrates that step 1) is obtained is put into APTMS soaks 1-2 hour, after taking-up, rinse, then dry up and obtain APTMS self-assembled film with nitrogen with ethanol, ultra-pure water successively;
3) APTMS self-assembled film surface amino groups original position phosphorylation: by step 2) the APTMS self-assembled film that obtains immerses containing phosphorous oxychloride and 2,3, in the acetonitrile solution of 5-trimethylpyridine, room temperature reaction 20-90 minute, take out with ultra-pure water flushing, dry up the APTMS self-assembled film that obtains phosphorylation with nitrogen;
4) preparation of LiFePO 4 nano particle: the APTMS self-assembled film of the phosphorylation that step 3) is obtained immerses in the ultra-pure water solution containing ferrous salt, phosphate, lithium salts and reacts 5 minutes-60 minutes, then take out with ultra-pure water flushing, nitrogen dries up and makes LiFePO 4 nano particle.
Press such scheme, described silicon chip is the bulk of (1 ~ 2) cm × (1 ~ 2) cm × 0.5mm.
Press such scheme, in described Piranha solution, the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 4:1.
Press such scheme, in the ethanolic solution of described APTMS, APTMS volumetric concentration is 0.1%-2%.
Press such scheme, in acetonitrile solution, the mol ratio of phosphorous oxychloride and 2,3,5-trimethylpyridine is 1:1 described in described step 3), and triclosan oxidation phosphorus concentration is 0.05-0.8mol/L.
Press such scheme, in the solution of ultra-pure water described in step 4), the mol ratio of ferrous salt, phosphate, lithium salts is 1 ~ 2:1 ~ 2:3 ~ 6, and ferrous salt concentration is 0.001-0.1mol/L.
Press such scheme, ferrous salt, phosphate, lithium salts are respectively ferrous sulfate heptahydrate, diammonium hydrogen phosphate, Lithium hydroxide monohydrate described in described step 4).
Press such scheme, it is 20 ~ 50 DEG C that the APTMS self-assembled film of the phosphorylation described in step 4) immerses the temperature of reacting in the ultra-pure water aqueous solution containing ferrous salt, phosphate, lithium salts.
Compared with prior art, beneficial effect of the present invention is:
1) compared with traditional preparation method, the prepared LiFePO 4 nano-particles size controllability of the present invention is high, the scale ratio of the LiFePO 4 nano particle that AFM 3 dimensional drawing result indicating template revulsion makes is more even, and the degree of crystallization of particle and reunion are less; Uniform particle diameter, size is little, detects to such an extent that average grain diameter is 10nm through AFM;
2) the present invention adopts template-mediated method, its principle is to utilize chemisorbed or the chemical reaction of solid-liquid interface, form chemical bond by surface of solids adsorption activity material and connect, tend to the ordered molecular film that molecular recognition is high closely, the LiFePO 4 nano particle product purity that preparation obtains is high;
3) preparation method's reaction temperature of the present invention is no more than 100 DEG C, without roasting and mechanical treatment, reaction temperature and, energy consumption is little;
4) raw material sources are abundant: preparation LiFePO
4the raw material of nano particle is basic industrial chemicals, is easy to obtain;
5) LiFePO preparing
4nano particle good combination property, Stability Analysis of Structures, security performance are good, nontoxic, non-secondary pollution.
Brief description of the drawings
Fig. 1 is the contact angle figure of the hydroxylated silicon-based substrates for preparing of the embodiment of the present invention 1;
Fig. 2 is the contact angle figure of the APTMS self-assembled film for preparing of the embodiment of the present invention 1;
Fig. 3 is the APTMS self-assembled film infrared spectrogram that the embodiment of the present invention 1 prepares;
Fig. 4 is the APTMS self-assembled film AFM figure that the embodiment of the present invention 1 prepares;
Fig. 5 is the surface contact angle figure of the APTMS self-assembled film of the phosphorylation for preparing of the embodiment of the present invention 2;
Fig. 6 is the infrared spectrogram of the APTMS self-assembled film of the phosphorylation for preparing of the embodiment of the present invention 2;
Fig. 7 is the atomic force microscope figure of the APTMS self-assembled film of the phosphorylation for preparing of the embodiment of the present invention 2;
Fig. 8 is the atomic force microscope figure of the lithium iron phosphate nano particle prepared of the embodiment of the present invention 3;
Fig. 9 is the atomic force microscope 3 dimensional drawing of the lithium iron phosphate nano particle prepared of the embodiment of the present invention 4;
Figure 10 is the xps energy spectrum figure of the lithium iron phosphate nano particle prepared of the embodiment of the present invention 4.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but the present invention is not only confined to the following examples.
