WO2010073493A1 - セラミック電子部品の製造方法およびセラミック電子部品 - Google Patents
セラミック電子部品の製造方法およびセラミック電子部品 Download PDFInfo
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- WO2010073493A1 WO2010073493A1 PCT/JP2009/006493 JP2009006493W WO2010073493A1 WO 2010073493 A1 WO2010073493 A1 WO 2010073493A1 JP 2009006493 W JP2009006493 W JP 2009006493W WO 2010073493 A1 WO2010073493 A1 WO 2010073493A1
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- ceramic
- ceramic body
- external electrode
- oil repellent
- repellent treatment
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 75
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/228—Terminals
- H01G4/232—Terminals electrically connecting two or more layers of a stacked or rolled capacitor
- H01G4/2325—Terminals electrically connecting two or more layers of a stacked or rolled capacitor characterised by the material of the terminals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T29/00—Metal working
- Y10T29/43—Electric condenser making
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T29/00—Metal working
- Y10T29/43—Electric condenser making
- Y10T29/435—Solid dielectric type
Definitions
- the present invention relates to a ceramic electronic component and a manufacturing method thereof, and more particularly to a ceramic electronic component in which an external electrode is disposed on a surface of a ceramic body constituting the ceramic electronic component and a manufacturing method thereof.
- the surface mounted by soldering the external electrode formed on the surface of the ceramic body to the land arranged on the wiring board by a method such as reflow soldering when mounted on the wiring board In recent years, the surface mounted by soldering the external electrode formed on the surface of the ceramic body to the land arranged on the wiring board by a method such as reflow soldering when mounted on the wiring board.
- Mounted ceramic electronic parts for example, ceramic inductors using magnetic ceramics, ceramic capacitors using dielectric ceramics, ceramic piezoelectric parts using piezoelectric ceramics, etc. are widely used.
- a plating film such as a Ni plating film or a Sn plating film is widely formed on an Ag electrode which is an external electrode main body (underlayer).
- an Ag electrode which is an external electrode main body (underlayer).
- an organosilicon compound is formed by dehydration condensation on the ceramic body surface, pores open to the surface, and external electrodes.
- a soldering technique used for mounting ceramic electronic components as a composition for preventing the solder flux from creeping up, a polymer containing a polymerized unit of an unsaturated ester containing a polyfluoroalkyl group, a fluorine-based polymer A composition containing a surfactant and an aqueous medium has been proposed (see Patent Document 2). And when this composition is used, it is supposed that it can prevent that a flux will be inhaled by the pore of a ceramic body at the time of soldering.
- the present invention solves the above-described problems, and can prevent a decrease in self-alignment property caused by flux being sucked into the pores of the ceramic body in a soldering process during mounting. It is an object of the present invention to provide an electronic component manufacturing method and a ceramic electronic component with high mounting reliability that can be manufactured by the method.
- a method for manufacturing a ceramic electronic component of the present invention includes: A ceramic electronic component manufacturing method comprising a ceramic body and an external electrode disposed on a surface of the ceramic body, After forming the external electrode on the surface of the ceramic body, an oil repellent treatment is performed on the surface of the ceramic body by applying an oil repellency treatment to the ceramic body using an oil repellent treatment agent.
- the oil repellent agent is at least one —CONH (CH 2 ) 3 Si (OR) 3 (However, OR is a methoxy group or an ethoxy group) It is characterized in that it contains a polyfluoropolyether compound containing as a main component and hydrofluoroether as a solvent.
- the method for producing a ceramic electronic component of the present invention includes: A ceramic electronic component manufacturing method comprising a ceramic body and an external electrode disposed on a surface of the ceramic body and having a plating film on the surface, An oil repellent treatment step of forming a plating film on the surface of the external electrode, then subjecting the ceramic body to oil repellent treatment using an oil repellent treatment agent, and forming a flux intrusion prevention film on the surface of the ceramic body.
- the oil repellent agent is at least one —CONH (CH 2 ) 3 Si (OR) 3 (However, OR is a methoxy group or an ethoxy group) It is characterized in that it contains a polyfluoropolyether compound containing as a main component and hydrofluoroether as a solvent.
- the method for producing a ceramic electronic component of the present invention includes: A ceramic electronic component manufacturing method comprising a ceramic body and an external electrode disposed on a surface of the ceramic body and having a plating film on the surface, After forming the external electrode and before forming the plating film, the ceramic body is subjected to an oil repellency treatment using an oil repellency treatment agent to form a flux penetration preventing film on the surface of the ceramic body.
- the oil repellent agent is at least one —CONH (CH 2 ) 3 Si (OR) 3 (However, OR is a methoxy group or an ethoxy group) It is characterized in that it contains a polyfluoropolyether compound containing as a main component and hydrofluoroether as a solvent.
- the polyfluoropolyether compound of the oil repellent treatment agent is at least one selected from the group consisting of the following (I), (II), (III), (IV), (V), and (VI). It is characterized by being. (I) C 3 F 7 O (CF (CF 3 ) CF 2 O) yCF (CF 3 ) -A (II) CF 3 O (C 2 F 4 O) yCF 2 -A (III) A-CF 2 O (CF 2 O) x (C 2 F 4 O) yCF 2 -A (IV) A-CF 2 O (C 2 F 4 O) xCF 2 -A (V) A-CF (CF 3 ) O (CF (CF 3 ) CF 2 O) yCF (CF 3 ) -A (VI) A- (CF 2 ) 3 O (C 4 F 8 O) y (CF 2 O) 3 -A However, said A is (I) -CONH (CH 2 ) 3 Si (OR) 3 (However, OR,
- ,And, X is 1 to 50, y is 4 to 40, and n is 1 to 4. That is, in the polyfluoropolyether compound of the oil repellent agent used in the present invention, A in the structural formula (molecule) of the above (I) and (II) is always the above (a), and (III) In the structural formulas (molecules) of (VI) to (VI), one A is necessarily the above (A), and the other A may be any one of the above (A) to (E).
- oil repellent treatment is preferably performed using the oil repellent treatment agent having a polyfluoropolyether compound concentration of 0.04 to 0.5% by weight.
- an oil repellent treatment agent removing step for removing excess oil repellent treatment agent is provided immediately after the oil repellent treatment step.
- a cleaning step of cleaning the ceramic body with hydrofluoroether is provided after the oil repellent treatment agent removing step.
- a step of heat-treating the ceramic body is provided between the oil repellent treatment agent removing step and the cleaning step.
- the ceramic constituting the ceramic body is preferably NiCuZn ferrite.
- the ceramic electronic component of the present invention is A ceramic electronic component comprising a ceramic body and external electrodes disposed on the surface of the ceramic body, At least F, Si, and N are detected from the ceramic surface constituting the ceramic body, and The atomic concentration ratio of each element to the ceramic surface is 2 ⁇ (F / ceramic body) ⁇ 12, 0.1 ⁇ (Si / ceramic body) ⁇ 1.0, 0.1 ⁇ (N / ceramic body) ⁇ 1.3, It is characterized by meeting the requirements of The “ceramic element” in each of the above formulas refers to the total atomic concentration of elements detected from the ceramic element.
- the ceramic electronic component of the present invention is A ceramic electronic component comprising a ceramic body and external electrodes disposed on the surface of the ceramic body, At least F, Si, and N are detected from the ceramic surface constituting the ceramic body and the external electrode surface, At the ceramic surface, the atomic concentration ratio of each element of F, Si, and N to the ceramic surface is 2 ⁇ (F / ceramic body) ⁇ 12, 0.1 ⁇ (Si / ceramic body) ⁇ 1.0, 0.1 ⁇ (N / ceramic body) ⁇ 1.3, Meet the requirements of On the surface of the external electrode, the atomic concentration ratio of each element of F, Si, and N to the surface of the external electrode is 0.4 ⁇ (F / external electrode) ⁇ 10, 0.06 ⁇ (Si / external electrode) ⁇ 0.8, 0.07 ⁇ (N / external electrode) ⁇ 1.0, It is characterized by meeting the requirements of The “ceramic element” in each of the above formulas refers to the total atomic concentration of the elements detected from the ceramic element excluding the oil
- a ceramic electronic component comprising a ceramic body and external electrodes disposed on the surface of the ceramic body, at least one ⁇ after the formation of the external electrodes on the surface of the ceramic body.
