US20060103060A1 - Process for producing nanoparticle apparatus therefor and method of storing nanoparticle - Google Patents

Process for producing nanoparticle apparatus therefor and method of storing nanoparticle Download PDF

Info

Publication number
US20060103060A1
US20060103060A1 US10/525,654 US52565405A US2006103060A1 US 20060103060 A1 US20060103060 A1 US 20060103060A1 US 52565405 A US52565405 A US 52565405A US 2006103060 A1 US2006103060 A1 US 2006103060A1
Authority
US
United States
Prior art keywords
laser light
light irradiation
irradiation portion
treated liquid
nanoparticle production
Prior art date
Legal status (The legal status 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 status listed.)
Abandoned
Application number
US10/525,654
Other languages
English (en)
Inventor
Tomonori Kawakami
Bo Li
Mitsuo Hiramatsu
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hamamatsu Photonics KK
Original Assignee
Hamamatsu Photonics KK
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.)
Filing date
Publication date
Application filed by Hamamatsu Photonics KK filed Critical Hamamatsu Photonics KK
Assigned to HAMAMATSU PHOTONICS K.K. reassignment HAMAMATSU PHOTONICS K.K. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LI, BO, KAWAKAMI, TOMONORI, HIRAMATSU, MITSUO
Publication of US20060103060A1 publication Critical patent/US20060103060A1/en
Priority to US12/213,977 priority Critical patent/US7922786B2/en
Abandoned legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/121—Coherent waves, e.g. laser beams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • B01J2219/00063—Temperature measurement of the reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00121—Controlling the temperature by direct heating or cooling
    • B01J2219/00123—Controlling the temperature by direct heating or cooling adding a temperature modifying medium to the reactants
    • B01J2219/00126—Cryogenic coolants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00132—Controlling the temperature using electric heating or cooling elements
    • B01J2219/00137—Peltier cooling elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0871—Heating or cooling of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0877—Liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0879—Solid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • This invention concerns a nanoparticle production method and production device and a nanoparticle preservation method, and to be more specific, concerns a nanoparticle production method and production device, with which nanoparticles are produced by irradiating a laser light irradiation portion of a to-be-treated liquid with a laser light, wherein suspended particles are suspended, to pulverize the suspended particles in the laser light irradiation portion, and a nanoparticle preservation method.
  • Nanoparticulation brings about extreme increase of surface area. Thus with nanoparticles, the reactivity with the surroundings is thus high and properties unique to a substance are exhibited readily. Also, in the case where the particles are of a poorly soluble or insoluble substance, by nanoparticulation, the nanoparticles can be put in state of pseudo-dissolution in a solvent (a state wherein the nanoparticles, though being suspended in the solvent, appear to be pseudo-dissolved due to the lack of light scattering).
  • Nanoparticulation arts thus have the possibility of providing methods of preparing new substances, and applications are anticipated in a wide range of fields.
  • This invention has been made in view of the above circumstance and an object thereof is to provide a nanoparticle production method and production device, with which nanoparticulation of high efficiency can be realized, and a nanoparticle preservation method.
  • the present inventors have found, as a result of diligent research towards resolving the above issue, that the efficiency of nanoparticulation is increased extremely by cooling a laser light irradiation portion and irradiating the portion with a laser light, and have thus come to complete the present invention.
  • this invention's nanoparticle production method comprises: a nanoparticle production step of producing nanoparticles by irradiating a laser light irradiation portion of a to-be-treated liquid with a laser light, wherein suspended particles are suspended, to pulverize the suspended particles in the laser light irradiation portion; and wherein the laser light irradiation portion of the to-be-treated liquid is cooled prior to irradiation of the laser light irradiation portion with the laser light.
  • the respective suspended particles are cooled in their entireties.
  • the laser light is absorbed at the surfaces of the suspended particles in the laser light irradiation portion. Since the to-be-treated liquid is cooled at this time, significant temperature differences arise between the interiors and surfaces of the suspended particles and between the surfaces of the suspended particles and the to-be-treated liquid at the laser light irradiation portion.
