TW543051B - Burning tool for electronic parts - Google Patents

Abstract

A burning tool for electronic parts is provided, which can reduce the burning time for a body to be burnt, and has a long service life. The burning tool for electronic parts is used for producing electronic parts by laminating the body to be burnt consisting of ceramic thereon, and burning the body to be sintered. The tool consists of a base material containing cordierite, or cordierite and alumina, and/or mullite, and at least one intermediate layer and a surface layer consisting of a material having low reactivity with the above body to be burnt.

Description

t 543051 五、發明說明（1) 【發明領域】 本發明關於用於電子元件的燒成夾具（後面簡稱為π 燒成夾具"），更具體地說，關於能夠縮短被燒成體的燒 成時間而且哥命長的用於電子元件的燒成夾具。 【發明背景】 以前，陶瓷電容、熱敏電阻、鐵氧體等由陶瓷構成的 電子元件的燒成是把電子元件放置在氧化鋁材質的燒成夾 具（例如***、燒盆、平板）上進行。這種燒成是多個 燒成夾具堆放在一起進行的，而且燒成夾具多次使用。 這種燒成夾具由馨土石夕石材質和/或碳化石夕材質的基 體材料和乳化錯材質表層構成’或者由蓉土石夕石材質和/ 或氧化锆材質的基體材料、礬土矽石材質的中間層和氧化 鍅材質的表層構成（見平1 0 - 1 5 8 0 8 1號特許公開公報、平 1 1 - 2 6 3 6 7 1號特許公開公報等）。 這些燒成夾具中由於基體材料使用礬土矽石材質、碳 化石夕材質、及氧化錯材質的材料，對以前的電子元件的燒 成速度很有承受力，若為了縮短電子元件的燒成時間，升 ’溫和降溫速度比以前提高，就存在抗裂性不夠，燒成夾具 發生裂缝的問題。 本發明就是針對以前的這種問題提出的。本發明的目 的是提供一種用於電子元件的燒成夾具，抗裂性比以前提 高，並能夠縮短電子元件的燒成時間而且寿命長。 【發明内容】 根據本發明，提供一種用於電子元件的燒成夾具，用t 543051 V. Description of the invention (1) [Field of the invention] The present invention relates to a firing jig for electronic components (hereinafter referred to as π firing jig "), and more specifically, it can shorten the firing of the object to be fired. It has a long life and a long life firing jig for electronic components. [Background of the Invention] In the past, the firing of electronic components made of ceramics, such as ceramic capacitors, thermistors, and ferrites, was performed by placing the electronic components on a firing fixture (such as a positioner, a baking pot, and a flat plate) made of alumina. get on. This firing is performed by stacking multiple firing jigs, and firing jigs are used multiple times. This firing jig is composed of a base material made of aragonite and / or carbonized carbide and a surface layer of emulsified material, or a base material made of arborite and / or zirconia, and alumina silica. The intermediate layer and the surface layer of the hafnium oxide material (see Hei 10-1 5 8 0 8 No. 1, Hei 1 1-2 6 3 6 7 No. 1). In these firing jigs, since the base material is made of alumina silica material, carbonized carbide material, and oxidized material, it is very resistant to the firing speed of previous electronic components. If you want to shorten the firing time of electronic components, If the temperature rise and temperature decrease is higher than before, there is a problem of insufficient crack resistance and cracks in the firing fixture. The present invention is made in response to such a problem. An object of the present invention is to provide a firing jig for an electronic component, which has higher crack resistance than the premise, can shorten the firing time of the electronic component, and has a long life. SUMMARY OF THE INVENTION According to the present invention, a firing jig for an electronic component is provided.

543051 五、發明說明（2) 於把由陶瓷構成的被燒成體裝載在上面，燒成該被燒成體 以製作電子元件，其特徵在於：由含有堇青石、或者堇青 石和氧化銘和/或富銘紅柱石的基體材料、至少為1層的中 間層、和與上述被燒成體反應性低的材料形成的表層構 成。 此時，理想的是由含有雜質量占質量2. 5 %以下的堇青 石、或者雜質量占質量2. 5 %以下的堇青石和氧化鋁和/或 富鋁紅柱石的基體材料、至少為1層的中間層、和與被燒 成體反應性低的材料形成的表層構成。含有雜質是氧化鐵 (F e203 )時，理想的是堇青石中含有的氧化鐵（F e203 )量 占質量1%以下。而且，含有雜質是氧化鐵（Fe2 03 )、氧化 鈉（Na20 )及氧化鉀（K20 )時，理想的是堇青石中含有的 氧化鐵（Fe203 )、氧化鈉（Na20 )及氧化鉀（K20 )量占質 量2%以下。 此時，理想的是基體材料含有的上述堇青石占質量 5 0 %以上；與中間層含有選自氧化铭、富銘紅柱石、氧化 銘和氧化錄的共晶物、及氧化铭和富紹紅柱石的混合物所 構成的組中的一種以上；表層含有氧化锆。且，理想的是 中間層通過噴鍍法或者喷塗法形成；而表層通過喷鍍法或 喷塗法形成。喷鍍法係水穩定化等離子體喷鍍法。 【發明概要】 本發明係用於電子元件的燒成夾具，用於把由陶瓷構 成的被燒成體裝載在上面，燒成該被燒成體而製作電子元 件，由含有堇青石、或者堇青石和氧化銘和/或富銘紅柱543051 V. Description of the invention (2) The method of loading a fired body made of ceramic on the fired body to produce an electronic component is characterized in that it comprises cordierite, or cordierite and an oxide and It is composed of a base material of Fuming Andalusite, an intermediate layer of at least one layer, and a surface layer formed of a material having low reactivity with the fired body. At this time, it is desirable that the base material contains cordierite with an impurity amount of 2.5% by mass or less, or cordierite with an impurity amount of 2.5% by mass or less, and alumina and / or mullite, at least A single-layered intermediate layer and a surface layer formed of a material having low reactivity with the fired body. When the impurity is iron oxide (F e203), it is desirable that the amount of iron oxide (F e203) contained in cordierite is 1% by mass or less. Further, when the impurities are iron oxide (Fe2 03), sodium oxide (Na20), and potassium oxide (K20), it is desirable that iron oxide (Fe203), sodium oxide (Na20), and potassium oxide (K20) contained in cordierite. The amount accounts for less than 2% of the mass. At this time, it is desirable that the above-mentioned cordierite contained in the base material accounts for more than 50% by mass; and the intermediate layer contains a eutectic material selected from the group consisting of oxide oxide, Fuming andalusite, oxide oxide and oxide record, and oxide oxide and Fushao One or more of the group consisting of a mixture of andalusite; the surface layer contains zirconia. Moreover, it is desirable that the intermediate layer is formed by a spraying method or a spraying method; and the surface layer is formed by a spraying method or a spraying method. The spraying method is a water-stabilized plasma spraying method. [Summary of the Invention] The present invention is a firing jig for electronic components. It is used to load a fired body made of ceramics on the fired body, and fire the fired body to produce electronic components. Bluestone and Oxygen and / or Fuming Red Post

