WO2016052373A1 - Poudre de cuivre - Google Patents

Poudre de cuivre Download PDF

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Publication number
WO2016052373A1
WO2016052373A1 PCT/JP2015/077253 JP2015077253W WO2016052373A1 WO 2016052373 A1 WO2016052373 A1 WO 2016052373A1 JP 2015077253 W JP2015077253 W JP 2015077253W WO 2016052373 A1 WO2016052373 A1 WO 2016052373A1
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Prior art keywords
copper powder
copper
mass
raw material
resin
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PCT/JP2015/077253
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English (en)
Japanese (ja)
Inventor
隆 向野
善仁 後藤
Original Assignee
三井金属鉱業株式会社
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Application filed by 三井金属鉱業株式会社 filed Critical 三井金属鉱業株式会社
Priority to JP2016551999A priority Critical patent/JP6303022B2/ja
Publication of WO2016052373A1 publication Critical patent/WO2016052373A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form

Definitions

  • the present invention relates to copper powder.
  • Copper powder is suitably used as a raw material for conductive compositions such as conductive paste.
  • the conductive composition is obtained by dispersing copper powder in a vehicle containing a binder resin and an organic solvent.
  • the conductive composition is used, for example, for forming an electric circuit or forming an external electrode of a ceramic capacitor.
  • Patent Document 2 describes a copper powder containing any one of Al, Mg, Ge, and Ga.
  • the copper powder described in Patent Documents 1 and 2 the copper powder is prevented from being oxidized by containing an element other than copper in the copper powder. Therefore, the element contained in the copper powder remains in the conductor formed from the conductive composition containing the copper powder. Depending on how the conductor is used and where it is used, the use of copper powder may be limited because the element may adversely affect the bonding reliability and conduction characteristics.
  • the object of the present invention is to improve copper powder. More specifically, the surface stability is excellent without using different elements, the denseness of the conductive composition, the adhesion with the oxygen-containing insulating material, and the uniform distribution. The object is to provide copper powder with excellent properties.
  • the present invention provides a peak intensity P 1 of Cu (I) with respect to a peak intensity P 2 of Cu (II) and A copper powder having a value of P 2 / (P 0 + P 1 ), which is a ratio of the peak intensity P 0 of Cu (0), is 0.15 or more and 1 or less.
  • this invention is as a suitable manufacturing method of the said copper powder, Copper which performs oxidation treatment by leaving the dried raw material copper powder to stand for 20 minutes or more and 650 minutes or less in an air atmosphere having a relative humidity of 40% RH to 80% RH and a temperature of 20 ° C to 120 ° C.
  • a method for producing a powder is provided.
  • the copper powder of the present invention is composed of an aggregate of copper particles.
  • the copper powder of the present invention consists essentially of copper particles, but it is allowed to contain inevitable impurities. Moreover, you may make the copper powder of this invention contain other powders etc. as needed.
  • the copper powder of this invention has one of the characteristics in the oxidation state of the copper which exists in the surface of a copper particle.
  • the copper particles constituting the copper powder of the present invention are metallic copper (that is, Cu (0)), monovalent copper (that is, Cu (I)), and divalent copper (that is, Cu) on the surface of the copper particles.
  • the ratio of (II)) is unique.
  • the abundance ratio of copper having various valences can be measured using an X-ray photoelectron spectrometer (XPS). According to XPS measurement, X-ray photoelectron spectroscopy spectra of various elements are obtained. In XPS, quantitative analysis can be performed on elemental components at a depth of about 10 nm from the surface of the copper particles.
  • the ratio of P 2 / (P 0 + P 1 ), which is the ratio of the peak intensity P 0 of Cu (0), is preferably 0.15 or more and 1 or less, more preferably 0.3 or more and 0.9 or less. Yes, more preferably 0.4 or more and 0.7 or less.
  • the value of P 2 / (P 1 + P 0 ) is referred to as “copper oxidation rate”.
  • the peak intensity is the height of the peak.
  • the peak of Cu (II) is mainly derived from CuO and Cu (OH) 2 and is observed in the range of 934.0 eV or more and 936.0 eV or less. Since these peaks are observed at the same position, they cannot be distinguished from each other.
  • the peak of Cu (I) is mainly derived from Cu 2 O.
