TWI237011B - Process for preparing aluminum-titanate-based sintered body - Google Patents

Process for preparing aluminum-titanate-based sintered body Download PDF

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TWI237011B
TWI237011B TW090127649A TW90127649A TWI237011B TW I237011 B TWI237011 B TW I237011B TW 090127649 A TW090127649 A TW 090127649A TW 90127649 A TW90127649 A TW 90127649A TW I237011 B TWI237011 B TW I237011B
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sintered body
titanate
weight
aluminum titanate
based sintered
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TW090127649A
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Tsutomu Fukuda
Masahiro Fukuda
Masaaki Fukuda
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Ohcera Co Ltd
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Description

1237011 A7 五、發明説明（1 ) 技術領域 本發明係關於鈦酸銘系燒結體之製造方法。 技術背景 鈇酉夂铭K體為熱膨脹係數小，且㈣性優良之燒結 〜抑U田做18、1呂合金、生鐵等之炼融金屬溶漿用的 容器、鑄桶、導流管等的材料使用時，就耐熔融金屬濕潤 f生耐餘性、耐剝洛性等而言，已知為發揮優良特性的财 …材料欽酸銘燒結體因構成燒結體的結晶粒為各 向異性，容易隨著熱膨脹而在結晶粒子界面產生受應力所 導致之細微裂紋，故有隨著微細裂紋或空隙的發展，機械 強度易於降低的缺點。 因此，習知之鈦酸鋁燒結體強度不足，尤其，在高溫 下使用於承受負荷的用途時，無法發揮足夠的耐用性。 另，鈦酸鋁在USOt；以下不安定，若在800〜128〇t左 右的高溫下使用，Ti〇AAl2〇3容易分解，難以在該溫度區 域下持續使用。 為使鈦酸鋁之燒結性提高並抑制熱分解，雖可將二氧 化矽等之添加劑加入原料再進行煅燒，惟該情形中，所獲 得之燒結體的耐火度容易降低，無法獲得同時具有可以在 14 0 0 C左右以上的高溫使用之耐火度與機械強度的鈦酸鋁 燒結體。 發明說明 本發明之主要四的在於提供一種鈦酸鋁系燒結體，既 可維持熱膨脹係數小且耐蝕性良好之所謂鈦酸鋁燒結體的 (請先閱讀背面之注意事項再填寫本頁) 訂— ♦
1237011 五、發明説明（2 ) 本來特性，又可使機械強度提高，而且即使在高溫下也可 以安定地使用。 本發明人有μ於如上所述的課題而重覆地銳意研究之 結果’發現在緞燒由二氧化鈦與氧化銘所組成的原料粉末 以製得鈦酸銘燒結體時，利用使特定的驗性長石存在原料 粉末中的做法，Si原子會固溶於鈦酸銘結晶中，結晶粒的 成長受到抑制而形成緻密的燒結體，所獲得之燒結體兼具 高機械強度與低膨脹係數’並且成為耐分解性、耐火度等 俱優的產品，進而完成本發明。 亦即，本發明提供下述之鈦酸鋁系燒結體的製造方法。 1·鈦酸鋁系燒結體之製造方法，特徵為，將相對於含 有Ti〇2與Al2〇3，前者··後者（重量比）=40 · 6〇〜6〇 · 4〇之 比例的混合物100重量分，調配有重量分之化學式： (NaxUAlShCMO $ x $丨）所表示的鹼性長石而組成之原 料混合物所形成的成形體，在125〇〜17〇〇它予以煅燒。 2.如第1項記載之鈦酸鋁系燒結體的製造方法，特徵 為’在還原性環境中實施成形體的烺燒。 3·如第1項或第2項記載之鈦酸鋁系燒結體的製造方 法，特徵為，化學式：（NaxKbX)AlSi308 *，使用〇1^χ$ 1的範圍之鹼性長石。 4.以上述第1〜3項之任一項的方法製得之鈦酸鋁系繞 結體。 本發明之鈦酸鋁系燒結體的製造方法係使用將化學 式：（NaxUAlSigCMO g X$丨）所表示的鹼性長石添加到含 (請先閲讀背面之注意事項再填寫本頁) 訂丨 Φ,