543051 五、發明說明（3) 石的基體材 反應性低的 此時， 石、或者雜 畐銘紅柱石 被燒成體反 本發明 堇青石。堇 的基體材料 燒成夹具， 性，能夠縮 夾具，在耐 溫度和電子 彎曲和表面 這裏， 熱膨脹小、 高頻電絕緣 然原料或者 1 40 0 °C燒成 而且，， 溫度和被燒 果這種彎曲 發生變形。 即使能夠堆 料、至少為1層的中間層、和與、 材料形成的表層構成。 &被燒成體 理想的是由含有雜質量占質量2 s 質量占質量2·則下的堇青石及=下的堇青 的基體材料、至少為1層的中間声、鋁和/或 應性低的材料形成的表層構成。 #舁上述 的燒成夾具’特徵在於基體材料使 青石純度高了 ，就變成溫度變化和承=純度的 、 、 發明的 逑升溫、降涊从 短電子元件的燒成時間 ，使用這種高純度堇青石基體材料二=性能強 與ί前比ί二ΐ ΐ耐快速升溫、降溫的強抗裂 而且 本發 受迅速燒成时机芩曲性強，由於能夠抑 元件的加麼產生的變形，且能夠防止焊j = f 剝離，因此壽命長。 疋n 堇青石的化學組成為2Mg0 —2A丨2〇3 — 5Si〇2，具有 抗熱衝擊性強、南度财酸性、耐驗性、_ π和 ，高等優點。混合高嶺土、菱鎂礦、粘=^天 氧化鋁、氧化鎂、矽石等人造原料在丨3 〇 〇至 製作。 1彎曲π是指如果燒成夾具反覆使用，由於燒成 成體的加壓燒成失具變形下垂的權宜說法。如 眭=，由於燒成夾具變形大，被燒成體即製品 通常燒成夾具堆積使用，但是變得不能堆放， 放’燒成夾具變得不穩定，容易發生在燒成爐 543051 五、發明說明（4) 内坍塌的事故。 下面更詳細地說明本發明，但是本發明並不限於下面 的實施例。 【具體實施方式】 (1 )用於電子元件的燒成夾具 在本說明書中，所說的π用於電子元件的燒成夾具π係 指燒成陶瓷電容、熱敏電阻、鐵氧體等由陶瓷構成的電子 元件時使用的部件，具體是包括用於放置被燒成體的定位 器、燒盆、平板等。· (2 )基體材料 本發明的燒成夾具，由含有堇青石、或者堇青石及氧 化鋁和/或富鋁紅柱石的基體材料、至少為1層的中間層 、和與上述被燒成體反應性低的材料形成的表層構成。 此時，理想的是基體材料由含有雜質量占質量2. 5 %以 下的堇青石、或者雜質量占質量2.5%以下的堇青石及氧化 鋁和/或富鋁紅柱石構成。雜質為氧化鐵（Fe2 03 )時，理 想的是堇青石中含有的氧化鐵（Fe203 )量占質量1%以下。 如果氧化鐵（Fe203 )量超過質量的1%以上，玻璃成分的生 成變強，這是表層耐剝離性下降的原因。而且，作為雜質 ，理想的是堇青石中含有氧化鐵（Fe2 03 )、氧化鈉 (Na20 )及氧化鉀（K20 )量占質量2%以下。 堇青石中含有的雜質主要是氧化鐵（Fe2 03 )、氧化鈉 (Na20 )及氧化if ( K20 )，雖然此外含有氧化妈 (CaO )、氧化鈦（Τι02 )，但是在本發明中作為雜質稱543051 V. Description of the invention (3) The base material of the stone is low in reactivity. At this time, the stone or mixed stigma andalusite is burned to reflect the present invention cordierite. The base material of the cordier firing fixture, can shrink the fixture, the temperature and the electronic bending and the surface here, the thermal expansion is small, the high-frequency electrical insulation is raw materials or firing at 1 40 ° C, and the temperature and the burned fruit This kind of bending is deformed. Even if it can be stacked, it has at least one intermediate layer and a surface layer made of materials. & The fired body is preferably composed of a base material containing cordierite and cordierite at a mass of 2 s and 2 s of mass, and at least one layer of intermediate sound, aluminum and / or A surface layer made of a material with low properties. # 舁 The above-mentioned firing jig 'is characterized in that the base material makes the purity of the bluestone high, and it becomes a temperature change and a high temperature. The invention's invention raises the temperature and reduces the temperature. From the short firing time of electronic components, this high purity is used. Cordierite base material II = strong performance compared with ί front ί ΐ ΐ strong resistance to rapid temperature rise, strong temperature resistance and crack resistance, and the hair is subject to rapid firing timing and flexibility, because it can suppress the deformation caused by the addition of components, and Can prevent welding j = f peeling, so long life. The chemical composition of 疋 n cordierite is 2Mg0 — 2A 丨 2〇3 — 5Si〇2, which has the advantages of strong thermal shock resistance, Nanducai acidity, endurance, π and and high. Blend kaolin, magnesite, sticky man-made raw materials such as alumina, magnesia, silica, etc. from 3,000 to 3,000. 1 Bending π is an expedient statement that if the firing jig is used repeatedly, it will lose its shape and sag due to the pressure firing of the fired body. If 眭 =, due to the large deformation of the firing jig, the fired body, ie the product, is usually stacked and used, but it cannot be stacked. The firing jig becomes unstable and easily occurs in the firing furnace. 543051 V. Invention Explanation (4) The accident that collapsed inside. The present invention is described in more detail below, but the present invention is not limited to the following examples. DETAILED DESCRIPTION (1) Firing jig for electronic components In this specification, the π firing jig for electronic components refers to the firing of ceramic capacitors, thermistors, ferrites, etc. The components used in the electronic component made of ceramics specifically include a positioner, a baking tray, a flat plate, and the like for placing a fired body. (2) Base material The firing jig of the present invention comprises a base material containing cordierite, or cordierite and alumina and / or mullite, an intermediate layer of at least one layer, and the fired body. A surface layer made of a material having low reactivity. At this time, it is desirable that the base material is composed of cordierite having an impurity amount of 2.5% by mass or less, or cordierite having an impurity amount of 2.5% by mass, and alumina and / or mullite. When the impurity is iron oxide (Fe2 03), it is desirable that the amount of iron oxide (Fe203) contained in cordierite is 1% by mass or less. If the amount of iron oxide (Fe203) exceeds 1% by mass or more, the generation of glass components becomes stronger, which is why the peel resistance of the surface layer decreases. Moreover, as the impurity, it is desirable that cordierite contains iron oxide (Fe2 03), sodium oxide (Na20), and potassium oxide (K20) in an amount of 2% by mass or less. The impurities contained in cordierite are mainly iron oxide (Fe2 03), sodium oxide (Na20), and if (K20). Although they also contain oxide (CaO) and titanium oxide (Ti02), they are referred to as impurities in the present invention.