  • the Cu (0) peak is derived from metallic copper. Since the peak of Cu (I) and the peak of Cu (0) are observed at the same position in the range of 930.0 eV to 933.5 eV, the two cannot be separated. Therefore, in the present invention, the definition of the copper oxidation rate is as described above.
  • the conductor obtained from the conductive composition containing the copper powder of the present invention can be made into a dense structure.
  • the affinity between the conductive composition and the oxygen-containing insulating material is high, the adhesion of the electronic component to the base material or the dielectric material is increased, and an electronic component with high adhesion reliability can be obtained. Therefore, the electrode for electronic components can be suitably manufactured using the copper powder of the present invention.
  • the conductive composition contains glass frit
  • the familiarity between the copper particles, the ceramic material, and the glass frit is improved when the conductive composition is used as an electrode of a ceramic electronic component. Therefore, when used as a conductive composition for ceramic electronic components that require sintering, it is possible to effectively prevent segregation of glass components during sintering. This also allows the conductor to have a dense structure.
  • the copper powder of this invention does not contain dissimilar elements other than copper substantially, it has an advantage also in the point that there are few restrictions of a use scene. “Substantially free of different elements” means that when the copper powder is subjected to elemental analysis, the total content of different elements other than copper and oxygen is 0.1% by mass or less. The suitable manufacturing method of the copper powder which satisfies the said copper oxidation rate is mentioned later.
  • the peak intensities P 0 , P 1 and P 2 described above have a ratio of P 2 : (P 0 + P 1 ) of 15:85 to 50:50, particularly 23:77 to 47:53, especially 29:71. It is also preferable from the viewpoint of increasing the oxidation resistance of the copper powder to be 41:59.
  • the measuring method of the copper oxidation rate of the copper particles by XPS is as follows.
  • Quantum 2000 manufactured by ULVAC-PHI Co., Ltd. can be used.
  • X-ray source Al—K ⁇ ray (1486.8 eV) can be used.
  • the condition of the X-ray source can be 17 kV ⁇ 0.023 A, for example.
  • the charge correction can be performed with the SiO 2 binding energy of 103.2 eV.
  • the beam diameter was 200 microns (40 W), and measurement was performed in a range of about 300 ⁇ 900 microns.
  • the peak intensities P 0 , P 1 and P 2 described above are in the range of 934.0 eV or more and 936.0 eV or less for Cu (II), and 930.0 eV or more and 933.5 eV or less for Cu (0) and Cu (I). It is calculated from the highest count number (c / s) in the range. These can be measured by a single copper particle, and can also be measured by a mixture with a binder component of a conductive composition. In that case, what is necessary is just to wash
  • the electrode member is a neutral organic solvent (ether, ketone, lactone, aromatic
  • ether, ketone, lactone aromatic
  • the copper powder of the present invention is characterized by a low oxygen content in addition to the surface oxidation state of the copper particles as described above.
  • the copper powder of the present invention preferably has an oxygen content of 0.15% by mass or more and 1.2% by mass or less, and preferably 0.4% by mass or more and 1.0% by mass or less. Further preferred.
  • a conductive composition is prepared using the copper powder of the present invention having an oxygen content within this range, and a conductor is formed from the conductive composition, the conductor is a dense one with few voids in the fired film. Become.
  • the conductive composition using the copper powder of the present invention in which the oxygen content is in this range has a high affinity with the oxygen-containing insulating material and tends to have high adhesion.
  • the oxygen-containing insulator examples include oxide ceramics.
  • oxide ceramics include oxide ceramics of single metal species such as alumina, zirconia, titania, ferrite, magnesia, silica, and mixtures thereof, and composite metal oxide ceramics such as barium titanate and strontium titanate. Is mentioned.
  • other oxygen-containing insulators include resins in which oxygen is included in the structure.
  • oxygen-containing resin examples include epoxy resin, cyanate resin, bismaleimide triazine resin (BT resin), polyphenylene ether resin, phenol resin, polyimide resin and polyamide resin, unsaturated polyester resin, liquid crystal polymer, polyethylene terephthalate resin, polyethylene naphthalene.
  • An insulating resin such as a resin may be used.
  • the resin contains filler particles made of various oxides such as silica and alumina, the resin has good adhesion to the conductive composition using the copper powder of the present invention.