1237011 A7 B7 五、發明説明（3 ) 有Ti〇2與Al2〇3的混合物而組成的混合物做為原料，再將所 形成之成形體在12 5 0〜17 0 〇。〇予以煅:燒的方法。 (請先閱讀背面之注意事項再填寫本頁) 做為原料使用之Τι〇2及八丨2〇3，只要是可以藉煅燒而合 成鈦酸紹的成分，即無特殊限制；通常，可以從當做氧化 鋁陶瓷（alumina ceramic)、二氧化鈦陶瓷（也⑽“ a% mics)、鈦酸鋁陶瓷等各種陶瓷的原料使用的成分中，適當 地遥用。尤其，Ti02選用銳鈦型（anatase) 丁丨〇2，選用 易燒結氧化鋁α型時，兩成分的反應性良好，可以在短時 間内即以高收率形成鈦酸鋁。
Ti〇2與Αΐ2〇3的混合比例可為Ti〇2 : Al2〇3(重量比）= 40 : 60〜60 : 40左右的範圍為，而以Ti〇2 : Al2〇3(重量比） =40 : 60〜45 : 55左右的範圍為佳。 做為添加劑使用的驗性長石係以化學式： (NaxKNx)AlSi308(〇$xS 1)表示，式中 。特別在 上述化學式中，以O.lSxg；!的範圍為佳，而以〇 15^χ^ 〇·85的範圍更佳。具有此種範圍的χ值之鹼性長石，融點比 鈦酸鋁的生成溫度低，對於鈦酸鋁的烺燒促進特別有效。 鹼性長石的使用量相對於Ti〇2與Al2〇3的合計量量1〇〇 重里分’可定為1〜15重量分左右，而以4〜1〇重量分左右 為佳。 若依據本發明之方法，利用將上述之特定的鹼性長石 當做添加劑調配於含有Ti0^A12〇3的混合物中，再將該混 a物成形為預定的形狀並加以煅燒的方式，鈦酸鋁的粒子 成長即會受到抑制而可以製得緻密的燒結體。其理由被認
1237011 五、發明説明 為係因，藉锻燒形成鈦酸銘時，鹼性長石令的Si固溶⑽ 晶格子内並與A1置換，因Sitt起竭子半徑小，故鱼周圍口 的氧：子之結合距離縮短’其結果，結晶乃被緻密化。 3有Τι〇2、Al2〇3及驗性長石的原料^合物經過充分混 合並粉碎成適當的粒徑之後，再成形為狀的形狀即可f 關於原料混合物之混合.粉碎方法並無特殊限制，依 ，吊法即可’例如，可以採用球磨機、媒介«拌研磨機 #以實施混合·粉碎。 關於原料此合物的粉碎程度雖無特殊限制，惟以粉碎 至1 V m左右以下為佳。 原料混合物中可依需要而進—步調配以成形_1 形助劑依成形方法，使用過去以來即已被使用之公 分即可。 风 ，此種成形助劑可使用例如，聚乙婦醇、微細職乳液、 竣酸纖維素等之黏結劑，硬脂酸乳液等之離型劑，η _辛醇、 «苯氧基乙醇等之消泡劑，二乙胺、三乙胺等之解膠劑 等。 關於此等成形助劑之使用量亦無特殊限制，只需依照 成形方法，從與f知相同的調配量範"做適當選擇即 可。例如，_成形用之成形助劑，相對於叫及八叫 的合計量1〇0重量分，可以使用黏結劑0.4〜〇·6重量分左 右’解膠劑0.5 4.5重量分左右，離型劑(固形分量)〇·2〜 0·7重量分左右，消泡劑0_03〜0·1重量分左右。 關於原料混合物之成形方法亦未特別限定，只要適當 1237011 五、發明説明 地採用例如，噴霧成形、壓板成形、_成形 射出成形、⑽成形等公知的成形方法即可。 關於锻燒溫度，只要在1250叫·。c左右即可，以剛 〜1700 C左右為佳。關於锻燒環境並未特別限定，一般所 採=之空氣中等含氧環境、還原性環境、惰性環境之任一 2了尤其，在氫雾圍氣、一氧化碳雾圍氣、天然氣雾 圍氟、、咖雾圍氣等之還原性環境中進行炮燒時，具有容 易形成緻密且高強度之燒結體的優點。 ㈣炮燒時間未特別限定，依照成形體㈣狀等，只 1二進行至充分地炮燒為止即可’通常’在上述溫度範 、’、#〜10小時左右即可。關於般燒時的昇溫速度及降溫 ^度亦無特殊限制，只要設定成燒結體不會出現裂紋的條 件即可。 體 .細 % 要 康本毛明所獲得之燒結體為Si固溶於鈦酸銘的結晶 並” A1置換之鈦酸銘系燒結體，和純粹的欽酸銘相 比’晶袼常數具有較小的數值。其結果，所獲得的燒結 成為結晶構造安定化，結晶粒成長受到抑制，且具有微细 的結晶粒之燒結體。此種結晶粒的成長受到抑制之燒結 體’因為將受熱膨脹而導致之歪斜予以緩和，故沒有必 產生裂紋，成為緻密且具有高機械強度的產品。 、_本發明方法而獲得之燒結體為具有此種優良特徵 2產阳，因兼具高機械強度與低熱膨脹率，而且結晶構造 f到安定化，故為具有優良的耐分解性與高耐火度的產 品。其結果，即使在數百度到1600t左右的高溫下，鈦酸 、’，尺度適用中國國家標準⑽）織格（2獻撕公着） 1237011 A7 p----- B7 _ 五、發明説明（6 ) 鋁的分解反應依然受到抑制而可以安定地使用，且，成為 具有遠超過鈦酸鋁之融點，即186(rC2SK4〇(192(rc)。以 上之耐火度的產品。