543051 五、發明說明（5) 為A L2 03、S i 02、M g 0以外的成分。這樣的成分容易形成低 融物，燒成時容易在燒成夾具中生成液相。如果堇青石中 含有這樣的雜質多，基體材料的抗彎曲性和中間層與基體 材料的抗剝離性下降，且給被燒成體的特性帶來不良影 響。 因此，必須使用這種雜質少的堇青石，高純度堇青石 與低純度堇青石比較，抗彎曲性強，且與氧化銘和富銘紅 柱石比較，抗裂性提高，能夠提高抗裂性和抗彎曲性。堇 青石中的雜質量如同後面的實施例所示，雜質總量占質量 2· 5%以下，作為主要雜質的氧化鐵（Fe203 )、氧化鈉 (Na20 )及氧化鉀（K20 )占質量2%以下就可以了。 而且，所述雜質的測定使用一般的濕式分析等就可以 完成，例如以日本工業標準R 2 2 1 2 ( 1 9 9 1 )為標準進行就 可以了。 又，本發明中，理想的是基體材料含有的上述堇青石 占質量50%以上。抗裂性和抗彎曲性強，如果基體材料含 有雜質總置占質置2. 5 %以下、作為主要雜質的氧化鐵 (Fe203 )、氧化鈉（Na20 )及氧化鉀（K20 )占質量2%的堇 青石占質量5 0%以上，如同後面的實施例所示，基體材料 的抗裂性顯著提高，即使反復燒成也不容易發生裂缝，能 夠實現燒成夹具壽命長。 (3 )中間層 本發明中所說的中間層，是位於基體材料和表層之間 的層，它的熱膨脹率在基體材料的熱膨脹率和表層的熱膨543051 V. Description of the invention (5) Components other than A L2 03, S i 02, and M g 0. Such a component easily forms a low-melting substance, and a liquid phase is easily generated in a firing jig during firing. If cordierite contains many such impurities, the bending resistance of the base material and the peel resistance of the intermediate layer and the base material are reduced, and the characteristics of the fired body are adversely affected. Therefore, cordierite with less impurities must be used. Compared with low-purity cordierite, high-purity cordierite has better bending resistance, and compared with oxidized and Fuming andalusite, it has improved crack resistance and can improve crack resistance and Resistance to bending. The amount of impurities in cordierite is as shown in the examples below. The total amount of impurities accounts for less than 2.5% by mass. Iron oxide (Fe203), sodium oxide (Na20), and potassium oxide (K20) as the main impurities account for 2% by mass. The following is fine. In addition, the measurement of the impurities can be performed using a general wet analysis or the like, and for example, it can be performed according to the Japanese Industrial Standard R 2 2 1 2 (19 9 1). In the present invention, it is preferable that the cordierite contained in the base material accounts for 50% by mass or more. Crack resistance and bending resistance are strong. If the base material contains impurities total 2.5% or less, iron oxide (Fe203), sodium oxide (Na20) and potassium oxide (K20) as main impurities account for 2% by mass. Cordierite accounts for more than 50% of the mass. As shown in the examples below, the crack resistance of the base material is significantly improved, and cracks are unlikely to occur even after repeated firing, and a long life of the firing jig can be achieved. (3) Intermediate layer The intermediate layer referred to in the present invention is a layer located between the base material and the surface layer, and its thermal expansion coefficient is between that of the base material and that of the surface layer.

