TW200526795A - Ceramic sintered compact, method for producing ceramic sintered compact, exothermic element for vapor deposition of metal - Google Patents

Ceramic sintered compact, method for producing ceramic sintered compact, exothermic element for vapor deposition of metal Download PDF

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Publication number
TW200526795A
TW200526795A TW093138429A TW93138429A TW200526795A TW 200526795 A TW200526795 A TW 200526795A TW 093138429 A TW093138429 A TW 093138429A TW 93138429 A TW93138429 A TW 93138429A TW 200526795 A TW200526795 A TW 200526795A
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Taiwan
Prior art keywords
ceramic sintered
sintered body
powder
nitride
mass
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TW093138429A
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English (en)
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TWI292784B (zh
Inventor
Hiroshi Yokota
Fumio Tokunaga
Kentaro Iwamoto
Masamitsu Kimura
Shoujiro Watanabe
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Denki Kagaku Kogyo Kk
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Publication of TWI292784B publication Critical patent/TWI292784B/zh

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    • 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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    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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  • Ceramic Engineering (AREA)
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  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Ceramic Products (AREA)
  • Physical Vapour Deposition (AREA)

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200526795 (1) 九、發明說明 【發明所屬之技術領域】 本發明係有關陶瓷燒結體、陶瓷燒結體製造方法，金 屬蒸鍍用發熱體。 【先前技術】 向來，金屬蒸鍍用發熱體已知以氮化硼 （BN)、氮化 鋁（A1N)、二硼化鈦（TiBO爲主成分所形成之平板形狀 (以下以「板材」稱之）（專利文獻1)，其市售品之一例如 (曰本）電氣化學工業公司製商品名「BN Compojet EC」。亦有無凹槽者。其使用方法爲板材之兩端以挾具 連接電極附加電壓而發熱，將裝入凹槽之鋁線材等之金屬 熔融·蒸發得到蒸鍍膜後冷卻。 如此之板材，熔融金屬將板材腐蝕’將板材之有效斷 面及電阻變動，不能取得充分之蒸鍍速度。例如，熔融金 屬爲鋁時，引起次反應式之腐蝕。 A1 (s) + TiB2 (s) — A1 ⑴ + TiB2 (1) 13 A1 (s) + 12 BN (s) 一 A1 B12 (s) + 12 AIN (s) 又，腐蝕多數發生於凹槽部份之局部’即熔融鋁浸濕 僅在凹槽中心部擴展，被蒸鍍物之膜厚分佈不充分，成爲 板材之壽命。爲延長板材之壽命’將板材之相對密度提至 9 5 %以上（專利文獻2 )，其所需之壓力必要爲1 0 0〜3 0 0 -5- (2) (2)200526795 MPa之高壓’設備費高’又生產性亦差。一方面，爲使板 材中B N之結晶配向不產生異方性’提案由熱壓燒結體切 取之方法（專利文獻3)。但是，不管此等如何改良，於 銘蒸鍍中之高溫下’上述反應緩緩進行，長壽命化尙有改 善的空間。 專利文獻1 :日本特公昭53-2 〇2 5 6號公報 專利文獻2 :日本特開昭6 0 - 2 1 8 6 6號公報 專利文獻3:日本特公平5-66906號公報 φ 【發明內容】 [發明之揭示] 有鑑於向來技術有關之上述問題點，本發明者更深入 硏究結果，使用含特定低結晶性ΒΝ粉末之混合粉末，使 其結晶化燒結時所得陶瓷燒結體的粒界相存在氮化鈦，發 現其與向來腐蝕進行迅速的非晶質且氧量多的粒界相不 同，完成本發明。一般，陶瓷材料幾乎由數/zm〜數十 Φ // m之粒子所燒結者，具有稱爲多結晶之型態，粒界相多 數於粒子與粒子之間有原料粉末濃縮之雜質。即，本發明 爲，含氮化硼、二硼化鈦、鈣化合物及氮化鈦所成之相對 密度爲92 %以上之陶瓷燒結體，鈣化合物之含有率以CaO 換算爲0.05〜0.8質量。/〇，由來自氮化鈦（2 00)面之X 線繞射之高峯強度，相對於BN之（002)面之高峯強度 爲0.06〜0.15爲其特徵之陶瓷燒結體。於此情況，氮化 鈦之一部份或全部以存在於粒界相爲理想。又’更以含氮 -6 - (3) (3)200526795 化鋁爲理想。又，同時滿足’陶瓷燒結體中所含氮化硼結 晶之C軸晶格係數爲6.6 7 5 A，陶瓷燒結體之氧量爲1〜2 質量％者更爲理想。 又’本發明係有關由上述陶瓷燒結體所構成爲特徵之 金屬蒸鍍用發熱體。 又’本發明爲將含二硼化鈦粉末與氮化硼粉末與鈣系 燒結助劑，依需要含有氮化鋁粉末所成之混合原料粉末， 於非氧化性氣體環境中以1 8 0 0〜2 1 0 0 °C燒結的方法，上 φ 述氮化硼粉末爲氮化硼結晶之C軸晶格係數爲6.6 90A以 下，累積平均徑爲4〜20//m、BET比表面積爲25〜70 m2 / g、氧量爲1 .0〜2 · 5質量％之氮化硼粉末，上述混合 粉末中之鈣系燒結助劑之含有率換算CaO爲0.09〜0.8質 量°/。爲特徵之陶瓷燒結體之製造方法。此時，鈣系燒結助 劑爲至少1種由CaO、Ca (OH)2及CaC03所選者爲理 想。 依本發明，可提供改善熔融金屬耐蝕性之陶瓷燒結 β 體，可適用於其之陶瓷燒結體之製造方法，及可達成長壽 命化之金屬蒸鍍用發熱體。 [用以實施發明之最佳型態] 構成本發明之陶瓷燒結體之主成分爲，氮化硼與二硼 化鈦。依此，陶瓷燒結體可爲絕緣性且導電性，例如可適 用作爲金屬蒸鍍用發熱體等之用途。此時，氮化硼作爲絕 緣材料之功能，可由同樣爲絕緣材料之氮化鋁取代最大 (4) (4)200526795 5 0質量％，由此可改善通電特性，又，可低成本化。