  • the suspended particles are thus pulverized readily and nanoparticulation of high efficiency is carried out.
  • this invention's nanoparticle production device comprises: a treatment chamber, containing a to-be-treated liquid; a nanoparticle production laser device, irradiating a laser light irradiation portion of the to-be-treated liquid with a nanoparticle production laser light; and a temperature adjustment device, enabled to cool the laser light irradiation portion of the to-be-treated liquid; and wherein nanoparticles are produced by irradiating the laser light irradiation portion of the to-be-treated liquid with the nanoparticle production laser light, wherein suspended particles are suspended, to pulverize the suspended particles in the laser light irradiation portion.
  • the above-described nanoparticle production method can be carried out effectively. That is, with this invention's device, by the to-be-treated liquid being set to a low temperature by the temperature adjustment device, the respective suspended particles are cooled in their entireties. When the laser light irradiation portion of the to-be-treated liquid is then irradiated with the nanoparticle production laser light by the nanoparticle production laser device, the nanoparticle production laser light is mainly absorbed at the surfaces of the suspended particles in the laser light irradiation portion.
  • the to-be-treated liquid is cooled at this point, significant temperature differences arise between the interiors and surfaces of the suspended particles and between the surfaces of the suspended particles and the to-be-treated liquid at the laser light irradiation portion.
  • the suspended particles are thus pulverized readily and nanoparticulation of high efficiency is carried out.
  • this invention's nanoparticle preservation method is characterized in that a to-be-treated liquid, in which nanoparticles are suspended, is preserved in a solid-phase state.
  • FIG. 1 is a schematic view showing an embodiment of a nanoparticle production device.
  • FIG. 2 is a schematic view showing another embodiment of a nanoparticle production device.
  • FIG. 3 is a perspective partial view of a treatment chamber.
  • FIG. 4 is a graph showing absorbance measurement results of an Example 1 and Comparative Examples 1 and 2.
  • FIG. 1 is a schematic view showing a first embodiment of this invention's nanoparticle production device.
  • a nanoparticle production device 1 is equipped with a treatment chamber 2 , containing a to-be-treated liquid 8 in which suspended particles are suspended, a constant-temperature device (temperature adjustment device) 3 , which can cool to-be-treated liquid 8 in treatment chamber 2 to a low temperature no more than room temperature and can rapidly cool to-be-treated liquid 8 , and a stirring device (not shown), which stirs to-be-treated liquid 8 inside treatment chamber 2 .
  • a constant-temperature device temperature adjustment device
  • stirring device not shown
  • Nanoparticle production device 1 is also equipped with a nanoparticle production laser device 5 , which irradiates a laser light irradiation portion 2 a of treatment chamber 2 with a nanoparticle production laser light 9 to thereby pulverize the suspended particles and produce nanoparticles, and a control device 6 , controlling constant-temperature device 3 and laser device 5 .
  • a suspension of vanadyl phthalocyanine (referred to hereinafter as “VOPc”) particles in water is used as to-be-treated liquid 8 .
  • VOPc vanadyl phthalocyanine
  • the stirring device comprises, for example, a magnetic stirrer and a stirring element.
  • constant-temperature device 3 for example, a cooling device that makes use of a Peltier element or a rapid cooling device that makes use of liquid nitrogen, etc., is favorably used.
  • Nanoparticle production laser device 5 is preferably one that emits laser light of a wavelength in the range of 400 to 180 nm. If the wavelength is longer than 400 nm, the nanoparticulation efficiency tends to decrease, and if the wavelength is shorter than 180 nm, the optical energy of laser irradiation tends to be absorbed by the solvent, which for example is water. Nanoparticle production laser device 5 is equipped with a laser light source.
  • an Nd:YAG laser is to be used as the laser light source
  • the fundamental wavelength of an Nd:YAG laser is 1064 nm
  • laser device 5 must be equipped furthermore with a higher harmonic unit that includes the nonlinear optic crystal KDP, in order to convert the light of fundamental wavelength to a light of the third harmonic (wavelength: 355 nm).
  • an excimer laser (193 nm, 248 nm, 308 nm, 351 nm) or a nitrogen laser (337 nm) may be used as the laser light source.
  • Control device 6 performs temperature control of the to-be-treated liquid, on/off control of laser irradiation, control of the irradiation time etc., for example, by activating laser device 5 when the temperature of constant-temperature device 3 falls to a predetermined value or less and stopping laser device 5 when the temperature of constant-temperature device 3 exceeds a predetermined value to thereby constantly maintain the nanoparticulation treatment at high efficiency.
