WO2003099708A1 - Procede de production de nanoparticules et nanoparticules produites selon ce procede - Google Patents
Procede de production de nanoparticules et nanoparticules produites selon ce procede Download PDFInfo
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- WO2003099708A1 WO2003099708A1 PCT/JP2003/006637 JP0306637W WO03099708A1 WO 2003099708 A1 WO2003099708 A1 WO 2003099708A1 JP 0306637 W JP0306637 W JP 0306637W WO 03099708 A1 WO03099708 A1 WO 03099708A1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/005—Epitaxial layer growth
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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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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
- C30B29/58—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/605—Products containing multiple oriented crystallites, e.g. columnar crystallites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02557—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/0256—Selenides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02587—Structure
- H01L21/0259—Microstructure
- H01L21/02601—Nanoparticles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02623—Liquid deposition
- H01L21/02628—Liquid deposition using solutions
Definitions
- the present invention relates to a method for producing nanoparticles of a compound semiconductor, a nanoparticle produced by the production method, and a composite comprising a nanoparticle and a protein produced in the production process of the production method.
- the energy levels of semiconductor nanoparticles are separated by energy level quantization, and they are controlled as a function of the particle size of the nanoparticles. Therefore, in semiconductor nanoparticles, the peak position of the exciton absorption band that appears slightly lower in energy than the long-wavelength absorption edge of the fundamental absorption of the semiconductor crystal can be controlled by changing the particle size of the semiconductor nanoparticles. It is expected to be used as a light-emitting material or a memory material because it exhibits a different absorption and generation ability of electromagnetic waves than bulk materials. For example, CdSe and ZnSe which are Group II-VI compound semiconductors Is known to fluoresce, but its fluorescence wavelength depends on the size of the particles. In order to utilize such quantum effects of semiconductor nanoparticles, it is necessary to produce nanoparticles with a uniform particle size. It becomes important.
- the method of producing nanoparticles has been performed by a physical pulverization method and a chemical synthesis method.
- physical comminution techniques are widely used to obtain starting materials for firing ceramics.
- chemical synthesis method there is a method of producing gold nanoparticles by reducing chloroauric acid between long-chain organic compounds.
- long-chain organic compounds prevent gold particles from growing and becoming giant.
- a composite of an organic compound and nanoparticles is formed and chemically reacted to produce uniform particles.
- gold nanoparticles with a SAM film formed on the surface are fixed by fixing gold atoms to the material for forming the SAM film and assembling the above materials around the gold atoms.
- micelles containing materials that form the nanoparticles are created, and nanoparticles are produced using chemical reactions in the micelles.
- Apoferritin is a protein that is widely found in the living world and plays a role in regulating the amount of iron, an essential trace element in living organisms.
- the complex of iron or iron compounds with apoferritin is called ferritin.
- FIG. 1 is a schematic diagram showing the structure of apoferritin.
- apoferritin 1 is a globular protein with a molecular weight of about 46,000 consisting of 24 non-covalently assembled monomeric subunits formed from a single polypeptide chain. It is about 12 nm in diameter and has higher thermostability and higher pH stability than normal proteins.
- the iron ions when divalent iron ions are incorporated into apoferritin 1, the iron ions enter through channel 3 and are oxidized at a place called ferrooxidase center (iron oxidation active center) in some subunits. It reaches the holding unit 4 and is concentrated in the negatively charged region on the inner surface of the holding unit 4. Then, the iron atom is 3 0 0 0-4 0 0 to 0 set, ferrihydrite (5 F e 2 0 3 ⁇ 9 H 2 0) is held by the holder 4 in crystalline form.
- the particle diameter of the nanoparticles containing metal atoms held in the holding section 4 is almost equal to the diameter of the holding section 4, that is, about 6 nm.
- the particle diameter of the nanoparticles made of these metals or metal compounds is also approximately equal to the diameter of the holding part 4 of apoferritin, that is, about 6 nm.