顯示 主成分之構成比例之一例時，如氮化硼40〜5 5質量％、 二硼化鈦45〜60質量％、氮化鋁〇〜20質量％。該主成 分，於陶瓷燒結體中以含有95質量％以上爲理想。 一方面，構成本發明陶瓷燒結體之上述主成分以外的 成分爲，鈣化合物與氮化鈦。鈣化合物係爲使陶瓷燒結體 之相對密度成爲9 2 %以上之必要成分，其含有率換算成 CaO爲0.05〜0.8質量％。低於0.05質量°/。時，相對密度 成爲92 %以上有困難，多於0.8質量％時，相對密度可成 爲9 2%以上，在陶瓷燒結中，機架夾具有產生燒結附著之 慮。相對密度爲92%以上之要件爲陶瓷燒結體之耐蝕性必 要成爲充分者。 氮化鈦，爲賦予陶瓷燒結體耐蝕性的成分，依耐蝕性 之改善觀點至少以一部份存在於粒界相爲理想。於粒界相 存在TiN，其斷面部可由ΕΡΜΑ (X線微分析計）之元素 分佈狀態與倂用粉末繞射法確認。氮化鈦之含有率爲由來 自氮化鈦 （200)面之X線繞射之高峯強度，相對於ΒΝ 之 （002)面之高峯強度爲0.06〜0.15的比例。即，X線 高峯強度比 （TiN (200)面 / (ΒΝ (002)面）爲〇·〇6〜 0.15的比率。該比低於0.06時，耐蝕性的改善效果不充 分，大於0.1 5時陶瓷燒結體之硬度過硬加工性惡化。 由粒界相至少存在TiN，可改善陶瓷燒結體耐蝕性之 理由，可說明爲TiN對熔融金屬之親和性比其他粒界相之 構成成分（B2〇3、Ti〇2、ai2o3)更小。SP，例如以熔融 (5) 200526795 金屬爲A1時加以說明，生成A1X (X =粒界構成 之自由能G以熱力學浸濕擴散溫度1 000 t求取時， 於 A1 - B2〇3 爲 56.1 kJ / mol、A1 - Ti02 爲 83.7 mol，Al - TiN 爲 12.2 kJ / mol，TiN 與 A1 之親和力 高耐蝕性。 有關本發明之陶瓷燒結體，由同時滿足氧量爲1 質量°/。，及於燒結體所含氮化硼結晶之C軸晶格係 6.6 7 5 A，更可改善耐蝕性。即，C軸晶格係數大於6 . 時結晶性低，成爲結晶應變大的B N容易受熔融金屬 蝕。換言之，低結晶性之B N粒子含有大量固溶氧或 缺陷，如此粒子內之構成缺陷成爲熔融金屬腐蝕之起 C軸晶格係數下限無限制，可爲理論値之6.6 62A，結 越高抗腐蝕強爲理想。 又’說明陶瓷燒結體之氧量以1〜2質量％爲理 理由’本發明之陶瓷燒結體，氧量主要爲存於粒界， 存在於BN(AIN)與TiB2粒子之間隙，一般其融 BN、A1N及TiB2低。氧量超過2質量。/。時，低融點 界相’於板材等陶瓷結體之使用溫度形成液相，與熔 屬容易引起反應，有損耐蝕性。又，氧量低於1質 時’ BN (A1N)與TiB2之粒子間結合力不充分，有損 性。 本發明之陶瓷燒結體之製造方法，係適合於製造 明之陶瓷燒結體者。以下說明其相關者。 於本發明所使用混合原料粉末，含二硼化鈦粉末 成分） 相對 k J / 小提 〜2 數爲 67 5 A 之腐 層合 因。 晶性 想之 知其 點比 之粒 融金 量％ 耐蝕 本發 (以 -9- (6) 200526795 下以「TiB2粉末」稱之）與氮化硼粉末（以下以「BN粉 末」稱之）與鈣系燒結助劑，依需要含有氮化鋁（以下以 「A1N粉末」稱之）所成。燒結前後成分之構成比例幾乎 無變化，各粉末之混合比例，可如上述陶瓷燒結體之構成 比例相同。如此之混合原料粉末，亦爲向來所使用者 > 本 發明重要的事項係使用特定低結晶性BN粉末，於特定量 鈣系燒結助劑之存在下，將低結晶性B N粉末一邊結晶化 一邊燒結。 0 於本發明所使用之BN粉末，C軸晶格係數爲6.690 A 以下，累積平均徑爲4〜20#m、BET比表面積爲25〜70 m2 / g、氧量爲1.0〜2.5質量％者。又，本發明所引用之 「累積平均徑」爲個數換算累積率50%之粒子徑 （D5〇)。 市售之BN粉末’由低結晶性至高結晶性的廣範圍， 由於至今適合之使用者爲高結晶性B N粉末，耐蝕性之改 善效果有限度。