- An oil repellent treatment agent comprising a polyfluoropolyether compound containing CONH (CH 2 ) 3 Si (OR) 3 (wherein OR is a methoxy group or an ethoxy group) as a main component and hydrofluoroether as a solvent. Since the ceramic body is subjected to oil repellency treatment and a flux intrusion prevention film is formed on the surface of the ceramic body, it prevents the flux from being sucked into the ceramic body and provides good mounting (Self-alignment) can be realized. In addition, since the flux intrusion prevention film is thin, electrical conductivity between the external electrode and the land electrode of the circuit board to be mounted and solderability of the external electrode are ensured.
- hydrofluoroether is used as a solvent for the oil repellent agent, and the hydrofluoroether that is the solvent for this oil repellent agent has a very low water solubility. Condensation due to hydrolysis of —CONH (CH 2 ) 3 Si (OR) 3 , which is a functional group of the main component, can be suppressed, and gelation can be prevented.
- a ceramic electronic component including a ceramic body and an external electrode having a plating film on the surface
- at least one —CONH (CH 2 ) 3 Si (OR) is formed after the plating film is formed on the surface of the external electrode.
- OR is a methoxy group or an ethoxy group
- the main body is a polyfluoropolyether compound, and the ceramic body is treated with an oil repellent using an oil repellent containing hydrofluoroether as a solvent. Even if a flux intrusion prevention film is formed on the surface of the ceramic body, the ceramic body having an external electrode having a plating film can be prevented by preventing the flux from being absorbed by the ceramic body.
- a thin flux penetration prevention film should be securely formed on the surface of the body, without sacrificing continuity and solderability. , It is possible to realize a good mountability (self alignment property). Moreover, the effect of preventing oxidation of the plating film of the external electrode by the flux penetration preventing film can be expected.
- a ceramic electronic component including a ceramic body and an external electrode having a plating film on the surface, at least one -CONH (CH 2 ) 3 after forming the external electrode and before forming the plating film.
- the ceramic body is made of an oil repellent agent containing a polyfluoropolyether compound containing Si (OR) 3 (wherein OR is a methoxy group or an ethoxy group) as a main component and hydrofluoroether as a solvent.
- OR is a methoxy group or an ethoxy group
- hydrofluoroether as a solvent.
- the present invention can be made more effective.
- Oil repellent treatment with a polyfluoropolyether compound concentration of 0.04 to 0.5% by weight makes it possible to prevent flux from entering with good workability. Therefore, it is possible to reliably form a flux intrusion prevention film having a large thickness and a film thickness that is not too large on the surface of the ceramic body, and the present invention can be more effectively realized.
- the oil repellency treatment agent removal step of removing excess oil repellency treatment agent it is possible to reliably form a uniform flux intrusion prevention film without uneven coating. It becomes possible.
- the excess oil repellent agent can be drained by a method such as contact with an air stream by suction or gas blowing, or centrifugation.
- the method of draining excess oil repellent agent is not limited to this.
- an unnecessary oil repellent treatment agent can be more reliably removed by performing a washing step of washing the ceramic body with hydrofluoroether.
- the heat treatment is usually preferably performed at 60 to 120 ° C. for about 30 minutes.
- NiCuZn ferrite as the ceramic constituting the ceramic body, it is possible to obtain an inductor with excellent mountability and high reliability.
- a ceramic electronic component in which F, Si, and N are detected from a ceramic surface constituting a ceramic body at a ratio (atomic concentration ratio) as defined in the tenth aspect. It is an electronic component and can be efficiently manufactured by the above-described method for manufacturing a ceramic electronic component of the present invention. In this ceramic electronic component, since the flux is not absorbed by the ceramic body in the soldering process, a good self-alignment property can be obtained.
- the ceramic electronic component according to claim 11 is a ratio (atomic concentration ratio) of F, Si, and N from the ceramic surface and the external electrode surface constituting the ceramic body, as defined in claim 11.
- the ceramic electronic component to be detected can be efficiently manufactured by the above-described method for manufacturing a ceramic electronic component of the present invention.
- this ceramic electronic component since the flux is not absorbed by the ceramic body in the soldering process, a good self-alignment property can be obtained.
- the thickness of the coating film (flux penetration preventing film) of the external electrode is thin (usually several tens of nm or less), sufficient conduction reliability can be ensured.
- FIG. 1 It is front sectional drawing which shows the structure of the ceramic electronic component (multilayer ceramic inductor) concerning the Example of this invention. It is a disassembled perspective view which shows typically the principal part structure of the multilayer ceramic inductor concerning the Example of this invention.
- (a) is a figure which shows the mounting state of the multilayer ceramic inductor concerning the Example of this invention
- (b) is a figure which shows the mounting state of the multilayer ceramic inductor of a comparative example.
- (a) is a figure which shows the soldering state of the multilayer ceramic inductor concerning the Example of this invention
- (b) is a figure which shows the soldering state of the multilayer ceramic inductor of a comparative example.
- (a) is an elemental mapping diagram of C by fluorescent X-ray analysis (WDX) when the multilayer ceramic inductor according to the example of the present invention is mounted, and (b) is mounted with the multilayer ceramic inductor of the comparative example. It is an elemental mapping figure of C by the fluorescent X ray analysis (WDX) in the case.
- WDX fluorescent X-ray analysis
- FIG. 1 is a cross-sectional view showing a configuration of a multilayer coil component (a multilayer ceramic inductor in the first embodiment) according to one embodiment (first embodiment) of the present invention
- FIG. 2 is an exploded perspective view schematically showing a main part configuration.
- the multilayer ceramic inductor of Example 1 is formed by connecting each coil conductor (coil pattern) 2 disposed in each ferrite layer 1 through a via hole 3 (FIG. 2).
- a ceramic body (ferrite body) 5 having a coil 4 is provided.
- External electrodes 6 a and 6 b are disposed on the end surfaces 5 a and 5 b of the ceramic body (ferrite body) 5 so as to be electrically connected to the lead electrodes 4 a and 4 b at both ends of the coil 4. Below, the manufacturing method is demonstrated.
- Ferric oxide (Fe 2 O 3 ), zinc oxide (ZnO), nickel oxide (NiO), and copper oxide (CuO) are weighed at a predetermined ratio into a ball mill as a raw material, for a predetermined time, Wet blending was performed. The powder obtained by drying and pulverizing the wet blended mixture was calcined at 700 ° C. for 1 hour. The obtained calcined powder was wet pulverized for a predetermined time with a ball mill, then dried and crushed to obtain a ferrite powder.
- a binder resin, a plasticizer, a wetting agent, and a dispersing agent were added to the ferrite powder, mixed for a predetermined time with a ball mill, and then defoamed under reduced pressure.
- the obtained slurry was applied onto a peelable film using a lip coater or a multi coater and dried to obtain a long ferrite green sheet having a desired film thickness.
- the obtained long ferrite green sheet was cut into a predetermined size, and a via hole was formed by a method such as laser processing to obtain a ferrite sheet having a via hole at a predetermined position.
- a conductive paste mainly composed of silver or a silver alloy is applied in a predetermined pattern by a method such as screen printing, and is heated and dried to form an electrode-forming ferrite provided with a coil conductor. A sheet was obtained.