第8頁 543051 五、發明說明（6) 脹率之間。 如果形成中間層，基體材料和表層之間的熱膨脹率差 被緩解，具有能夠防止表層剝離的優點。 本發明中的燒成夾具中，理想的是中間層含有選自氧 化銘、富銘紅柱石、氧化銘和氧化錯的共晶物、及氧化I呂 和富鋁紅柱石的混合物所構成的組中的一種以上。 如果考慮對被燒成體的特性的影響，理想的是與表層 相連的中間層的S i 02量占質量2 0 %以下。 本發明中的中間層如果使用上述化合物作為材料，使 用以前的噴鍍法或者喷塗法層疊在基體材料表面上就可以 了。例如，如果使用氣體等離子體喷鍍法，最好中間層的 膜厚為5 0微米（// m )〜1 0 0微米（// m )水平，如果使用水穩定 化等離子體喷鍍法，最好中間層的膜厚為1 0 0微米 (// m)〜150微米（/zm)水平。 如果使用喷塗法，理想的是中間層的膜厚為5 0微米 (//m)〜500微米（wm)水平。 本發明中，構成為中間層是多層、使熱膨脹率緩慢變 化也可以。例如，在1 0 0 0 °C時的熱膨脹率，堇青石為 0 . 2 % ’富銘紅柱石為0 · 4 % ’氧化結為0 . 8 % ’氧化錯為 0. 9%，如果燒成夾具按照這樣的順序層疊，能夠把熱膨脹 率的差抑制在最小限度内，在燒成時能夠緩解層與層之間 的剝離應力。 這裏，所謂共晶物是指從熔融體中同時析出的2種以 上的物質的混合物。它的各種組成成分形成為細微混合組Page 8 543051 V. Description of the invention (6) Between expansion rates. If the intermediate layer is formed, the difference in thermal expansion coefficient between the base material and the surface layer is reduced, and there is an advantage that the surface layer can be prevented from peeling. In the firing jig of the present invention, it is desirable that the intermediate layer contains a group selected from the group consisting of oxidized indium, fuming andalusite, oxidized indium and oxidized eutectic, and a mixture of oxidized aluminum and mullite. More than one. Considering the influence on the characteristics of the fired body, it is desirable that the amount of Si 02 in the intermediate layer connected to the surface layer accounts for less than 20% by mass. If the intermediate layer in the present invention uses the above-mentioned compound as a material, it may be laminated on the surface of the base material by a conventional spraying method or a spraying method. For example, if a gas plasma spraying method is used, it is preferable that the film thickness of the intermediate layer is 50 micrometers (// m) to 100 micrometers (/ m). If a water-stabilized plasma spraying method is used, Preferably, the film thickness of the intermediate layer is at a level of 100 micrometers (// m) to 150 micrometers (/ zm). If a spraying method is used, it is desirable that the film thickness of the intermediate layer is 50 micrometers (// m) to 500 micrometers (wm). In the present invention, the intermediate layer may be composed of a plurality of layers, and the thermal expansion coefficient may be gradually changed. For example, the thermal expansion rate at 1000 ° C, cordierite is 0.2% 'Fuming andalusite is 0.4%' oxidation junction is 0.8% 'oxidation error is 0.9%, if burned The jigs are stacked in this order, and the difference in thermal expansion coefficient can be minimized, and the peeling stress between layers can be alleviated during firing. Here, the eutectic means a mixture of two or more substances that are simultaneously precipitated from a melt. Its various components are formed into subtle mixed groups

543051 五、發明說明（7) 織。共晶物如同其他純粹 ^^ 合物不同，具有熔點 .只是凝固、熔融點與 優點。 在。構成成分的渡合物系中為最小的匕 間層的表面，利用J : : : f f膜能夠對著基體材料和中 鑛時，進一步浸入基體材料和容易溶解，在嘴 含有共晶物的喷鍍覆膜與 & x =的凸凹處。因此 高，難以發生剝離。 &材科和中間層的結合性提 本發明中，雖然使用氧化鋁和 在呂（mp，2015。〇 *氧化錯〜，2 677 i :rf，氧化 化鍅是指沒有穩定化的氧化 二曰;物中的氧 .6時獲得最小溶點mGt，在 ^置比為57.4 : 42. 水平）共晶物變換。 (4 )表層 又俠 表面：5：：表層’是指基體材料的表面或者中門 :。如杲形成表層，防止基體#料和中間層中：：的接觸 地:元件材料接觸。本發明的燒成爽：中的反應 有是應性低的材芯化：想、 ΐΓί電容，理想地是選擇與鈦酸鋇反應性低的ί:構成 表層中的氧化鍅除了未穩定化的氧化錯之外錯。 543051 五、發明說明（8) 氧化鈣（CaO )、三氧化二釔（Y203 )等穩定化的穩定化氧 化锆。因此，考慮上述反應性適當選擇最合適的氧化锆就 可以了。 而且，根據電子元件的種類，也可以使用含有氧化銘 和氧化錘的共晶物的喷鍍覆膜作為表層。 本發明中的表層，以上述的化合物作為材料，利用以 前的噴鍍或者喷塗方法在基體材料的表面或者中間層的表 面上層疊就可以了。本發明中，不特別限於能夠確保上述 效果的表層膜厚。 如上所述，本發明的燒成夾具，特別理想地是基體材 料含有的上述堇青石占質量50%以上；中間層含有選自氧 化紹、昌銘紅柱石、氧化銘和氧化錯'的共晶物、及氧化銘 和富銘紅柱石的混合物所構成的組中的一種以上；表層含 有氧化锆。 (5 )製造方法 本發明的燒成夾具能夠通過如下方式製造，即利用噴 鍍法或者喷塗法，在所希望形狀的基體材料表面上形成中 間層、然後形成表層。 所謂喷鐘法是把金屬或陶究細微粉末（下面稱為π喷 鍍材料π )加熱成半熔融狀態，喷鑛在鍍膜物件的表面上 形成喷鍍覆膜的方法。根據加熱方法不同存在，使用燃燒 焰的氣體噴鍍法、使用電弧的電弧喷鍍法等各種方法，但 是本發明中最好通過使用等離子體喷嘴的等離子體喷鍍法 形成喷鍍覆膜。543051 V. Description of Invention (7) Weaving. Eutectics are different from other pure ^^ compounds in that they have a melting point. They have only solidification, melting points and advantages. in. It is the surface of the smallest dagger layer among the constituents of the conjugate system. When the J ::: ff film can be used to face the base material and the middle ore, it can be further immersed in the base material and easily dissolved. The eutectic contains spray in the mouth. Laminated with & x = convex and concave. Therefore, it is high and peeling is hard to occur. & Combinability of Materials and Intermediate Layers In the present invention, although alumina and aluminum oxide are used (mp, 2015. 〇oxidation error ~, 2 677 i: rf, osmium oxide refers to the second oxide without stabilization. The minimum melting point mGt is obtained at 6 o'clock, and the eutectic transformation is achieved at a ratio of 57.4: 42. (4) Surface layer Xia surface: 5 :: surface layer 'refers to the surface of the base material or the middle door :. If 杲 forms a surface layer, prevent contact between the base material and the intermediate layer :: Ground: The component material is in contact. The firing of the present invention has a low-response material core reaction: ideally, 电容 Γί capacitor, ideally choose Γ, which has low reactivity with barium titanate: rhenium oxide in the surface layer except for unstabilized Oxidation is wrong. 543051 V. Description of the invention (8) Stabilized stabilized zirconia such as calcium oxide (CaO), yttrium trioxide (Y203). Therefore, it is sufficient to appropriately select the most suitable zirconia considering the above reactivity. In addition, depending on the type of the electronic component, a spray-coated film containing a eutectic substance of an oxide name and an oxide weight may be used as the surface layer. The surface layer in the present invention can be laminated on the surface of the base material or the surface of the intermediate layer by using the aforementioned thermal spraying or spraying method using the aforementioned compound as a material. In the present invention, the thickness of the surface layer which can ensure the above-mentioned effects is not particularly limited. As described above, the firing jig of the present invention is particularly preferably such that the cordierite contained in the base material accounts for more than 50% by mass; the intermediate layer contains a eutectic selected from the group consisting of Shaoxing, Changming andalusite, oxidizing oxide, and oxidizing oxide. One or more of the group consisting of a mixture of oxides and fuming andalusite; the surface layer contains zirconia. (5) Manufacturing method The firing jig of the present invention can be manufactured by forming an intermediate layer on the surface of a base material having a desired shape using a spraying method or a spraying method, and then forming a surface layer. The so-called clock spray method is a method of heating a metal or ceramic fine powder (hereinafter referred to as π spray coating material π) to a semi-fused state, and spraying ore to form a spray coating on the surface of a coating object. Various methods exist depending on the heating method, such as a gas spray method using a combustion flame, an arc spray method using an electric arc, but in the present invention, it is preferable to form a thermal spray coating by a plasma spray method using a plasma nozzle.

