CN108284231A - A kind of method that photocuring prepares the extra small nano particle of carbon coating - Google Patents
A kind of method that photocuring prepares the extra small nano particle of carbon coating Download PDFInfo
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- CN108284231A CN108284231A CN201810022878.3A CN201810022878A CN108284231A CN 108284231 A CN108284231 A CN 108284231A CN 201810022878 A CN201810022878 A CN 201810022878A CN 108284231 A CN108284231 A CN 108284231A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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Abstract
The invention discloses a kind of methods that photocuring prepares the extra small nano particle of carbon coating.This method operating procedure is：Under the conditions of black out, persursor material is dissolved completely in photaesthesia polymeric material；Then solution is placed in crucible, is exposed under ultraviolet light or visible light, pass through the thorough curing solution of photocuring；Finally crucible is placed in tube furnace to carry out calcining in protective atmosphere cracking and obtains the extra small nano particle of carbon coating.The method of the present invention has synthetic method simple, and the simple and easy to do feature of preparation process, obtained extra small nano particle diameter is uniform and does not assemble.
Description
Technical field
The invention belongs to nano material synthesis technical fields, specifically, it is super to disclose a kind of photocuring preparation carbon coating
The method of small nano particle.
Background technology
The features such as nano material has crystal grain tiny, and defect concentration is high, and specific surface is larger, pass through due to its special light,
The properties such as heat, electricity, magnetic, are greatly paid close attention to by people in recent years.With the development of nanosecond science and technology, the preparation method of nano material
Also become the emphasis of scientific research.Currently, the preparation method of nano material generally can be divided into vapor phase method by states of matter, liquid phase method, consolidate
Xiang Fa.Common vapor phase method has physical vaporous deposition, chemical vapour deposition technique etc..These method flexibilities are larger, can prepare
Better quality nano material, but its synthesis rate is relatively low and appliance arrangement is expensive, it is difficult to it mass produces.Liquid phase method includes chemistry
The precipitation method, sol-gel method, spray-on process, hydro-thermal method, microemulsion method etc., these methods are generally easier, but there is synthesis production
The shortcomings of object purity is relatively low, and the reaction time is longer, and particle size is larger.Solid phase method includes high-energy ball milling method, solid reaction process etc..
This method advantage is that product component is unrestricted, at low cost, yield is big, but there is also particle sizes to be distributed larger, production
The not high problem of product purity.So novel easy, the favorable for large-scale production, Product size of exploitation it is controllable, have it is pervasive
Property nano material synthesis preparation method, will greatly push information technology, medicine, environment, automatic technology and energy science
Development.
Photo-curing material is the general designation of the materials such as the coating, ink and binder of photocuring.This kind of material is with prepolymer
Basis is added specific activated monomer, photoinitiator and multiple additives and is formulated.Wherein photoinitiator function is to attract light
Can, it is answered with causing polymerization hair, is divided into free radical type, cationic.Prepolymer is the main body of material, determines material after curing
Main performance, including epoxy acrylate etc..Monomer can influence to cure film property to adjust viscosity and participate in curing reaction
Can, it is divided into single functionality, bifunctionality and polyfunctionality.In addition, some additives can be suitably added this light depending on purposes difference
Polymerization system.Photocuring belongs to chemical method, it is light-initiated chemical reaction as a result, compared with other curings, and light is solid
Changing has many unique advantages, for example reaction rate is fast, most soon can be to cure in 0.05-1 seconds time；Expense is relatively low,
Equipment investment is relatively cheap；Pollution is few, and basic 100% solidification of photo-curing material can reduce the environment caused by solvent volatilizees
Pollution.
Invention content
The characteristics of for photopolymerization reaction, the present invention provide a kind of method that photocuring prepares extra small nano particle, have
Preparation process is easy to operate, and the advantage that controllability is strong.