  • the oxygen content in the copper powder of the present invention is measured by the following method.
  • an oxygen / nitrogen analyzer EMGA-620 manufactured by Horiba, Ltd. can be used as an apparatus. After weighing 0.1 g of copper powder and putting it in a nickel capsule, the oxygen content can be determined by burning it in a graphite crucible.
  • the copper powder of the present invention has a volume cumulative particle size D 50 at a cumulative volume of 50% by volume measured by a laser diffraction / scattering particle size distribution measurement method of 0.3 ⁇ m or more and 10 ⁇ m or less, particularly 1.0 ⁇ m or more and 5.5 ⁇ m or less. preferable.
  • a volume cumulative particle size D 50 at a cumulative volume of 50% by volume measured by a laser diffraction / scattering particle size distribution measurement method of 0.3 ⁇ m or more and 10 ⁇ m or less, particularly 1.0 ⁇ m or more and 5.5 ⁇ m or less. preferable.
  • the particle size of the copper particles constituting the copper powder is reduced to this level, the copper particles are easily oxidized due to an increase in the specific surface area.
  • the copper powder of the present invention the copper on the surface of the copper particles As a result, the progress of oxidation due to changes over time can be prevented.
  • the volume cumulative particle diameter D 50 of the above can be carried out, for example, by the following method.
  • 0.1 g of a measurement sample is mixed with 100 ml of a 20 mg / L aqueous solution of sodium hexametaphosphate and dispersed with an ultrasonic homogenizer (US-300T manufactured by Nippon Seiki Seisakusho) for 10 minutes. Thereafter, the particle size distribution is measured using a laser diffraction / scattering particle size distribution measuring apparatus, for example, Microtrack MT-3000 manufactured by Nikkiso Co., Ltd.
  • the copper powder of the present invention may be used after being sintered, or may be used in the form of a powder that is not sintered.
  • the copper powder preferably has a shrinkage start temperature of 480 ° C. or higher and 620 ° C. or lower. In particular, it is preferably 500 ° C. or higher and 580 ° C. or lower.
  • a conductive composition is prepared using the copper powder of the present invention having a shrinkage start temperature in this range, and a conductor is formed from the conductive composition, a “sink” of the fired film due to low temperature shrinkage, or conversely, insufficient firing. Thus, a fired film with less “necking failure” can be formed.
  • the shrinkage start temperature can be measured by a thermomechanical analyzer (TMA).
  • TMA thermomechanical analyzer
  • EXSTAR60006TMA / SS6200 manufactured by Seiko Instruments Inc. can be used as the measuring device.
  • a sample for measuring the shrinkage start temperature for example, a cylindrical molded body is used in which 0.2 g of copper powder weighed in advance is placed in an aluminum case with an inner diameter of 3.8 mm ⁇ and molded with a load of 4835N.
  • This cylindrical molded body was mounted on a thermomechanical analyzer (TMA), and the thermal expansion coefficient (%) in the vertical direction when the temperature was raised at a rate of 10 ° C./min under a load of 98 mN and nitrogen was monitored. Measure the temperature (° C) that first changed from positive to negative. That temperature can be defined as the shrinkage onset temperature.
  • TMA thermomechanical analyzer
  • the copper particles constituting the copper powder of the present invention are not particularly limited in shape, and can be used in various shapes such as a spherical shape, a flake shape, a plate shape, and a dendritic shape. What shape copper particles are used may be appropriately determined according to the specific application of the copper powder of the present invention.
  • the shape of the copper particles generally depends on the manufacturing method. Spherical copper particles can be produced, for example, by an atomization method or a wet reduction method.
  • the flaky particles can be produced, for example, by mechanically plastically deforming spherical particles.
  • the plate-like particles can be produced, for example, by a wet reduction method.
  • Dendritic copper particles can be produced, for example, by an electrolytic method.
  • the copper powder of the present invention may be a mixture of copper particles having various shapes.
  • the copper particle which comprises the copper powder of this invention exhibits each said shape
  • the copper powder of this invention is observed by electron microscope observation (for example, 1000 time)
  • grains which exhibit said each shape Meaning that the number accounts for 80% or more.
  • the copper powder of this invention is suitably manufactured by oxidizing the raw material copper powder manufactured by various methods on a suitable condition in a predetermined atmosphere.
