WO2012150802A2 - Dispositif de préparation de nanoparticule fixée à un support - Google Patents

Dispositif de préparation de nanoparticule fixée à un support Download PDF

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Publication number
WO2012150802A2
WO2012150802A2 PCT/KR2012/003420 KR2012003420W WO2012150802A2 WO 2012150802 A2 WO2012150802 A2 WO 2012150802A2 KR 2012003420 W KR2012003420 W KR 2012003420W WO 2012150802 A2 WO2012150802 A2 WO 2012150802A2
Authority
WO
WIPO (PCT)
Prior art keywords
metal
carrier
stirring
nanoparticles
metal compound
Prior art date
Application number
PCT/KR2012/003420
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English (en)
Korean (ko)
Other versions
WO2012150802A3 (fr
Inventor
고석근
Original Assignee
주식회사 나노케미
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by 주식회사 나노케미 filed Critical 주식회사 나노케미
Publication of WO2012150802A2 publication Critical patent/WO2012150802A2/fr
Publication of WO2012150802A3 publication Critical patent/WO2012150802A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
    • 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

Definitions

  • the present invention relates to an apparatus for producing nanoparticles using a carrier.
  • Nanoparticles are formed by the chemical process in the initial process of converting metal ions into metal solid particles by adding a reducing agent and a dispersant to the metal ions present in an aqueous solution.
  • Such chemical method is not easy to control the nanoparticle size and separation of the nanoparticles, and the characteristics of the nanoparticles vary depending on the type of redox agent, dispersant, PH, temperature, etc., the flammability side in the production of nanoparticles Has many problems.
  • the above chemical method because the first to dissolve the metal in acid or base to oxidize to the next form, and then to reduce the metal back to the metal element using a reducing agent to use a number of redox reagents for the treatment of the reagent waste used It costs a lot.
  • the nanoparticles when manufacturing the nanoparticles by the chemical method as described above, in order to use in the industry, it is necessary to treat other chemicals such as a mixture, stabilizer, organic solvent, compatibilizer, resulting in unexpected with other chemicals As a result of the reaction, discoloration of the final product occurs, and the commerciality is lowered.
  • the dispersant is dissociated because the initial dispersant loses the linkage between the chemicals of the final product, and the nanoparticles aggregate with each other to increase in size. Because of the problem that cannot be obtained, the application of nanoparticles to the industry is limited.
  • a metal atom vapor which is a metal or a metal compound.
  • the method uses a high temperature of a metal or metal compound to produce steam, or uses electron or energy using DC sputtering, DC-RF sputtering, ECR, and laser beam sputtering.
  • the atomic vapor generated by irradiating a solid having a particle with a solid is injected into a gas of a low temperature or passed through a region of a low temperature so that the atomic vapor is rapidly condensed to form nano-sized particles.
  • Another physical method is a mechanical grinding method in which a mechanical force is applied to the material to grind the material into fine particles. In order to process the material into nano particles having a size of 10 nm, a long grinding process is required.
  • the physical methods are 80 to 90% of the particles in the powder is formed in a micrometer size significantly larger than the -nano particles, when the nano-particles by the physical method using the vacuum equipment, the particle size is non-uniform and productivity is low and economical There is a falling problem.
  • the method is a method of vaporizing a metal or metal compound by a physical method in a vacuum state, and depositing a metal or metal compound vapor on a stirred carrier to form nanoparticles.
  • a carrier mainly containing oxides and precious metals as a raw material was stirred to form nanoparticles on the stirred carrier.
  • the nano horses manufactured using the carrier as described above were easy to handle and could simplify the manufacturing process of the applied product when the constituent material of the final product was used as the carrier.
  • the nanopowder manufacturing apparatus of the 1980s and 1990s had problems such as low deposition efficiency, wide distribution of nanoparticle size, load applied to a stirred carrier of heterogeneous carrier, and low equipment durability.
  • Korean Patent No. 10-0644219 discloses a method for forming nanoparticles by horizontal stirring, in which the stirring vessel is vertically formed so that the carrier is scattered in vacuum and easily escapes from the stirring tank.