  • a nanoparticle production method using the above-described nanoparticle production device 1 shall now be described.
  • to-be-treated liquid 8 in which the suspended particles to be subject to nanoparticulation are suspended, is loaded into treatment chamber 2 .
  • To-be-treated liquid 8 is then stirred by the stirring device. The suspended state of suspended particles in to-be-treated liquid 8 is thereby maintained.
  • To-be-treated liquid 8 is then cooled by constant-temperature device 3 .
  • the respective suspended particles are thereby cooled in their entireties.
  • to-be-treated liquid 8 is cooled to room temperature or less and preferably to 10° C. or less.
  • laser device 5 When the temperature has dropped to a predetermined temperature or less, laser device 5 is activated by control device 6 , and the laser light irradiation portion 2 a of to-be-treated liquid 8 , contained inside treatment chamber 2 , is irradiated with laser light 9 from laser device 5 (nanoparticle production step).
  • the laser light is mainly absorbed at the surfaces of the suspended particles in laser light irradiation portion 2 a. Since the to-be-treated liquid is set to a low temperature no more than the predetermined temperature, significant temperature differences arise between the interiors and surfaces of the suspended particles and between the surfaces of the suspended particles and the to-be-treated liquid. The suspended particles are thus pulverized readily and nanoparticulation of high efficiency is carried out.
  • nanoparticles are thus formed, since the nanoparticles become less likely to scatter light, a pseudo-dissolution state, in other words, a transparent state is achieved as nanoparticulation progresses.
  • the formation of nanoparticles can thus be judged by the transparency of the to-be-treated liquid.
  • the pulse repetition frequency is preferably a high repetition frequency in consideration of the treatment efficiency.
  • the pulse repetition frequency since the to-be-treated liquid is heated at high frequency, the pulse repetition frequency must be set so as to be of a heating energy with which the performance of the constant-temperature device can be maintained.
  • nanoparticles that are formed as described above are normally active. Thus when laser device 5 is stopped after nanoparticle formation and the nanoparticles are left as they are in this state for some time, the nanoparticles aggregate. The aggregation of nanoparticles must thus be prevented to maintain the dispersed state of the nanoparticles.
  • to-be-treated liquid 8 is subject to rapid cooling solidification (rapid cooling solidification step) by constant-temperature device 3 .
  • rapid cooling solidification step rapid cooling solidification step
  • rapid cooling refers to a state of cooling with which the rate of progress of solidification of the laser light irradiation portion is higher than the rate of Brownian motion of the nanoparticles. With gradual cooling solidification that does not meet this state, the probability that the nanoparticles will be captured inside the solidified solid phase will be low and the nanoparticles will tend to aggregate in the non-solidified liquid phase.
  • to-be-treated liquid 8 is maintained at a temperature no more than its solidification point after rapid cooling solidification. That is, to-be-treated liquid 8 is maintained in the solid phase state. Thus after rapid cooling solidification, storage in a normal freezer is adequate. The nanoparticles can thereby be preserved in the suspended state over a long period of time.
  • FIG. 2 is a schematic view showing the second embodiment of this invention's nanoparticle production device.
  • this embodiment's nanoparticle production device 10 differs from nanoparticle production device 1 of the first embodiment firstly in being further equipped with an XYZ stage 11 for moving treatment chamber 2 , a thawing laser device 12 , which, when to-be-treated liquid 8 inside treatment chamber 2 is made a solidified body, thaws laser light irradiation portion 2 a of that solidified body, an optical trapping laser device 13 , which gathers suspended particles to the center of the thawed laser light irradiation portion 2 a by the optical trapping action of a laser light, and an optical system 16 , which irradiates the same portion of the to-be treated liquid with the respective laser lights from thawing laser device 12 , optical trapping laser device 13 , and nanoparticle production laser device 5 .
  • thawing laser device 12 a laser device that emits laser light of a wavelength at which absorption by the to-be-treated liquid or the suspended particles occurs is preferable.
  • the suspended particles are VOPc
  • an argon ion laser (488 nm, 514 nm) is used for example as thawing laser device 12 .
  • optical trapping laser device 13 a laser device that emits laser light of a wavelength at which there is no absorption by the to-be-treated liquid or the suspended particles is preferable.