另，依據本發明方法所獲得之燒結體， 對熔融金屬表現出極為優異之不沾濕性及耐蝕性，其結 果，對於流動的熔融金屬，可以發揮在截至目前為止的材 料中所完全無法思及的程度之優良的耐侵蝕性。 本發明之鈦酸鋁燒結體可以利用上述的優良特性而應 用於例如，金屬用坩堝、鑄桶（ladle)、導流管等之高融點 金屬用容器，航空機用喷射引擎的高溫部用零件，喷射噴 鳴，各種内燃機關之熱線點火塞（gl〇w plug)、汽缸活塞頭 (piston head)等之高溫部用零件，太空船等之外壁用隔熱及 遮蔽板等的各種用途；此外，利用其低膨脹性，也可以有 效地應用做為LSI製造程序中之印刷加工上的定盤等。 如上所述，依據本發明之製造方法所獲得之鈦酸鋁系 燒結體，除維持鈦酸鋁原來的低膨脹率以外，具有高機械 強度，耐熱衝擊性亦佳。且，該鈦酸鋁系燒結體2JISR22〇4 中規定之耐火度，顯示為SK40(192(rc)以上之非常高的耐 火度，耐分解性亦佳，也可以在高溫下安定地使用。 實施例 以下例舉實施例，更詳細地說明本發明。 實施例1 相對於以銳鈦型氧化鈦43.9重量％與易燒結氧化鋁^ 型56.1重1 %組成之混合物1〇〇重量分，添加福島產鹼性長 石（(NaowKuOAlShO8) 4重量分做為添加劑，二乙醇胺 本紙張尺度適用中國國家標準（CNS) A4規格（210X297公釐）~--- 1237011 A7 _______ _B7 五 " 一一 anol amine) 1.5重量分做為解膠劑，聚乙稀醇ο 4重 量分做為黏結劑，及水30重量分，製得原料混合物。將該 原料混合物置入球磨機㈣3小時後，將取_ J蚪其後再錄鑄成掛禍型，2小時後取出，得到直徑6 cm、高度8 em之圓筒狀成形體。 使α亥成形體自然乾燥24小時後，在乾燥機中，以6〇。。 以下的溫度乾燥至含水率成為1%以下。 將该成形體自乾燥機取出後，以13小時的時間昇溫至 1600 C為止，在160(rc煅燒2小時以後，將之放冷。煅燒係 在大氣裝境中進行。 關於所獲得之燒結體，從χ射線繞射圖形算出來的晶 格常數示於下列表1。 表1
_、τ. (請先閲讀背面之注意事項再填寫本頁)
本紙張尺度適用中國國家標準（CNS) Α4規格（210X297公釐) 晶格常數(Α) 真密度 3.713 a b c 實施例1之燒結體 9.423 9.626 3.586 鈦酸症呂 9.429 9.636 3.590 ------ 3.704 溫度 °c 熱膨脹係數(％)(昇溫） 實施例1之燒結體 鈦酸ί呂 30 0 0 80 -0.007 -0.005 130 -0.016 -0.011 180 -0.023 -0.019 230 -0.03 -0.027 280 -0.036 -0.034 330 -0.04 -0.04 380 -0.043 -0.044 430 -0.045 -0.048 480 -0.045 -0.049 530 -0.044 -0.048 580 -0.041 -0.046 630 -0.037 -0.042 680 -0.03 -0.037 730 -0.02 -0.032 780 -0.006 -0.028 830 0.008 -0.026 880 0.022 -0.023 930 0.039 -0.017 980 0.056 -0.012 1000 0.063 -0.011 1237011 A7 B7 五、發明説明（8 ) 表2 本紙張尺度適用中國國家標準（CNS) A4規格（210X297公釐） 11 (請先閲讀背面之注意事項再填寫本頁)
1237011 A7 B7 五、發明説明（9 ) 表3 溫度 °c 熱膨脹係數(％)(降溫） 實施例1之燒結體 欽酸ί呂 1000 0.019 -0.072 980 0.004 -0.085 930 -0.029 -0.112 880 -0.063 -0.131 830 -0.099 -0.146 780 -0.137 -0.159 730 -0.174 -0.173 680 -0.21 -0.187 630 -0.241 -0.192 580 -0.246 -0.184 530 -0.233 -0.17 480 -0.216 -0.155 430 -0.196 -0.138 380 -0.177 -0.121 330 -0.155 -0.101 280 -0.132 -0.081 230 -0.108 -0.06 180 -0,082 -0.037 130 -0.056 -0.011 80 -0.027 0.018 50 -0.003 0.038 (請先閲讀背面之注意事項再填寫本頁) 訂丨 本紙張尺度適用中國國家標準（CNS) A4規格（210X297公釐） 12 1237011 五、發明説明（l〇 由以上結果可知，以上述方法製得之燒結體，判定係 熱膨脹係數小’且維持鈦酸輯來的低膨脹性之產品。 