所以，本發明由使用氧量爲1.0〜2.5質 量％且C軸晶格係數爲6.690A以下，低氧量且低結晶性 鲁 之B N粉末，耐蝕之水準可凌越向來使用高結晶性b n粉 末者，又將BN粉末之粒度限於累積平均徑4〜20 ^ m、 BET比表面積爲25〜70 m2 / g，助長該效果。 即，將上述特定低氧且低結晶性之B N粉末，於特定 量的鈣系燒結助劑下，以特定條件燒結時，所得之陶瓷燒 結體之粒界相爲以TiN爲主相者，即陶瓷燒結體之上述X 線禹峯強度比（TiN (200)面/ BN (002)面）爲〇·〇6〜 〇-. 1 5，撇淸耐蝕性之改善。TiN相生成之機構未確定，可 -10- (7) 200526795 考慮其爲燒結過程中存在於TiB2粒子之表面氧化層之 Ti〇2與BN粉末之表面之B2〇3反應形成液相，BN粒子溶 解該液相再析出的同時，Ti02接受氮化生成TiN。 於本發明，C軸晶格係數超過6.6 9 0A時，所得之陶 瓷燒結體殘留低結晶性BN耐蝕性不能提高。累積平均徑 低於4 μ m，控制氧量爲2.5質量％以下有困難。累積平均 徑超過20#m時，或BET比表面積低於25 m2 / g，不能 製造相對密度爲92%以上之陶瓷燒結體。BET比表面積超 φ 過 7 0 m2 / g時燒結前之成形體密度變小，此亦不能製造 相對密度爲 92%以上之陶瓷燒結體。BN粉末之氧量低於 1.0質量％時燒結必要之氧量不足，又超過2.5質量％時， 於粒界相之氧量過剩而析出成爲耐蝕性不充分。 於本發明所使用之BN粉末，例如可由硼砂與尿素之 混合物於氨環境中加熱至8 00 °C以上的方法，將硼酸或氧 化硼與磷酸鈣之混合物，與氨、二氰二醯胺等含氮化物加 熱至1300 °C之方法等製造。任一者之BN粉末，氧量1.0 # 〜2 · 5質量％之控制，係於氮、氬等之非氧化性氣體環境 下’以1 100〜1 3 0 0 °C進行加熱處理3〜5小時完成。加熱 處理溫度超過1 3 00 °C時，BN粉末之C軸晶格係數小於 6.690A以下，成爲高結晶性BN粉末。又，加熱處理後以 〇 · 1〜1 %之硝酸等稀酸洗淨爲理想。 鈣系燒結助劑於混合原料粉末中之含有率，換算爲 CaO低於〇.〇9質量％時，將低結晶性BN粉末邊結晶邊燒 結有困難，又超過〇 · 8質量。/。時，於粒界相之殘留量增 -11 - (8) (8)200526795 加’耐蝕性不充分。作爲鈣系燒結助劑，各種鈣的氧化物 以外’例如可使用CaCN2、硝酸鈣等之氮化物，或例如 α ·α3(Ρ〇4)2、Ca4(P〇4)2〇等，由加熱變化爲鈣之氧化 物，理想爲CaO、Ca (〇H)2、CaC03。鈣系燒結助劑之平 均粒子徑爲〇 . 8 # m以下，特別以〇 . 5 μ m以下者爲理想。
TiB2粉末、A1N粉末，使用係將Ti粉末、A1粉末直 接氮化反應或直接硼化反應所製造者；將Ti02粉末或 Ah〇3粉末還元氮化反應或還元硼化反應所製造者，平均 粒子徑以5〜2 5 // m者爲理想。此等以市售者即已充分。 混合原料粉末理想爲製粒後，於非氧化性氣體環境 1 8 0 0〜2 1 0 0 °C燒結。例如，單軸加壓或冷各方等壓加壓 後’於1 8 0 0〜2 1 0 0 °C燒結，或於〇 . 8 MP a以下之氣體環 境下以常壓燒結。又，可於1800〜21001：、1〜100 MPa 之熱壓或熱各方等壓熱壓燒結。燒結溫度低於1800。(：燒 結不充分又超過2100 °C時不能製造相對密度92 %以上之 陶瓷燒結體。非氧化性氣體環境可使用氮、氬、二氧化 碳、氨等之環境。 又，燒結以收容於石墨製容器、氮化硼製容器、內襯 氮化硼之容器，於非氧化性氣體環境中進行爲理想。熱壓 法係使用石墨或氮化硼製襯套、內襯氮化之襯套燒結。 由本發明之陶瓷燒結體，製造本發明之金屬蒸鍍用發 熱體，例如板材，依常法加工適宜之形狀。其尺寸之一 例’如縱30〜150mmx福25〜35mmx高8〜12ηιιη 之長片狀，板材於其上面中央形成凹槽（縱90 mm〜120 -12- 200526795 Ο) mm x 幅20〜32 mm χ 深0.5〜2.0 )。加工由機械加 工、雷射加工等進行。 【實施方式】 實施例1〜1 0、比較例1〜1 1 .