- channel 3 On the surface of channel 3 (see Fig. 1), which connects the outside and inside of apoferritin 1, negatively charged amino acids are exposed under conditions of pH 7 to 8, and positively charged F e 2+ ions are incorporated into channel 3 by electrostatic interaction.
- the iron ions sequentially taken in adhere to the nuclei of the crystal, and nuclei composed of iron oxide grow, and nanoparticles having a particle diameter of 6 nm are formed in the holding section 4.
- the above is an outline of the uptake of iron ions and the formation of nanoparticles composed of iron oxide.
- An object of the present invention is to solve the above-mentioned conventional problems, and provides a method for producing nanoparticles capable of obtaining semiconductor nanoparticles having a uniform particle diameter.
- the compound semiconductor nanoparticles are formed in the protein cavity in a solution containing ions of a protein having a cavity therein and an element serving as a raw material of the compound semiconductor. Process.
- the method includes forming nanoparticles of a group II-VI compound semiconductor in a cavity of the protein in a solution containing a protein, a group II element ion, and a group VI element ion.
- group II element referred to in the present specification is a group 12 element of the periodic table, and specifically means Zn and Cd.
- Group VI elements are Group 16 elements of the Periodic Table, specifically, 0, S, and Ce.
- the solution is a complex having the group II element ion as a central metal.
- PC leakage Contains 37 ions.
- a complex ion having the group II element ion as a central metal is contained in the cavity of the protein.
- the solution further contains ammonium ions.
- a complex ion in which the group II element ion is a central metal and ammonia is a ligand is present in the solution.
- a complex ion in which the group II element ion is the central metal and ammonia is a ligand is present in the cavity of the protein.
- the supply of the group VI element ion (X 2 —) into the solution is by adding H 2 NCXNH 2 into the solution.
- the X is S e or S.
- the group II element is zinc (Zn) or cadmium (Cd)
- the group VI element is zeolite (S) or selenium (Se).
- the nanoparticles are formed from at least one compound semiconductor selected from the group consisting of CdSe, ZnSe and 33-113.
- the protein is at least one of apoferritin, Dps protein, CCMV protein, and TMV protein-further comprising a step of removing the protein by heat treatment after forming the nanoparticles. There may be.
- the present invention is a nanoparticle produced by the production method. Further, the present invention is a composite comprising nanoparticles and a protein, which is produced in a production process of the method for producing nanoparticles.
- the protein may have a portion that specifically binds to a specific protein.
- FIG. 1 is a schematic diagram showing the structure of apoferritin.
- FIG. 2 is a flowchart showing a method for producing semiconductor nanoparticles.
- FIG. 3 is a schematic diagram showing step St1 and step St2 shown in FIG.
- FIG. 4 is a schematic diagram showing a reaction considered to be occurring in step St 2 shown in FIG.
- Figs. 5 (a) to (c) are electron micrographs showing the state of formation of nanoparticles.
- FIGS. 6 (a) and (b) are schematic diagrams showing states in which semiconductor nanoparticles having different particle diameters are respectively bound to actin filaments and nuclei of cells.
- FIGS. 7 (a) and (b) are schematic diagrams showing a method of labeling a protein with a semiconductor nanoparticle protein complex using an antibody.
- 8 (a) to 8 (d) are cross-sectional views illustrating a method for manufacturing a nonvolatile memory cell.
- FIG. 9 is a process cross-sectional view showing a method of arranging and fixing the dot bodies two-dimensionally on the surface of the substrate.
- FIG. 10 is a diagram for explaining a method of arranging and fixing the composites two-dimensionally on the surface of the substrate.
- the surface of the cavity has a positive or negative charge and has a potential difference to the outside.
- the channel is large enough to allow ions to pass, and has no obstacles to hinder the passage of ions.
- the protein may be a protein composed of a single subunit or a protein composed of a plurality of subunits.
- the shape of the protein is not limited to a spherical shape, and the protein may have a hollow shape such as a rod shape or a ring shape.