- the obtained electrode-formed ferrite sheets are stacked so that the coil conductors are connected to each other to form a coil, and the ferrite green sheets not coated with the conductive paste are stacked on the upper and lower sides of the stacked laminate.
- a fired laminate was obtained.
- the electrode-forming ferrite sheet provided with the coil conductor is laminated, the coil conductor is interlayer-connected through the via hole described above, and a coil is formed inside the unfired laminate.
- the obtained unfired laminate was pressure-bonded at 45 ° C. and a pressure of 1.0 t / cm 2 .
- this laminated pressurization body was cut
- FIGS. 1 and 2 an unfired ceramic element having a coil 4 in which each coil conductor (coil pattern) 2 disposed in each ferrite layer 1 is connected by a via hole 3 is provided.
- a body (ferrite body) 5 is formed.
- FIG. 1 shows a multilayer ceramic inductor in which external electrodes 6 a and 6 b are formed on end faces 5 a and 5 b of a ceramic body (ferrite body) 5.
- an electrode material paste for forming external electrodes is applied to the end faces 5a and 5b of the obtained fired body (ceramic body 5) where the lead electrodes 4a and 4b at both ends of the coil 4 are exposed by an immersion method. After applying and drying at 120 ° C. for 10 minutes, an electrode material paste was baked at 800 ° C. for 15 minutes to form an external electrode body (underlayer).
- the oil repellent treatment agent was put in a container, and the ceramic body in which the electrode material paste was baked to form the external electrode main body (underlayer) as described above was immersed in the container for about 5 minutes. Thereafter, the ceramic body was taken out from the oil repellent treatment agent, drained by suction and contacted with an air current, and then heat treated at 80 ° C. for about 30 minutes. Thereby, a flux intrusion prevention film is formed on the surface of the ceramic body and the surface of the external electrode main body (underlayer).
- a multilayer ceramic inductor in which a flux intrusion prevention film was formed on the surface of the ceramic body and the surface of the external electrode main body (underlayer) was obtained.
- illustration of the flux intrusion prevention film and the Ni and Sn plating films is omitted.
- the mounting coordinate is shifted from the center by 150 ⁇ m in the width direction (W direction) of the multilayer ceramic inductor so that mounting displacement occurs intentionally.
- the multilayer ceramic inductor should be mounted on the land by soldering the external electrode of the multilayer ceramic inductor on the land by the reflow soldering method.
- the self-alignment property was evaluated by examining whether or not it returned to the position.
- FIG. 3 (a) shows the mounting state of the multilayer ceramic inductor according to Example 1 of the present invention that was subjected to oil repellent treatment
- FIG. 3 (b) was the multilayer ceramic of Comparative Example 1 that was not subjected to oil repellent treatment. The mounting state of the inductor is shown.
- FIG. 4A shows the soldered state of the multilayer ceramic inductor according to Example 1 of the present invention that had been subjected to oil repellency treatment
- FIG. 4B shows Comparative Example 1 that had not been subjected to oil repellency treatment. The soldering state of the multilayer ceramic inductor is shown.
- the multilayer ceramic inductor after the self-alignment test is removed from the mounting substrate, and is included in the flux by wavelength dispersive X-ray fluorescence analysis (WDX).
- WDX wavelength dispersive X-ray fluorescence analysis
- the flux intrusion prevention film is formed on the surface of the ceramic body, so that the flux is prevented from being sucked into the ceramic body. Good self-alignment properties could be obtained.
- (1) Water repellent treatment was performed using water-repellent CH 3 (CH 2 ) 9 Si (OCH 3 ) 3 after the external electrode body was formed and before the plating film was formed (the oil repellent treatment in the above examples is
- the multilayer ceramic inductor of Comparative Example 2 was produced in the same manner as the multilayer ceramic inductor of Example 1 except that (2) After forming the external electrode body and before forming the plating film, water-repellent treatment was performed using water-repellent CF 3 CH 2 CH 2 Si (OCH 3 ) 3 (the oil-repellent treatment in the above embodiment was performed).
- the multilayer ceramic inductor of Comparative Example 3 was produced in the same manner as the multilayer ceramic inductor of Example 1 except that The self-alignment properties of the multilayer ceramic inductors of Comparative Examples 2 and 3 were also evaluated.
- Table 1 summarizes the self-alignment evaluation results of the multilayer ceramic inductor of Example 1 and the multilayer ceramic inductors of Comparative Examples 1 to 3.
- An electrode material paste for forming an external electrode was applied to the end face of the same fired body as the ceramic body (fired body) produced in the step (6) of Example 1 above by exposing the lead electrode to 120 ° C. For 10 minutes. Then, an electrode material paste was baked at 800 ° C. for 15 minutes to form an external electrode body (underlayer). Then, a multilayer ceramic inductor (see FIG. 1) is formed on the external electrode main body (underlayer) by forming a two-layered plating film in which the lower layer is a Ni plating film and the upper layer is a Sn plating film (or solder plating film). Got.
- an oil repellent treatment agent is put in a container, and an electrode material paste is baked into the container to form an external electrode as described above, and a ceramic body (multilayer ceramic inductor) on which a plating film is formed is formed for about 5 minutes. Soaked. Thereafter, the ceramic body was taken out from the oil repellent treatment agent, drained by a method of contacting with an air current by suction, and then heat-treated at 80 ° C. for about 30 minutes.
- FIG. 1 a multilayer ceramic inductor (see FIG. 1) having a flux intrusion prevention film formed on the surface of the ceramic body and the surface of the external electrode was obtained.
- FIG. 1 the illustration of the flux intrusion prevention film and the Ni and Sn plating films is omitted as described above.
- the multilayer ceramic inductor of Example 2 was superior in self-alignment properties to the multilayer ceramic inductors of Comparative Examples 1 to 3 as in Example 1.
- the flux intrusion prevention film of the multilayer ceramic inductor of Example 2 is very thin, after the plating film is formed, oil repellent treatment is performed to prevent flux intrusion on the surface of the ceramic body and the surface of the external electrode. Even when the film was formed, it was confirmed that there was no problem in solderability and conductivity.
- the flux intrusion prevention film is formed on the plating film, it is confirmed that the oxidation of the plating film formed on the external electrode body (underlayer) is suppressed and prevented, and the reliability is improved. .
- An electrode material paste for forming an external electrode was applied to the end face of the same fired body as the ceramic body (fired body) produced in the step (6) of Example 1 above by exposing the lead electrode to 120 ° C. For 10 minutes. Thereafter, an electrode material paste was baked at 800 ° C. for 15 minutes to form an external electrode body (underlayer). Thereafter, a plating film having a two-layer structure in which the lower layer is a Ni plating film and the upper layer is a Sn plating film (or solder plating film) is formed on the external electrode body (underlayer).
- an oil repellent treatment was performed by the method described below.
- the concentration of the polyfluoropolyether compound as the oil repellent treatment agent is 0.5 wt%, 0.2 wt%, 0.1 wt%, 0.05 wt%, 0.04
- a weight percent treatment solution was prepared.
- the ceramic body (multilayer ceramic inductor) provided with the external electrode formed by forming a plating film on the external electrode body (underlayer) using each processing solution whose concentration is adjusted as described above. Oil repellent treatment was performed.
- FIG. 1 a multilayer ceramic inductor (see FIG. 1) having a flux intrusion prevention film formed on the surface of the ceramic body and the surface of the external electrode was obtained.
- FIG. 1 the illustration of the flux intrusion prevention film and the Ni and Sn plating films is omitted as described above.
- Example 3 the multilayer ceramic inductor obtained in Example 3 was evaluated for self-alignment property, solderability, and external electrode conductivity. The results are shown in Table 2.
- the flux intrusion prevention film is formed on the plating film formed on the external electrode body (underlayer), so that oxidation of the plating film is suppressed and prevented. It has been confirmed that reliability is improved.
