1226880 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公f ) A7 B7 五、發明說明（1 ) [技術領域] 本發明有關氧化鋁•模來石系多孔質片狀耐火物及其 製造方法，特別是有關優於耐熱衝擊性（resistance t0 thermal Shock)，且經大幅改善高溫，例如16〇〇t下的撓 曲抵抗性（resistance to flexture)，而適合於用為陶瓷 基板等之燒成或氧化鋁陶瓷之燒成的氧化鋁•模來石系多 孔質片狀耐火物及其製造方法。 [背景技術] 以往技術t，當燒成電子部件等之際，係使用氧化鋁 質或锆質之燒成用器具（firingt〇al)，例如氧化鋁磁器製 片，並在此氧化鋁磁器製片上載置被燒成物以實施燒成 者。然而，以往之氧化鋁磁器製片係在耐熱衝擊性或熱間 的撓曲抵抗性方面較為劣差，以致如於15〇(rc以上溫度使 用時，不能耐久。 又，氧化鋁•模來石質之壓製品，係作為氧化鋁基板 燒成用碼磚器（setter)使用者，惟難以製造厚度5_以下 之單薄的碼磚器，以致難於製得均勻的組織，且又不耐久。 再者，如欲將燒成用器具之表面粗糙度（surface | roughness)為按JIS B 060 1所定義的以所求出的3vm 以下時，則必需作成為非常細的粒子集中於其表面的構| 造，從而難於採用加壓成型的製造。 | 本發明以提供一種優於耐熱衝擊性，且經大幅改善高| 溫，例如160(TC下的撓曲抵抗性，而適合於用為陶瓷基板！ 等之燒成或氧化鋁陶瓷之燒成的氧化鋁•模來石系多孔質 311923 -裝---------訂---------- (請先閱讀背面之注意事項再填寫本頁) 1226880 A71226880 Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs The paper size is applicable to the Chinese National Standard (CNS) A4 (210 X 297 male f) A7 B7 V. Description of the invention (1) [Technical Field] The invention relates to alumina Lacite-based porous flaky refractory and its manufacturing method, in particular, it is better than resistance to thermal shock (resistance t0 thermal shock), and has been greatly improved in high temperature, for example, resistance to flexture at 160 ° t ), Which is suitable for firing alumina substrates such as ceramic substrates, or alumina ceramics, and a method for producing the same. [Background Art] In the conventional technology, when firing electronic components and the like, firing tools such as alumina or zircon are used, such as alumina magnets, and the alumina magnets are manufactured here. A fired object is placed on the sheet to perform firing. However, the conventional alumina magnet sheet is inferior in thermal shock resistance and resistance to thermal deflection, so that it cannot be durable when used at a temperature of 150 ° C or more. In addition, alumina and mullite High-quality pressed products are users of setters for firing alumina substrates, but it is difficult to manufacture thin code blocks with a thickness of 5_ or less, which makes it difficult to produce a uniform structure and is not durable. If the surface roughness of the firing device is 3 vm or less as defined in JIS B 060 1, it is necessary to make a structure in which very fine particles are concentrated on the surface. | This makes it difficult to manufacture by press molding. | The present invention is suitable for use as a ceramic substrate to provide a resistance to thermal shock resistance and greatly improved high temperature, such as 160 (TC flex resistance at TC) ！ Alumina and sintered alumina ceramics made by waiting for firing or alumina ceramics 311923 -pack --------- order ---------- (Please read the back first (Notes on this page, please fill out this page) 1226880 A7