  • a vertical stirring method such as a nanoparticle manufacturing method using the vertical transfer method of Figure 2 has been developed (China Patent Application No. 200810004352.9).
  • the vertical stirring method improves the problems of the horizontal stirring method, in particular, the blowing phenomenon of the powder, and the problem of scattering to the deposition source even in the case of a relatively light carrier.
  • the present invention provides a nanoparticle manufacturing apparatus characterized in that by evaporating a metal or a metal compound by using physical vapor deposition (vapor), and depositing nanoparticles on a carrier. It aims to do it.
  • an object of the present invention is to provide a nanoparticle manufacturing apparatus that can effectively control the size and content of the nanoparticles by controlling the growth of the nanoparticles.
  • an object of the present invention is to provide an apparatus for producing nanoparticles with superior deposition efficiency and durability superior to existing carrier stirring methods.
  • the present invention is a vacuum deposition tank; A stirring tank provided in the vacuum deposition tank; A screw provided in the stirring tank and stirring the carrier; And an evaporation source provided above the stirring vessel in the vacuum evaporation tank and evaporating the metal or metal compound, the metal or metal compound nanoparticle manufacturing apparatus attached to the carrier.
  • the upper end of the side of the stirring vessel is bent 1 to 90 degrees in the center direction on the basis of the vertical surface,
  • the screw stirs only the lower portion of the carrier having a total depth of 1/5 to 3/4 of the carrier charged into the stirring vessel, and causes the carrier of the upper portion of the stirring vessel to flow by stirring the lower portion to continuously move the carrier to the lower portion.
  • an apparatus for producing metal or metal compound nanoparticles attached to a carrier characterized in that the scattering by stirring can prevent the scattering of the carrier in the upper layer due to the weight of the upper layer.
  • Nanoparticle manufacturing apparatus by transporting the carrier at a constant speed and uniformly stirring the carrier to increase the deposition efficiency of the nanoparticles to produce nanoparticles of uniform size, mechanical load and The durability of the equipment can be improved by minimizing the load on the equipment.
  • 1 and 2 is a schematic diagram of a conventional horizontal stirring type nanoparticle manufacturing apparatus and vertical stirring type nanoparticle manufacturing apparatus.
  • Figure 3 is a schematic diagram showing that the upper end of the side of the stirring tank of the nanoparticle manufacturing apparatus according to the present invention has a feature that is bent 1 to 90 degrees in the center direction with respect to the vertical plane.
  • Figure 4 is a schematic diagram showing that the movement of the metal or metal compound vapor supplied from the deposition source of the nanoparticle manufacturing apparatus according to the present invention uses an average free path.
  • Figure 5 is a schematic diagram showing that the nanoparticle manufacturing apparatus according to the present invention has a feature that the screw is loaded into the carrier.
  • FIG. 6 is a schematic view of a nanoparticle manufacturing apparatus according to an embodiment of the present invention.
  • 7 is a schematic diagram showing the growth control process of the nanoparticles according to the present invention.
  • Figure 8a shows the position of the metals deposited on the specimen to make the aluminum vaporized by thermal evaporation after a certain time to determine the direction of movement of aluminum vapor
  • Figure 8b is a photograph of the slide glass with aluminum deposited on each specimen It is a photograph.
  • FIG. 9A shows the direction of vapor flow through the specimen observation at each position after a certain time by making Si02 by steam
  • FIG. 9B is a photograph of Si02 vapor deposited on each specimen.
  • FIG. 10A is an example of manufacturing nanoparticles using the nanoparticle manufacturing apparatus of the present invention.
  • FIG. 10A is a photograph of an initial glucose carrier powder when glucose is used as a carrier and copper is used as a deposition source.
  • FIG. 10B illustrates an example in which nanoparticles are manufactured using the nanoparticle manufacturing apparatus of the present invention.
  • glucose is used as a carrier and copper is used as a deposition source, glucose with copper nanoparticles adhered to a concentration of about 10,000 ppm. For micrographs.
  • FIG. 10C shows the results of EDS analysis of the points 1, 2 ′ 3 and 4 displayed on the glucose having the copper nanoparticles of FIG. 10B attached thereto.
  • 10D is a photograph of the copper nanoparticles attached to the copper nanoparticles after dissolving in water, flowing in a slide glass and dried, and then observed the copper nanoparticles under a microscope.