What the invention is realized by the following technical scheme：
A kind of method that photocuring prepares the extra small nano particle of carbon coating：It is under the conditions of black out, persursor material is completely molten
Solution is in photaesthesia polymeric material；Then solution is placed in crucible, is exposed under ultraviolet light or visible light, passes through photocuring
Thorough curing solution；Finally crucible is placed in tube furnace and carries out calcining cracking in protective atmosphere and obtains that carbon coating is extra small to be received
Rice grain.
Preferably, the persursor material is the compound for including at least one of following element：Li、Na、K、Mg、
Ca、Sr、Ba、Al、Ga、In、Ge、Sn、Sc、Ti、V、Mn、Fe、Co、Ni、Cu、Zn、Y、Zr、Nb、Mo、Ag、Ce、W、H、B、C、N、
O, F, Si, P, S, Cl, As, Te, I or Br；And persursor material can be dissolved in photaesthesia polymeric material.
Preferably, the persursor material is one or more of acid, alkali or salt.
Preferably, photocuring principle is free radical type photocuring processes or cationic process for photocuring.
Preferably, the photaesthesia polymeric material includes one or more of prepolymer, photoactive monomer and light-initiated
Agent.
Preferably, the photaesthesia polymeric material further includes auxiliary agent.
Preferably, the prepolymer is polyethylene glycol double methyl methacrylate；The photoactive monomer is methyl-prop
One or more of olefin(e) acid hydroxyl ethyl ester, pentaerythritol triacrylate；The photoinitiator is bis- (2,4, the 6- front threes of phenyl
Base benzoyl) phosphine oxide.
Preferably, the photaesthesia polymeric material is polyvinyl alcohol ring contracting Ethenylbenzene formalin.
Preferably, time for exposure >=1 minute, until solution is fully cured.
Preferably, protective atmosphere is the mixed atmosphere of argon gas, nitrogen, hydrogen or more gas.
Preferably, 1200 degrees Celsius >=calcination temperature >=400 degree Celsius, calcination time >=1 hour.
When the principle of the present invention is that solute is dissolved in solution, dispersion is extremely uniform, and solute molecule is with lewis' acid
Form exists in solution.Under the conditions of this makes black out, when persursor material is dissolved in photaesthesia polymeric material, dispersed pole
It is good.After the solidification of photoinduction light sensitive material instaneous polymerization, after this makes persursor material also uniformly be dispensed into solidification
In light sensitive material.At this point, after protective atmosphere high-temperature calcination, light sensitive material is cracked into carbon material, and presoma material
Expect that fixation in situ in carbon material, forms extra small nano particle.
The advantageous effects of the present invention：The synthetic method of the extra small nano particle of the present invention is simple, and reaction condition is mild, root
The extra small nano particle diameter prepared according to the present invention is uniform and does not assemble, and the method has universality, can be used for big absolutely
The synthesis of most nano materials.
Description of the drawings
Fig. 1 is the X-ray diffractogram of the extra small cobalt nano-particle of carbon coating obtained in embodiment 1；
Fig. 2 is the transmission electron microscope picture of the extra small cobalt nano-particle of carbon coating obtained in embodiment 1；
Fig. 3 is the transmission electron microscope picture of the extra small cobalt nano-particle of carbon coating obtained in embodiment 2；
Fig. 4 is the X-ray diffractogram of the extra small manganous oxide nano particle of carbon coating obtained in embodiment 3；
Fig. 5 is the transmission electron microscope picture of the extra small manganous oxide nano particle of carbon coating obtained in embodiment 3；
Fig. 6 is the X-ray diffractogram of the extra small lithium manganese phosphate nano particle of carbon coating obtained in embodiment 4；
Fig. 7 is the transmission electron microscope picture of the extra small lithium manganese phosphate nano particle of carbon coating obtained in embodiment 4；
Fig. 8 is the transmission electron microscope picture of the extra small tin nanoparticles of carbon coating obtained in embodiment 5.