另，有關在實施例1所獲得之燒結體，當實施將1250 t之加熱狀態下的燒結體置人代的冰水中之急冷試驗，和 將-251之燒結體以煤氣喷燈（gas burner)急速加熱至丨5〇〇 C為止之急速加熱試驗，以當做耐熱衝擊性試驗時，燒結 體上未產生裂紋，顯示出優良的耐熱衝擊性。 實施例2 將和在實施例1中所使用的成分相同之原料混合物，以 球磨機攪拌3小時而獲得之漿狀物，在uot乾燥4小時後， 以60 Mpa的成形壓成形為120 mm X 35 mm x 25 mm (厚 度）’或120 mm χ 35 mm χ 20 mm (厚度）（測定熱間線性膨 脹率用）的形狀。 關於所製得之成形體，以下列的煅燒模式1或煅燒模式 2緞燒後，放冷而得到鈦酸鋁系燒結體。 般燒模式1 (1540°c煅燒） 0 〜180°C 4小時 180〜250°C .3小時 250〜450〇C 3小時 450〇C 保持3小時 450 〜1540〇C 6小時 1540〇C 保持2小時 2·煅燒模式2 (1600°C烺燒） 0〜180°C 4小時 本紙張尺度適用中國國家標準（CNS) A4規格（210X297公釐） 13 (請先閲讀背面之注意事項再填寫本頁)
1237011 A7 B7
五、發明説明（11 ) 180〜250°C 250 〜450°C 450〇C 450 〜1600°C 1600°C 3小時 3小時 保持3小時 6小時 保持2小時 關於所製得之燒結體，物性數值的測定結果示於下列 表4。 表4 煅燒溫度（°c) 1540 1600 煅燒收縮率（％) -9.63 -9.55 外表氣孔率(％) 7.3 5.5 吸水率（％) 2.2 1.7 外觀比重 3.56 3.49 容積比重 3.30 3.30 耐火度（SK) 40以上 40以上 彎曲強度(MPa) 室溫 50 40 熱間線性熱膨脹率(％) 500°C -0.09 ±0 750〇C -0.08 ^0.02 1000°C +0.04 +0.10 由以上的結果判斷，以上述方法製得之燒結體熱膨脹 率小’且具有南耐火度’而且強度南。 本紙張尺度適用中國國家標準（CNS) A4規格（210X297公釐） 14 (請先閲讀背面之注意事項再填窝本頁) 1237011 A7 B7 五、發明説明（12 ) 另，關於以實施例2製得之燒結體，當與實施例1同樣 地處理並實施耐熱衝擊性試驗時，不產生裂紋，且顯示出 優良的耐熱衝擊性。 15 (請先閲讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS) A4規格（210X297公釐）

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  1. mron 1公告本.j A8 ^ t g ..:88 -r *08 I ^
    六、申請專利範圍 第90127649號專利申請案申請專利範圍修正本 修正曰期：94年3月18曰 1· 一種鈦酸鋁系燒結體之製造方法，其特徵為，將相對於 含有τι〇2與Ai2〇3，前者：後者（重量比）=4〇 : 60〜6〇 ·· 40的比例之混合物1〇〇重量分，調配有卜15重量分之化 學式·（NaxUAlShOdO.iSx^i)所表示的驗性長石 而組成之原料混合物所形成的成形體，在125〇〜17〇〇 °C予以緞燒。 . 2·如申請專利範圍第1項之鈦酸鋁系燒結體之製造方法， 其特徵為，在還原性環境中進行成形體的煅燒。 3· —種鈦酸鋁燒結體，係以申請專利範圍第項之任一 種方法製得。 16 本紙张尺度適用中國國家標準（CNS〉A4规格（21〇X297公釐）
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KR20020092935A (ko) 2002-12-12
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EP2014627A1 (en) 2009-01-14
DE60137531D1 (de) 2009-03-12
CA2396857A1 (en) 2002-05-16
US20030015829A1 (en) 2003-01-23
WO2002038519A1 (fr) 2002-05-16
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US7011788B2 (en) 2006-03-14
ATE421489T1 (de) 2009-02-15
USRE42582E1 (en) 2011-08-02

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