543051 五、發明說明（9) 本發明中，等離子體喷鍍法中的水释 鍍法更為理想。利用氣體等離子體喷錢子體喷 小膜厚為20微米（_)〜50微米（”）水平膜的最 定化等離子體噴鍍法能夠形成最小 用水穩 表面結合力方面是優秀的選擇。 a e表面的 所明噴塗法，是指把陶瓷粉末製成漿噴 上、漿在基體表面上流動然後燒形成噴塗覆2 土體表面 塗法與喷鍍法比較容易形成厚膜，而且噴= ^法。喷 粒度在1 0 0微米（V m)至2 〇 〇微米（V m)水平鉍、、此夠使用 能夠使用粒度在數微米至5 〇 〇微米（“ m) 騎料，喷塗法 因此，喷塗法與噴鍍法比較，所述覆犋能二：，的材料。 硬度和表面粗糙度等優良的特性。而且，+广侍氣孔率、 比較，還有成本不高的優點。 贺塗法與噴鍍法 下面，利用實施例更詳細地說明 具。 很據本發明的燒成夾 (實施例1〜3 ’比較例1〜3 ) 體 在實施例1〜3和比較例丨〜3中，對 具的基體材料進行評價。實施例丨〜3和 本每明的燒成夾 材料，通過如下方式製成：使用（a 較例卜3中的基 U )含（Fe203 )占質量〇 . i %、氧化鈉 b )作為原料 (LO)占質量〇.3%、其他雜質含量占及氧化鉀 石；（b )含（Fe2〇3 )量占質量2. 7%、貝人里,3%的堇青 3氧化鈉（Na9〇 ) 543051 五、發明說明（ίο) 及氧化鉀（Κ20 )量占質量1. 4%、其他雜質含量占質量 1 . 7 %的堇青石，把它們混合，在輪碾機上混勻後，通過油 壓機在1噸/平方公分的壓力下形成為長150釐米（mm )χ 寬 1 50釐米（mm)x 厚4釐米（mm)，在1 3 0 0 ° C燒成3小時作成。 而且，堇青石基體材料中含的雜質量通過適當混合上述 (a ) 、 （ b )原料進行調整。 根據實施例1〜3和比較例1〜3對抗裂性和抗彎曲性的評 價結果在表1中示出。抗裂性的評價是以如下方式進行， 即在製作的基體材料中央部分放置大小為所述基體材料 6 5%大小的氧化锆材質的燒成夾具，然後放置在小型電爐 内，從3 5(TC開始每次升溫5(TC，直到1 0 0 0 °C，然後觀察 放置在常溫下時有無裂缝。在各個溫度下，加熱1小時 。表1中，不滿6 0 0 °C時發生裂缝的為X ，從6 0 0 °C開始至 不滿7 0 0 °C時範圍内發生裂缝的為△，從7 0 0 °C開始至不滿 8 0 0 °C時發生裂缝的為〇，在8 0 0 °C時沒有發生裂缝的為 ◎。 抗彎曲性的評價通過如下方式完成，即在製作的基體 材料中央部分載入4kg/cm2在120 0°C下保持5小時，然後去 掉載入時，觀察從載入前開始發生的彎曲量。表1中彎曲 量大於1.5釐米（mm)的為X ，彎曲量小於1.5釐米（mm)大於 1.0釐米（mm)的為△，彎曲量小於1.0釐米（mm)大於 0.5釐米（mm)的為〇，彎曲量小於0.5爱米（mm)的為©)。543051 V. Description of the invention (9) In the present invention, the water release plating method in the plasma spraying method is more preferable. The most optimized plasma spraying method using a gas plasma spraying sub-body spraying a small film thickness of 20 microns (_) to 50 microns (") horizontal film can form the smallest water-stable surface bonding force. Ae The surface spraying method refers to spraying ceramic powder onto the slurry, flowing the slurry on the surface of the substrate, and then firing to form a spray coating. 2 The soil surface coating method is easier to form a thick film than the spray coating method, and spraying = ^ method The spray particle size is between 100 micrometers (V m) and 2000 micrometers (V m). The bismuth is sufficient, which can use the particle size of several micrometers to 500 micrometers (“m). The spray method therefore Compared with the spraying method and the spraying method, the coating can be made of two materials. Excellent properties such as hardness and surface roughness. Moreover, the + porosity porosity and comparison have the advantage of low cost. Concoction method and thermal spray method Next, the tool will be described in more detail using examples. The firing clips according to the present invention (Examples 1 to 3 'and Comparative Examples 1 to 3) were evaluated in Examples 1 to 3 and Comparative Examples 1 to 3. Examples 丨 3 and Benjamin's sintered clip material were made by using (a the base U in Example 3) containing (Fe203) 0.1% by mass, sodium oxide b) as a raw material (LO) accounts for 0.3% by mass, the content of other impurities and potassium oxide stones; (b) (Fe2O3) accounts for 2.7% by mass, Beirenli, 3% cordierine 3 sodium oxide (Na9 〇) 543051 V. Description of the invention (ίο) and potassium oxide (κ20) accounted for 1.4% by mass, and other impurities contained 1.7% by mass of cordierite. After mixing them, mixing them on a wheel mill, It was formed into a length of 150 cm (mm) x a width of 150 cm (mm) x a thickness of 4 cm (mm) by a hydraulic press under a pressure of 1 ton / cm2, and it was fired at 1,300 ° C for 3 hours. The amount of impurities contained in the cordierite base material is adjusted by appropriately mixing the above-mentioned (a) and (b) raw materials. The evaluation results of crack resistance and bending resistance according to Examples 1 to 3 and Comparative Examples 1 to 3 are shown in Table 1. The evaluation of crack resistance was performed by placing a firing jig of zirconia material having a size of 65% of the base material in the central portion of the produced base material, and then placing it in a small electric furnace from 3 5 ( TC starts to heat up 5 ° C (until 100 ° C), and then observes whether there are cracks when placed at normal temperature. At each temperature, it is heated for 1 hour. In Table 1, cracks occur when the temperature is less than 60 ° C. X is △, cracks occurred in the range from 600 ° C to less than 7 0 ° C, △, cracks occurred from 7 0 ° C to less than 8 0 0 ° C, 0, 8 0 No crack occurred at 0 ° C is ◎. The evaluation of bending resistance is completed by loading 4kg / cm2 in the central part of the produced base material and holding it at 120 0 ° C for 5 hours, and then removing the loading, Observe the amount of bending that occurs from before loading. In Table 1, the amount of bending greater than 1.5 cm (mm) is X, the amount of bending less than 1.5 cm (mm) is greater than 1.0 cm (mm) is △, and the amount of bending is less than 1.0 cm ( (mm) is greater than 0.5 centimeters (mm) is 0, and the amount of bending is less than 0.5 millimeters (mm) is ©).