  • the present invention is a vacuum deposition tank; A stirring tank provided in the vacuum deposition tank; A screw provided in the stirring tank and stirring the carrier; And a deposition source provided above the stirring vessel in the vacuum deposition tank and evaporating the metal or metal compound, wherein the upper end of the side surface of the stirring vessel is a vertical plane. Bends 1 to 90 degrees in the center direction relative to the
  • the screw provides a device for producing metal or metal compound nanoparticles attached to the carrier, characterized in that the horizontal or vertical direction, provided to stir 1/5 to 3/4 of the total depth of the carrier charged into the stirring vessel. .
  • the nanoparticle manufacturing apparatus is characterized in that the side of the stirring vessel is bent 1 to 90 degrees in the center direction with respect to the vertical plane.
  • FIG 3 is a schematic diagram of this, in the case of inclining the side of the stirring vessel in this way when the carrier having a viscosity can be prevented from being separated to the outside by riding the stirring vessel wall.
  • the screw is a horizontal or vertical screw, which stirs the carrier in the horizontal or vertical direction.
  • the nanoparticle manufacturing apparatus is characterized in that the screw is provided to stir 1/5 to 3/4 of the total depth of the carrier charged into the stirring vessel.
  • Nanoparticles according to the present invention is a result, the weight of the support, even when high-speed stirring by having fully charged the s horizontal or vertical screw carrier increases prevent carriers are scattered over the carrier to be stagnant in the central wall or portion Carriers were easily moved up and down inside the carrier stir bath (FIG. 5).
  • the deposition source of the metal or metal compound is thermal vapor deposition, DC sputtering, DC-RF sputtering, electron beam deposition (E ⁇ Beam) Evaproation) or laser sputtering may be used, but is not necessarily limited thereto.
  • the metal may be cobalt, copper, silver, nickel, manganese, palladium, indium iron, tungsten, titanium, alloys thereof, and the like, but is not limited thereto.
  • the metal compound may be metal oxide, metal nitride, metal carbide, metal carbon nitride, but is not necessarily limited thereto.
  • the metal compound may include alumina (A1 0) as a metal oxide, tungsten carbide (WC) as a metal carbide, nitrogen aluminum (A1N) as a metal nitride, and titanium carbonitride (TiCN) as a metal carbonitride. It is not limited to this.
  • the carrier may be activated carbon, a hydrocarbon compound, alumina (A1 0), tungsten carbide (WC), glass, sand, a material soluble in water or a solvent, such as glucose, sugar, salt, PMMA, etc. It is not limited.
  • the vacuum degree of the vacuum deposition tank is preferably 10 to 4 to 1 torr.
  • the vacuum degree of the vacuum deposition tank is adjusted to include an inert gas, the inert gas may be argon, neon, N Ar, 0, CH and the like, but is not necessarily limited thereto.
  • the apparatus for producing nanoparticles according to the present invention is a nanoparticle of the metal or metal compound from the deposition source using the principle of the average free path under an atmosphere in which the vacuum degree of the vacuum deposition tank is adjusted to 1 ( ⁇ 4 to 1 torr using an inert gas). It is characterized by scattering the particles in the downward direction.
  • the direction in which the metal vapor was scattered was in the carrier direction.
  • the scattering direction of the atomized vapor is the carrier direction, it is mainly deposited around the deposition source, causing loss of vapor to be deposited, and when producing steam at high speed to increase the production rate, many vapors are formed inside the nozzle. It was difficult to produce small size nanoparticles by clustering at.
  • the metal vapor since the vaporization direction of the atomized vapor is opposite to the carrier, the metal vapor is scattered upwards, but the vacuum degree is 1 to 4 to 1 torr, so that a layer stone is formed between the metal vapor and the inert gas due to the inert gas filled therein. The path is shortened so that the metal vapor moves downward by gravity to form nanoparticles on the stirred carrier.
  • the aluminum metal mass was loaded on a tungsten boat and heat was applied using a DC power source as a deposition heat source to cause the aluminum metal to evaporate upward.
  • a DC power source as a deposition heat source to cause the aluminum metal to evaporate upward.
  • the circular slide glass was placed at various positions and aluminum was deposited, the circular slide glass was observed, and the moving direction of steam was schematically illustrated in FIG. 8A.
  • the argon gas to form a low vacuum atmosphere at least 10- 3 torr.