TiB2粉末（平均粒子徑12 // m、純度99.9質量°/〇以 上），A1N粉末（平均粒子徑10 // m、純度98.5質量％以 上），CaO粉末（平均粒子徑0.5 // m、純度99.9質量％以 φ 上），及如表1所示之各種Β Ν粉末依表1所示之比例混 合調整各種混合料粉末。此處，各種ΒΝ粉末係將硼砂與 尿素之混合物於氨環境中加熱所得之ΒΝ粉末，於氮環境 下’變更1 1 0 0〜1 3 0 0 °C、3〜5小時的各種熱處理條件進 行熱處理而製造。將其塡充於石墨模中，於氮環境中如表 2所示之條件進行熱壓製造陶瓷燒結體（直徑200 mm χ 高20 mm之圓柱形）。 由該燒結體，切取直方角柱體（長1 50 mm χ幅30 φ mm χ 厚10 mm )，其表面之中央部以機械加工形成凹槽 製造板材。板材之 （1)耐蝕性與 （2)壽命依以下測 疋° (1)耐蝕性：板材頂端以挾具連接電極設定附加電壓 使凹槽中央部份之溫度成爲1 5 00 °C。於真空度2M(T2Pa 之真空中，將直徑1.5 mm之鋁線以6.5 g /分鐘之速度 於40分鐘供給凹槽一邊進行蒸鍍後冷卻至室溫爲1循 環’重複進行。每次，將樣本取出凹槽部最浸蝕之深度使 -13- (10) (10)200526795 用雷射變位計（機器：日本KEYENCE公司製「乙丁-9 0 0 0」）測定’求出板材於4 0分鐘被浸蝕之速度。浸蝕 之速度越小即爲耐蝕性良好的陶瓷燒結體。 (2) 壽命：以上述耐蝕性試驗之條件爲基準，板材上 方2 0 0 mm之位置重複進行於樹脂薄膜上之蒸鍍，求1循 環鋁蒸鍍膜厚度成爲低於2 0 0 0人時之循環數。 又’陶瓷燒結體之相對密度、B N之C軸晶格係數、 氧量、鈣化合物量、粒界相、及上述X線高峯強度比（TiN φ (200)面 / BN (002)面）依以下測定。其結果如表2所 示。 (3) 相對密度：由實測密度與理論密度算出。實測密 度’一般依所得測定値正確度與再現性觀點依阿基米德法 測定。理論密度依原料之毛比重與配合比所求出之値。 (4) C軸晶格係數：由粉末X線繞射法（機器：日本 理學公司製「RAD - B」），於40kV、1 00 mA之條件將試 料於2 0 1(Γ〜7 0。的範圍測定，依Lead Belt法計算BN結 φ 晶之C軸晶格係數而求得。將燒結體粉碎之方法一般的方 法係於瑪瑙硏鉢粉碎數次，將其小片於硏鉢硏磨微細化。 又，將其微粉以200 mesh過篩可準備成爲適於粉末X線 繞射法之試料。 (5) 氧量：依氧氮分析裝置（昇溫分析法）（機器： LECO公司製「TC-436」）測定。 (6) 鈣化合物量：使用衍生結合電漿發光分析裝置 (日本 SCHADEL ASSH 製「ICP - AES，MODEL ICAP — -14- (11) (11)200526795 1 ο ο o s」）測定。 (7) 粒界相：有關粒界相存在之 TiN，將板材加工 成直徑5 mm之斷面形狀。將其斷面硏磨部由ΕΡΜΑ (X線 微分析計）測定元素分佈狀態。更由粉末X線繞射法鑑 定粒界相。. (8) X線高峯強度比（TiN (200)面 /ΒΝ (002)面）： 由上述粉末X線繞射結果求出。