- An electrode material paste for forming an external electrode was applied to the end face of the same fired body as the ceramic body (fired body) produced in the step (6) of Example 1 above by exposing the lead electrode to 120 ° C. For 10 minutes. Thereafter, an electrode material paste was baked at 800 ° C. for 15 minutes to form an external electrode body (underlayer). Thereafter, a plating film having a two-layer structure in which the lower layer is a Ni plating film and the upper layer is a Sn plating film (or solder plating film) is formed on the external electrode body (underlayer).
- an oil repellent treatment was performed by the method described below.
- an oil repellent treatment agent comprising hydrofluoroether as a solvent.
- an oil repellent treatment agent is put in a container, and an electrode material paste is baked into the container to form an external electrode body as described above, and a ceramic body (multilayer ceramic inductor) on which a plating film is further formed is about 5 Immerse for a minute.
- Example 4 the liquid drainage is accommodated in a mesh basket container having a diameter of about 12 cm or less, and the mesh basket container is accommodated in a cylindrical liquid draining jig having a diameter of 12 cm. This was carried out by sucking from below and allowing gas (air) to flow from top to bottom in the liquid draining jig. However, the draining time was 150 seconds.
- the degree of suction was set to 3.0 kPa as a differential pressure from the atmospheric pressure, and the liquid was drained so that the air flow rate was 5 m 3 / min. And after completion
- FIG. 1 a multilayer ceramic inductor (see FIG. 1) having a flux intrusion prevention film formed on the surface of the ceramic body and the surface of the external electrode was obtained.
- FIG. 1 the illustration of the flux intrusion prevention film and the Ni and Sn plating films is omitted as described above.
- the method of draining is not limited to the method of draining the suction liquid as described above, and a method of bringing an air current into contact with the ceramic body by blowing (pushing) air, a method using centrifugal force, or the like is applied. It is also possible to do.
- An electrode material paste for forming an external electrode was applied to the end face of the same fired body as the ceramic body (fired body) produced in the step (6) of Example 1 above by exposing the lead electrode to 120 ° C. For 10 minutes. Thereafter, an electrode material paste was baked at 800 ° C. for 15 minutes to form an external electrode body (underlayer). Thereafter, a plating film having a two-layer structure in which the lower layer is a Ni plating film and the upper layer is a Sn plating film (or solder plating film) is formed on the external electrode body (underlayer).
- an oil repellent treatment agent is put in a container, and an electrode material paste is baked into the container to form an external electrode body as described above, and a ceramic body (multilayer ceramic inductor) on which a plating film is further formed is about 5 Immerse for a minute.
- the suction liquid was removed by the same method and under the same conditions as in Example 4 to remove excess oil-repellent treatment liquid on the ceramic body.
- the ceramic body from which the excess oil repellent treatment liquid was removed was heat treated at 80 ° C. for about 30 minutes.
- the ceramic body was ultrasonically cleaned for 5 minutes with the same hydrofluoroether used as the solvent for the oil repellent agent.
- a multilayer ceramic inductor in which a flux penetration preventing film was formed on the surface of the ceramic body and the surface of the external electrode was obtained.
- FIG. 1 the illustration of the flux intrusion prevention film and the Ni and Sn plating films is omitted as described above.
- the self-alignment property of the obtained multilayer ceramic inductor was examined, and for comparison, the self-alignment property was also examined for a multilayer ceramic inductor manufactured without performing the above cleaning.
- the above-mentioned liquid draining step is omitted, and a multilayer ceramic inductor (a sample with uneven flux intrusion prevention film) in which an excessive oil repellent agent is intentionally left is prepared.
- a multilayer ceramic inductor a sample with uneven flux intrusion prevention film in which an excessive oil repellent agent is intentionally left is prepared.
- hydrofluoroether which is the same solvent as the oil repellent treatment agent, excess oil repellent treatment agent can be efficiently removed from the multilayer ceramic inductor and good self-alignment property can be secured. It was.
- An electrode material paste for forming an external electrode was applied to the end face of the same fired body as the ceramic body (fired body) produced in the step (6) of Example 1 above by exposing the lead electrode to 120 ° C. For 10 minutes. Thereafter, an electrode material paste was baked at 800 ° C. for 15 minutes to form an external electrode body (underlayer).
- an oil repellent treatment agent is put in a container, and an electrode material paste is baked into the container to form an external electrode body as described above, and a ceramic body (multilayer ceramic inductor) on which a plating film is further formed is about 5 Immerse for a minute.
- the suction liquid was removed by the same method and under the same conditions as in Example 4 to remove excess oil-repellent treatment liquid on the ceramic body.
- the ceramic body from which the excess oil repellent treatment liquid was removed was heat treated at 80 ° C. for about 30 minutes.
- the ceramic body was ultrasonically cleaned for 5 minutes with the same hydrofluoroether used as the solvent for the oil repellent agent. And after completion
- Example 6 the oil repellency of the surface of the multilayer ceramic inductor (ceramic body) was adjusted by adjusting the concentration of the oil repellent agent, liquid draining conditions, ultrasonic cleaning conditions, etc. Multilayer ceramic inductors of sample numbers 1, 2, and 3 containing F, Si, and N were produced on the surface of the ceramic body (ferrite body) at the ratio shown.
- the surface of the obtained multilayer ceramic inductor was subjected to qualitative and quantitative analysis by XPS (X-ray photoelectron spectroscopy) using Quantum 2000 manufactured by PHYSICAL ELECTRONICS.
- the measurement area was 100 ⁇ m ⁇ .
- Table 3 shows the evaluation results of the surface oil repellency, the self-alignment property, and the continuity of the Ni plating film, in which the multilayer ceramic inductor of Example 6 was examined.
- the “ceramic body” in each of the above formulas is an element excluding an oil repellent component element and an oxygen element among elements (Ni, Cu, Zn, Fe, etc.) detected from the ceramic body.
- the atomic concentration ratio of each element of F, Si, N to the ceramic body (ferrite body) surface is 2 ⁇ F / ceramic body ⁇ 12, 0.1 ⁇ Si / ceramic body ⁇ 1.0 0.1 ⁇ N / ceramic body ⁇ 1.3 It was confirmed that good self-alignment properties and Ni plating continuity can be obtained when the above requirements are satisfied.
- An electrode material paste for forming an external electrode was applied to the end face of the same fired body as the ceramic body (fired body) produced in the step (6) of Example 1 above by exposing the lead electrode to 120 ° C. For 10 minutes. Thereafter, an electrode material paste was baked at 800 ° C. for 15 minutes to form an external electrode body (underlayer). Then, a two-layer plating film in which the lower layer is a Ni plating film and the upper layer is a Sn plating film (or solder plating film) is formed on the external electrode main body (underlayer).
- an oil repellent treatment agent is put in a container, and an electrode material paste is baked into the container to form an external electrode body as described above, and a ceramic body (multilayer ceramic inductor) on which a plating film is further formed is about 5 Immerse for a minute.
- the suction liquid was removed by the same method and under the same conditions as in Example 4 to remove excess oil-repellent treatment liquid on the ceramic body.
- the ceramic body from which the excess oil repellent treatment liquid was removed was heat treated at 80 ° C. for about 30 minutes.
- the ceramic body was ultrasonically cleaned for 5 minutes with the same hydrofluoroether used as the solvent for the oil repellent agent. And after completion
- Example 7 the oil repellency state of the surface of the multilayer ceramic inductor was adjusted by adjusting the concentration of the oil repellent agent, the liquid draining condition, the ultrasonic cleaning condition, and the like as shown in Table 4.
- multilayer ceramic inductors of sample numbers 4, 5, and 6 containing F, Si, and N were fabricated on the surface of the ceramic body and the surface of the external electrode.