  • a YAG laser (1064 nm) is for example used as optical trapping laser device 13 .
  • a first half-mirror 14 and a second half-mirror 15 are disposed, for example, as optical system 16 .
  • the thawing laser light that is emitted from thawing laser device 12 is arranged to be reflected by first half-mirror 14 , pass along optical axis 17 of nanoparticle production laser device 5 , and the same portion as the above-mentioned laser light irradiation portion 2 a is irradiated with the thawing laser light.
  • optical trapping laser light emitted from optical trapping laser device 13 is arranged to be reflected by second half-mirror 15 , pass along optical axis 17 of nanoparticle production laser device 5 , and the same portion as the above-mentioned laser light irradiation portion 2 a is irradiated with the optical trapping laser light.
  • nanoparticle production device 10 by moving XYZ stage 11 , laser light irradiation position 2 a in treatment chamber 2 can be changed freely.
  • nanoparticle production device 10 differs from nanoparticle production device 1 of the first embodiment in that control device 6 controls nanoparticle production laser device 5 , thawing laser device 12 , and optical trapping laser device 13 in association with constant-temperature device 3 and XYZ stage 11 .
  • nanoparticulation of suspended particles is carried out in the following manner.
  • XYZ stage 11 is moved to set laser light irradiation portion 2 a in treatment chamber 2 .
  • laser irradiation portion 2 a is the region through which laser light passes.
  • the entirety of to-be-treated liquid 8 is then cooled and solidified and made into a solidified body by means of constant-temperature device 3 (cooling solidification step). Thereafter, this temperature is maintained.
  • thawing laser device 12 is activated and made to emit the thawing laser light.
  • the thawing laser light is reflected by first half-mirror 14 and the laser light irradiation portion 2 a of the solidified body is irradiated with the thawing laser light.
  • the thawing laser light is thus absorbed by to-be-treated liquid 8 or the suspended particles in laser light irradiation portion 2 a, heat is thereby generated, and laser light irradiation portion 2 a is thawed by this heat (thawing step).
  • optical trapping laser device 13 is activated and made to emit the optical trapping laser light.
  • the optical trapping laser light is reflected by second half-mirror 15 and the laser light irradiation portion 2 a is irradiated with the optical trapping laser light (optical trapping step).
  • suspended particles of large particle diameter that exist in the thawed laser irradiation portion 2 a gather along optical axis (center of the laser irradiation portion) 17 due to the optical trapping action of the optical trapping laser light.
  • the optical trapping action is stronger the larger the particle diameter of a particle, and selective positioning of particles of large particle diameter along optical axis 17 is thereby enabled.
  • the concentration of suspended particles along optical axis 17 of laser light irradiation portion 2 a thus increases.
  • Such an art provides the merits of preventing the aggregation of nanoparticles with each other at portions outside the laser light irradiation portion and enabling a cooling treatment to be carried out in a comparatively simple manner since thawing of just a localized portion is performed.
  • nanoparticle production laser device S is activated.
  • the nanoparticle production laser light is transmitted successively through first half-mirror 14 and second half-mirror 15 and the laser light irradiation portion 2 a is irradiated with the nanoparticle 6 production laser light (nanoparticle production step).
  • the suspended particles in laser light irradiation portion 2 a are in a state of high concentration.
  • the laser light intensity is normally high at the center of laser light irradiation portion 2 a.
  • the irradiations with laser light by thawing laser device 12 , optical trapping laser device 13 , and nanoparticle production laser device 5 are stopped (laser irradiation stopping step).
  • the cooling of the thawed portion thus begins, and since this portion is localized, rapid cooling solidification occurs naturally.
  • this solidified body By then keeping this solidified body at a low temperature no more than the solidification point of the to-be-treated liquid, the suspended state of the nanoparticles can be maintained over a long period of time.
  • VOPc which is an organic compound
  • the suspended particles are not limited to those of VOPc and may be those of other organic compounds.
  • Ibuprofen, clobetasone butyrate, etc., which are insoluble medical agents, can be cited as examples.
  • water is used as the solvent for suspending VOPc
  • the combination of suspended particles and solvent is not limited thereto, and any combination with which suspended particles are suspended in a solvent may be used.
  • a surfactant for example, SDS or other ionic surfactant, Igepal or other nonionic surfactant -that does not become ionized, Tween, which is permitted to be added to medical products, etc.