  • FIG. 8B is photographs of the slide glass on which aluminum is deposited in FIG. 8A.
  • the slide glass close to the steam generator can see that a large amount of aluminum is deposited, while the far slide glass can see that very little aluminum is deposited.
  • slide glass 1 and 2 a large amount of aluminum is deposited to reflect the metallic gloss, and the same color appears in the picture, but this is a phenomenon caused by reflection.
  • Slide 4 shows a small amount of actual deposition, making it opaque black.
  • slide glasses 5 to 8 aluminum is hardly deposited, so that the transparent slide glass can be confirmed.
  • FIG. 9A is a photograph confirming that SiO vapor is deposited on the slide glass in FIG. 9A.
  • Slide glass 1 and 2 is a slide glass located directly below the electron beam, it can be seen that the oxide vapor is not reached directly below the steam source because the oxide vapor is not deposited on the slide glass.
  • the deposition amount of Si02 vapor decreases as it moves away from the steam source from slide glasses 3 to 8.
  • the speed of the screw is preferably adjusted to 1 to 200 rpm.
  • stirring speed is less than 1 rpm, agitation is not sufficiently performed, so that the metal nanoparticles are not uniformly attached to the surface of the carrier. If the stirring speed exceeds 200 rpm, each of the carriers is heavy. Powders charged in the stirring tank may be scattered by the high speed rotation, and when the weight of each carrier is light, the stirring may be performed only in the inside of the carrier barrel, thereby making it difficult to move the carrier in the vertical direction by the weight.
  • Nanoparticles manufacturing apparatus as shown in FIG. By controlling the deposition rate, stirring speed, etc., the growth of the nanoparticles can be controlled to effectively control the size and content of the nanoparticles.
  • a metal or metal compound vapor is deposited on a carrier to form a nucleus for forming a metal or metal compound nanoparticle, and the nucleus is then nanoparticles by further deposition of metal vapor.
  • the carrier was stirred and rotated to form a mixture of metal or metal vapor.
  • the nanoparticle production apparatus is controlled by the deposition rate of the metal or metal compound vapor on the carrier at a thickness of 1 A (low speed steam discharge rate) to 10 (high speed steam discharge rate) per unit area per minute, high speed in low speed deposition It does not cause problems until deposition, and even if a large amount of steam is generated from the steam source, all of them can be made into nanoparticles on the stirred carrier.
  • the nanoparticle manufacturing apparatus according to the present invention has enhanced deposition efficiency and superior durability compared to the conventional carrier stirring method.
  • the nanoparticle manufacturing apparatus uses a vertical or horizontal screw to stir the carrier, and the horizontal or vertical screw is loaded into the carrier to prevent excessive scattering in the vacuum chamber. , Can transport the carrier at a constant speed by minimizing the mechanical load, improve the deposition efficiency by making the stirring of the carrier uniform, and manufacture nanoparticles of uniform size, and minimize the mechanical load and equipment load Durability can be improved.
  • the direction in which the copper vapor is scattered was set so as to be in the opposite direction, that is, upward direction, of the stirring vessel in which glucose, which is a carrier, is contained.
  • the glucose is agitated by a rotary screw provided in the stirring vessel, wherein the stirring speed of the glucose by the screw is maintained below lOOrpm.
  • the copper vapor was deposited on a glucose carrier to prepare glucose with copper nanoparticles at a concentration of about laOO ppm.
  • Example 1 the appearance change of the glucose carrier was observed by visual and electron microscopy.
  • Example 1 The copper-glucose nanoparticles prepared in Example 1 were subjected to quantitative and qualitative analysis of the components using an energy dispersive spectrometry (EDS).
  • EDS energy dispersive spectrometry
  • Example 1 After dissolving the copper ⁇ glucose nanoparticles prepared in Example 1 in water and observed the recrystallized form of the copper nanoparticles using an electron microscope. As shown in FIG. 10C, the points 1, 2, 3, and 4 shown in the photomicrograph of the copper / glucose carriers, which were observed by 400 times magnification of the glucose carrier with the copper nanoparticles, were analyzed by EDS. The amounts of C, 0 and Cu were the same. C ⁇ 0 detected by elemental analysis is a component constituting the glucose carrier, and Cu is a component generated from nanoparticles formed on the glucose carrier. On the other hand, copper was not detected at the position 4, and C and 0 were detected.