In following embodiment, 3-aminopropyl-trimethoxy silane (APTMS) used is that Sigma aldrich company produces, acetone is that the huge chemical reagent factory in Dongli District, Tianjin is produced, hydrogen peroxide is that Tianjin great Mao chemical reagent factory is produced, the concentrated sulfuric acid is the production of Kaifeng chemical reagent work of Dong great Chemical Co., Ltd., 2,3,5-trimethylpyridine, phosphorous oxychloride, acetonitrile, ferrous sulfate heptahydrate, lithium hydroxide, diammonium hydrogen phosphate are that Chemical Reagent Co., Ltd., Sinopharm Group produces.It is pure that above medicine is analysis.Ultrapure resistivity of water used in experiment is not less than 18 MWcm.
Described in following embodiment, in Piranha solution, the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 4:1.
Embodiment 1
The preliminary treatment of silicon chip: the successively Ultrasonic Cleaning 5min in acetone, ultra-pure water of bulk silicon that will cut into 1cm × 1cm × 0.5mm, then put into Piranha solution and soak 30min in 60 DEG C, take out silicon chip and rinse with ultra-pure water, then dry up and obtain hydroxylated silicon-based substrates with nitrogen;
The preparation of 3-aminopropyl-trimethoxy silane (APTMS) thin-film template: the ethanolic solution that the hydroxylated silicon-based substrates obtaining through above-mentioned steps is put into volumetric concentration 0.2%APTMS soaks and carries out self assembly for 1 hour, after taking-up, rinse, then dry up and obtain APTMS self-assembled film with nitrogen with ethanol, ultra-pure water successively;
Accompanying drawing 1 is the contact angle figure of the hydroxylated silicon-based substrates for preparing of embodiment 1, almost drawout completely of water droplet, and contact angle is very little.
Accompanying drawing 2 is contact angle figure of the APTMS self-assembled film for preparing of embodiment 1, and contact angle increases, and hydrophobicity obviously strengthens.
Accompanying drawing 3 is APTMS self-assembled film infrared spectrograms that embodiment 1 prepares, 1617 cm
-1belong to the interior flexural vibrations absworption peak of N=H, 1107 cm
-1for the characteristic absorption peak of C-N, 817 cm
-1for the outside sweep vibration of N-H, 740 cm
-1belong to the characteristic absorption peak of Si-C, position and the bibliographical information of each diffraction maximum are basically identical, show that APTMS is successfully assembled into hydroxylated silicon-based substrates surface.
Accompanying drawing 4 is APTMS self-assembled film AFM figure prepared by embodiment 1, can find out the very even compact of surface of APTMS self-assembled film.
embodiment 2
1) preliminary treatment of silicon chip: the successively Ultrasonic Cleaning 15min in acetone, ultra-pure water of silicon chip that will cut into 2cm × 2cm × 0.5mm, then put into Piranha solution and soak 60min in 100 DEG C, take out silicon chip and rinse with ultra-pure water, then dry up and obtain hydroxylated silicon-based substrates with nitrogen;
2) preparation of 3-aminopropyl-trimethoxy silane (APTMS) thin-film template: the hydroxylated silicon-based substrates that step 1) is obtained is put into 2%(volume fraction) ethanolic solution of APTMS soaks and within 1-2 hour, carries out self assembly, after taking-up, rinse, then dry up and obtain APTMS self-assembled film with nitrogen with ethanol, ultra-pure water successively;
3) APTMS self-assembled film surface amino groups original position phosphorylation: by step 2) the APTMS self-assembled film that obtains immerses containing phosphorous oxychloride, 2,3, in the acetonitrile solution of 5-trimethylpyridine, wherein the mol ratio of phosphorous oxychloride and 2,3,5-trimethylpyridine is 1:1, triclosan oxidation phosphorus concentration is: 0.1mol/L, after room temperature reaction 90 minutes, take out with ultra-pure water flushing, dry up the APTMS self-assembled film that obtains phosphorylation with nitrogen;
Accompanying drawing 5 is surface contact angle figure of the APTMS self-assembled film of the phosphorylation prepared of embodiment 2, film surface-NH
2group is gradually by-PO (OH)
2after group replaces, hydrophily strengthens, and drop can soak film surface preferably.
