EP2608629B1 - Keramischer Heizer und Herstellungsverfahren dafür, und Heizvorrichtung - Google Patents

Keramischer Heizer und Herstellungsverfahren dafür, und Heizvorrichtung Download PDF

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Publication number
EP2608629B1
EP2608629B1 EP12199164.0A EP12199164A EP2608629B1 EP 2608629 B1 EP2608629 B1 EP 2608629B1 EP 12199164 A EP12199164 A EP 12199164A EP 2608629 B1 EP2608629 B1 EP 2608629B1
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EP
European Patent Office
Prior art keywords
heat
generating portion
generating
ceramic heater
substrate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP12199164.0A
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English (en)
French (fr)
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EP2608629A2 (de
EP2608629A3 (de
Inventor
Yohei Kan
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Niterra Co Ltd
Original Assignee
NGK Spark Plug Co Ltd
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Publication of EP2608629A2 publication Critical patent/EP2608629A2/de
Publication of EP2608629A3 publication Critical patent/EP2608629A3/de
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Publication of EP2608629B1 publication Critical patent/EP2608629B1/de
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/017—Manufacturing methods or apparatus for heaters
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/027—Heaters specially adapted for glow plug igniters
    • 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
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49082—Resistor making
    • Y10T29/49083—Heater type

Definitions

  • the present invention relates to a ceramic heater in which a heat-generating element is held in a substrate, to a method of manufacturing the ceramic heater, and to a heating apparatus having the ceramic heater.
  • a glow plug used, for example, to help startup of a diesel engine includes a tubular metallic shell and a heater having an incorporated heat-generating element which generates heat through energization.
  • the heater may be a ceramic heater.
  • the ceramic heater is configured such that a heat-generating element made of electrically conductive ceramic is held in a substrate made of an electrically insulating ceramic (refer to, for example, Japanese Patent Application Laid-Open (kokai) No. 2006-351446 ).
  • a recently proposed ceramic heater employs a heat-generating element formed from a material which contains, for example, a silicide or a carbide of molybdenum or tungsten as a main component so as to improve heat resistance of the heat-generating element, whereby, even when quick temperature rise (e.g., the temperature of the surface of the substrate is raised to 1,000°C or higher within two seconds) is repeated within a combustion chamber, the heat-generating element is unlikely to suffer an electrical disconnection (refer to, for example, Japanese Patent Application Laid-Open (kokai) No. 2010-181125 ).
  • European Patent Application EP1998596 A1 describes a ceramic heater having the features cited in the preamble of claim 1, comprising an insulating substrate formed from an insulating ceramic, and a heat-generating resistor formed from a conductive ceramic embedded in the insulating substrate.
  • European Patent Application EP1139693 A2 describes a method for manufacturing a ceramic heater having the features cited in the preamble of claim 5, including the steps of joining together two half green bodies consisting of a ceramic substrate to accommodate a unitary green body, comprising electrically conductive material and subsequent hot-pressing to provide the ceramic heater.
  • EP 1213 274 A2 discloses a silicon nitride tungsten carbide composite sintered material adapted to be used within the heat of a glow plug, of which a test piece having dimensions of 3 mm x 4 mm x 50 mm has a fracture toughness of 4.7 to 5.8 MPa*m ⁇ 0.5.
  • the inventors of the present invention carried out extensive studies and found the following: conventionally, durability of the heat-generating element in terms of electrical disconnection (service life of the heat-generating element) is determined mainly from heat resistance; however, repeated application of a large thermal stress to the heat-generating element is responsible for the occurrence of an electrical disconnection in the heat-generating element.
  • the present invention has been conceived in view of the above circumstances.
  • the present invention provides a ceramic heater with the features of claim 1 which can exhibit effective restraint of the occurrence of an electrical disconnection in a heat-generating element even upon energization for heating under the condition of ultrahigh-speed temperature raising, thereby providing long service life.
  • Another aspect of the present invention is a method with the features of claim 5 of manufacturing a ceramic heater as described above.
  • a ceramic heater of the present configuration that comprises a substrate and a heat-generating element.
  • the substrate is formed from an electrically insulating ceramic and extends rearward from the forward end of the ceramic heater in the direction of an axis.
  • the heat-generating element has a heat-generating portion formed from an electrically conductive ceramic which contains silicon nitride and an electrically conductive material, disposed in a forward end portion of the substrate, and having a shape resembling a letter U as viewed along the direction of the axis.
  • the heat-generating portion has a fracture toughness of 4.3 MPa ⁇ m 0.5 or more.
  • the heat-generating portion of the heat-generating element has a fracture toughness of 4.3 MPa ⁇ m 0.5 or more.
  • the heat-generating portion disposed in a forward end portion of the substrate has such a high strength as to resist, over a long period of time, a very large thermal stress which is repeatedly applied thereto.
  • the ceramic heater can provide long service life.
  • a ceramic heater as described in the above configuration 1, wherein the heat-generating element has electrically conductive lead portions connected to respective ends of the heat-generating portion located on the rear end side of the heat-generating portion, and the thickness of the heat-generating portion is 30% or less that of the lead portions.
  • the thickness of the heat-generating portion is 30% or less than that of the lead portions (corresponding to power supply paths to the heat-generating portion). Therefore, the cross-sectional area of the heat-generating portion can be greatly smaller than that of the lead portions, and thus, the electrical resistivity of the heat-generating portion can be far more higher than that of the lead portions. As a result, at the time of energization, the temperature of the heat-generating portion can be raised quite quickly without being influenced by the lead portions, so that ultrahigh-speed temperature raising (the temperature of the surface of the substrate is raised to 1,000°C or higher within one second) can be implemented relatively easily.
  • the above configuration 2 involves concern about the occurrence of an electrical disconnection in the heat-generating element (heat-generating portion) at the time of ultrahigh-speed temperature raising, since the heat-generating portion is considerably thin as compared with the lead portions.
  • the concern can be eradicated through employment of the above configuration 1.
  • the above configuration 1 is particularly significant for a ceramic heater which has the heat-generating portion having a thickness of 30% or less that of the lead portions and thus involves much concern about the occurrence of an electrical disconnection in the heat-generating portion.
  • different materials may be used to form the heat-generating portion and the lead portions, or the heat-generating portion and the lead portions may be formed from the same material.
  • a material used to form the lead portions may be a metal material or an electrically conductive ceramic.
  • damage, such as cracking may arise to a certain extent at the joints between the heat-generating portion and the lead portions.
  • a ceramic heater as described in configuration 2 which is configured such that the heat-generating portion and the lead portions are formed from the same material. Employment of the present configuration can prevent the occurrence of damage, such as cracking, at the joints between the heat-generating portion and the lead portions and can improve productivity because of use of the same material.
  • a heating apparatus having an energization control unit configured to adjust supply power to the heat-generating element, and adapted to control heat generation of the heat-generating portion through adjustment of the supply power.
  • the energization control unit supplies power to the heat-generating element in such a manner as to raise the surface temperature of a heating portion of the substrate corresponding to the heat-generating portion from room temperature to 1,000°C within one second.
  • a heating apparatus such as that of the above configuration 4, in which the energization control unit supplies power to the heat-generating element in such a manner as to raise the surface temperature of a heating portion of the substrate located around the heat-generating portion from room temperature to 1,000°C within one second; i.e., in a heating apparatus in which the heat-generating element executes ultrahigh-speed temperature raising, an electrical disconnection is more likely to occur in the heat-generating element (heat-generating portion).
  • the ceramic heater of the above configuration 1, etc. the occurrence of an electrical disconnection in the heat-generating element can be more reliably prevented.
  • the ceramic heater of the above configuration 1, etc. fully exhibits its superior durability against ultrahigh-speed temperature raising when used in a heating apparatus in which power is supplied to the heat-generating element in such a manner as to raise the surface temperature of a heating portion of the substrate from room temperature to 1,000°C within one second.
  • a method of manufacturing a ceramic heater which comprises a substrate formed from an electrically insulating ceramic and extending rearward from the forward end of the ceramic heater in the direction of an axis, and a heat-generating element having a heat-generating portion containing silicon nitride and an electrically conductive material, disposed in a forward end portion of the substrate, and having a shape resembling a letter U as viewed along the direction of the axis.
  • the method comprises: a green element forming step of forming a green element body which is to become the heat-generating element, from an element material which contains an electrically conductive material powder and silicon nitride; a holding body forming step of forming a holding body in which the green element body is embedded in a green insulation body which is formed from a substrate material containing an electrically insulating ceramic powder and which is to become the substrate; a debindering step of debindering the holding body; and a firing step of firing, after the debindering step, the holding body under pressure.
  • the green element body has a prospective heat-generating portion which is to become the heat-generating portion. As measured after the debindering step and before the firing step, a portion of the green insulation body located around the prospective heat-generating portion has a relative density of 46.3% or more.
  • relative density means a proportion of the density of the green insulation body located around the prospective heat-generating portion expressed as a percent of the theoretical density of the substrate material as measured after the debindering step and before the firing step.
  • a portion of the green insulation body located around the prospective heat-generating portion has a relative density of 46.3% or more. Therefore, in the firing step, a large pressure can be applied from the green insulation body to the prospective heat-generating portion, whereby there can be accelerated the grain growth of silicon nitride which constitutes the green element body. As a result, the fracture toughness of the heat-generating portion can be more reliably increased, so that the ceramic heater having superior durability against ultrahigh-speed temperature raising can be more reliably manufactured.
  • the above configuration 5 is particularly significant in manufacture of the ceramic heater in which power is supplied to the heat-generating element in such a manner as to raise the surface temperature of a heating portion of the substrate from room temperature to 1,000°C within one second.
  • FIG. 1 is a block diagram showing the schematic configuration of a heating apparatus 101.
  • the heating apparatus 101 includes a ceramic glow plug 1 (hereinafter, referred to as the "glow plug 1") having a ceramic heater 4, and a glow control unit (GCU) 102 (an energization control unit) to control energization of the glow plug 1.
  • FIG. 1 shows only a single glow plug 1. However, an actual engine has a plurality of cylinders, and the glow plug 1 and a switch 104, which will be described later, are provided for each of the cylinders.
  • the GCU 102 operates by power supplied from a battery VA and includes a microcomputer 103 having a CPU, a ROM, a RAM, etc., and the switch 104 adapted to turn ON/OFF the supply of power to the glow plug 1 from the battery VA.
  • the GCU 102 controls energization of the glow plug 1 under PWM control such that the switch 104 turns ON/OFF the supply of power to the glow plug 1 under instructions from the microcomputer 103.
  • the switch 104 is configured such that an FET (field effect transistor) having a current detecting function is operated via an NPN transistor, etc.
  • the microcomputer 103 is connected to the power supply terminals of the glow plug 1 via a voltage-dividing resistor (not shown), and a voltage obtained by dividing a voltage to be applied to the glow plug 1 (a voltage output from the GCU 102) is input to the microcomputer 103.
  • the microcomputer 103 can calculate an applied voltage to the glow plug 1 on the basis of the input voltage and can measure the resistance of the glow plug 1 from the applied voltage and current which flows through the glow plug 1 and is measured by the switch 104.
  • the microcomputer 103 is designed to perform, when the engine key is turned ON, preglow energization for quickly raising the temperature of the glow plug 1 (the ceramic heater 4), and thereafter, after-glow energization for maintaining the glow plug 1 at a predetermined temperature for a predetermined period of time.
  • preglow energization power is supplied to the glow plug 1 in such a manner as to raise the temperature of the surface of a substrate 21, which will be described later, of the glow plug 1 from room temperature to 1,000°C within one second (ultrahigh-speed temperature raising).
  • the temperature of the glow plug 1 is quickly raised to a target temperature irrespective of characteristics of the glow plug 1, by matching, with a predetermined reference curve, a curve indicative of the relationship between power to be supplied to the glow plug 1 and elapsed time. Specifically, by use of a relational expression or a table indicative of the predetermined reference curve, power to be supplied at a point of elapsed time from start of energization is obtained. From the relationship between current flowing through the glow plug 1 and power to be supplied at a point of elapsed time, voltage to be applied to the glow plug 1 is obtained, and voltage to be applied to the glow plug 1 (effective voltage) is controlled under PWM control.
  • supply power to the glow plug 1 is adjusted such that the surface temperature of the substrate 21 is maintained at a high temperature (e.g., 1,200°C or higher) for a relatively long period of time (e.g., about 180 seconds).
  • a high temperature e.g., 1,200°C or higher
  • a relatively long period of time e.g., about 180 seconds
  • FIG. 2A is a sectional view of the glow plug 1
  • FIG. 2B is a front view of the glow plug 1.
  • FIG. 3 is a fragmentary, enlarged, sectional view of the glow plug 1, primarily showing the ceramic heater 4.
  • the lower side of the glow plug 1 (the ceramic heater 4) is referred to as the forward side of the glow plug 1, and the upper side as the rear side of the glow plug 1.
  • the glow plug 1 includes a housing 2, an axial rod 3, the ceramic heater 4, a sleeve 5, and a terminal pin 6 or a like.
  • the housing 2 is formed from a predetermined metal material (e.g., an iron-based material, such as S45C) and has an axial bore 7 extending along the direction of an axis CL1. Furthermore, as viewed externally, the housing 2 has an externally threaded portion 8 formed at its central portion with respect to the direction of the axis CL1. The externally threaded portion 8 is adapted to mount the glow plug 1 to, for example, the cylinder head of an engine. Also, as viewed externally, the housing 2 has a flange-like tool engagement portion 9 formed at its circumference of the rear end portion and having a hexagonal cross section. When the glow plug 1 (the externally threaded portion 8) is to be mounted to, for example, the cylinder head, a mounting tool is engaged with the tool engagement portion 9.
  • a predetermined metal material e.g., an iron-based material, such as S45C
  • the axial bore 7 of the housing 2 accommodates the axial rod 3 made of metal and having a circular cross section.
  • a forward end portion of the axial rod 3 is press-fitted into a rear end portion of a cylindrical connection member 10 formed from a metal material (e.g., an iron-based material, such as SUS).
  • a rear end portion of the ceramic heater 4 is press-fitted into a forward end portion of the connection member 10.
  • the axial rod 3 and the ceramic heater 4 are mechanically and electrically connected to each other via the connection member 10.
  • the axial rod 3 has a diameter-reduced portion 13 formed at its intermediate portion that is smaller in outside diameter than its forward and rear end portions. The diameter-reduced portion 13 mitigates stress transmitted to the axial rod 3.
  • predetermined lead wires or the like may be used to electrically connect the axial rod 3 and the ceramic heater 4 to each other.
  • a terminal pin 6 made of metal is fixedly crimped to a rear end portion of the axial rod 3.
  • An electrically insulating bushing 11, formed from an electrically insulating material, is disposed between a forward end portion of the terminal pin 6 and a rear end portion of the housing 2 in order to prevent direct electrical communication (short circuit) therebetween.
  • an O-ring 12 formed from an electrically insulating material is provided between the housing 2 and the axial rod 3 in such a manner as to be in contact with a forward end portion of the electrically insulating bushing 11 in order to improve gastightness or a like within the axial bore 7.
  • the sleeve 5 is formed into a cylindrical shape from a predetermined metal material.
  • the sleeve 5 holds an intermediate portion, along the direction of the axis CL1, of the ceramic heater 4.
  • a forward end portion of the ceramic heater 4 projects and is exposed from the forward end of the sleeve 5.
  • the sleeve 5 is joined to the housing 2 through laser welding along the outer circumference of the contact surface between the housing 2 and the sleeve 5 in a state in which a rear end portion of the sleeve 5 is inserted into the axial bore 7.
  • the ceramic heater 4 includes the round rodlike substrate 21 extending rearward from the forward end of the ceramic heater 4 along the direction of the axis CL1, and a heat-generating element 22 embedded in the substrate 21.
  • the substrate 21 is formed from an electrically insulating ceramic (e.g., silicon nitride or alumina or a like).
  • the heat-generating element 22 is formed from an electrically conductive ceramic which contains silicon nitride as a main component, and an electrically conductive material (in the present embodiment, a silicide, a nitride, or a carbide of molybdenum or tungsten).
  • the heat-generating element 22 includes a heat-generating portion 23 disposed in a forward end portion of the substrate 21, and a pair of rodlike lead portions 24 and 25 extending rearward from respective rear ends of the heat-generating portion 23.
  • the heat-generating portion 23 functions as a so-called heat-generating resistor and has a shape resembling the letter U so as to follow the curved surface of a curved forward end portion of the ceramic heater 4. More specifically, the U-shaped heat-generating portion 23 has a turnback subportion 231 provided at its front end side and straight subportions 232 and 233 extending from the turnback subportion 231.
  • the lead portions 24 and 25 extend rearward substantially in parallel with each other directed toward the rear end portion of the ceramic heater 4.
  • One lead portion 24 has an electrode lead portion 26, located toward its rear end, projecting radially outward in such a manner as to be exposed at the outer circumferential surface of the ceramic heater 4.
  • the other lead portion 25 has an electrode lead portion 27, located toward its rear end, projecting radially outward in such a manner as to be exposed at the outer circumferential surface of the ceramic heater 4.
  • the electrode lead portion 26 of the one lead portion 24 is located rearward of the electrode lead portion 27 of the other lead portion 25 with respect to the direction of the axis CL1.
  • the exposed surface of the electrode lead portion 26 is in contact with the inner circumferential surface of the connection member 10, thereby establishing electrical communication between the lead portion 24 and the axial rod 3 connected to the connection member 10.
  • the exposed surface of the electrode lead portion 27 is in contact with the inner circumferential surface of the sleeve 5, thereby establishing electrical communication between the lead portion 25 and the housing 2 connected to the sleeve 5. That is, in the present embodiment, the axial rod 3 and the housing 2 function as an anode and a cathode for supplying power to the heat-generating portion 23 of the ceramic heater 4 in the glow plug 1.
  • the heat-generating portion 23 and the lead portions 24 and 25 are formed from the same material (a material which contains silicon nitride and an electrically conductive material). As shown in FIG. 4 , as measured in a direction orthogonal to a plane which contains the center axes of the lead portions 24 and 25, a thickness T1 of the heat-generating portion 23 is 30% or less a thickness T2 of the lead portions 24 and 25 Accordingly, the cross-sectional area of the heat-generating portion 23 (the area of a section taken orthogonally to the axis CL1) is far smaller than that of the lead portions 24 and 25. Thus, the (electrical) resistivity of the heat-generating portion 23 can be far higher than that of the lead portions 24 and 25, whereby, upon energization, the temperature of the heat-generating portion 23 can be raised quite quickly.
  • the thickness T1 of the heat-generating portion 23 is the thickness of a region of the heat-generating portion 23 having a substantially fixed thickness (an average thickness). Also, the thickness T2 of the lead portions 24 and 25 is the thickness of a region of the lead portions 24 and 25 having a substantially fixed thickness (an average thickness).
  • the heat-generating portion 23 has a fracture toughness of 4.3 MPa ⁇ m 0.5 or more.
  • the fracture toughness of the heat-generating portion 23 is calculated according to the IF method of JIS R1607.
  • the surface of the ceramic heater 4 (the substrate 21) is started from a direction perpendicular to the direction of the axis CL1 and along an overlapping direction of the straight subportions 232 and 233 of the heat-generating portion 23 (in other words, grinding is started in the horizontal direction from the right side or the left side on the paper on which FIG. 3 appears), and grinding is continued until the center of the width (the horizontal length on the paper on which FIG. 3 appears) of one of the straight subportion 232 or 233 is reached.
  • finish-polishing is performed so as to impart a surface roughness of 0.100 ⁇ mRa or less to the surface, thereby forming a surface-to-be-measured S of the heat-generating portion 23 (see FIG. 17 ).
  • a diamond indenter is driven with a predetermined indentation load P (2 kgf) for a predetermined time (15 seconds) on the surface-to-be-measured S of the heat-generating portion 23 at a position P (see FIG. 17 ) corresponding to the above-specified length A.
  • a portion of the surface of the substrate 21 which corresponds to the heat-generating portion 23 is the “heating portion” in the present invention.
  • a portion of the surface of the substrate 21 whose temperature becomes the highest upon energization in the present embodiment, a portion of the surface located 2 mm rearward from the forward end of the substrate 21 may be the “heating portion.”
  • a silicon nitride powder is added to an electrically conductive material (e.g., a carbide of W); the resultant mixture is slurried in water; and the resultant slurry is spray-dried.
  • an electrically conductive material e.g., a carbide of W
  • the resultant mixture is slurried in water
  • the resultant slurry is spray-dried.
  • a binder, a plasticizer, a dispersant, etc. are added, followed by mixing so as to yield a powdery element material.
  • a green element body 32 (see FIG. 6 ) which is to become the heat-generating element 22 is formed.
  • a first mold 51 and a second mold 52 are mated with each other.
  • a heated liquid element material M1 is then injected into a cavity 53 corresponding to the shape of the heat-generating element 22 that is formed in the molds 51 and 52.
  • the injection-molded element material M1 is dried and solidified at a predetermined temperature (e.g., 100°C to 250°C), thereby yielding the green element body 32 having, at its forward end portion, a prospective heat-generating portion 33 which is to become the U-shaped heat-generating portion 23.
  • a predetermined temperature e.g. 100°C to 250°C
  • a halved green insulation body 31X (see FIG. 6 ) separately from formation of the green element body 32, a halved green insulation body 31X (see FIG. 6 ) corresponding to half of the substrate 21 is formed.
  • an electrically insulating ceramic e.g., silicon nitride
  • a binder is added to the slurry; and the resultant slurry is spray-dried, thereby yielding a substrate material.
  • the halved green insulation body 31X is formed by use of a tubular outer frame 61 having an inner space having a rectangular cross section.
  • a lower mold 62 is disposed on a side toward one opening of the outer frame 61.
  • An upper mold 63 is disposed on a side toward the other opening of the outer frame 61 and is vertically movable in relation to the outer frame 61.
  • a portion of the lower mold 62 to be disposed within the outer frame 61 has a curved surface corresponding to the outer surface of the halved green insulation body 31X.
  • a portion of the upper mold 63 to be disposed within the outer frame 61 has, on its surface, a forming protrusion 63A having a shape resembling the letter U as viewed in plane for forming an accommodation cavity 31A (see FIG. 6 ) which accommodates half of the green element body 32.
  • the upper mold 63 has rectangular-parallelepiped protrusions 63B and 63C located on opposite sides of a portion of the forming protrusion 63A adapted to form an accommodation cavity which accommodates the prospective heat-generating portion 33.
  • a substrate material M2 is charged in a predetermined amount from the upper opening of the outer frame 61.
  • the upper mold 63 is disposed in such a manner as to close the upper opening of the outer frame 61.
  • the upper mold 63 is then moved toward the lower mold 62 so as to press the substrate material M2 under a predetermined load.
  • This procedure yields, as shown in FIG. 6 , the halved green insulation body 31X having the accommodation cavity 31A formed by the forming protrusion 63A, and cavities 31B and 31C formed by the protrusions 63B and 63C.
  • a holding body 30 (see FIG. 11 ) is formed by use of the halved green insulation body 31X, the green element body 32, and the substrate material M2.
  • the holding body forming step uses an outer frame 71 having an inner space having a rectangular cross section.
  • a lower mold 72 is disposed on a side toward one opening of the outer frame 71.
  • An upper mold 73 is disposed on a side toward the other opening of the outer frame 71 and is vertically movable in relation to the outer frame 71.
  • a surface of the lower mold 72 and a surface of the upper mold 73 which are disposed within the outer frame 71 are curved so as to correspond to the outer surface of the holding body 30.
  • the outer frame 71 has inclined surfaces 71A inclined inward and formed on its upper end surface at positions located on opposite sides of the prospective heat-generating portion 33 to be disposed.
  • the outer frame 71 and the lower mold 72 are assembled together, and then the halved green insulation body 31X is set on the lower mold 72. Then, as shown in FIG. 6 , the green element body 32 is placed in the accommodation cavity 31A of the halved green insulation body 31X. Subsequently, the substrate material M2 is charged into the outer frame 71 in such a manner as to cover the green element body 32.
  • the substrate material M2 is also charged onto the inclined surfaces 71A, and, since the cavities 31B and 31C of the halved green insulation body 31X are filled with the substrate material M2, the associated charged substrate material M2 in the region near cavities 31B, 31C is thicker than the substrate material M2 charged in the other regions.
  • the lower mold 72 is moved downward in relation to the outer frame 71, whereby the substrate material M2 charged in the outer frame 71 moves downward. Accordingly, as shown in FIG. 13 , the substrate material M2 on the inclined surfaces 71A slides down into the outer frame 71.
  • the upper mold 73 is disposed in such a manner as to close the upper opening of the outer frame 71 and is then moved toward the lower mold 72 so as to press the substrate material M2 under a predetermined load.
  • the holding body 30 configured such that the green element body 32 is held within a green insulation body 31.
  • the packing density of a portion of the green insulation body 31 located around the prospective heat-generating portion 33 is increased through the synergy of the following: as mentioned above, the substrate material M2 charged on the inclined surfaces 71A slides down into the outer frame 71, and the substrate material M2 is charged in a relatively large amount in the cavities 31B and 31C.
  • a debindering step (S5), the holding body 30 is heated at a predetermined temperature (e.g., about 800°C) in a nitrogen gas atmosphere, thereby removing the plasticizer and the binder from the green element body 32 and the green insulation body 31.
  • a portion of the green insulation body 31 located around the prospective heat-generating portion 33 has a relatively high packing density
  • after the debindering step a portion of the green insulation body 31 located around the prospective heat-generating portion 33 has a relative density of 46.3% or more.
  • relative density means a proportion of the density of the green insulation body 31 located around the prospective heat-generating portion 33 expressed as a percent of the theoretical density of the substrate material M2 as measured after the debindering step.
  • a parting agent is applied to the entire outer surface of the holding body 30.
  • the holding body 30 is subjected to a firing step (S7).
  • firing is performed by a so-called hot pressing process.
  • the holding body 30 is heated under pressure in a non-oxygen atmosphere under, for example, the following conditions: heating temperature 1,800°C; heating time 1.5 hours; and hot pressing pressure 25 MPa.
  • the firing step uses a carbon jig having a cavity whose shape corresponds to the external form of the above-mentioned ceramic heater 4.
  • the holding body 30 is uniaxially pressed.
  • the fired body 40 undergoes various types of grinding, thereby yielding the above-mentioned ceramic heater 4.
  • the employed types of grinding include centerless grinding for grinding the outer circumferential surface of the fired body 40 by use of a publicly known centerless grinding machine, so as to expose the electrode lead portions 26 and 27 from the outer circumferential surface, and R-grinding for imparting a curved surface to a forward end portion of the fired body 40 so as to establish a uniform distance between the extreme heat-generating portion 23 and the outer circumferential surface of the forward end portion.
  • the thus-manufactured ceramic heater 4 is assembled with the housing 2 and other members manufactured by publicly known methods.
  • the above-mentioned glow plug 1 is yielded.
  • the heat-generating portion 23 whose temperature becomes high upon energization has a fracture toughness of 4.3 MPa ⁇ m 0.5 or more.
  • the heat-generating portion 23 has such a high strength as to resist, over a long period of time, a very large thermal stress which is repeatedly applied thereto.
  • the occurrence of an electrical disconnection in the heat-generating element 22 can be effectively restrained, whereby the ceramic heater 4 can provide long service life.
  • the same material is used to form the heat-generating portion 23 and the lead portions 24 and 25.
  • the present embodiment can eradicate such concerns.
  • the electrical resistivity of the extreme heat-generating portion 23 can be far more higher than that of the lead portions 24 and 25.
  • the temperature of the heat-generating portion 23 can be raised quite quickly, so that ultrahigh-speed temperature raising (the temperature of the surface of the substrate is raised to 1,000°C or higher within one second) can be implemented relatively easily.
  • a portion of the green insulation body 31 located around the prospective heat-generating portion 33 has a relative density of 46.3% or more. Therefore, in the firing step, a large pressure can be applied from the green insulation body 31 to the prospective heat-generating portion 33, whereby there can be accelerated the grain growth of silicon nitride which constitutes the green element body 32. As a result, the fracture toughness of the heat-generating portion 23 can be more reliably increased, so that the ceramic heater 4 having superior durability against ultrahigh-speed temperature raising can be more reliably manufactured.
  • One test cycle consisted of one-second energization conducted so as to raise the temperature of the substrate surface (heating portion) from room temperature to 1,000°C in 0.5 second and such that the substrate surface reaches a maximum temperature of 1,350°C at the temperature-raising gradient, and subsequent air blast cooling for 30 seconds.
  • the samples which exhibited 50,000 electrical-disconnection cycles or more were evaluated as "Good,” indicating that the samples were superior in durability against quick temperature raising. Meanwhile, the samples which exhibited less than 50,000 electrical-disconnection cycles were evaluated as "Poor,” indicating that the samples were somewhat inferior in durability against quick temperature raising. Table 1 shows the results of the durability evaluation test.
  • the samples having a fracture toughness of 4.3 MPa ⁇ m 0.5 or more have superior durability against quick temperature raising. Conceivably, this is for the following reason: the heat-generating portion had such a high strength as to resist, over a long period of time, a very large thermal stress which is repeatedly applied thereto.
  • the establishment of a relative density of 46.3% or more as measured after the debindering step more reliably ensures that the heat-generating portion can have a fracture toughness of 4.3 MPa ⁇ m 0.5 or more.
  • this is for the following reason: by virtue of the relative density being increased, in the firing step, the green insulation body applied a higher pressure to the prospective heat-generating portion; as a result, in the prospective heat-generating portion, the grain growth of silicon nitride was accelerated.
  • the heat-generating portion has a fracture toughness of 4.3 MPa ⁇ m 0.5 or more.
  • a portion of the green insulation body located around the prospective heat-generating portion has a relative density of 46.3% or more.
  • the present invention is not limited to the above-described embodiment, but may be embodied, for example, as follows. Of course, applications and modifications other than those exemplified below are also possible.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Resistance Heating (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)

Claims (6)

  1. Keramik-Heizeinrichtung (4), die umfasst:
    ein Substrat (21), das aus einem elektrisch isolierenden Keramikmaterial besteht und sich von einem vorderen Ende der Keramik-Heizeinrichtung (4) in einer Richtung einer Achse (CL1) nach hinten erstreckt, sowie
    ein Wärmeerzeugungs-Element (22), das einen Wärmeerzeugungs-Abschnitt (23) aufweist, der aus einem elektrisch leitenden Keramikmaterial besteht, das Siliziumnitrid und ein elektrisch leitendes Material enthält, wobei der Wärmeerzeugungs-Abschnitt (23) in einem vorderen Endabschnitt des Substrats (21) angeordnet ist und eine Form hat, die, in der Richtung der Achse (CL1) gesehen, einem Buchstaben U ähnelt,
    dadurch gekennzeichnet, dass
    der Wärmeerzeugungs-Abschnitt (23) eine Bruchzähigkeit von 4,3 MPa·m0,5 oder mehr hat.
  2. Keramik-Heizeinrichtung nach Anspruch 1, wobei:
    das Wärmeerzeugungs-Element (22) elektrisch leitende Zuleitungs-Abschnitte (24, 25) aufweist, die mit jeweiligen Enden des Wärmeerzeugungs-Abschnitts (23) verbunden sind, wobei sich die Zuleitungs-Abschnitte (24, 25) an einer Seite des hinteren Endes des Wärmeerzeugungs-Abschnitts (23) befinden, und
    eine Dicke des Wärmeerzeugungs-Abschnitts (23) 30 % oder weniger der der Zuleitungs-Abschnitte (24, 25) beträgt.
  3. Keramik-Heizeinrichtung nach Anspruch 2, wobei der Wärmeerzeugungs-Abschnitt (23) und die Zuleitungs-Abschnitte (24, 25) aus dem gleichen Material bestehen.
  4. Heizvorrichtung, die umfasst:
    eine Keramik-Heizeinrichtung nach einem der Ansprüche 1 bis 3, sowie
    eine Energiezufuhr-Steuerungseinheit (102), die so konfiguriert ist, dass sie Speisestrom für das Wärmeerzeugungs-Element (22) reguliert, und so eingerichtet ist, dass sie Wärmeerzeugung des Wärmeerzeugungs-Abschnitts (23) über Regulierung des Speisestroms steuert,
    wobei die Energiezufuhr-Steuerungseinheit (102) dem Wärmeerzeugungs-Element (22) Strom so zuführt, dass eine Oberflächentemperatur eines Heiz-Abschnitts des Substrats (21), der dem Wärmeerzeugungs-Abschnitt entspricht, innerhalb von einer Sekunde von Raumtemperatur auf 1000 °C erhöht wird.
  5. Verfahren zum Herstellen einer Keramik-Heizeinrichtung nach Anspruch 1, die umfasst:
    ein Substrat (21), das aus einem elektrisch isolierenden Keramikmaterial besteht und sich in einer Richtung einer Achse (CL1) erstreckt, sowie
    ein Wärmeerzeugungs-Element (22), das in dem Substrat (21) eingebettet ist und einen Wärmeerzeugungs-Abschnitt (23) aufweist, der Siliziumnitrid und ein elektrisch leitendes Material enthält, das ein Silizid, ein Nitrid oder ein Carbid von Molybdän oder Wolfram enthält, wobei der Wärmeerzeugungs-Abschnitt (23) in einem vorderen Endabschnitt des Substrats (21) angeordnet ist und eine Form hat, die, in der Richtung der Achse (CL1) gesehen, einem Buchstaben U ähnelt,
    wobei das Verfahren umfasst:
    Ausbilden eines ungebrannten Grund-Körpers (32), aus dem das Wärmeerzeugungs-Element (22) wird, wobei der ungebrannte Grund-Körper (32) aus einem Grund-Material besteht, das ein Pulver aus elektrisch leitendem Material und Siliziumnitrid enthält;
    Ausbilden eines Aufnahme-Körpers (30), in dem der ungebrannte Grund-Körper (32) in einem ungebrannten Isolier-Körper (31X) eingebettet ist, wobei der ungebrannte Isolier-Körper (31X) aus einem Substrat-Material besteht, das ein Pulver aus elektrisch isolierendem Keramikmaterial enthält und aus dem das Substrat (21) wird;
    Entbindern des Aufnahme-Körpers (30); und
    Brennen des Aufnahme-Körpers (30) unter Druck;
    wobei der ungebrannte Grund-Körper (32) einen potentiellen Wärmeerzeugungs-Abschnitt (33) aufweist, aus dem der Wärmeerzeugungs-Abschnitt (23) wird, und
    dadurch gekennzeichnet, dass
    ein Abschnitt des ungebrannten Isolier-Körpers (31X), der um den potentiellen Wärmeerzeugungs-Abschnitt (33) herum angeordnet ist, gemessen nach dem Entbinderungs-Schritt und vor dem Brenn-Schritt, eine relative Dichte von 46,3 % oder mehr hat.
  6. Verfahren zum Herstellen einer Keramik-Heizeinrichtung nach Anspruch 5, wobei die Keramik-Heizeinrichtung so betrieben werden kann, dass eine Oberflächentemperatur eines Heiz-Abschnitts des Substrats (21), der dem Wärmeerzeugungs-Abschnitt (33) entspricht, innerhalb von einer Sekunde von Raumtemperatur auf 1000 °C erhöht wird.
EP12199164.0A 2011-12-21 2012-12-21 Keramischer Heizer und Herstellungsverfahren dafür, und Heizvorrichtung Active EP2608629B1 (de)

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JP6370754B2 (ja) * 2015-09-10 2018-08-08 日本特殊陶業株式会社 セラミックヒータおよびグロープラグ
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CN107046739B (zh) * 2016-11-24 2019-10-29 常德科锐新材料科技有限公司 大功率氮化硅陶瓷加热片及其内硬外软的制作方法
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CN207869432U (zh) * 2018-03-07 2018-09-14 东莞市国研电热材料有限公司 一种多温区陶瓷发热体
CN114263535B (zh) * 2021-12-14 2023-11-14 西安现代控制技术研究所 一种有效提高微型涡喷发动机点火可靠性的方法

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US20130160730A1 (en) 2013-06-27

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