- proteins that satisfy the first to fifth conditions there are many proteins that satisfy the first to fifth conditions, and typical proteins include apoferritin, Dps protein, and virus protein.
- viral proteins include CPMV, CCMV, HSV, Rotavirus, Reovirus, LA-1, Polymoma, CaMV, HPV, Ross River, SpV-4, ⁇ 174, FHV, HRV— 14, viral proteins such as Pioio.
- virus proteins of CPMV and CCMV can be used.
- nanoparticles are formed according to the shape and size of the cavity of the protein to be used.
- nanoparticle refers to a particle having a major axis of 5 O nm or less and a size not less than a size that exists stably as a particle.
- nanoparticles with a major diameter of l nm to 50 nm correspond to nanoparticles.
- Proteins are made from DNA information and replicate in large numbers by known methods It is easy. It is also well known that proteins replicated in large numbers from the same DNA have the same structure with angstrom accuracy. Therefore, it is easy to prepare a protein that satisfies the above first condition.
- apoferritin which is a protein having a function of retaining a metal or a metal compound, is used.
- FIG. 2 is a flowchart showing a method for producing semiconductor nanoparticles of the present embodiment. All the steps of the method of the present embodiment described below are performed at room temperature on a 200 ml scale. Unless otherwise specified, the term “solution” used herein refers to a solution using water as a solvent.
- step St1 50 mgZm1 of apoferritin solution, 10 OmM cadmium acetate solution, 1 M ammonium acetate solution, and 10 OmM aqueous ammonia are prepared. Also, selenourea (H 2 NCSeNH 2 ) is dissolved in a small amount of ethanol (about 101), and pure water is added to make a 10 OmM concentration to prepare a 10 OmM selenourea solution. I do. Since selenourea is unstable when dissolved in water, prepare a selenourea solution immediately before the next step.
- step St2 each solution prepared in step St1 is mixed, and pure water is added until the total volume becomes 200 ml, thereby preparing a reaction solution.
- Apoferritin, cadmium acetate, ammonium acetate, selenourea and ammonium in the above reaction solution Each concentration of your is as shown in Figure 3.
- FIG. 3 is a schematic diagram showing Step St1 and Step St2.
- the reaction proceeds while stirring the reaction solution.
- the reaction starts spontaneously immediately after preparation.
- the reaction solution is further stirred for one day and night.
- the reaction that occurs here is not rapid, but is completed in minutes to hours.
- CdSe is introduced into the apoferritin holding portion, and a CdSe-apoferritin complex (hereinafter, also simply referred to as a complex) is generated.
- Step St3 the reaction solution is placed in a container, and centrifuged at 300,000 rpm for 20 minutes using a centrifuge to remove the precipitate. At this time, the complex exists in the supernatant in a dispersed state.
- step St4 the supernatant liquid after removing the precipitate is further centrifuged at 100,000 rotations per minute for 30 minutes to precipitate the complex.
- step St5 the precipitate obtained in step St4 is suspended in a 15 O mM NaCl solution to prepare a complex solution.
- FIG. 4 is a schematic diagram for explaining a mechanism of forming a CdSe-apoferritin complex.
- Fig. 4 apoferritin shown in Fig. 1 is further simplified for easier understanding. are doing. Therefore, in FIG. 4, the same reference numerals as those in FIG. 1 are used.
- reaction formula 1 Reaction formula 1
- selenourea Since selenourea has no charge, it is uniformly present inside and outside the holding portion 4 of apoferritin 1. Selenourea, when dissolved in water at room temperature, begins to decompose slowly but immediately. All decompositions take several hours and generate S e 2 —.
- step St1 of this embodiment the amount of added ammonia was changed to form CdSe nanoparticles, and the reaction solution was observed with an electron microscope immediately after step St2 in FIG. (A) to (c) are shown.
- Figure 5 (a) ⁇ (c) is, tweezers aqueous ammonia added to the reaction solution tone, 0 mM concentration of ammonia (NH 3) in the reaction solution, respectively, when a 0. 5 mM and 1.