Accompanying drawing 6 is infrared spectrograms of the APTMS self-assembled film of the phosphorylation prepared of embodiment 2,1260cm
-1belong to the stretching vibration of P=O; 1048cm
-1belong to the antisymmetric stretching vibration of P-O; 950cm
-1, 653cm
-1belong to the symmetrical stretching vibration of P-O; 577 cm
-1for the flexural vibrations of O=P-O antisymmetry; 546cm
-1for the vibration of O=P-O symmetric curvature; APTMS self-assembled film surface-NH
2group is all by-PO (OH)
2group replaces.
Accompanying drawing 7 is AFM figure of the APTMS self-assembled film of the phosphorylation prepared of embodiment 2, and roughness further reduces, and surface becomes even compact more.
embodiment 3
Template-mediated legal system is for the method for LiFePO 4 nano particle, and it comprises the following steps:
1) preliminary treatment of silicon chip: the silicon chip that is 1cm × 1cm × 0.5mm by size is Ultrasonic Cleaning 10min in acetone, ultra-pure water successively, then put into Piranha solution and soak 45min in 80 DEG C, take out silicon chip and rinse with ultra-pure water, then dry up and obtain hydroxylated silicon-based substrates with nitrogen;
2) preparation of 3-aminopropyl-trimethoxy silane (APTMS) thin-film template: the hydroxylated silicon-based substrates that step 1) is obtained is put into 0.5%(volume fraction) ethanolic solution of APTMS soaks and within 1.5 hours, carries out self assembly, after taking-up, rinse, then dry up and obtain APTMS self-assembled film with nitrogen with ethanol, ultra-pure water successively;
3) APTMS self-assembled film surface amino groups original position phosphorylation: by step 2) the APTMS self-assembled film that obtains immerses containing phosphorous oxychloride and 2,3, in the acetonitrile solution of 5-trimethylpyridine, wherein the mol ratio of phosphorous oxychloride and 2,3,5-trimethylpyridine is 1:1, triclosan oxidation phosphorus concentration is: 0.8mol/L, room temperature reaction 60 minutes, takes out with ultra-pure water flushing, dries up the APTMS self-assembled film that obtains phosphorylation with nitrogen;
4) preparation of LiFePO 4 nano particle: the APTMS self-assembled film of the phosphorylation that step 3) is obtained immerses in the ultra-pure water aqueous solution that contains ferrous sulfate heptahydrate, diammonium hydrogen phosphate, Lithium hydroxide monohydrate, in the aqueous solution, the mol ratio of ferrous sulfate heptahydrate, diammonium hydrogen phosphate, Lithium hydroxide monohydrate is 1:1:3, ferrous sulfate heptahydrate concentration is 0.003mol/L, at 35 DEG C, react 5 minutes, then take out with ultra-pure water flushing, nitrogen dries up and makes LiFePO 4 nano particle.
Accompanying drawing 8 is AFM plane graphs of the lithium iron phosphate nano particle prepared of embodiment 3, and sweep limits is 2 um × 2um, and lithium iron phosphate nano particle is evenly distributed in substrate surface, and coverage is large, and its average grain diameter is about 10 ± 1nm, and mean roughness is 1.127nm.