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<N Ο '〇 IK镗匡 _ 17 . (14) (14)200526795 口表 〜所不’本發明之陶瓷燒結體由於浸蝕速度抑制 於6 // m / min以下，大幅改善耐蝕性’又使用其製造之 板材知其爲具1 5循環以上之長壽命。 已參照特定之實施型態詳細說明本發明，本業者了解 在不逸出本發明之精神與範圍可加以種種變更或修正。 本申請係依據2 0 0 3年12月1 1日申請之日本特許出 願（日本特願2003 - 4 1 3 5 3 )者，其內容納入此處作爲參 [產業上之利用領域] 本發明之陶瓷燒結體，例如作爲板材等之金屬蒸鍍用 發熱體，又本發明之金屬蒸鍍用發熱體，可作爲將鋁、 銅、銀、鋅等之金屬蒸鍍於薄膜、陶瓷等基材時之機架挾 具使用。
-18-

Claims (1)

  1. 200526795 (1) 申請專利範圍 欽、 結體 由來 BN ^ 鈦之 其中 燒結 數爲 硼、 硼、 者。 範圍 化鈦 鋁粉 1800 1 . 一種陶瓷燒結體，其特徵爲含有氮化硼、二硼化 鈣化合物及氮化鈦所成相對密度爲92%以上之陶瓷燒 ，鈣化合物的含有率換算CaO爲0.05〜0.8質量％， 自氮化鈦 （200)面之X線繞射之高峯強度.，相對於 1 (〇〇2)面之高峯強度爲0.06〜0.15者。 2 ·如申請專利範圍第1項之陶瓷燒結體，其中氮化 一部份或全部存在於粒界相者。 3 ·如申請專利範圍第1項或第2項之陶瓷燒結體， 更含有氮化鋁所成者。 4.如申請專利範圍第1項、第2項或第3項之陶瓷 體’其中含於陶瓷燒結體之氮化硼結晶之C軸晶格係 6 ·6 7 5 Α以下’陶瓷燒結體之氧量爲1〜2質量％者。 5 ·如申請專利範圍第1項之陶瓷燒結體，其中氮化 ~硼化欽之合計含有率爲95質量％以上者。 6 ·如申請專利範圍第3項之陶瓷燒結體，其中氮化 二硼化鈦及氮化鋁之合計含有率爲9 5質量％以上 7 · 一種金屬蒸鍍用發熱體，其特徵係由如申請專利 第1項至第6項中任一項之陶瓷燒結體所構成。 8 · 一種陶瓷燒結體之製造方法，其特徵爲將含二硼 粉末與氮化硼粉末與鈣系燒結助劑，依需要含有氮化 $所成之混合原料粉末，於非氧化性氣體環境中以 〜2 1 〇〇 °C燒結的方法，上述氮化硼粉末爲氮化硼結 -19- (2) (2)200526795 晶之C軸晶格係數爲6.6 9 0A以下，累積平均徑爲4〜20 #m、BET比表面積爲25〜70 m2 / g、氧量爲1.0 ~ 2.5 質量％之氮化硼粉末，上述混合原料粉末中之鈣系燒結助 劑之含有率換算CaO爲0.09〜0.8質量％者。 9.如申請專利範圍第 8項之陶瓷燒結體之製造方 法，其中鈣系燒結助劑爲至少1種由CaO、Ca (OH)2及 CaC〇3所選者。
    -20- 200526795 七、（ )、本案指定之代表圖為：無 )、本代表圖之元件代表符號簡單說明：無 八、本案若有化學式時，請揭示最能顯示發明特徵的化學式：
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