- the surface of the obtained multilayer ceramic inductor was subjected to qualitative and quantitative analysis by XPS (X-ray photoelectron spectroscopy) using Quantum 2000 manufactured by PHYSICAL ELECTRONICS.
- the measurement area was 100 ⁇ m ⁇ .
- Table 4 shows the evaluation results of the surface oil repellency, the self-alignment property, and the continuity of the Ni plating film, in which the multilayer ceramic inductor of Example 7 was examined.
- the “ceramic body” in each of the above formulas is an element excluding an oil repellent component element and an oxygen element among elements (Ni, Cu, Zn, Fe, etc.) detected from the ceramic body.
- the “external electrode” in each of the above formulas is the total atom of elements excluding the oil repellent agent component element and the oxygen element among the elements (Ni, Ag, Zn, etc.) detected from the external electrode.
- Concentration: Unit is atom%. That is, the atomic concentration ratio of F, Si, and N to the external electrode surface refers to the atomic concentrations of F, Si, and N such as Ni, Ag, Zn detected from the surface of the external electrode. It is not the ratio but the ratio of the elements detected from the surface of the external electrode to the total atomic concentration of the elements excluding the oil repellent agent component element and the oxygen element.
- the atomic concentration ratio of each element of F, Si, N to the ceramic body (ferrite body) surface is 2 ⁇ F / ceramic body ⁇ 12 0.1 ⁇ Si / ceramic body ⁇ 1.0 0.1 ⁇ N / ceramic body ⁇ 1.3
- the atomic concentration ratio of each element of F, Si, N to the external electrode surface is 0.4 ⁇ F / external electrode ⁇ 10 0.06 ⁇ Si / External electrode ⁇ 0.8 0.07 ⁇ N / External electrode ⁇ 10 It was confirmed that good self-alignment properties and Ni plating continuity can be obtained when the above requirements are satisfied.
- a multilayer ceramic inductor has been described as an example of a ceramic electronic component.
- the present invention is not limited to a multilayer ceramic inductor, and has a structure in which external electrodes are disposed on the surface of a ceramic body.
- the present invention can be widely applied to various ceramic electronic parts such as multilayer ceramic capacitors and ceramic piezoelectric parts.
- the present invention is not limited to the above-described examples in other points as well, and relates to the type of polyfluoropolyether compound that is the main component of the oil repellent treatment agent, the blending ratio with the solvent, and the like. It is possible to add various applications and modifications.
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Abstract
Description
そして、この方法によれば、めっき液、水などがセラミック素体内部に浸入することを防いで、電気特性の劣化を抑制することができるとされている。
そして、この組成物を用いた場合、はんだ付け時にフラックスがセラミック素体の細孔に吸い込まれてしまうことを防止できるとされている。
セラミック素体と、前記セラミック素体の表面に配設された外部電極とを備えるセラミック電子部品の製造方法であって、
前記セラミック素体の表面に前記外部電極を形成した後に、撥油処理剤を用いて前記セラミック素体に撥油処理を施し、前記セラミック素体の表面にフラックス浸入防止膜を形成する撥油処理工程を備え、かつ、
前記撥油処理剤は、少なくとも1つの
-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基)
を含有するポリフルオロポリエーテル化合物を主成分とし、ハイドロフルオロエーテルを溶媒として含むものであること
を特徴としている。
セラミック素体と、前記セラミック素体の表面に配設され、表面にめっき膜を有する外部電極とを備えるセラミック電子部品の製造方法であって、
前記外部電極の表面に前記めっき膜を形成した後に、撥油処理剤を用いて前記セラミック素体に撥油処理を施し、前記セラミック素体の表面にフラックス浸入防止膜を形成する撥油処理工程を備え、かつ、
前記撥油処理剤は、少なくとも1つの
-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基)
を含有するポリフルオロポリエーテル化合物を主成分とし、ハイドロフルオロエーテルを溶媒として含むものであること
を特徴としている。
セラミック素体と、前記セラミック素体の表面に配設され、表面にめっき膜を有する外部電極とを備えるセラミック電子部品の製造方法であって、
前記外部電極を形成した後、前記めっき膜を形成する前に、撥油処理剤を用いて前記セラミック素体に撥油処理を施し、前記セラミック素体の表面にフラックス浸入防止膜を形成する撥油処理工程を備え、かつ、
前記撥油処理剤は、少なくとも1つの
-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基)
を含有するポリフルオロポリエーテル化合物を主成分とし、ハイドロフルオロエーテルを溶媒として含むものであること
を特徴としている。
(I) C3F7O(CF(CF3)CF2O)yCF(CF3)-A
(II) CF3O(C2F4O)yCF2-A
(III) A-CF2O(CF2O)x(C2F4O)yCF2-A
(IV) A-CF2O(C2F4O)xCF2-A
(V) A-CF(CF3)O(CF(CF3)CF2O)yCF(CF3)-A
(VI) A-(CF2)3O(C4F8O)y(CF2O)3-A
ただし、前記Aは、
(イ)-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基),