543051 抗彎曲性 Ο Ο 〇 <! X X 抗裂性 ◎ ◎ ◎ ◎ ◎ ◎ m ΕξΠΕ m 雜質量 (%) 合計 2. 3 1. 2 0. 7 Ο Ο 00 CO ^ LO 其他 卜寸 CO Ο Ο 〇 ^~t 卜 〇 1~( 1~( A*+B 氺 CD 00 寸 -η Ο Ο cy^ r~^ oi cvi ^ 卜寸 CO Ο Ο 〇 Oi O 寸 τ~< r~( 0· 9 0. 4 0. 1 Ν ⑦卜 r-H i—l CS3 材料 堇青石 堇青石 堇青石 堇青石 堇青石 堇青石 賨施例1 賨施例2 實施例3 比較例1 比較例2 比較例3 (0£)騷^¥<*543051 Anti-bending resistance 〇 〇 〇 & XX Crack resistance ◎ ◎ ◎ ◎ ◎ ◎ m ΕξΠΕ m Miscellaneous mass (%) Total 2. 3 1. 2 0. 7 Ο OO 00 CO ^ LO 〇 ^ ~ t Bu 〇1 ~ (1 ~ (A * + B 氺 CD 00 inch -η Ο Ο cy ^ r ~ ^ oi cvi ^ Bu inch CO Ο Ο 〇Oi O inch τ ~ < r ~ (0 · 9 0. 4 0. 1 Ν ⑦ rrH i-1 CS3 Material Cordierite Cordierite Cordierite Cordierite Cordierite Cordierite Cordierite Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 (0 £) Sao ^ ¥ < *