五、發明說明（3 ) 之。 經 濟 部 智 慧 財 產 局 員 工 消 費 合 作 社 印 製 3 311923 [為實施發明之最佳形態] 兹將本發明之實施形態詳細說明如下，惟本發明不限 定於此。 本發明之氧化銘.模來石系多孔質片狀耐火物中，由 電融氧化銘及/或燒結氧化㈣電融模來石而成的粒徑ι〇 至之骨材成分佔有50至85質量％，由氧化紹及模 來石而成的結合材成分佔有15至5G f量％，又存在有不 可避免的不純物，而其氣孔率為1〇至4〇%。 本發明之氧化銘•模來石系多孔質片狀耐火物中，如 分析其組成時之化學成分而言，^〇3含量較佳$85至95 質量％，更佳為87至93質量Us%含量較佳為5至 15質量。/。，更佳為7至13質量％。 本發明之氧化銘·模來石系多孔質片狀耐火物中’如 分析其組成時之化學成分而言’如Al2〇3含有量較95質量 %為多的情形，亦即S102含有量較5質量%為少的情形，則 有耐熱衝擊性、熱剝落抵抗性（reslstance t0 themal spaing)會低落的傾向之故不佳。又，如ai办含有量較 85質量%為少的情形，亦即叫含有量較15質量%為多的 情形’則有作為目的之本發明之效果不足的傾向 佳。 ^本發明之氧化鋁·模來石系多孔質片狀耐火物中如 乳孔率較10%為小的情形，有熱剝落抵抗性會低落的傾向 _ ^^不^_反之’如氣40%為大的情形，則有在強 本紙張尺度剌巾_|鮮（CNS)A4規格_----,---- — — — — — III — — · Γ I I I I I I < I — I — III— (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 1226880 A7 ^ " —------------ 五、發明說明（4 ) ' 度方面可能會發生問題之故不佳。 本發明之製造方法中，為製作多孔質片，使用電融氧 化鋁及/或由燒結氧化鋁與電融模來石而成的粒徑1〇至 1 50//m之骨材。如此的骨材可依常法調製之。又，骨材中 之電融氧化鋁及/或燒結氧化鋁及電融模來石之組成比 〇率，係在使用骨材50至85質量％及結合材15至5〇質量 所製得的氧化鋁·模來石系多孔質片狀耐火物中，將其 組成分析為化學成分，並適當選定為能成為含有Ai2〇j85 ^ 95質量％，Si〇2 5至15質量％及不可避免的不純物的狀 恕。如此的選定，係同業者所容易做到的。 t ’本發明之製it方法中M吏用按燒成後能成為氧化 鋁及模來合的組成比所混合的由氧化鋁與氧化矽微粉及/ 或黏土而成的粒徑1〇//m以下之結合材。結合材中之氧化 鋁與氧化矽微粉及/或黏土的組成比率，係於使用骨材5〇 至85質！ ％及結合材15至50質量％所製得的氧化銘•模 來石系多孔質片狀耐火物中，將其組成分析成為化學成、 分，並適當選定為能成為含有Μ"3 85至95質量％、 5至1 5質量％及不可避免的不純物的狀態。如此的選定， 係同業者所容易做到的。 本發明之製造方法中，為確保多孔性且獲得充分的強 度對月材50至85質量％按能成為15至50質量％的量使 用結合材。混合預定量之骨材、和結合材、和對混練•成 型有效的量的甲基纖維素等之有機黏合劑和水，並將其混 合物例如使用3只輥子（r〇n)充分予以混練〇其後，例: 本紙張尺度適用中國國家標準（CNS)A4規格⑵〇 X 297公爱）一 4-- 裝---------訂--------- (請先閱讀背面之注意事項再填寫本頁) 1226880 A7 五、發明說明) 依擠出成型或滾子成型予以成型為厚度〇3至5_之片 將其成型片於1 600至1800°C燒成3至10小時程度以製得 多孔質片。 & 依上述的製造方法所得的本發明之氧化鋁•模來石系 多孔質片狀耐火物之表面粗糙度Ra為3//m以下，再於必 要時藉由兩面研磨，即可作成為表面更平滑的多孔質片狀 耐火物。又，耐熱衝擊性，熱剝落抵抗性優，於從1〇〇〇它 的急冷耐久性試驗中亦不會發生破損、龜裂，而於高溫， 例如160CTC下的撓曲抵抗性經已大幅改善。再者，氣孔率 雖為10至40%，但因具有充分的強度之故，亦能進行架 棚，厚度1.5mm而直徑300mm之大形品，亦堪於實用。 因而，可作為網狀皮帶（嶋hbe_所用的燒成用二板， 或多孔質片狀耐火物使用，而適用於陶瓷基板或氧化鋁陶 瓷之燒成。 茲將舉實施例及比較例以具體說明本發明如下，惟本 發明係不被此等例子所限定者。 實施例1 混合包含電融氧化鋁60質量％與電融模來石4〇質量 %而粒徑範圍為1〇至15G//m之骨材！⑽f量份和包含 锻燒氧化紹75質量％與氧化石夕微粉25質量％而粒徑範圍 為i—以下之結合材30質量部、和作為有機黏合劑的 曱基纖維素5質量份、和水10質量份’並將此等混合物以 3只親子充分混練。其後，藉由擠出成型，成型為1〇〇議 _^_〇〇mmXi.5mm之片。待此等成型片之乾燥後於丨700t： Μ氏張尺度適用中國國家標準（CNS)A4規格（2Ί〇 X 297公爱)--- (請先閱讀背面之注意事項再填寫本頁) 壯衣· *-------訂--------- 經濟部智慧財產局員工消費合作社印製 311923 1226880 B7 經濟部智慧財產局員工消費合作社印：¾ 五、發明說明（6 ) t成5小時，並製得多孔質片。所得多孔質片之鬆密度、 =。:按，件下所測定的威下的挽曲抵 ▲ 心冷耐久性，係如第1表所示。 1 及比鲂 、又為比較例1，U乍與實施例之片@ _狀之氧化 紹磁器製片，為比較， ^ ^ 2 I作與實施例之片同樣形狀之 乳化鋁99 /。之多孔質片。此等片之鬆密度氣孔率、“ο。 。。下的撓曲抵抗性、從1〇〇{Γς的急冷耐久性，係如第u 所示。 <撓曲抵抗性試驗條件〉 •试驗片形狀：l〇〇mmx 1〇〇mmx i 5mm •荷重 ：於中央500g •電氣爐中’於160(TC下保持3小時 〈從1000 c的急冷耐久性試驗條件> •試驗片形狀·· l〇0mmx 100mmx i 5mm •將試驗片置於電氣爐中’以升溫速度1000。。~從 室溫升溫至HKHTC，並在1〇〇(rc下保持3〇分鐘斧後迅 速取出電氣爐，於外氣中放冷並觀察龜裂發生狀況。 表15. Description of the invention (3). Printed by the Consumer Goods Agency of the Intellectual Property Office of the Ministry of Economic Affairs 3 311923 [The best form for implementing the invention] The embodiment of the present invention is described in detail below, but the present invention is not limited thereto. In the oxidized inscription of the present invention, the mullite-based porous flake refractory has a particle size of 50 to 85, which is composed of electrofused oxidized inscription and / or sintered hafnium oxide electrofused mold fused stone. Mass%, the composition of the binding material made of sulphur oxide and mullite occupies 15 to 5G f%, and there are