Abstract

La présente invention concerne un dispositif de préparation d'un métal ou d'une nanoparticule à composé métallique fixée à un support. Ledit dispositif comprend une chambre d'évaporation sous vide; une chambre d'agitation prévue dans la chambre d'évaporation sous vide; une vis disposée à l'intérieur de la chambre d'agitation servant à agiter le support; et une source d'évaporation située sur la partie supérieure de la chambre d'agitation à l'intérieur de la chambre d'évaporation sous vide pour engendrer l'évaporation du métal ou du composé métallique. L'extrémité supérieure de la surface latérale de la chambre d'agitation est pliée de 1 à 90 degrés en direction du centre, le plan perpendiculaire servant de base, et la vis se situe dans une direction horizontale ou verticale, de manière à agiter 1/5-3/4 de la profondeur totale du support chargé dans la chambre d'agitation.
PCT/KR2012/003420 2011-05-02 2012-05-02 Dispositif de préparation de nanoparticule fixée à un support WO2012150802A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR20110041583A KR101484572B1 (ko) 2011-05-02 2011-05-02 담체에 부착된 나노 입자 제조 장치
KR10-2011-0041583 2011-05-02

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Publication Number Publication Date
WO2012150802A2 true WO2012150802A2 (fr) 2012-11-08
WO2012150802A3 WO2012150802A3 (fr) 2013-01-17

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070044879A (ko) * 2005-10-26 2007-05-02 주식회사 피앤아이 금속, 합금 및 세라믹 나노 입자가 균일하게 진공 증착된파우더의 형성 방법 및 그 제조 장치
KR100835207B1 (ko) * 2007-05-31 2008-06-09 대한민국(관리부서:농촌진흥청장) 은 나노입자를 함유한 천연실크 및 그의 제조방법
JP2009079251A (ja) * 2007-09-26 2009-04-16 Ulvac Japan Ltd 金属蒸着装置および同装置における粉体状担体の撹拌方法
KR20100086907A (ko) * 2009-01-23 2010-08-02 세종대학교산학협력단 진공 건식 증착 분말 교반장치

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070044879A (ko) * 2005-10-26 2007-05-02 주식회사 피앤아이 금속, 합금 및 세라믹 나노 입자가 균일하게 진공 증착된파우더의 형성 방법 및 그 제조 장치
KR100835207B1 (ko) * 2007-05-31 2008-06-09 대한민국(관리부서:농촌진흥청장) 은 나노입자를 함유한 천연실크 및 그의 제조방법
JP2009079251A (ja) * 2007-09-26 2009-04-16 Ulvac Japan Ltd 金属蒸着装置および同装置における粉体状担体の撹拌方法
KR20100086907A (ko) * 2009-01-23 2010-08-02 세종대학교산학협력단 진공 건식 증착 분말 교반장치

Also Published As

Publication number Publication date
KR101484572B1 (ko) 2015-01-20
WO2012150802A3 (fr) 2013-01-17
KR20120123939A (ko) 2012-11-12

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