  • a surfactant for example, SDS or other ionic surfactant, Igepal or other nonionic surfactant -that does not become ionized, Tween, which is permitted to be added to medical products, etc.
  • a surfactant for example, SDS or other ionic surfactant, Igepal or other nonionic surfactant -that does not become ionized, Tween, which is permitted to be added to medical products, etc.
  • nanoparticulation of higher efficiency is carried out when the to-be-treated liquid is irradiated with the nanoparticle production laser light.
  • the aggregation of the nanoparticles formed is prevented adequately.
  • nanoparticles produced by the above described nanoparticle production methods are used as the nanoparticles to be preserved
  • the nanoparticles preserved by this invention's nanoparticle preservation method is not limited to just the nanoparticles produced by the above-described nanoparticle production methods and may instead be nanoparticles that have been produced by a production method other than the above-described nanoparticle production methods.
  • a sample solution prepared by suspending a VOPc powder in water (VOPc: 0.5 mg/ml), were dispensed in a 10 mm ⁇ 10 mm ⁇ 40 mm rectangular quartz cell, and thereafter the temperature of the sample solution was lowered to 5° C. using a constant-temperature device (131-0040 Constant-Temperature Cell Holder with Temperature Display, made by Hitachi).
  • VOPc 0.5 mg/ml
  • the absorbance of the sample solution after laser light irradiation was then measured by an absorbance measuring device.
  • the result is shown in FIG. 4 .
  • the absorbance was found to be significantly high in the vicinity of 500 to 900 nm, which is the absorbance wavelength range of VOPc. Since when VOPc particles that are suspended in a to-be-treated liquid are made fine, the inherent light absorption of the particles increase due to the increase of surface area, the above result shows that nanoparticles were formed efficiently by the light irradiation treatment. Of the four absorbance curves, the absorbance curve at the lowest position is that prior to laser light irradiation.
  • nanoparticulation treatment of VOPc was carried out as follows using the device of FIG. 2 .
  • XYZ stage 11 was moved to set the laser light irradiation portion in the 10 mm ⁇ 10 mm ⁇ 40 mm rectangular quartz cell. 3 ml of a sample solution, prepared by suspending VOPc powder in water (VOPc: 0.5 mg/ml), was then dispensed in the rectangular quartz cell. Thereafter, using the same constant-temperature device as in Example 1, the sample solution was cooled to and solidified at ⁇ 5° C., thereby obtaining a solidified body.
  • VOPc 0.5 mg/ml
  • the above-mentioned laser light irradiation portion was irradiated with a thawing laser light.
  • optical trapping laser device 13 using a YAG laser (1064 nm) as optical trapping laser device 13 , an optical trapping laser light was emitted and the above-mentioned laser light irradiation portion was irradiated with the optical trapping laser light.
  • the laser light irradiation portion was irradiated with a nanoparticle production laser light. After 10 seconds of irradiation, the laser light irradiation portion of the solidified body became transparent. Comparison of this result with that of Example 1 in consideration of the cross-section of the irradiation laser shows that, since the treatment of making the entire to-be-treated liquid of 3 ml transparent was completed in 15 minutes with Example 1 and in 7 to 8 minutes with Example 2, nanoparticulation occurred at is a higher efficiency than in the case of Example 1.
  • the irradiations with laser light by the argon ion laser, YAG laser, and the third harmonic of the Nd:YAG laser were stopped.
  • the laser light irradiation portion remained transparent. It is thus considered that by rapid cooling of the thawed portion, it was possible to maintain the pseudo-dissolution state of the nanoparticles and adequately prevent the aggregation of the nanoparticles.
  • this invention's nanoparticle production method and production device can be used as a production method and production device that can realize nanoparticulation of high efficiency by lowering of the temperature of the to-be-treated liquid. Furthermore, long-term maintenance of the suspended state of the nanoparticles is enabled by rapid cooling solidification after the nanoparticulation treatment.
  • this invention's nanoparticle preservation method can be used as a preservation method that enables long term preservation of the state in which nanoparticles are suspended.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Optics & Photonics (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Disintegrating Or Milling (AREA)
  • Lasers (AREA)
US10/525,654 2002-08-30 2003-08-28 Process for producing nanoparticle apparatus therefor and method of storing nanoparticle Abandoned US20060103060A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US12/213,977 US7922786B2 (en) 2002-08-30 2008-06-26 Nanoparticle production method and production device and nanoparticle preservation method