- Omm 5 is an electron micrograph showing the state of formation of nanoparticles.
- ammonium that dissociates from ammonium acetate Nia is very small and is considered to have little effect on the ammonia concentration shown here.
- the C d Se semiconductor nanoparticles are typically indicated by open arrows in FIGS. 5 (a), (b) and (c). As shown in Fig. 5 (a) to (c), the formation of semiconductor nanoparticles of CdSe depends on the concentration of ammonia, and when the concentration of ammonia is 0.5 mM, The formation is best.
- the reaction solution shown in Fig. 5 (a) has a pH of 6.6
- the reaction solution shown in Fig. 5 (b) has a pH of 7.4
- the reaction solution shown in Fig. 5 (c) has a pH of 7. 9 Therefore, it is considered that ammonia coordinates with C d 2+ and stabilizes it, and at the same time, keeps the reaction solution containing no buffer at a high pH, and also has a function of facilitating precipitation of Cd Se.
- the pH of the reaction solution is preferably maintained in the range of pH 7.0 to 9.5. The same effect can be obtained by increasing the mixing ratio of ammonia to 20000 in Table 1.
- semiconductor nanoparticles composed of CdSe can be preferentially formed in apoferritin.
- Proteins, including apoferritin, are made from DNA information and are easily replicated in large numbers by known methods. It is also well known that proteins that have been replicated many times from the same DNA have the same structure with angstrom accuracy. Therefore, all of the hollow holding portions of the apoferritin used in the present embodiment have the same shape.
- the particle size of the semiconductor nanoparticles is determined by the protein, so that semiconductor nanoparticles having a uniform particle size can be obtained. can get.
- the CdSe nanoparticles obtained in the present embodiment in which the reaction solution had the form shown in FIG. 3 were spherical and had a diameter of 6 nm (standard deviation 1 nm). That is, it can be said that nanoparticles having a uniform particle size were obtained.
- apoferritin was used as a protein.
- Dps protein diameter 9 nm, spherical shell-shaped protein having a 4 nm diameter holding portion inside
- Semiconductor nanoparticles with a particle size of 4 nm can be produced.
- a viral protein such as CCMV and TMV
- semiconductor nanoparticles according to the shape of the internal holding portion of each protein can be produced.
- a zinc acetate solution is mixed into the reaction solution instead of the acetic acid dome solution used in the form.
- Other conditions are as described in the present embodiment.
- a thiourea (H 2 NCSNH 2 ) solution is mixed in the reaction solution instead of the selenourea solution used in the present embodiment.
- Other conditions are as described in the present embodiment.
- a zinc acetate solution is mixed in the reaction solution instead of the acetic acid domium solution and a thiourea solution instead of the selenourea solution.
- Other conditions are as described in the present embodiment.
- Group II-VI compound semiconductors are direct-transition wide-bandgap semiconductors, which can utilize such properties in addition to the properties of nanoparticles, and are useful in various applications.
- fluorescent stains such as rhodamine have been used for fluorescence observation of cells and the like.
- fluorescent dyes such as rhodamine are weak in fluorescence, and in a few seconds, do not emit light due to a fluorescent bleaching called quenching.
- the fluorescence extends to the red (longer wavelength side) (called red tilling) and enters the fluorescent region of other fluorescent dyes, causing crosstalk. I do.
- a sharp wavelength filter is required because the difference between the excitation light wavelength irradiated for observing the fluorescence and the fluorescence wavelength from the fluorescent dye is about several tens of nm. For this reason, the number of excitation light devices and wavelength filters required by the number of fluorescent dyes is required, and the configuration of a fluorescence observation device (for example, a fluorescence microscope) is complicated. If the configuration of the fluorescence observation device becomes complicated, it becomes difficult to secure the light amount, and a bright lens is required. Therefore, the design of the fluorescence observation device becomes difficult, and the price of the fluorescence observation device becomes extremely high.