embodiment 4
Template-mediated legal system is for the method for LiFePO 4 nano particle, and it comprises the following steps:
1) preliminary treatment of silicon chip: the silicon chip that is 2cm × 2cm × 0.5mm by size is Ultrasonic Cleaning 15min in acetone, ultra-pure water successively, then put into Piranha solution and soak 30min in 80 DEG C, take out silicon chip and rinse with ultra-pure water, then dry up and obtain hydroxylated silicon-based substrates with nitrogen;
2) preparation of 3-aminopropyl-trimethoxy silane (APTMS) thin-film template: the hydroxylated silicon-based substrates that step 1) is obtained is put into 0.2%(volume fraction) ethanolic solution of APTMS soaks and within 1 hour, carries out self assembly, after taking-up, rinse, then dry up and obtain APTMS self-assembled film with nitrogen with ethanol, ultra-pure water successively;
3) APTMS self-assembled film surface amino groups original position phosphorylation: by step 2) the APTMS self-assembled film that obtains immerses containing phosphorous oxychloride and 2,3, in the acetonitrile solution of 5-trimethylpyridine, wherein the mol ratio of phosphorous oxychloride and 2,3,5-trimethylpyridine is 1:1, triclosan oxidation phosphorus concentration is 0.6mol/L, room temperature reaction 90 minutes, takes out with ultra-pure water flushing, dries up the APTMS self-assembled film that obtains phosphorylation with nitrogen;
4) preparation of LiFePO 4 nano particle: the APTMS self-assembled film of the phosphorylation that step 3) is obtained immerses in the ultra-pure water aqueous solution that contains ferrous sulfate heptahydrate, diammonium hydrogen phosphate, Lithium hydroxide monohydrate, in the aqueous solution, the mol ratio of ferrous sulfate heptahydrate, diammonium hydrogen phosphate, Lithium hydroxide monohydrate is 1:1:3, ferrous sulfate heptahydrate concentration is 0.01mol/L, at 45 DEG C, react 60 minutes, then take out with ultra-pure water flushing, nitrogen dries up and makes LiFePO 4 nano particle.
Accompanying drawing 9 is AFM 3 dimensional drawings of the lithium iron phosphate nano particle prepared of embodiment 4, can observe local particle and occur agglomeration, form " island " formula structure, but most of particle is not reunited.
Accompanying drawing 10 is XPS spectrum figure of the lithium iron phosphate nano particle prepared of embodiment 4.A in Figure 10, b, c, C1s in d, O1s, P2p, Fe2p(Fe2p
1/2and Fe2p
3/2) respectively corresponding combination can be 284.6eV, 531.44eV, 133.31eV, 725.80eV, 711.80eV.In Figure 10 e, Li1s peak and Fe3p peak are overlapping serious near 55.72eV, the existence that cannot draw intuitively Li1s peak and elemental lithium.
Table 1 is lithium iron phosphate nano particle samples XPS analysis initial data prepared by the embodiment of the present invention 4.
Table 2 is lithium iron phosphate nano particle samples XPS analysis initial data prepared by the embodiment of the present invention 4.
In conjunction with d, e figure and table 1 in Figure 10, if without elemental lithium, XPS detects the Fe2p that obtains and the molar content of Fe3p should equate.The molar content of the testing result Fe2p that above-mentioned hypothesis obtains as shown in table 1 and Fe3p be respectively 3.81% and 4.66%(4.66% >3.81%), obviously, peak in Figure 10 d is the overlap peak of Li1s and Fe3p, has indirectly proved the existence of elemental lithium.Therefore in Figure 10 e, carry out swarming, utilize known Fe molar content (Fe2p calculates) Fe3p peak to be separated to each element molar content after the correction that (first Fe3p peak is separated from overlap peak, the remaining peak then obtaining is Li1s peak) out obtain with the matching of Li1s peak in table 2.The Fe3p that matching obtains and Li1s are in conjunction with being respectively 55.95eV and 54.47eV.