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2002255973A JP4293586B2 (ja) 2002-08-30 2002-08-30 ナノ粒子の製造方法及び製造装置
JP2002-255973 2002-08-30
PCT/JP2003/010962 WO2004020086A1 (fr) 2002-08-30 2003-08-28 Procede de production de nanoparticules, appareil associe et procede de stockage de nanoparticules

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US12/213,977 Division US7922786B2 (en) 2002-08-30 2008-06-26 Nanoparticle production method and production device and nanoparticle preservation method

Publications (1)

Publication Number Publication Date
US20060103060A1 true US20060103060A1 (en) 2006-05-18

Family

ID=31972929

Family Applications (2)

Application Number Title Priority Date Filing Date
US10/525,654 Abandoned US20060103060A1 (en) 2002-08-30 2003-08-28 Process for producing nanoparticle apparatus therefor and method of storing nanoparticle
US12/213,977 Expired - Fee Related US7922786B2 (en) 2002-08-30 2008-06-26 Nanoparticle production method and production device and nanoparticle preservation method

Family Applications After (1)

Application Number Title Priority Date Filing Date
US12/213,977 Expired - Fee Related US7922786B2 (en) 2002-08-30 2008-06-26 Nanoparticle production method and production device and nanoparticle preservation method

Country Status (6)

Country Link
US (2) US20060103060A1 (fr)
EP (1) EP1541228B1 (fr)
JP (1) JP4293586B2 (fr)
CN (1) CN1305558C (fr)
AU (1) AU2003261804A1 (fr)
WO (1) WO2004020086A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070264350A1 (en) * 2006-05-15 2007-11-15 Ebara Corporation Water-insoluble medicine
US20070284769A1 (en) * 2006-05-15 2007-12-13 Ebara Corporation Apparatus for forming ultrafine particles
US20080237376A1 (en) * 2006-05-15 2008-10-02 Tsuyoshi Asahi Method of producing medicinal nanoparticle suspension
US20180114867A1 (en) * 2015-03-23 2018-04-26 Universität Duisburg-Essen Method for production of components comprising a schottky diode by means of printing technology
JP2019188364A (ja) * 2018-04-27 2019-10-31 株式会社コガネイ 光照射反応装置