Specific implementation mode
Embodiment 1
Under the conditions of black out, hydroxyethyl methacrylate (HEMA, 45wt%), polyethylene glycol double methyl methacrylate are prepared
The mixed solution of (PEGDA, 50wt%) and pentaerythritol triacrylate (PETA, 5wt%) are added mixed solution 3wt%'s
Bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides (819) of photoinitiator phenyl, after mixing as photaesthesia polymeric material.
Under the conditions of black out, by 0.01g cabaltous nitrate hexahydrates (Co (NO)3·6H2O it is prepared above-mentioned) to be dissolved completely in 1g
In photaesthesia polymeric material, mixed liquor is poured into crucible.Later, cured after ultraviolet light 2h at room temperature
Mixture.At this point, cobalt element is infinitely uniformly scattered in the photopolymerization material after solidification.The solidfied material of gained is being protected
(volume ratio 1 under property atmosphere:19 hydrogen and argon-mixed) in 800 DEG C, be heat-treated after 2h obtain it is unformed carbon-coated extra small
Cobalt nanometer particle.Its X-ray diffractogram is as shown in Figure 1, it can be seen from the figure that material is strictly by cobalt nano-particle and without fixed
Type carbon is constituted, and the diffraction maximum peak width of cobalt granule is wider, illustrates that cobalt nano-particle grain size is smaller.The transmission electron microscope picture of material
As shown in Figure 2.There is relatively narrow particle diameter distribution from the cobalt nano-particle of the transmission electron microscope picture of Fig. 2 display gained, grain size is about
For 3nm or so.
Embodiment 2
Under the conditions of black out, hydroxyethyl methacrylate (HEMA, 45wt%), polyethylene glycol double methyl methacrylate are prepared
The mixed solution of (PEGDA, 50wt%) and pentaerythritol triacrylate (PETA, 5wt%) are added mixed solution 4wt%'s
Bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides (819) of photoinitiator phenyl, after mixing as photaesthesia polymeric material.
Under the conditions of black out, by 0.1g cabaltous nitrate hexahydrates (Co (NO)3·6H2O) it is dissolved completely in the prepared above-mentioned light of 1g
In sensitive polymeric material, mixed liquor is poured into crucible.Later, it at room temperature after ultraviolet light 2h, obtains cured
Mixture.At this point, cobalt element is infinitely uniformly scattered in the photopolymerization material after solidification.By the solidfied material of gained in protectiveness
(volume ratio 1 under atmosphere:19 hydrogen and argon-mixed) in 800 DEG C, obtain unformed carbon-coated extra small cobalt after being heat-treated 2h
Nano-particle.The transmission electron microscope picture of material is as shown in Figure 3.From the cobalt nano-particle of the transmission electron microscope picture of Fig. 2 display gained
With relatively narrow particle diameter distribution, grain size is about 7nm or so.It follows that as nano material grain size can be by precursor concentration
Control.
Embodiment 3
Under the conditions of black out, hydroxyethyl methacrylate (HEMA, 45wt%), polyethylene glycol double methyl methacrylate are prepared
The mixed solution of (PEGDA, 50wt%) and pentaerythritol triacrylate (PETA, 5wt%) are added mixed solution 5wt%'s
Bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides (819) of photoinitiator phenyl, after mixing as photaesthesia polymeric material.
Under the conditions of black out, by 0.2g manganese acetates (Mn (CH3COO)2) it is dissolved completely in the prepared above-mentioned photaesthesia polymerizations of 1g
In material, mixed liquor is poured into crucible.Later, at room temperature after ultraviolet light 2h, cured mixture is obtained.This
When, manganese element is infinitely uniformly scattered in the photopolymerization material after solidification.By the solidfied material of gained under protective atmosphere (argon
Gas) in 900 DEG C, be heat-treated 2h after obtain unformed carbon-coated extra small manganous oxide (MnO) nano-particle.Its X-ray diffraction
Figure is as shown in figure 4, it can be seen from the figure that material is strictly to be made of with agraphitic carbon MnO nano particles, and MnO particles
Diffraction maximum peak width it is wider, illustrate that MnO nano particle diameters are smaller.The transmission electron microscope picture of material is as shown in Figure 5.From Fig. 5's
The MnO nano particles of transmission electron microscope picture display gained have relatively narrow particle diameter distribution, and grain size is about 5nm or so.