(ロ)(CnF2n+1)
(ハ)(CnF2n+1O)
(ニ)(HCnF2nO)
(ホ)(HCnF2n+1O)
からなる群より選ばれる少なくとも1種であり、(I)~(VI)の構造式において、少なくとも一つの前記Aは、前記(イ)の-CONH(CH2)3Si(OR)3であり、かつ、
前記xは1~50、yは4~40、nは1~4。
すなわち、本発明で用いられる撥油処理剤のポリフルオロポリエーテル化合物において、上記(I),(II)の構造式(分子)におけるAは、必ず上記(イ)であり、また、(III)~(VI)の構造式(分子)における一方のAは、必ず上記(イ)であり、他方のAは、上記(イ)~(ホ)のいずれでもよい。
セラミック素体と、前記セラミック素体の表面に配設された外部電極を備えるセラミック電子部品であって、
前記セラミック素体を構成するセラミック表面から、少なくともF、Si、およびNが検出され、かつ、
前記各元素の前記セラミック表面に対する原子濃度比が、
2≦(F/セラミック素体)≦12、
0.1≦(Si/セラミック素体)≦1.0、
0.1≦(N/セラミック素体)≦1.3、
の要件を満たすことを特徴としている。
なお、上記の各式における「セラミック素体」とは、セラミック素体から検出される元素の合計の原子濃度をいう。
セラミック素体と、前記セラミック素体の表面に配設された外部電極を備えるセラミック電子部品であって、
前記セラミック素体を構成するセラミック表面、および、外部電極表面から、少なくともF、Si、およびNが検出され、
前記セラミック表面では、F、Si、およびNの各元素の前記セラミック表面に対する原子濃度比が、
2≦(F/セラミック素体)≦12、
0.1≦(Si/セラミック素体)≦1.0、
0.1≦(N/セラミック素体)≦1.3、
の要件を満し、
前記外部電極表面では、F、Si、およびNの各元素の前記外部電極表面に対する原子濃度比が、
0.4≦(F/外部電極)≦10、
0.06≦(Si/外部電極)≦0.8、
0.07≦(N/外部電極)≦1.0、
の要件を満たすことを特徴としている。
なお、上記の各式における「セラミック素体」とは、セラミック素体から検出される元素のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度をいう。
また、上記の各式における「外部電極」とは、外部電極から検出される元素のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度をいう。
また、本発明では、撥油処理剤の溶媒として、ハイドロフルオロエーテルを使用しており、この撥油処理剤の溶媒であるハイドロフルオロエーテルは、水分溶解性が非常に低いため、撥油処理剤の主成分の官能基である-CONH(CH2)3Si(OR)3の加水分解による縮合を抑制し、ゲル化を防止することができる。
また、フラックス浸入防止膜による外部電極のめっき膜の酸化防止の効果も期待できる。
なお、過剰な撥油処理剤の液切りは、例えば、吸引や気体吹き付けなどによる気流との接触、遠心分離などの方法で行うことができる。ただし、過剰な撥油処理剤の液切りの方法は,これに限られるものではない。
そして、このセラミック電子部品は、はんだ付け工程でフラックスがセラミック素体に吸収されないため、良好なセルフアライメント性が得られる。
そして、このセラミック電子部品は、はんだ付け工程でフラックスがセラミック素体に吸収されないため、良好なセルフアライメント性が得られる。
なお、このセラミック電子部品の場合、外部電極のコーティング膜(フラックス浸入防止膜)の厚みが薄いため(通常、数10nm以下),十分な導通信頼性を確保することができる。
図1,図2に示すように、この実施例1の積層セラミックインダクタは、各フェライト層1に配設された各コイル用導体(コイルパターン)2がビアホール3(図2)により接続されてなるコイル4を有するセラミック素体(フェライト素体)5を備えている。そして、セラミック素体(フェライト素体)5の端面5a,5bには、コイル4の両端部の引き出し電極4a,4bと導通するように、外部電極6a,6bが配設されている。
以下に、その製造方法について説明する。
湿式調合した混合物を乾燥、粉砕することにより得られる粉末を700℃で1時間仮焼した。得られた仮焼粉末をボールミルにて所定の時間湿式粉砕した後、乾燥、解砕し、フェライト粉末を得た。
得られたスラリーをリップコータ、またはマルチコータを用いて、剥離性のフィルム上に塗布し、乾燥させることにより、所望の膜厚を有する長尺フェライトグリーンシートを得た。
このフェライトシート上に、スクリーン印刷などの方法により、銀または、銀合金を主成分とする導体ペーストを所定のパターンとなるように塗布し、加熱乾燥して、コイル用導体を備えた電極形成フェライトシートを得た。
なお、コイル用導体を備えた電極形成フェライトシートが積層されると、コイル用導体が、上述のビアホールを介して層間接続され、未焼成積層体の内部にコイルが形成される。
なお、図1は、セラミック素体(フェライト素体)5の端面5a,5bに外部電極6a,6bを形成した積層セラミックインダクタを示している。
まず、A-CF2O(CF2O)x(C2F4O)yCF2-A
ただし、A:-CONH(CH2)3Si(OCH3)3
x、y:8~12
の化合物と、溶媒であるハイドロフルオロエーテルを含む撥油処理剤を準備した。
その後、セラミック素体を撥油処理剤から取り出し、吸引により、気流と接触させる方法で液切りした後、80℃で約30分間熱処理を行った。
これにより、セラミック素体の表面および外部電極本体(下地層)の表面にフラックス浸入防止膜が形成される。
これにより、セラミック素体の表面および外部電極本体(下地層)の表面にフラックス浸入防止膜が形成された積層セラミックインダクタ(図1参照)を得た。なお、図1においては,フラックス浸入防止膜、および、NiおよびSnめっき膜の図示を省略している。
上述のように、撥油処理の工程を経て作製したこの実施例1の積層セラミックインダクタと、比較のため撥油処理を施さずに作製した積層セラミックインダクタ(比較例1)について、実装性を調べる試験(セルフアライメント試験)を行い、実装性(セルフアライメント性)を調べた。
また、撥油処理を行った本発明の実施例1にかかる積層セラミックインダクタのはんだ付け状態を確認したところ、図4(a)に示すように、はんだが濡れ上がっていることが確認された。
また、撥油処理を行っていない比較例1の積層セラミックインダクタのはんだ付け状態を確認したところ、図4(b)に示すように、はんだが,粒状のまま凝固しており、いわゆる「いもはんだ状態」になっていることが確認された。
(1)外部電極本体形成後、めっき膜形成前に、撥水性のあるCH3(CH2)9Si(OCH3)3を用いて撥水処理を施した(上記実施例の撥油処理は施していない)こと以外は上記実施例1の積層セラミックインダクタと同様の方法で比較例2の積層セラミックインダクタを作製するとともに、
(2)外部電極本体形成後、めっき皮膜形成前に、撥水性のあるCF3CH2CH2Si(OCH3)3を用いて撥水処理を施した(上記実施例の撥油処理は施していない)こと以外は上記実施例1の積層セラミックインダクタと同様の方法で比較例3の積層セラミックインダクタ作製し、
これらの比較例2,3の積層セラミックインダクタについてもセルフアライメント性を評価した。
なお、本発明の実施例にかかる積層セラミックインダクタのフラックス浸入防止膜は、非常に薄いため、外部電極本体(下地層)を形成した後、めっき膜を形成する前に、撥油処理を施してフラックス浸入防止膜を形成しても、その後のめっき工程で形成されるNiめっきの連続性は損なわれないことが確認されている。
それから、800℃にて15分間電極材料ペーストを焼き付けることにより、外部電極本体(下地層)を形成した。
それから、外部電極本体(下地層)に、下層がNiめっき膜、上層がSnめっき膜(またははんだめっき膜)からなる2層構造のめっき膜を形成することにより、積層セラミックインダクタ(図1参照)を得た。
まず、A-CF2O(CF2O)x(C2F4O)yCF2-A
ただし、A:-CONH(CH2)3Si(OCH3)3
x、y:8~12
の化合物と、溶媒であるハイドロフルオロエーテルを含む撥油処理剤を準備した。
その後、セラミック素体を撥油処理剤から取り出し、吸引により気流と接触させる方法で液切りした後、80℃で約30分間熱処理を行った。
また、本実施例2の積層セラミックインダクタのフラックス浸入防止膜は、非常に薄いため、めっき膜を形成した後に、撥油処理を行って、セラミック素体の表面および外部電極の表面にフラックス浸入防止膜を形成した場合にも、はんだ付け性、導通性は問題がないことが確認された。
また、めっき膜上にフラックス浸入防止膜が形成されているため、外部電極本体(下地層)上に形成されためっき膜の酸化が抑制、防止され、信頼性が向上することが確認されている。
その後、外部電極本体(下地層)上に、下層がNiめっき膜、上層がSnめっき膜(またははんだめっき膜)からなる2層構造のめっき膜を形成した。