第14頁 543051 五、發明說明（12) (評價） 從1可以知道，雜質總量占質量2, 5 %以上，而且作為 主要雜質的氧化鐵（Fe2 03 )、氧化納（Na20)及氧化_ (K20 )占質量2%以上的堇青石基體材料，在8 0 0 ° C以下 不發生裂缝，抗裂性良好，但是彎曲量大於1. 0 釐米 (mm)，表明抗彎曲性不夠。雜質總量占質量2· 5%以下，而 且作為主要雜質的氧化鐵（Fe2 03 )、氧化納（Na20 )及氧 化鉀（K20 )占質量2%以下的堇青石基體材料，結果抗裂 性和抗彎曲性都很好。而且，實施例1〜3和比較例1〜3中， 獲得即使在1 0 〇 trc時也不發生裂缝的結果。 (實施例4〜9，比較例4、5 ) 實施例4〜9和比較例4、5與實施例1〜3 —樣，對根據本 發明的燒成夾具的基體材料進行評價。實施例4〜9的基體 材料，通過如下方式製成··使用上述（a ) 、 （ b )的堇青 石和（c ) 、 ( d ) 、 （ e )作為原料，（c )最大粒子直徑 為2 5 0微米（// m)及4 4微米（// m )的電融氧化銘（d )最大粒 子直徑為1 50微米（// m)及44微米（// m)的電融富鋁紅柱石 (e )平均粒子直徑為3微米（// m)的煆燒氧化鋁為原料， 成型為與實施例1〜3相同的形狀，在1 4 5 0 °C燒成5小時作 成。而且，基體材料中含的氧化链量、富銘紅柱石量及雜 質量通過適當混合上述（a )〜（e )原料進行調整。比較 例4、5的基體材料，除了以上述（c ) 、 （ d ) 、 （ e )為 原料外，與實施例卜3相同方式製作。根據實施例4〜9和比 較例4、5對抗裂性和抗彎曲性的評價結果在表2中示出。Page 14 543051 V. Description of the invention (12) (Evaluation) It can be known from 1 that the total amount of impurities accounts for more than 2.5% by mass, and the main impurities are iron oxide (Fe2 03), sodium oxide (Na20) and oxidation_ (K20) The cordierite base material, which accounts for more than 2% by mass, has no cracks below 800 ° C and good crack resistance, but the bending amount is greater than 1.0 cm (mm), indicating that the bending resistance is insufficient. The total amount of impurities accounts for less than 2.5% by mass, and iron oxide (Fe2 03), sodium oxide (Na20), and potassium oxide (K20) as the main impurities account for less than 2% by mass of the cordierite matrix material. As a result, the crack resistance and Bend resistance is very good. Furthermore, in Examples 1 to 3 and Comparative Examples 1 to 3, results were obtained in which cracks did not occur even at 100 trc. (Examples 4 to 9 and Comparative Examples 4 and 5) Examples 4 to 9 and Comparative Examples 4 and 5 were the same as Examples 1 to 3, and the base material of the firing jig according to the present invention was evaluated. The base materials of Examples 4 to 9 were prepared as follows: ... using the cordierite (a), (b) and (c), (d), (e) as raw materials, and (c) the maximum particle diameter was Electrolytic fusion oxide (d) with a maximum particle diameter of 250 micrometers (// m) and 44 micrometers (/ m) and a maximum diameter of 150 micrometers (/ m) and 44 micrometers (/ m) The mullite (e) sintered alumina having an average particle diameter of 3 micrometers (/ m) was used as a raw material, molded into the same shape as in Examples 1 to 3, and fired at 1,450 ° C for 5 hours to prepare. In addition, the amount of oxidized chains, the amount of fuming andalusite, and the amount of impurities contained in the base material are adjusted by appropriately mixing the above-mentioned (a) to (e) raw materials. The base materials of Comparative Examples 4 and 5 were produced in the same manner as in Example 3 except that (c), (d), and (e) were used as raw materials. The evaluation results of crack resistance and bending resistance according to Examples 4 to 9 and Comparative Examples 4 and 5 are shown in Table 2.

第15頁 543051 五、發明說明（13) 抗裂性和抗彎曲性的評價是 成 完 式 方 同 相 3 - I·*- 例 施 實 與 以 的表 Ο ο ο ο ο ο 0 ◎ ◎◎◎οο◎Page 15 543051 V. Description of the invention (13) The evaluation of crack resistance and bending resistance is completed in the same phase 3-I · *-Examples of implementation and table 〇 ο ο ο ο ο 0 ◎ ◎◎◎ οο ◎

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Lo羣鎰Ή H势鎰^ ((5^0霸^_<* M3〇5i 五、發明說明（14) (評價） 且作：表2所示，可以知道雜質總量占質量2 π 作為主要雜質的氧化鐵（Fe : · 5%以下， 化卸U20)占質量2%以下的堇匕2化納（Na2〇) f ； ，, , f , , , , ί ； ς柱石構成的基體材料雖然抗 虱化鋁和富 就發生裂缝，因此可以知道抗；子，是在_ (貧施例1〇〜19，比較例6〜δ)、抗衣性不夠。 通過實施例1 〇〜丨9，比較 丨夹3具广亍評價。實施例10,以及比較發明的燒成 離子體喷鍍法或者嘖舍、、^表面上，通過水穩定化耸J 燒成夹具。中間成中.間層、然後形成表声制寺 中間層水穩定ί = 3厚均為100微米（-Π)。 试米（㈣)〜15。微米（J ^鑛=的材料使用粒度為75 f ’膜壓通過噴鍍:欠數^二乳化鋁和電融富鋁紅柱 ::用易燒結氧化 二整。而且’中間層的噴塗材 45链米（^)以下的带s /未（㈣）以下的電融氧化鋁及 時。 包融§鋁紅桎石，在HOO它下燒5小 表層水穩定化〜 (VnO〜150微米（以夸離子體喷鍍的材料使用粒度為75微米 壓通過喷鏡:欠數^2,電融三氧化二紀穩定化氧化錯，膜 锨米（// m )以下的^订^周整。而且，表層的噴塗材料使用4 4 燒5小時。 氣化_纪穩定化氧化鍅，在1 4⑽。c下Lo group 镒 Ή H potential 镒 ((5 ^ 0 霸 ^ _ < * M3〇5i V. Description of the invention (14) (evaluation)) As shown in Table 2, we can know that the total amount of impurities accounts for 2 π as the main Impurity of iron oxide (Fe: · 5% or less, U20) accounts for 2% or less of mass (Na2〇) f;,,,, f,,,, ί Anti-lice aluminum and rich cracks occur, so you can know the resistance; sub, is in _ (lean Example 10 ~ 19, Comparative Examples 6 ~ δ), insufficient clothing resistance. According to Example 1 〇 ～ 丨 9, Comparison 丨 3 extensive evaluations. Example 10, and the comparatively invented sintered plasma spraying method or sintering, sintering fixtures on the surface with water to stabilize the J sintering jig. Middle to middle. Interlayer, Then form the middle layer of the surface-acoustic temple with water stable = 3 thick and 100 microns (-Π). Test meters (㈣) ~ 15. Micron (J ore = material using a particle size of 75 f 'film pressure through spray coating : Under number ^ Emulsified aluminum and fused aluminum-rich red pillars ::: Easily sintered and oxidized oxidized. Also, the spraying material of the intermediate layer is 45 chain meters (^) or less, and the electrofusion oxidation is less than or equal to (s). Aluminum in time Encapsulated § alumina vermiculite, burned under HOO for 5 small surface water stabilization ~ (VnO ~ 150 μm (with a particle size of 75 μm sprayed with quart ion plasma through a spray lens: less than ^ 2, electric The second-order stabilized oxidized trioxide is oxidized, and the film thickness is less than 锨 meters (// m). Moreover, the surface spraying material is burned for 5 hours using 4 4. 4⑽.c