Table 1 lithium iron phosphate nano particle XPS detects initial data
Table 2 lithium iron phosphate nano particle XPS detects swarming correction data
Claims (7)
1. template-mediated legal system, for the method for LiFePO 4 nano particle, is characterized in that it comprises the following steps:
1) preliminary treatment of silicon chip: by silicon chip successively Ultrasonic Cleaning 5 ~ 15min in acetone, ultra-pure water, then put into Piranha solution and soak 30-60min in 60 ~ 100 DEG C, take out silicon chip and rinse with ultra-pure water, then dry up and obtain hydroxylated silicon-based substrates with nitrogen;
2) preparation of APTMS thin-film template: the ethanolic solution that the hydroxylated silicon-based substrates that step 1) is obtained is put into APTMS soaks 1-2 hour, rinses, then dries up and obtain APTMS self-assembled film with nitrogen with ethanol, ultra-pure water successively after taking-up;
3) APTMS self-assembled film surface amino groups original position phosphorylation: by step 2) the APTMS self-assembled film that obtains immerses containing phosphorous oxychloride and 2,3, in the acetonitrile solution of 5-trimethylpyridine, room temperature reaction 20-90 minute, take out with ultra-pure water flushing, dry up the APTMS self-assembled film that obtains phosphorylation with nitrogen;
4) preparation of LiFePO 4 nano particle: the APTMS self-assembled film of the phosphorylation that step 3) is obtained immerses in the ultra-pure water solution containing ferrous salt, phosphate, lithium salts and reacts 5 minutes-60 minutes, then take out with ultra-pure water flushing, nitrogen dries up and makes LiFePO 4 nano particle;
In the described ultra-pure water aqueous solution, the mol ratio of ferrous salt, phosphate, lithium salts is 1 ~ 2:1 ~ 2:3 ~ 6, and ferrous salt concentration is 0.001-0.1mol/L.
2. template-mediated legal system according to claim 1 is for the method for LiFePO 4 nano particle, it is characterized in that the bulk that silicon chip is (1 ~ 2) cm × (1 ~ 2) cm × 0.5mm described in step 1).
3. template-mediated legal system according to claim 1 is for the method for LiFePO 4 nano particle, it is characterized in that described in step 1) that in Piranha solution, the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 4:1.
4. template-mediated legal system according to claim 1, for the method for LiFePO 4 nano particle, is characterized in that step 2) APTMS volumetric concentration is 0.1%-2% in the ethanolic solution of described APTMS.
5. template-mediated legal system according to claim 1 is for the method for LiFePO 4 nano particle, it is characterized in that in described step 3) phosphorous oxychloride and 2 in acetonitrile solution, the mol ratio of 3,5-trimethylpyridine is 1:1, and triclosan oxidation phosphorus concentration is 0.05-0.8mol/L.
6. template-mediated legal system according to claim 1 is for the method for LiFePO 4 nano particle, and it is 20 ~ 50 DEG C that the APTMS self-assembled film that it is characterized in that the phosphorylation described in step 4) immerses the temperature of reacting in the ultra-pure water aqueous solution containing ferrous salt, phosphate, lithium salts.
7. the method for LiFePO 4 nano particle according to the template-mediated legal system described in claim 1 or 6, is characterized in that institute's ferrous salt, phosphate, lithium salts are respectively ferrous sulfate heptahydrate, diammonium hydrogen phosphate, Lithium hydroxide monohydrate.
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| US5997958A (en) * | 1997-03-13 | 1999-12-07 | Hitachi Europe Limited | Method of depositing nanometer scale particles |
| CN1356543A (en) * | 2001-12-10 | 2002-07-03 | 中国科学院长春应用化学研究所 | Process for preparing film electrode of gold-monocrystal nano island array |
| CN1786268A (en) * | 2005-12-15 | 2006-06-14 | 复旦大学 | Self assembly chemical silver plating method on non metal material surface |
| CN101012109A (en) * | 2007-02-01 | 2007-08-08 | 上海交通大学 | Method of manufacturing phosphate group silicane-carbon nano tube composite film on glass substrate surface |
-
2012
- 2012-11-23 CN CN201210479256.6A patent/CN102945960B/en not_active Expired - Fee Related
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| US5997958A (en) * | 1997-03-13 | 1999-12-07 | Hitachi Europe Limited | Method of depositing nanometer scale particles |
| CN1356543A (en) * | 2001-12-10 | 2002-07-03 | 中国科学院长春应用化学研究所 | Process for preparing film electrode of gold-monocrystal nano island array |
| CN1786268A (en) * | 2005-12-15 | 2006-06-14 | 复旦大学 | Self assembly chemical silver plating method on non metal material surface |
| CN101012109A (en) * | 2007-02-01 | 2007-08-08 | 上海交通大学 | Method of manufacturing phosphate group silicane-carbon nano tube composite film on glass substrate surface |
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