まず、ハイドロフルオロエーテルを用いて、撥油処理剤であるポリフルオロポリエーテル化合物の濃度が0.5重量%、0.2重量%、0.1重量%、0.05重量%、0.04重量%の処理液を用意した。
そして、上述のようにして濃度調整を行った各処理液を用いて、外部電極本体(下地層)上にめっき膜を形成してなる外部電極を備えた上記セラミック素体(積層セラミックインダクタ)に撥油処理を行った。
その結果を表2に示す。
撥油処理剤であるポリフルオロポリエーテル化合物の濃度を0.5重量%、0.2重量%、0.1重量%、0.05重量%、0.04重量%に調整した処理液を用いて撥油処理を施した各積層セラミックインダクタは、セルフアライメント性、はんだ付け性、および外部電極の導通性のいずれについても良好な特性を備えていることが確認された。
その後、外部電極本体(下地層)上に、下層がNiめっき膜、上層がSnめっき膜(またははんだめっき膜)からなる2層構造のめっき膜を形成した。
まず、A-CF2O(CF2O)x(C2F4O)yCF2-A
ただし、A:-CONH(CH2)3Si(OCH3)3
x、y:8~12
の化合物と、溶媒であるハイドロフルオロエーテルを含む撥油処理剤を準備した。
それから、撥油処理剤を容器に入れ、その中に上述のようにして,電極材料ペーストを焼き付けて外部電極本体を形成し、さらにめっき膜を形成したセラミック素体(積層セラミックインダクタ)を約5分間浸漬した。
この実施例4では液切りを、多数個のセラミック素体を直径が約12cm弱の網かご状容器に収容し、この網かご状容器を直径12cmの筒状の液切り治具に収容し、下方から吸引して、液切り治具内に上から下に向かって気体(空気)を流通させる方法により実施した。ただし、液切りの時間は150秒とした。なお、この実施例4では、吸引の度合いを、大気圧との差圧で3.0kPaとし、空気の流量が5m3/minとなるようにして液切りを行った。
そして、液切りの終了後に、セラミック素体を80℃で約30分間熱処理した。
その後、外部電極本体(下地層)上に、下層がNiめっき膜、上層がSnめっき膜(またははんだめっき膜)からなる2層構造のめっき膜を形成した。
まず、A-CF2O(CF2O)x(C2F4O)yCF2-A
ただし、A:-CONH(CH2)3Si(OCH3)3
x、y:8~12
の化合物と、溶媒であるハイドロフルオロエーテルを含む撥油処理剤を準備した。
浸漬終了後、直ちに、上記実施例4の方法と同じ方法および同じ条件で吸引液切りを行い、セラミック素体上の過剰な撥油処理液を除去した。
そして、過剰な撥油処理液を除去したセラミック素体を80℃で約30分間熱処理した。
これにより、セラミック素体の表面および外部電極の表面にフラックス浸入防止膜が形成された積層セラミックインダクタ(図1参照)を得た。ただし、図1において,フラックス浸入防止膜、および、NiおよびSnめっき膜の図示を省略していることは上述の通りである。
また、洗浄液として、ハイドロフルオロエーテルの代わりに、イソプロピルアルコール、水を洗浄液として用いた場合、いずれの場合も、ハイドロフルオロエーテルを洗浄液として用いた場合ほどの、セルフアライメント性の改善は認められなかった。
まず、A-CF2O(CF2O)x(C2F4O)yCF2-A
ただし、A:-CONH(CH2)3Si(OCH3)3
x、y:8~12
の化合物と、溶媒であるハイドロフルオロエーテルを含む撥油処理剤を準備した。
浸漬終了後、直ちに、上記実施例4の方法と同じ方法および同じ条件で吸引液切りを行い、セラミック素体上の過剰な撥油処理液を除去した。
そして、過剰な撥油処理液を除去したセラミック素体を80℃で約30分間熱処理した。
そして、超音波洗浄の終了後に、上記実施例4の方法と同じ方法および同じ条件で吸引液切りを行い、洗浄液であるハイドロフルオロエーテルを除去した。
それから、外部電極本体(下地層)に、下層がNiめっき膜、上層がSnめっき膜(またははんだめっき膜)からなる2層構造のめっき膜を形成することにより、積層セラミックインダクタ(図1参照)を得た。
表3に、この実施例6の積層セラミックインダクタについて調べた、表面の撥油状態、セルフアライメント性およびNiめっき膜の連続性の評価結果を示す。
(イ)試料番号1の試料では、F、Si、およびNの、X線光電子分光法(XPS)による、セラミック素体(フェライト素体)表面に対する原子濃度比が、
(F/セラミック素体)=12
(Si/セラミック素体)=1.0
(N/セラミック素体)=1.3
であった。
(ロ)試料番号2の試料では、F、Si、およびNの、X線光電子分光法(XPS)による、セラミック素体(フェライト素体)表面に対する原子濃度比が、
(F/セラミック素体)=8
(Si/セラミック素体)=0.6
(N/セラミック素体)=0.8
であった。
(ハ)試料番号3の試料では、F、Si、およびNの、X線光電子分光法(XPS)による、セラミック素体(フェライト素体)表面に対する原子濃度比が、
(F/セラミック素体)=2
(Si/セラミック素体)=0.1
(N/セラミック素体)=0.1
であった。
なお、上記の各式における「セラミック素体」とは、セラミック素体から検出される元素(Ni,Cu,Zn,Feなど)のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度:単位atom%をいう。
すなわち、上記のF、Si、およびNの、セラミック素体表面に対する原子濃度比とは、F、Si、およびNの、セラミック素体の表面から検出されるNi,Cu,Zn,Feなどのそれぞれの原子濃度に対する比ではなく、セラミック素体の表面から検出される元素のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度に対する比である。
2≦F/セラミック素体≦12、
0.1≦Si/セラミック素体≦1.0
0.1≦N/セラミック素体≦1.3
の要件を満たすとき、良好なセルフアライメント性およびNiめっき連続性が得られることが確認された。
それから、外部電極本体(下地層)に、下層がNiめっき膜、上層がSnめっき膜(またははんだめっき膜)からなる2層構造のめっき膜を形成した。
まず、A-CF2O(CF2O)x(C2F4O)yCF2-A
ただし、A:-CONH(CH2)3Si(OCH3)3
x、y:8~12
の化合物と、溶媒であるハイドロフルオロエーテルを含む撥油処理剤を準備した。
浸漬終了後、直ちに、上記実施例4の方法と同じ方法および同じ条件で吸引液切りを行い、セラミック素体上の過剰な撥油処理液を除去した。
そして、過剰な撥油処理液を除去したセラミック素体を80℃で約30分間熱処理した。
そして、超音波洗浄の終了後に、上記実施例4の方法と同じ方法および同じ条件で吸引液切りを行い、洗浄液であるハイドロフルオロエーテルを除去し、積層セラミックインダクタ(図1参照)を得た。
表4に、この実施例7の積層セラミックインダクタについて調べた、表面の撥油状態、セルフアライメント性およびNiめっき膜の連続性の評価結果を示す。
(イ)試料番号4の試料の場合、F、Si、およびNの、X線光電子分光法(XPS)による、セラミック素体(フェライト素体)表面に対する原子濃度比が、
(F/セラミック素体)=12
(Si/セラミック素体)=1.0
(N/セラミック素体)=1.3
であった。
(ロ)試料番号5の試料の場合、F、Si、およびNの、X線光電子分光法(XPS)による、セラミック素体(フェライト素体)表面に対する原子濃度比が、
(F/セラミック素体)=8
(Si/セラミック素体)=0.6
(N/セラミック素体)=0.8
であった。
(ハ)試料番号6の試料の場合、F、Si、およびNの、X線光電子分光法(XPS)による、セラミック素体(フェライト素体)表面に対する原子濃度比が、
(F/セラミック素体)=2
(Si/セラミック素体)=0.1
(N/セラミック素体)=0.1
であった。
(ニ)試料番号4の試料の場合、F、Si、およびNの、X線光電子分光法(XPS)による、外部電極(最上層めっき膜)表面に対する原子濃度比が、
(F/外部電極)=10
(Si/外部電極)=0.8
(N/外部電極)=1.0
であった。
(ホ)試料番号5の試料の場合、F、Si、およびNの、X線光電子分光法(XPS)による、外部電極(最上層めっき膜)表面に対する原子濃度比が、
(F/外部電極)= 4.0
(Si/外部電極)=0.4
(N/外部電極)=0.6
であった。
(ヘ)試料番号5の試料の場合、F、Si、およびNの、X線光電子分光法(XPS)による、外部電極(最上層めっき膜)表面に対する原子濃度比が、
(F/外部電極)= 0.4
(Si/外部電極)=0.06
(N/外部電極)=0.07
であった。
なお、上記の各式における「セラミック素体」とは、セラミック素体から検出される元素(Ni,Cu,Zn,Feなど)のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度:単位atom%をいう。