- CdSe semiconductor nanoparticles with a uniform particle size can be obtained for each of several types of particle sizes, it will be possible to label proteins in cells and perform fluorescence observation at very low cost.
- the produced CdSe and ZnSe semiconductor nanoparticles are not uniform in particle size. Particles of various fluorescent wavelengths are mixed. Therefore, semiconductor nanoparticles produced by a conventional physical pulverization method or a chemical synthesis method cannot be used as they are for a fluorescent label. For this reason, the above report requires a precise purification process that separates CdSe and ZnSe semiconductor nanoparticles by nanometer-order particle sizes in order to use them as fluorescent label materials. I have. Therefore, the mass productivity of semiconductor nanoparticles is very low, and the cost for fluorescence observation is also very high.
- the above report proposes that the surface of the semiconductor nanoparticles be coated with an organic material.
- the mass productivity of the semiconductor nanoparticles is further low, and the manufacturing cost for fluorescence observation is extremely high.
- the semiconductor nanoparticles obtained in the first embodiment have a uniform particle size. Therefore, if several types of proteins having different diameters of the holding portion for holding the semiconductor nanoparticles are used, CdSe semiconductor nanoparticles having a uniform particle size can be easily obtained for each of several types of particle sizes, There is no need for a precise purification step to separate semiconductor nanoparticles by particle size. Therefore, it becomes possible to label the protein in the cell and observe the fluorescence at a very low cost.
- amino acid residues are exposed on the surface of the protein.
- Amino acid residues exposed on the surface can be modified by genetic engineering techniques such as recombination. This allows the semiconductor nanoparticle-protein complex to have a positive or negative charge at any position on the surface of the protein complex, Alternatively, hydrophobicity or hydrophilicity can be imparted. Therefore, the dispersion and aggregation of the semiconductor nanoparticles can be controlled without coating the surface of the semiconductor nanoparticles with an organic material or the like.
- FIGS. 7 (a) and (b) are schematic diagrams showing a method of labeling a protein with a semiconductor nanoparticle-protein complex using an antibody.
- the semiconductor nanoparticle-protein complex C1 is a complex composed of the Dps protein 11 and the CdSe semiconductor nanoparticle 14a.
- the semiconductor nanoparticle-protein complex C2 is a composite composed of apoferritin 1 and CdSe semiconductor nanoparticles 4a.
- the semiconductor nanoparticle-protein complexes C1 and C2 contain CdSe semiconductor nanoparticles having a uniform particle size for each of two different particle sizes. Further, the semiconductor nanoparticle-protein complex C 1 specifically binds to protein X, and the semiconductor nanoparticle-protein complex C 2 specifically binds to protein Y. Therefore, by irradiating a single wavelength of excitation light (for example, ultraviolet light), different fluorescent colors are expressed for each of the proteins X and Y, and the two proteins can easily move in the cell 0306637
- a single wavelength of excitation light for example, ultraviolet light
- the semiconductor nanoparticle-protein complex obtained in the first embodiment has a configuration in which the semiconductor nanoparticle is covered with the protein, and therefore, the fluorescence is used by modifying the protein. It is easy to use for observation of a living body.
- CdSe semiconductor nanoparticles are used as the fluorescent material.
- other fluorescent materials ZnSe, CdS, and ZnS, etc.
- non-volatile memory cell including a dot body formed using the nanoparticle overnight protein composite produced in Embodiment 1 as a floating gate will be described.
- 8 (a) to 8 (d) are process cross-sectional views illustrating a method for manufacturing the nonvolatile memory cell of the present embodiment.
- an element isolation oxide film 102 surrounding the active region is formed on the p-type Si substrate 101 by the LO COS method, and then a tunnel insulating film is formed on the substrate.
- a gate oxide film 103 functioning as a gate oxide film is formed by a thermal oxidation method.
- a dot body 104 made of nanoparticles having a particle size of about 6 nm is formed on the substrate. The method for forming the dot body 104 on the substrate will be described later.