unavoidable impurities, and its porosity is 10 to 40%. According to the oxidized inscription of the present invention, the mullite-based porous flake refractory, in terms of chemical composition when analyzing its composition, the content of ^ 〇3 is preferably $ 85 to 95% by mass, and more preferably 87 to 93% by mass. The content is preferably 5 to 15 mass. /. And more preferably 7 to 13% by mass. The oxidized ingot and mullite-based porous sheet-shaped refractory of the present invention is "in terms of chemical composition when analyzing its composition", as in the case where the content of Al203 is more than 95% by mass, that is, the content of S102 is greater than When 5 mass% is small, the thermal shock resistance and thermal spalling resistance (resltance t0 themal spaing) tend to decrease, which is not preferable. In addition, if the content of ai is less than 85% by mass, that is, when the content is more than 15% by mass', the effect of the present invention, which is the purpose, tends to be insufficient. ^ If the porosity of the alumina and mullite-based porous sheet refractory of the present invention is smaller than 10%, there is a tendency that the resistance to thermal spalling will decrease _ ^^ 不 ^ _ Conversely, such as gas 40 In the case where the% is large, there is a paper towel in the strong paper size _ | fresh (CNS) A4 specifications _----, ---- — — — — — III — — · Γ IIIIII < I — I — III— (Please read the precautions on the back before filling out this page) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economy 1226880 A7 ^ " —------------ V. Description of Invention (4) 'There may be problems with the degree and is not good. In the manufacturing method of the present invention, in order to produce a porous sheet, fused aluminum oxide and / or aggregates having a particle size of 10 to 150 // m made of sintered alumina and fused mold are used. Such aggregates can be prepared in the usual way. In addition, the composition ratio of the fused alumina and / or sintered alumina and fused mullite in the aggregate is 0, which is obtained by using 50 to 85 mass% of the aggregate and 15 to 50 mass of the bonding material. The composition of alumina · mullite-based porous flaky refractory is analyzed as a chemical component, and it is appropriately selected so as to contain Ai20j85 ^ 95% by mass, Si〇2 5-15% by mass, and unavoidable The state of impurities. Such a selection is easy for the industry. t 'In the manufacturing method of the present invention, the particle size of the alumina and silica fine powder and / or clay mixed with the composition ratio that can be alumina and mold after firing is 10 // m or less. The composition ratio of the aluminum oxide to the fine silica powder and / or clay in the bonding material is based on the use of aggregates 50 to 85! %, And 15 to 50% by mass of the bonded material. The mullite-based porous flaky refractory prepared by analyzing the composition into chemical components and components, and appropriately selected to