Embodiment 4
Under the conditions of black out, hydroxyethyl methacrylate (HEMA, 45wt%), polyethylene glycol double methyl methacrylate are prepared
The mixed solution of (PEGDA, 50wt%) and pentaerythritol triacrylate (PETA, 5wt%) are added mixed solution 3wt%'s
Bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides (819) of photoinitiator phenyl, after mixing as photaesthesia polymeric material.
Under the conditions of black out, by 0.1g manganese acetates (Mn (CH3COO)2), 0.47g trimethyl phosphates (C3H9PO4) and 0.03g
Lithium nitrate (LiNO3) be dissolved completely in the prepared above-mentioned photaesthesia polymeric materials of 1g, mixed liquor is poured into crucible.It
Afterwards, at room temperature after ultraviolet light 2h, cured mixture is obtained.At this point, manganese element is infinitely uniformly scattered in admittedly
In photopolymerization material after change.By the solidfied material of gained under protective atmosphere 900 DEG C in (argon gas), nothing is obtained after being heat-treated 2h
Shape carbon-coated extra small lithium manganese phosphate (LiMnPO4) nano-particle.Its X-ray diffractogram is as shown in fig. 6, can from figure
Go out, material is strictly by LiMnPO4Nano particle is constituted with agraphitic carbon, and LiMnPO4The diffraction maximum peak width of particle is wider,
Illustrate LiMnPO4Nano particle diameter is smaller.The transmission electron microscope picture of material is as shown in Figure 7.It is aobvious from the transmission electron microscope picture of Fig. 7
Show the LiMnPO of gained4Nano particle has relatively narrow particle diameter distribution, and grain size is about 15nm or so.
Embodiment 5
Under the conditions of black out, it is with polyvinyl alcohol ring contracting ethylene benzaldehyde (PVA-SbQ) aqueous solution that mass concentration is 15%
Photaesthesia polymeric material, PVA-SbQ have special molecular structure, itself include polymerized monomer and light-initiated group.
Under the conditions of black out, by 0.5g isopropanols tin (Sn (OCH (CH3)2)4) it is dissolved completely in 0.2g PVA-SbQ aqueous solutions
In, mixed liquor is poured into crucible and is dried.Later, at room temperature after ultraviolet light 5h, cured mixture is obtained.This
When, tin element is infinitely uniformly scattered in the photopolymerization material after solidification.By the solidfied material of gained under protective atmosphere (argon
Gas) in 700 DEG C, be heat-treated 2h after obtain unformed carbon-coated extra small sijna rice corpuscles.Transmission electron microscope picture such as Fig. 8 of material
It is shown.There is relatively narrow particle diameter distribution from the tin nanoparticles of the transmission electron microscope picture of Fig. 8 display gained, grain size is about 3nm
Left and right.
The foregoing is merely the Illustrative embodiments of the present invention, are not intended to limit the invention, all the present invention's
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within spirit and principle.
Claims (10)
1. a kind of method that photocuring prepares the extra small nano particle of carbon coating, which is characterized in that under the conditions of black out, by presoma material
Material is dissolved completely in photaesthesia polymeric material；Then solution is placed in crucible, is exposed under ultraviolet light or visible light, led to
Cross the thorough curing solution of photocuring；Finally crucible is placed in tube furnace to carry out calcining in protective atmosphere cracking and obtains carbon packet
Cover extra small nano particle.
2. the method that photocuring according to claim 1 prepares the extra small nano particle of carbon coating, which is characterized in that before described
It is the compound for including at least one of following element to drive body material：Li、Na、K、Mg、Ca、Sr、Ba、Al、Ga、In、Ge、
Sn、Sc、Ti、V、Mn、Fe、Co、Ni、Cu、Zn、Y、Zr、Nb、Mo、Ag、Ce、W、H、B、C、N、O、F、Si、P、S、Cl、As、Te、
I, or Br；And persursor material can be dissolved in photaesthesia polymeric material.