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4545690B2 (ja) 2003-11-20 2010-09-15 浜松ホトニクス株式会社 微粒子の製造方法、及び製造装置
JP4482322B2 (ja) 2003-12-18 2010-06-16 浜松ホトニクス株式会社 微粒子の製造方法、及び製造装置
JP4846248B2 (ja) * 2004-02-27 2011-12-28 学校法人東京理科大学 微結晶粒の製造方法、該微結晶粒を分散してなる固体の製造方法、バイオセンシング用透明発光液体、及び透明発光固体。
JP4786205B2 (ja) 2005-03-14 2011-10-05 浜松ホトニクス株式会社 カーボンナノチューブの加工方法、及び加工装置
TWI388344B (zh) * 2005-08-23 2013-03-11 Celsion Corp 儲存奈米微粒調合物之方法
US9849512B2 (en) * 2011-07-01 2017-12-26 Attostat, Inc. Method and apparatus for production of uniformly sized nanoparticles
CN102921961B (zh) * 2012-11-30 2016-01-20 南京大学 一种飞秒激光制备金属纳米材料的方法
CN105834434B (zh) * 2016-04-27 2017-12-05 广东工业大学 一种粒径分布可控的铜微纳颗粒的化学激光复合制备方法
CN108057406A (zh) * 2017-12-14 2018-05-22 中国科学院长春光学精密机械与物理研究所 一种酞菁纳米材料及其制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4482375A (en) * 1983-12-05 1984-11-13 Mcdonnell Douglas Corporation Laser melt spin atomized metal powder and process
US5582957A (en) * 1995-03-28 1996-12-10 Eastman Kodak Company Resuspension optimization for photographic nanosuspensions
US6068800A (en) * 1995-09-07 2000-05-30 The Penn State Research Foundation Production of nano particles and tubes by laser liquid interaction
US6251159B1 (en) * 1998-12-22 2001-06-26 General Electric Company Dispersion strengthening by nanophase addition
US6939388B2 (en) * 2002-07-23 2005-09-06 General Electric Company Method for making materials having artificially dispersed nano-size phases and articles made therewith
US7144441B2 (en) * 2003-07-03 2006-12-05 General Electric Company Process for producing materials reinforced with nanoparticles and articles formed thereby

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09171920A (ja) * 1995-12-18 1997-06-30 Bridgestone Corp ボンド磁石用組成物
KR20010016692A (ko) * 1999-08-02 2001-03-05 최만수 레이저 가열에 의한 입자 소결 제어를 이용한 구형의 미세입자 제조방법
JP4457439B2 (ja) * 1999-10-14 2010-04-28 Ｄｉｃ株式会社 有機化合物の微粒子の製造方法
CN1180912C (zh) * 2000-12-22 2004-12-22 中国科学院金属研究所 激光气相制备纳米银粒子方法和装置
DE10160817A1 (de) * 2001-12-11 2003-06-26 Degussa Verfahren und Vorrichtung zur Erzeugung von nanoskaligen Pulvern durch Laserverdampfung
JP4545690B2 (ja) * 2003-11-20 2010-09-15 浜松ホトニクス株式会社 微粒子の製造方法、及び製造装置
JP4482322B2 (ja) * 2003-12-18 2010-06-16 浜松ホトニクス株式会社 微粒子の製造方法、及び製造装置

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4482375A (en) * 1983-12-05 1984-11-13 Mcdonnell Douglas Corporation Laser melt spin atomized metal powder and process
US5582957A (en) * 1995-03-28 1996-12-10 Eastman Kodak Company Resuspension optimization for photographic nanosuspensions
US6068800A (en) * 1995-09-07 2000-05-30 The Penn State Research Foundation Production of nano particles and tubes by laser liquid interaction
US6251159B1 (en) * 1998-12-22 2001-06-26 General Electric Company Dispersion strengthening by nanophase addition
US6939388B2 (en) * 2002-07-23 2005-09-06 General Electric Company Method for making materials having artificially dispersed nano-size phases and articles made therewith
US7144441B2 (en) * 2003-07-03 2006-12-05 General Electric Company Process for producing materials reinforced with nanoparticles and articles formed thereby

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070264350A1 (en) * 2006-05-15 2007-11-15 Ebara Corporation Water-insoluble medicine
US20070284769A1 (en) * 2006-05-15 2007-12-13 Ebara Corporation Apparatus for forming ultrafine particles
US20080237376A1 (en) * 2006-05-15 2008-10-02 Tsuyoshi Asahi Method of producing medicinal nanoparticle suspension
US7597278B2 (en) 2006-05-15 2009-10-06 Osaka University Method of producing medicinal nanoparticle suspension
US7815426B2 (en) * 2006-05-15 2010-10-19 Absize Inc. Apparatus for forming ultrafine particles
US20110059183A1 (en) * 2006-05-15 2011-03-10 Ebara Corporation Water-insoluble medicine
US8399024B2 (en) * 2006-05-15 2013-03-19 Ebara Corporation Water-insoluble medicine
US20180114867A1 (en) * 2015-03-23 2018-04-26 Universität Duisburg-Essen Method for production of components comprising a schottky diode by means of printing technology
US10411142B2 (en) * 2015-03-23 2019-09-10 University Duisburg-Essen Method for production of components comprising a schottky diode by means of printing technology
JP2019188364A (ja) * 2018-04-27 2019-10-31 株式会社コガネイ 光照射反応装置
JP7078223B2 (ja) 2018-04-27 2022-05-31 株式会社コガネイ 光照射反応装置