contain M " 3 85 to 95% by mass, 5 to 15% by mass, and inevitable impurities. Such a selection is easy for the industry. In the manufacturing method of the present invention, in order to ensure porosity and obtain sufficient strength, the bonding material is used in an amount of 50 to 85% by mass to 15 to 50% by mass. A predetermined amount of bone material, a binding material, and an organic binder such as methyl cellulose and water in an amount effective for kneading and molding are mixed, and the mixture is thoroughly kneaded using, for example, three rollers (ron). Thereafter, for example: This paper size applies to the Chinese National Standard (CNS) A4 specification ⑵〇X 297 公 爱) a 4--pack --------- order --------- (please Read the precautions on the back before filling in this page) 1226880 A7 V. Description of the invention) Extruded or roller formed into a thickness of 0 to 5_, and the formed sheet is fired at 1 600 to 1800 ° C About 3 to 10 hours to obtain a porous sheet. & The surface roughness Ra of the alumina and mullite porous flake refractory of the present invention obtained by the above-mentioned manufacturing method is 3 // m or less, and if necessary, it can be made by grinding on both sides to form Porous flake refractory with smoother surface. In addition, it has excellent thermal shock resistance and resistance to thermal spalling. It does not break or crack in the rapid cold endurance test from 10,000, and its flex resistance at high temperatures, such as 160CTC, has been greatly improved. . In addition, although the porosity is 10 to 40%, it can also be shed because of its sufficient strength. Large shapes with a thickness of 1.5 mm and a diameter of 300 mm are also practical. Therefore, it can be used as a mesh belt (嶋 hbe_ two plates for firing or porous sheet refractory), and is suitable for firing ceramic substrates or alumina ceramics. Examples and comparative examples will be given below. The present invention is specifically described as follows, but the present invention is not limited by these examples. Example 1 A mixture including fused alumina 60% by mass and fused mullite 40% by mass with a particle size range of 10 to 15G // The bone material of m! ⑽ f parts and 75% by mass of calcined oxide and 25% by weight of oxidized stone powder with a particle size range of i—30 parts by mass of the following, and fluorene group as an organic binder 5 parts by mass of cellulose and 10 parts by mass of water were used, and these mixtures were thoroughly kneaded with 3 parent-child members. Thereafter, they were extruded into a 100 mm _ ^ _ 00 mm x 5 mm sheet. After these shaped pieces are dried, it will be at 700t: The M's scale is applicable to China National Standard (CNS) A4 (2Ί〇X 297 public love) --- (Please read the precautions on the back before filling this page) Zhuang Clothing * ------- Order --------- Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 311923 1226880 B7 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs: ¾ 5. Description of the invention (6) 5 hours, and made porous tablets. The obtained porous tablets have a bulk density of =. The resistance to the cold bend of ▲ is shown in Table 1. 