  • the method for producing the raw material copper powder there are no particular restrictions on the method for producing the raw material copper powder, but when producing copper powder composed of spherical copper particles, for example, it is preferable to use the atomizing method, which produces fine copper powder having an average particle size of 3 ⁇ m or less. In this case, a wet method is preferable.
  • a gas atomizing method or a water atomizing method can be preferably employed.
  • a gas atomizing method In order to make the particle shape uniform, it is preferable to employ a gas atomizing method.
  • a water atomizing method when the particles are miniaturized.
  • the high pressure atomization method is particularly preferable because the particles can be produced finely and uniformly.
  • the high-pressure atomizing method is a method of atomizing at a water pressure of about 50 MPa to 150 MPa in the water atomizing method.
  • atomization is performed at a gas pressure of about 0.5 MPa to 3 MPa.
  • a reduction precipitation method in which a reducing agent is added to a slurry obtained by adding an alkaline aqueous solution to a copper salt aqueous solution can be employed.
  • first reducing agents such as reducing sugar, hypophosphorous acid and sodium sulfite are added to the slurry to prepare a cuprous oxide slurry, and then hydrazine such as hydrated hydrazine and hydrazine sulfate.
  • a two-step reduction method in which a strongly basic reducing agent such as a compound or sodium borohydride is added is preferred.
  • the raw material copper powder may be classified before being subjected to oxidation treatment. This classification can be easily carried out by separating coarse powder and fine powder from the obtained raw material copper powder using an appropriate classification apparatus so that the target particle size becomes the center. Classification, the value of D 50 of the raw material copper powder, is preferably performed such that the ranges set forth above.
  • Suitable oxidation conditions include, for example, conditions for standing in an air atmosphere having a relative humidity of 40% RH to 80% RH and a temperature of 60 ° C. to 120 ° C. as industrial treatment conditions.
  • the treatment time is on condition that the atmospheric conditions are within the above range. It is preferably 20 minutes or longer and 650 minutes or shorter, more preferably 30 minutes or longer and 600 minutes or shorter, and even more preferably 30 minutes or longer and 180 minutes or shorter.
  • the relative humidity is low, the oxidation rate tends to be slow.
  • the temperature may be set higher.
  • the treatment temperature is preferably 70 ° C. or more and 130 ° C. or less.
  • the treatment temperature is 60 ° C. or more and 90 ° C. or less. Is preferred.
  • the copper powder to be oxidized for example, dry powder having a low moisture content can be used.
  • the moisture content can be set to 0.1% by mass or less, for example.
  • the oxidation rate tends to be slow, but the oxidation rate can be increased by adding moisture to the copper powder.
  • the oxidation treatment of the copper powder can be performed in a state where moisture is added in the range of 1% by mass to 5% by mass with respect to the mass of the dry copper powder.
  • the target copper powder can be successfully produced.
  • the copper powder thus obtained is preferably sealed in a non-moisture permeable material container and stored at a temperature of room temperature (25 ° C.) or lower for the purpose of maintaining the oxidized state of the copper particle surface. .
  • the copper powder of the present invention has excellent conductive properties, high oxidation resistance, and good compatibility with glass frit, a conductive resin composition such as a conductive paste or a conductive adhesive, or a conductive paint
  • a conductive resin composition such as a conductive paste or a conductive adhesive, or a conductive paint
  • it can be suitably used as a main constituent material of various conductive materials.
  • the copper powder of the present invention may be mixed with a binder and a solvent. By doing so, a high-temperature fired conductive paste can be obtained. Or the copper powder of this invention can also be mixed with a binder and a solvent, and also a hardening
  • binder examples include, but are not limited to, a liquid epoxy resin, an acrylic resin, a phenol resin, and an unsaturated polyester resin.
  • solvent examples include terpineol, ethyl carbitol, carbitol acetate, butyl cellosolve, butyl carbitol acetate and the like.
  • curing agent examples include 2-ethyl 4-methylimidazole.
  • the curing accelerator include tertiary amines, tertiary amine salts, imidazoles, phosphines, phosphonium salts and the like.
  • the conductive paste when used for an oxide ceramic electronic component that needs to be sintered, it is preferable to further mix a glass frit in the conductive paste for the purpose of improving adhesion to the oxide ceramic.