- an SiO 2 film for filling the dot body 104 is deposited on the substrate by sputtering or CVD.
- an Al film is deposited on the substrate.
- One Zui using the photoresist mask P r 1, a silicon oxide film serving as the S I_ ⁇ 2 film and A 1 film Pas evening insulating film by performing an training
- first and second n-type diffusion layers 107a and 107b are formed.
- a well-known method is used to form an interlayer insulating film 108, open a contact hole 109 in the interlayer insulating film 108, and bury tungsten in the contact hole 109.
- the formation of the tungsten plug 110 and the formation of the first and second aluminum wirings 111 and 111b are performed.
- the P-type Si substrate is used as the substrate.
- an n-type Si substrate may be used, and further, a compound semiconductor such as GaAs and other semiconductors may be used.
- a substrate may be used.
- the method for forming the dot body 104 on the substrate is not limited to the method described below, and other known methods can be applied.
- the nanoparticle-protein complex (hereinafter, abbreviated as “complex”) 150 obtained in Embodiment 1 above is prepared, and this complex 150 is attached to the substrate 1. Place on 30 surfaces. Thus, a composite film in which the composite 150 is arranged on the surface of the substrate 130 with high density and high precision is formed.
- the substrate 130 is a process shown in FIG. 8 (a) in which a device isolation oxide film 102 surrounding the active region is formed on the p-type Si substrate 101 by the LOCOS method.
- a gate oxide film 103 serving as a tunnel insulating film is formed on the Pointed out. The same applies to the following description.
- the protein 140 of the complex 150 is removed, and only the nanoparticles 104a are left. A dot body 104 is formed.
- the complex 150 is arranged with high density and high precision on the surface of the substrate 130, ie, two-dimensionally on the surface of the substrate 130.
- a method of arranging and fixing in a shape is described.
- a method described in Japanese Patent Application Laid-Open No. 11-45990 will be described below with reference to FIG.
- a liquid 160 in which the complex 150 is dispersed is prepared.
- a liquid in which the nanoparticle-protein complex is dispersed in a mixed solution (pH 5.8) of a 2 OmM NaC1 solution and a 2 OmM MES buffer solution is used as the liquid 160.
- MES means 2-morpholinoethanesulfonic acid.
- PBLH P01y-1-Benzil-L-Histidin
- a polypeptide film 170 made of PBLH is formed on the surface of the liquid 170. After this, adjust the pH of the liquid 160.
- the complex 150 adheres to the polypeptide membrane 100 with time, and a two-dimensional crystal of the complex 150 is formed. This is because the polypeptide membrane 170 has a positive charge, while the complex 150 has a negative charge.
- the substrate 130 is placed (floated) on the polypeptide film 170, and the polypeptide film 170 is attached to the substrate 130. Let it. PC so-called back 637
- the nanoparticle 104 a remains on the 0 as a two-dimensional, high-density, high-precision, regularly arranged dot body 104.
- the nanoparticles 104a held by the composite 150 are caused to appear two-dimensionally on the substrate 130, and In addition, it is possible to form dot bodies 104 arranged with high precision.
- the memory cell 100 of the present embodiment includes an A1 electrode 106 functioning as a control gate, and first and second n cells functioning as a source or a drain. It has a MOS transistor (memory cell transistor) consisting of a diffusion layer 107a and 107b, and the amount of electric charge stored in the dot body 104 functioning as a floating gate. This is a non-volatile memory cell utilizing the change in threshold voltage.
- This non-volatile memory cell can function as a memory for storing binary values, but by controlling not only the presence / absence of charges stored in the dot body 104 but also the amount of charges stored, it is possible to obtain three or more values. Multi-valued memory can also be realized.
- FN Lowler-Nordhe im
- Use current or direct tunneling current When erasing data, FN (Fowler-Nordhe im) Use current or direct tunneling current.
- FN current through an oxide film direct tunneling current, or channel hot electron (CHE) injection is used for writing data overnight.