1 and the ratio are also Comparative Example 1. U and the film of the example @ _ 状 之 Oxide Shao magnetic device, for comparison, ^ ^ 2 I made a porous sheet of emulsified aluminum 99 /. Having the same shape as the sheet of the example. The porosity of these sheets, the porosity of the bulk density, "o ...", the flexural resistance from 100% The quenching durability is shown in Section u. ≪ Deflection resistance test conditions> • Test piece shape: 100 mm x 100 mm x i 5 mm • Load: 500 g in the center • In an electric furnace '160 ( Hold at TC for 3 hours <Chilling endurance test conditions from 1000 c> • Shape of test piece · 100mm x 100mm x i 5mm • Place the test piece in an electric furnace 'at a temperature increase rate of 1000. ~ Temperature increase from room temperature To HKHTC, and hold the axe at 100 (rc) for 30 minutes, quickly remove the electric furnace, let it cool in the outside air and observe the occurrence of cracks Status Table 1
本纸張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 鬆密度 g/cm3 視氣孔率 % 實施例~Γ _ 3.02 25 比較例1 0 比較例"Τ 3.78 22 6 311923 (請先閱讀背面之注意事項再填寫本頁) 零裝---------訂---------. 1226880 A7 ----—--_B?__ 五、發明說明（7 ) 由表1之數據可知，比較例丨之氧化鋁磁器製片中， 於1600 C的撓曲抵抗性不充分，而⑼1〇〇〇<t的挽曲抵抗性 不充分，而從100CTC的急冷耐久性試驗，則發生破損。又， 比較例2之氧化鋁99%之多孔質片中，於16〇〇〇c的撓曲抵 抗性不充分，而從1000X：的急冷耐久性試驗，則發生小龜 裂。然而，實施例1之本發明之氧化鋁•模來石系多孔質 片狀对火物中，經已改善於16〇(rc的撓曲抵抗性，而從 1 0 0 0 °c的急冷耐久性試驗，則並未發生龜裂。 ------------壯衣-------訂·-------I (請先閱讀背面之注意事項再填寫本頁} 經濟部智慧財產局員工消費合作社印制衣 本纸張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 7 311923 ^ ^ 經濟部智慧財產局員工消費合作社印製 1226880 A7This paper size is in accordance with Chinese National Standard (CNS) A4 (210 X 297 mm) bulk density g / cm3 apparent porosity% Example ~ Γ _ 3.02 25 Comparative Example 1 0 Comparative Example " T 3.78 22 6 311923 ( (Please read the precautions on the back before filling this page) Zero-loading -------- Order ---------. 1226880 A7 ------------ B? __ 5. Description of the invention (7) From the data in Table 1, it can be seen that in the aluminum oxide magnet sheet of Comparative Example 丨, the flex resistance at 1600 C was insufficient, and the resistance to flexion at 10,000 ° was not sufficient. In the 100CTC quenching durability test, breakage occurred. Further, in the porous sheet of 99% of alumina of Comparative Example 2, the flex resistance at 1600c was insufficient, and from the quenching test at 1000X :, small cracks occurred. However, the alumina and mullite porous flakes of the present invention in Example 1 have been improved in flex resistance to 160 ° C, and have been rapidly quenched from 1000 ° C. Sex test, no cracks occurred. ------------ Zhuang Yi ------- Order · --------- I (Please read the precautions on the back before Fill in this page} The printed paper size of the employees ’cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs applies the Chinese National Standard (CNS) A4 (210 X 297 mm) 7 311923 ^ ^ Printed by the employees’ cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 1226880 A7