3. the method that photocuring according to claim 2 prepares the extra small nano particle of carbon coating, which is characterized in that before described
It is one or more of acid, alkali or salt to drive body material.
4. the method that photocuring according to claim 1 or 2 prepares the extra small nano particle of carbon coating, which is characterized in that light
It is cured as free radical type photocuring processes or cationic photocuring processes.
5. the method that photocuring according to claim 4 prepares the extra small nano particle of carbon coating, which is characterized in that the light
Sensitive polymeric material includes one or more of prepolymer, photoactive monomer and photoinitiator.
6. the method that photocuring according to claim 5 prepares the extra small nano particle of carbon coating, which is characterized in that the light
Sensitive polymeric material further includes auxiliary agent.
7. the method that photocuring according to claim 5 prepares the extra small nano particle of carbon coating, which is characterized in that described
Prepolymer is polyethylene glycol double methyl methacrylate；The photoactive monomer is hydroxyethyl methacrylate, pentaerythrite three
One or more of acrylate；The photoinitiator is bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides of phenyl.
8. the method that photocuring according to claim 4 prepares the extra small nano particle of carbon coating, which is characterized in that the light
Sensitive polymeric material is polyvinyl alcohol ring contracting Ethenylbenzene formalin.
9. the method that the photocuring according to claim 5 or 8 prepares the extra small nano particle of carbon coating, which is characterized in that institute
Time for exposure >=1 minute is stated, until solution is fully cured.
10. the method that photocuring according to claim 9 prepares the extra small nano particle of carbon coating, which is characterized in that described
Protective atmosphere be argon gas, nitrogen, hydrogen or more gas mixed atmosphere；1200 degrees Celsius >=calcination temperature >=400 are taken the photograph
Family name's degree, calcination time >=1 hour.
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| CN101857217A (en) * | 2009-04-07 | 2010-10-13 | 清华大学 | Carbon nano tube metal composition and preparation method thereof |
| US20120236065A1 (en) * | 2011-03-17 | 2012-09-20 | Xerox Corporation | Magnetic Curable Inks |
| CN103310869A (en) * | 2012-03-08 | 2013-09-18 | 清华大学 | Carbon nanotube slurry and preparation method thereof, and method for preparing cathode emitter with the carbon nanotube slurry |
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| CN105098136A (en) * | 2015-08-27 | 2015-11-25 | 中国科学院宁波材料技术与工程研究所 | Preparation method and application of silicon oxycarbide/carbon composite micronano material |
| CN105251979A (en) * | 2015-09-29 | 2016-01-20 | 中国航空工业集团公司北京航空材料研究院 | Method for preparing materials including metal nanoparticles/graphene/carbon nano tubes |
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- 2018-01-10 CN CN201810022878.3A patent/CN108284231A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857217A (en) * | 2009-04-07 | 2010-10-13 | 清华大学 | Carbon nano tube metal composition and preparation method thereof |
| US20120236065A1 (en) * | 2011-03-17 | 2012-09-20 | Xerox Corporation | Magnetic Curable Inks |
| CN103310869A (en) * | 2012-03-08 | 2013-09-18 | 清华大学 | Carbon nanotube slurry and preparation method thereof, and method for preparing cathode emitter with the carbon nanotube slurry |
| KR20140011642A (en) * | 2012-07-18 | 2014-01-29 | 금오공과대학교 산학협력단 | Uv curable epoxy resin/carbon nanomaterial composite films and process for producing the same |
| WO2015105514A1 (en) * | 2014-01-13 | 2015-07-16 | Unipixel Displays, Inc. | Coated nano-particle catalytically active composite inks |
| CN105098136A (en) * | 2015-08-27 | 2015-11-25 | 中国科学院宁波材料技术与工程研究所 | Preparation method and application of silicon oxycarbide/carbon composite micronano material |
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