  • a glass frit for example, silica as an essential component, alumina, boron oxide, calcium carbonate, titanium oxide, zinc oxide, bismuth oxide, vanadium oxide, phosphoric acid, antimony oxide, iron oxide, tellurium oxide, tin oxide, cerium oxide, Examples thereof include a mixture obtained by heating, melting and pulverizing a mixture to which at least one oxide selected from the group consisting of lanthanum oxide and tin oxide is added.
  • the conductive paste containing the copper powder of the present invention can be suitably used, for example, for forming a conductor circuit by screen printing or for electrical contact members of various electronic components.
  • electronic components for example, internal electrodes of multilayer ceramic capacitors, chip components such as inductors and resistors, single plate capacitor electrodes, tantalum capacitor electrodes, resin multilayer substrates, low temperature co-fired ceramic (LTCC) multilayer substrates, antenna switch modules, PA modules and high frequency active filters And the like.
  • insulating materials for ceramic electronic parts include oxide ceramics such as alumina, zirconia, titania, ferrite, magnesia, and silica, and ceramic composite oxides such as barium titanate and strontium titanate.
  • Electrodes for printed wiring boards such as flexible printed circuit boards (FPCs) and build-up multilayer wiring boards for electronic components that use resin as an insulating material
  • electromagnetic shielding films for PDP front and back plates PDP color filters, and crystals
  • conductive adhesive EMI shield
  • RF-ID membrane switch
  • PC keyboard anisotropic conductive film
  • ACF / ACP anisotropic conductive film
  • the resin When using a resin as the insulating material, specific examples of the resin include epoxy resin, cyanate resin, bismaleimide triazine resin (BT resin), polyphenylene ether resin, phenol resin, polyimide resin, polyamide resin, unsaturated polyester resin, Examples thereof include an insulating resin such as a liquid crystal polymer, a polyethylene terephthalate resin, and a polyethylene naphthalene resin.
  • the resin may also contain filler particles made of various oxide inorganic particles such as silica and alumina.
  • the obtained copper powder was classified by a classifier (“Turbo Classifier (trade name) TC-25 (model number)” manufactured by Nissin Engineering Co., Ltd.), and the classified copper powder was used as the raw material copper powder A.
  • the raw material copper powder A was a spherical dry powder, and the D 50 and oxygen content ratios were as shown in Table 1 below.
  • the raw material copper powder B was obtained in the same manner as the raw material copper powder A, except that the classification point of the classifier was changed.
  • the raw material copper powder B was a spherical dry powder, and the D 50 and oxygen content ratios were as shown in Table 1 below.
  • the raw material copper powder C was obtained in the same manner as the raw material copper powder A, except that the classification point of the classifier was changed.
  • the raw material copper powder C was a spherical dry powder, and the D 50 and oxygen content ratios were as shown in Table 1 below.
  • Example 1 1000 g of the raw material copper powder A was left in a constant temperature and humidity chamber adjusted to 80 ° C. and 80% RH for 30 minutes and subjected to an oxidation treatment in an air atmosphere. Thus, the target copper powder was obtained.
  • Example 2 The target copper powder was obtained in the same manner as in Example 1 except that the raw material copper powder shown in the same table was oxidized under the conditions shown in Table 2 below.
  • Examples 11 and 12 The same as Example 1 except that 3% by mass of water is added to the mass of the raw material copper powder shown in Table 2 and the raw copper powder is moistened under the conditions shown in the same table. Thus, the intended copper powder was obtained.
  • Example 13 The same as Example 1 except that 1% by mass of water is added to the mass of the raw material copper powder shown in Table 2 and the raw copper powder is moistened under the conditions shown in the same table. Thus, the intended copper powder was obtained.
  • Example 5 The target copper powder was obtained in the same manner as in Example 1 except that the raw material copper powder shown in the same table was oxidized under the conditions shown in Table 2 below.
  • Example 8 Example 1 except that 3% by mass of water is added to the mass of the raw material copper powder shown in Table 2 below and the raw copper powder is moistened under the conditions shown in the same table. In the same manner as above, the intended copper powder was obtained.
  • a conductive paste (1) To the copper powder obtained in Examples and Comparative Examples, terpineol and acrylic resin were added and mixed to prepare a conductive paste (1).