すなわち、上記のF、Si、およびNの、セラミック素体表面に対する原子濃度比とは、F、Si、およびNの、セラミック素体の表面から検出されるNi,Cu,Zn,Feなどのそれぞれの原子濃度に対する比ではなく、セラミック素体の表面から検出される元素のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度に対する比である。
また、上記の各式における「外部電極」とは、外部電極から検出される元素(Ni,Ag,Znなど)のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度:単位atom%をいう。
すなわち、上記のF、Si、およびNの、外部電極表面に対する原子濃度比とは、F、Si、およびNの、外部電極の表面から検出されるNi,Ag,Znなどのそれぞれの原子濃度に対する比ではなく、外部電極の表面から検出される元素のうち、撥油処理剤成分元素と酸素元素とを除いた元素の合計の原子濃度に対する比である。
2≦F/セラミック素体≦12
0.1≦Si/セラミック素体≦1.0
0.1≦N/セラミック素体≦1.3
の要件を満たし、かつ、
F、Si、Nの各元素の、外部電極表面(最外層めっき膜)に対する原子濃度比が、
0.4≦F/外部電極≦10
0.06≦Si/外部電極≦0.8
0.07≦N/外部電極≦10
の要件を満たすとき、良好なセルフアライメント性およびNiめっき連続性が得られることが確認された。
本発明は、さらにその他の点においても、上記実施例に限定されるものではなく、撥油処理剤の主成分であるポリフルオロポリエーテル化合物の種類、溶媒との配合割合などに関し、発明の範囲内において、種々の応用、変形を加えることが可能である。
2 コイル用導体(コイルパターン)
3 ビアホール
4 コイル
4a,4b 引き出し電極
5 セラミック素体
5a,5b セラミック素体の端面
6a,6b 外部電極
Claims (11)
- セラミック素体と、前記セラミック素体の表面に配設された外部電極とを備えるセラミック電子部品の製造方法であって、
前記セラミック素体の表面に前記外部電極を形成した後に、撥油処理剤を用いて前記セラミック素体に撥油処理を施し、前記セラミック素体の表面にフラックス浸入防止膜を形成する撥油処理工程を備え、かつ、
前記撥油処理剤は、少なくとも1つの
-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基)
を含有するポリフルオロポリエーテル化合物を主成分とし、ハイドロフルオロエーテルを溶媒として含むものであること
を特徴とするセラミック電子部品の製造方法。 - セラミック素体と、前記セラミック素体の表面に配設され、表面にめっき膜を有する外部電極とを備えるセラミック電子部品の製造方法であって、
前記外部電極の表面に前記めっき膜を形成した後に、撥油処理剤を用いて前記セラミック素体に撥油処理を施し、前記セラミック素体の表面にフラックス浸入防止膜を形成する撥油処理工程を備え、かつ、
前記撥油処理剤は、少なくとも1つの
-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基)
を含有するポリフルオロポリエーテル化合物を主成分とし、ハイドロフルオロエーテルを溶媒として含むものであること
を特徴とするセラミック電子部品の製造方法。 - セラミック素体と、前記セラミック素体の表面に配設され、表面にめっき膜を有する外部電極とを備えるセラミック電子部品の製造方法であって、
前記外部電極を形成した後、前記めっき膜を形成する前に、撥油処理剤を用いて前記セラミック素体に撥油処理を施し、前記セラミック素体の表面にフラックス浸入防止膜を形成する撥油処理工程を備え、かつ、
前記撥油処理剤は、少なくとも1つの
-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基)
を含有するポリフルオロポリエーテル化合物を主成分とし、ハイドロフルオロエーテルを溶媒として含むものであること
を特徴とするセラミック電子部品の製造方法。 - 前記撥油処理剤のポリフルオロポリエーテル化合物が、下記の(I),(II),(III),(IV),(V),(VI)からなる群より選ばれる少なくとも1種であることを特徴とする請求項1~3のいずれかに記載のセラミック電子部品の製造方法:
(I) C3F7O(CF(CF3)CF2O)yCF(CF3)-A
(II) CF3O(C2F4O)yCF2-A
(III) A-CF2O(CF2O)x(C2F4O)yCF2-A
(IV) A-CF2O(C2F4O)xCF2-A
(V) A-CF(CF3)O(CF(CF3)CF2O)yCF(CF3)-A
(VI) A-(CF2)3O(C4F8O)y(CF2O)3-A
ただし、前記Aは、
(イ)-CONH(CH2)3Si(OR)3
(ただし、ORは、メトキシ基、もしくは、エトキシ基),
(ロ)(CnF2n+1)
(ハ)(CnF2n+1O)
(ニ)(HCnF2nO)
(ホ)(HCnF2n+1O)
からなる群より選ばれる少なくとも1種であり、(I)~(VI)の構造式において、少なくとも一つの前記Aは、前記(イ)の-CONH(CH2)3Si(OR)3であり、かつ、
前記xは1~50、yは4~40、nは1~4。 - 前記撥油処理剤として、ポリフルオロポリエーテル化合物の濃度が0.04~0.5重量%のものを用いて撥油処理することを特徴とする請求項1~4のいずれかに記載のセラミック電子部品の製造方法。
- 前記撥油処理工程の直後に、過剰な前記撥油処理剤を取り去る撥油処理剤除去工程を備えていることを特徴とする請求項1~5のいずれかに記載のセラミック電子部品の製造方法。
- 前記撥油処理剤除去工程の後に、前記セラミック素体を、ハイドロフルオロエーテルで洗浄する洗浄工程を備えていることを特徴とする請求項6記載のセラミック電子部品の製造方法。
- 前記撥油処理剤除去工程と前記洗浄工程との間に、前記セラミック素体を加熱処理する工程を備えていることを特徴とする請求項7記載のセラミック電子部品の製造方法。
- 前記セラミック素体を構成するセラミックがNiCuZnフェライトであることを特徴とする請求項1~8のいずれかに記載のセラミック電子部品の製造方法。
- セラミック素体と、前記セラミック素体の表面に配設された外部電極を備えるセラミック電子部品であって、
前記セラミック素体を構成するセラミック表面から、少なくともF、Si、およびNが検出され、かつ、
前記各元素の前記セラミック表面に対する原子濃度比が、
2≦(F/セラミック素体)≦12、
0.1≦(Si/セラミック素体)≦1.0、
0.1≦(N/セラミック素体)≦1.3、
の要件を満たすこと
を特徴とするセラミック電子部品。 - セラミック素体と、前記セラミック素体の表面に配設された外部電極を備えるセラミック電子部品であって、
前記セラミック素体を構成するセラミック表面、および、外部電極表面から、少なくともF、Si、およびNが検出され、
前記セラミック表面では、F、Si、およびNの各元素の前記セラミック表面に対する原子濃度比が、
2≦(F/セラミック素体)≦12、
0.1≦(Si/セラミック素体)≦1.0、
0.1≦(N/セラミック素体)≦1.3、
の要件を満し、
前記外部電極表面では、F、Si、およびNの各元素の前記外部電極表面に対する原子濃度比が、
0.4≦(F/外部電極)≦10、
0.06≦(Si/外部電極)≦0.8、
0.07≦(N/外部電極)≦1.0、
の要件を満たすこと
を特徴とするセラミック電子部品。
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JP2021064702A (ja) * | 2019-10-15 | 2021-04-22 | 株式会社村田製作所 | コイル部品およびその製造方法、ならびにコイル部品を実装した電子部品 |
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JP2012164966A (ja) * | 2011-01-21 | 2012-08-30 | Murata Mfg Co Ltd | セラミック電子部品 |
EP2816046B1 (en) * | 2012-02-17 | 2019-01-23 | AGC Inc. | Fluorinated ether compound, fluorinated ether composition and coating fluid, and substrate having surface-treated layer and method for its production |
JP6127985B2 (ja) * | 2012-02-17 | 2017-05-17 | 旭硝子株式会社 | 含フッ素エーテル化合物、含フッ素エーテル組成物およびコーティング液、ならびに表面処理層を有する基材およびその製造方法 |
CN104114566B (zh) * | 2012-02-17 | 2017-05-31 | 旭硝子株式会社 | 含氟醚化合物、含氟醚组合物及涂覆液以及具有表面处理层的基材及其制造方法 |
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