片狀耐火物及其製造方法為目的。 [發明揭示] 士發明人等’為達成上述目的而—意研究的結果發 現，藉由以氧化鋁及模來石構成，並以特定量含有特定之 骨材成分及結合成分，且使之保持特定範圍之氣孔率，而 可具有上述諸特性並可製得適合用為上述料的氧化銘· 模來石系多孔質片狀耐火物的事實，以及如此的氧化鋁· 模來石系多孔質片狀耐火物可由使用特定之骨材原料及結 合原料的特定之製造方法製得的事實，而完成本發明。 ^亦即’本發明之氧化鋁•模來石系多孔質片狀耐火物， ,由：電融氧化|g(electr。fused alumina)及/或由燒結 氧化鋁（sintered alumina)與電融模來石而成的粒徑1〇 至150/zm之骨材（aggregate)成分5〇至85質量％、和由氧 化鋁及模來石而成的結合材成分15至5〇質量％、和不可 避免的不純物而成的燒成體’而其特徵為：厚度為0.3至 5mm、氣孔率為10至40%者。 、又、’本發明之氧化鋁•模來石系多孔質片狀耐火物之 製造方法之特徵為：混合由；電融氧化鋁及/或由燒結氧化 電融模來石而成的粒徑10至15〇#m之骨材5〇至85 貝β 和由ί知：燒成後能成為氧化銘及模來石之方式的 組成比混合的氧化鋁與氧化矽微粉及/或黏土而成的粒徑 以下之結合材15至50質量％、和對混練.成型有 機黏合_*0、和水’並經充分混練後成型 為厚度0.3至5mm之片’待乾燥後於16⑼至丨綱。c燒成 本紙張尺匕適用中國國豕標準（CNS)A4規格⑵〇心97公髮） '—- (請先閱讀背面之注意事項再填寫本頁) # 訂---------線- 2(修正頁） 311923The sheet-like refractory and its manufacturing method are aimed at. [Disclosure of the invention] In order to achieve the above-mentioned object, the inventors of the present invention and other studies have found that the structure is composed of alumina and mold stone, and contains a specific bone component and a binding component in a specific amount, and maintains the same. The porosity of a specific range, and the fact that it can have the above-mentioned characteristics and can be used as the above-mentioned oxidized ingots · mullite-based porous flake refractories, and such alumina · mullite-based porous materials The present invention has been completed by the fact that the sheet-like refractory can be produced by a specific manufacturing method using a specific aggregate material and a combination of raw materials. ^ That is, the alumina and mullite porous flake refractory of the present invention is composed of: electrofusion oxidation | g (electr. Fused alumina) and / or sintered alumina and electrofusion mold Aggregate components with a particle size of 10 to 150 / zm from 50 to 85% by mass, and 15 to 50% by mass of a composite material composed of alumina and mullite. The sintered body made of impure substances is characterized by a thickness of 0.3 to 5 mm and a porosity of 10 to 40%. The method of manufacturing the alumina-mollite-based porous flake refractory of the present invention is characterized in that: the particle size is made by mixing fused alumina and / or sintered oxidized fused mullite 10 to 15〇 # m 的 骨材 50 ～ 85 贝 β and made from the knowledge that after firing, the composition ratio of the method that can become oxidized enamel and mullite is made by mixing alumina and silica fine powder and / or clay. 15 to 50% by mass of the binding material with a particle size of less than 50% by weight, and mixed with each other. Molded organic bonding _ * 0, and water 'and fully kneaded to form a sheet with a thickness of 0.3 to 5mm. c Burning cost paper ruler is applicable to China National Standard (CNS) A4 specification ⑵〇97 97 issued) '—- (Please read the precautions on the back before filling out this page) # Order --------- Line-2 (correction page) 311923