  • the proportion of copper powder in the conductive paste (1) was 70% by mass, the proportion of terpineol was 25% by mass, and the proportion of acrylic resin was 5% by mass.
  • This conductive paste (1) was applied on an alumina substrate with a film thickness of 50 ⁇ m to form a coating film.
  • This coating film was baked at 845 ° C. for 20 minutes in a nitrogen atmosphere to obtain a baked film.
  • the surface of the obtained fired film was magnified with a scanning electron microscope (1000 times), and images of 10 fields of view were taken.
  • the void area ratio is a value obtained by calculating the area of voids (5 ⁇ m or more) included in one visual field by image analysis and arithmetically averaging the values of the ten visual fields. If the void area is too large, the denseness is insufficient. Conversely, if the void area is too small, the denseness is too high and adversely affects the glass distribution uniformity described later. The quality of the denseness was evaluated in the following three stages.
  • ⁇ The void area ratio is 1% or more and less than 3%, or more than 7% and 10% or less.
  • X Void area ratio is less than 1% or more than 10%.
  • Adhesion of fired film II The adhesiveness of the fired film was evaluated from another viewpoint. Specifically, after the fired film is immersed in the ultrasonic cleaner for 30 seconds together with the substrate, the surface of the fired film is observed with a scanning electron microscope (1000 times), and the fired film in an observation field of about 100 ⁇ m square is observed. The quality of adhesion was evaluated in the following three stages. A: No peeling of the fired film is observed. ⁇ : 70% or more of the fired film area is in close contact. X: The area of the fired film in close contact is less than 30%.
  • the surface of the fired film was subjected to EDX analysis on an image obtained at a field of view of about 100 ⁇ m square and 1000 times, and the glass distribution uniformity was evaluated from the amount of Si derived from the glass frit.
  • the evaluation criteria are as follows.
  • the amount of Si is an amount defined by Si ⁇ 100 / (Si + Cu).
  • Si and Cu represent peak intensities of Si and Cu in EDX analysis.
  • ⁇ Si amount is 0.5% or more and less than 1%, or more than 10% and 20% or less
  • X The amount of Si is less than 0.5% or more than 20%.
  • A Two or more items among the denseness I, the adhesion II, and the uniformity evaluation are A.
  • ⁇ One item or more among the denseness I, the adhesiveness II, and the uniformity evaluation is ⁇ .
  • X Among the denseness I, the adhesiveness II and the uniformity evaluation, there is x in one or more items.
  • the copper powder obtained in each example has a higher oxidation start temperature and superior oxidation resistance compared to the copper powder of the comparative example.
  • the fired film manufactured using the copper powder obtained in each example as a raw material has a higher film density than the fired film manufactured using the copper powder of the comparative example as a raw material, and copper powder and glass It turns out that familiarity with is good.
  • copper powder excellent in shrinkage temperature control is provided. Since this copper powder has good compatibility with the glass frit at the time of firing, a fired film having excellent denseness can be obtained by using this copper powder. Moreover, when this copper powder is made into a conductive composition, it is possible to obtain an electronic component having a high affinity with an oxygen-containing insulating material and a high adhesion reliability.

Abstract

Selon la présente invention, cette poudre de cuivre présente un spectre de spectroscopie photoélectronique X (XPS) qui est obtenu par mesure de la surface de particules de cuivre à l'aide d'un spectroscope photoélectronique X, dans lequel le rapport P2/(P1+P0), qui est le rapport de l'intensité de crête P1 de Cu (I) et de l'intensité P0 de Cu(0) avec l'intensité de crête P2 de Cu(II), est de 0,15-1. La teneur proportionnelle en oxygène est de préférence de 0,15-1,2 % en masse. Le diamètre de particules d'accumulation volumique D50 au niveau d'un volume d'accumulation de 50 % en volume, tel que mesuré par la technique de classement granulométrique de particules par diffusion de lumière, est de préférence de 0,3–10 µm.
PCT/JP2015/077253 2014-10-03 2015-09-28 Poudre de cuivre WO2016052373A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018181482A1 (fr) * 2017-03-31 2018-10-04 三井金属鉱業株式会社 Particules de cuivre et leur procédé de fabrication
JP2021055127A (ja) * 2019-09-27 2021-04-08 Dic株式会社 銅／酸化銅微粒子ペースト

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