- CHE channel hot electron
- the floating gate is formed of nanoparticles having a small particle size that can function as a quantum dot, the amount of accumulated charge is small. Therefore, the amount of current for writing and erasing can be reduced, and a low power consumption nonvolatile memory cell can be configured.
- the nanoparticles constituting the floating gate have a uniform particle size, the characteristics at the time of charge injection and extraction are uniform among the nanoparticles. Control can be easily performed in these operations.
- Nanoparticles of iron, cobalt, etc. which have been obtained using apoferritin, exist as oxides inside apoferritin. For this reason, when a dot body is formed using nanoparticles such as iron and cobalt, in order to make the nanoparticles into a dot body having charge retention characteristics in the step shown in FIG. 8 (b), The nanoparticles need to be reduced.
- the nanoparticles used in the present embodiment such as CdSe, ZnSe, CdS, ZnS, FePt, and CoPt, obtained by the first embodiment, can be used without reduction. Has retention characteristics. This eliminates the need for a nanoparticle reduction step. Therefore, it is possible to reduce the cost for forming the dot body. (Other embodiments)
- nanoparticles can be integrated on a substrate at a nanometer scale. Therefore, for example, it is thought that it is also possible to fabricate an arithmetic element utilizing transfer of light energy between semiconductor nanoparticles that generate fluorescence.
- semiconductor nanoparticles having a uniform particle size can be obtained.
- excitation light is applied to semiconductor nanoparticles with a uniform particle size, they emit fluorescent light of a specific wavelength.
- Cobalt acetate solution in place of acetic force Domiumu solution used in 1, mixing the K 2 P t C 1 4 solution to the reaction solution instead of Serre Bruno urea solution.
- Other conditions are as described in the first embodiment.
- the semiconductor nanoparticles of the present invention can be used for various light-emitting materials and storage materials by utilizing their characteristics. For example, chemical sensing, DNA sequencing, high-throughput screening, fluorescence polarization inomasthesia, time-gated inomasthesia, time-resolved inomasthesia, enzyme-linked immunosorbent assay (ELISA) assays, filtration tests, and targeted evenings Available to Further, the semiconductor nanoparticles of the present invention are blended with a polymer or the like to form a thin film. It can also be used for play panels, light-emitting diodes, super-resolution films for optical disks, optical waveguides, etc.
- ELISA enzyme-linked immunosorbent assay
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE60328492T DE60328492D1 (de) | 2002-05-28 | 2003-05-28 | Verfahren zur erzeugung von nanoteilchen |
EP03730654A EP1514838B1 (en) | 2002-05-28 | 2003-05-28 | Process for producing nanoparticles |
AU2003241813A AU2003241813A1 (en) | 2002-05-28 | 2003-05-28 | Process for producing nanoparticle and nanoparticle produced by the process |
JP2004507375A JP3683265B2 (ja) | 2002-05-28 | 2003-05-28 | ナノ粒子の製造方法及び該製造方法によって製造されたナノ粒子 |
US10/727,648 US7129058B2 (en) | 2002-05-28 | 2003-12-05 | Method of production of a nanoparticle of a compound semiconductor in a cavity of protein |
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EP (1) | EP1514838B1 (ja) |
JP (1) | JP3683265B2 (ja) |
AU (1) | AU2003241813A1 (ja) |
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- 2003-05-28 AU AU2003241813A patent/AU2003241813A1/en not_active Abandoned
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Also Published As
Publication number | Publication date |
---|---|
EP1514838B1 (en) | 2009-07-22 |
US20040110347A1 (en) | 2004-06-10 |
DE60328492D1 (de) | 2009-09-03 |
EP1514838A1 (en) | 2005-03-16 |
JPWO2003099708A1 (ja) | 2005-09-22 |
US7129058B2 (en) | 2006-10-31 |
EP1514838A4 (en) | 2008-06-25 |
AU2003241813A1 (en) | 2003-12-12 |
JP3683265B2 (ja) | 2005-08-17 |
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