Also Published As

Publication number Publication date
CN1305558C (zh) 2007-03-21
US20080265070A1 (en) 2008-10-30
JP2004089890A (ja) 2004-03-25
EP1541228A4 (fr) 2006-09-20
JP4293586B2 (ja) 2009-07-08
AU2003261804A1 (en) 2004-03-19
WO2004020086A1 (fr) 2004-03-11
CN1671468A (zh) 2005-09-21
EP1541228B1 (fr) 2012-07-11
US7922786B2 (en) 2011-04-12
EP1541228A1 (fr) 2005-06-15

Similar Documents

Publication Publication Date Title
US7922786B2 (en) Nanoparticle production method and production device and nanoparticle preservation method
Zhang et al. Laser synthesis and processing of colloids: fundamentals and applications
Huang et al. Atomistic view of laser fragmentation of gold nanoparticles in a liquid environment
Tsuji et al. Preparation of silver nanoparticles by laser ablation in polyvinylpyrrolidone solutions
Jimenez et al. Laser-ablation-induced synthesis of SiO2-capped noble metal nanoparticles in a single step
JP6076742B2 (ja) 高繰返周波数の超高速パルスレーザ溶発による、有機化合物のナノ粒子の液中生成方法
US7597277B2 (en) Microparticles, microparticle production method, and microparticle production apparatus
US8246714B2 (en) Production of metal and metal-alloy nanoparticles with high repetition rate ultrafast pulsed laser ablation in liquids
CN100423847C (zh) 微粒、微粒的制造方法及制造装置
Dorranian et al. Photoluminescence of ZnO nanoparticles generated by laser ablation in deionized water
Cavicchi et al. Single laser pulse effects on suspended-Au-nanoparticle size distributions and morphology
Jiang et al. Controllably tuning the near-infrared plasmonic modes of gold nanoplates for enhanced optical coherence imaging and photothermal therapy
Khaniabadi et al. Structure, morphology and absorption characteristics of gold nanoparticles produced via PLAL method: Role of low energy X-ray dosage
Chubilleau et al. Laser fragmentation in liquid medium: A new way for the synthesis of PbTe nanoparticles
Arndt et al. Implantation and spectroscopy of metal atoms in solid helium
EP1733836B1 (fr) Procede de traitement pour cristal organique
JP2007045674A5 (ja) フラーレン分散液の製造方法
JP2005125258A (ja) 微粒子、微粒子の製造方法、及び製造装置
Abdulla-Al-Mamun et al. Plasmon-induced photothermal cell-killing effect of gold colloidal nanoparticles on epithelial carcinoma cells
Loicq et al. Non-linear optical measurements and crystalline characterization of CdTe nanoparticles produced by the ‘electropulse’technique
JP4717376B2 (ja) 微粒子の製造方法、及び製造装置
Talukder et al. Power dependence of size of laser ablated colloidal silver nanoparticles
Shibatani et al. Synergistic Effect of High Irradiation Power and Antisolvent Addition for Enhanced Microwave Assisted Nanoparticle Synthesis Process
JP2010144201A (ja) パラジウムナノ粒子およびその製造方法
Atsuya et al. Synergistic E ect of High Irradiation Power and Antisolvent Addition for Enhanced Microwave Assisted Nanoparticle Synthesis Process

Legal Events

Date Code Title Description
AS Assignment

Owner name: HAMAMATSU PHOTONICS K.K., JAPAN

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:KAWAKAMI, TOMONORI;LI, BO;HIRAMATSU, MITSUO;REEL/FRAME:017499/0043;SIGNING DATES FROM 20050303 TO 20050323

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION