JP2019009051A - スパークプラグ - Google Patents
スパークプラグ Download PDFInfo
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- JP2019009051A JP2019009051A JP2017125610A JP2017125610A JP2019009051A JP 2019009051 A JP2019009051 A JP 2019009051A JP 2017125610 A JP2017125610 A JP 2017125610A JP 2017125610 A JP2017125610 A JP 2017125610A JP 2019009051 A JP2019009051 A JP 2019009051A
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- Prior art keywords
- insulator
- component
- spark plug
- alumina
- crystal grain
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- 239000012212 insulator Substances 0.000 claims abstract description 78
- 239000013078 crystal Substances 0.000 claims abstract description 73
- 239000000523 sample Substances 0.000 claims abstract description 51
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 25
- 238000010894 electron beam technology Methods 0.000 claims abstract description 24
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- 238000001514 detection method Methods 0.000 claims abstract description 6
- 230000005540 biological transmission Effects 0.000 claims abstract description 4
- 229910052788 barium Inorganic materials 0.000 claims description 10
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 abstract description 13
- 238000005259 measurement Methods 0.000 description 48
- 239000000843 powder Substances 0.000 description 34
- 239000012071 phase Substances 0.000 description 29
- 239000002245 particle Substances 0.000 description 22
- 229910015999 BaAl Inorganic materials 0.000 description 21
- 238000000034 method Methods 0.000 description 17
- 238000005245 sintering Methods 0.000 description 17
- 239000011521 glass Substances 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 13
- 125000001475 halogen functional group Chemical group 0.000 description 13
- 238000005452 bending Methods 0.000 description 12
- 238000009826 distribution Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000011230 binding agent Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 9
- 238000010586 diagram Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 238000010304 firing Methods 0.000 description 8
- 229910052746 lanthanum Inorganic materials 0.000 description 8
- 229910052791 calcium Inorganic materials 0.000 description 7
- 238000000280 densification Methods 0.000 description 7
- 238000002524 electron diffraction data Methods 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000002159 abnormal effect Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910052779 Neodymium Inorganic materials 0.000 description 3
- 229910052777 Praseodymium Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910052769 Ytterbium Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000007561 laser diffraction method Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- -1 rare earth compound Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 241000978776 Senegalia senegal Species 0.000 description 1
- 229910002794 Si K Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T13/00—Sparking plugs
- H01T13/02—Details
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
- C04B35/117—Composites
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- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T13/00—Sparking plugs
- H01T13/20—Sparking plugs characterised by features of the electrodes or insulation
- H01T13/38—Selection of materials for insulation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T13/00—Sparking plugs
- H01T13/58—Testing
- H01T13/60—Testing of electrical properties
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
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- Combustion & Propulsion (AREA)
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- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
原料粉末として、平均粒径が0.2〜2.1μmのアルミナ粉末、SiO2粉末、及び、Ba,Ca,Mg,Laの炭酸塩粉末を準備した。これらの粉末を種々の割合で混合した原料粉末と、バインダーとしてのポリビニルアルコールと、溶媒としての水とを混合して種々のスラリーを調製した。
サンプル1〜12における焼結体の組成、即ち各成分の含有率を、ICP発光分光分析により検出した。検出された各成分の酸化物換算の質量の合計を100wt%としたときの質量割合(%)として、各成分の含有率を算出した。
サンプル1〜23,27〜29における焼結体について、STEM−EDS(日立製作所製HD−2000)を用いて組成に関する情報を得た。加速電圧は200kV、電子線のプローブ径は1.0nmとし、EDSによる元素分析、元素マッピング、電子線回折を50,000倍の倍率で行った。
サンプル1〜29における焼結体(絶縁体11)について、軸線O(図1参照)を含む断面を鏡面研磨した後、熱エッチング処理を行った。熱エッチング処理の代わりに化学エッチング処理を行っても良い。SEMを用いて、エッチング処理を行った断面を観察した。SEMの加速電圧は15kV、作動距離は10〜12mmとした。1視野の大きさを200μm×200μmとする矩形領域のSEM画像を、無作為に10視野撮影した。
図6に示す耐電圧試験装置30を用いて、サンプル1〜20,24〜26における有底筒状の試料41(アルミナ基焼結体)の800℃における高温耐電圧試験を行った。図6は耐電圧試験装置30の断面図である。
JIS R1601:2008年に基づいて、室温(5〜35℃)における3点曲げ強さを測定した。
サンプル21〜23における焼結体(絶縁体11)について、形状測定レーザマイクロスコープVK−X110/X100(キーエンス社製)を用いて、絶縁体11の先端部の軸線O方向における算術平均粗さを測定した。
サンプル21〜23における焼結体(絶縁体11)について、材料試験機を用いて、周方向における異なる3方向から絶縁体11(図1参照)の先端部に対して軸線Oと直交する向きの荷重を加え、絶縁体11に破壊が生じたときの荷重(破壊荷重)を測定した。
サンプル24〜26における焼結体に研磨処理を施した後、株式会社リガク製のX線回折装置(型式:Smart Lab)を用いて、X線:CuKα(λ1.54Å)、X線出力:40kV−30mA、スキャンスピード(計数時間):20.0、サンプリング幅:0.02deg、入射スリット:1/2deg、受光スリット(1):15.000mm、受光スリット(2):20.000mmの測定条件でX線回折分析をした。
11 絶縁体
21 結晶粒界
Claims (6)
- アルミナ基焼結体からなる絶縁体を備え、
前記絶縁体は、酸化物換算で、Al成分を90〜98wt%含有するスパークプラグであって、
前記絶縁体は、酸化物換算で、Si成分を1〜5wt%、Mg成分を0.1〜1wt%、Ca成分を2wt%以下、Ba成分を0.3〜6wt%、希土類成分を0.11〜5wt%含有し、
電子線のプローブ径が1nmの走査透過型電子顕微鏡を用いた分析において、厚さ15nm以下の結晶粒界にSi及び希土類元素が検出され、前記結晶粒界におけるアルカリ土類金属は検出限界未満であるスパークプラグ。 - 前記Ba成分の含有率は1〜6wt%である請求項1記載のスパークプラグ。
- 前記Ca成分の含有率は0.3wt以下である請求項1又は2に記載のスパークプラグ。
- 前記Si成分の含有率は1〜2.7wt%である請求項1から3のいずれかに記載のスパークプラグ。
- 前記絶縁体の相対密度は94〜99%であり、前記絶縁体の任意の断面を鏡面研磨した面内に存在する気孔のうち1μm以上の大きさの気孔の割合が1%以下である請求項1から4のいずれかに記載のスパークプラグ。
- 前記絶縁体は、酸化物換算で、Na成分を100〜2000ppm含有する請求項1から5のいずれかに記載のスパークプラグ。
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