第17頁 543051 、發明說明（15) 么 在貝％例1 2〜1 5中，中間層的材料使用氧化鋁和富鋁 1柱石的混合物。所述混合在中間層使用喷鍍法的實施例 ^ 5中，把粒度為1 5 0微米（# m )〜7 5微米（v m)的氧化鋁 ϋ富鋁紅柱石在振動混合機上混合5分鐘完成。而且，在 ’層使用噴塗法的實施例i 2、1 3 +，把粒度為4 5微米 α以下的晏鋁紅柱石粉末、易燒結氧化鋁、以及粒度 合。微米（//Π〇以下的電融氧化鋁適當調和，在製漿時混 物。:的中間層材料使用氧化銘和氧化錯的共晶 微二利用氧化㈣化鍅以1 ]比例混合，是細 1又、'、口日日的混合組織物質。 根據實施例1 0〜丨9和比較例6〜8對抗 的評價結果在表3中示出。抗剝離性的^價^和抗反綠 進仃，即在製作的燒成夾具上塗抹作 °下方工、 =，在、2小時條件下反復在小$型電貝溶 =疋直到發生中間層或表層從基盈、凡 表3中，不滿3次時發生剝離的為x 上^離時的次數。 範圍内發生制離的為△’從5次開始 \始至不滿5次 為〇 :到8次沒有發生剝離的為◎。侧-人發生剝離的 抗反應性的評價通過與抗剝離性 然後在不加埶护 a > + U豫方式反復燒成， 表3中，撓曲旦It Γ 1㈣前㈣的挽曲量。 於1釐米(_)2Γ 的為x，小於2釐米(_)大 ^ π 的為△，小於1釐米（mm)大於0.5釐丨& 為〇，小於〇· 5釐米（_)的為◎。 未（_)的P.17 543051, description of the invention (15) In Example 1 2 to 15, the material of the intermediate layer is a mixture of alumina and alumina-rich pillared stone. In Example ^ 5 in which the spraying method was used for the intermediate layer, alumina and mullite with a particle size of 150 micrometers (#m) to 75 micrometers (vm) were mixed on a vibration mixer. Minutes to complete. Furthermore, Example i 2, 1 3 + using a spraying method was used for the layer, and a mullite powder having a particle size of 45 μm or less, an easily sintered alumina, and a particle size were combined. Micron (// ΠΠ fused aluminum oxide is properly blended and mixed during pulping .: The intermediate layer material is made of oxidized oxide and oxidized eutectic microsecondary oxide, and mixed with osmium oxide at a ratio of 1]. It is a mixed tissue material that is fine, thin, and fine. The evaluation results of confrontation according to Examples 1 to 9 and Comparative Examples 6 to 8 are shown in Table 3. The peel resistance and the anti-green resistance are shown in Table 3. Into the sintering jig, apply it to the bottom of the firing jig, and then repeatedly dissolve it in the small $ type electric shell under the condition of 2 hours until the intermediate layer or surface layer occurs from the base surplus, where in Table 3, The number of occurrences of peeling when less than 3 times is the number of times when x is separated. The number of occurrences of peeling within the range is Δ ', starting from 5 times, starting from 5 times and less than 5 times: 0: 8 times without peeling is ◎. Side- The anti-peeling resistance of humans was evaluated by repeated firing with anti-peeling resistance and then without a protection method> Table 3. In Table 3, the deflection amount of the deflection dendrite It Γ 1㈣ before ㈣. Centimeter (_) 2Γ is x, less than 2 cm (_) large ^ π is △, less than 1 cm (mm) is greater than 0.5 centimeter 丨 & is 0, less than 0.5 cm ( _) Is ◎. Not (_)

543051543051

抗反應性 〇 〇 〇 〇 〇 〇 〇 〇 ◎ 〇 〇 &lt;] &lt;1 fWtA 破 ) \ 1 ^ S' 〇 〇 〇 〇 Ο 〇 〇 〇 ◎ 〇 &lt;1 X X 表層 施工方法 ί _1 噴鍍 噴鍍 噴鍍 噴鍍 噴鍍 噴鍍 &lt;H^ 督 噴塗 噴鍍 i嘖鍍 1噴鍍 噴鈹 材料 氧化鉻 氧化鉻 氧化鉻 氧化鉻i 氧化锆 氧化鉻 氧化锆 氧化锆 氧化錯 氧化鉻 氧化銷 氧化鉻 氧化锆 中間層 —._ .. _ί 施工方法 噴塗 噴塗i 噴塗 1 噴塗 噴鍍 噴鍍 噴塗 噴鍍 噴鍍 噴鍍 噴塗 噴塗 噴塗 材料 1 i 氧化鋁 | 氧化鋁 氧化鋁（50%)+富鋁紅柱石(50%) | 氧化鋁（15%) +富鋁紅柱石(85%) 氧化鋁(50%) +富鋁紅柱石(50%) 氧化鋁（15%) +富鋁紅柱石(85%) 氧化鋁 氧化鋁 氧化鋁 i 氧化鋁和氧化锆的共晶體 氧化鋁 氧化鋁 氧化鋁 基 體 材料 雜 質（% ) 合計1 CO CSI CSI r—ί 卜 〇 卜 〇 卜 〇 卜 〇 卜 d 卜 〇 卜 CD 卜 〇 〇 CO 〇 00 LO 其他 卜 d 寸 〇 CO 〇 00 〇 CO 〇 〇〇 〇 CO ο 〇〇 〇 CO Ο CO 〇 05 〇 r—( r—ί 卜 1 A*+B* ① T—Η 00 〇 寸 Ο 寸 C? 寸 〇 寸 〇 寸 ο 寸 〇 寸 ο 寸 d Γ—Η ⑦ cn〇 τ—&lt; 寸 卜 〇 寸 〇 CO 〇 00 〇 CO d 〇〇 ό CO d CO ό 〇0 ο co ο ⑦ d ο t ^ 寸 r— d 寸 〇 Τ—1 〇 T &quot;1 〇 1—1 〇 〇 11 〇 1—^ 〇 τ—^ Ο r—^ Ο CM T—&lt; 1 卜 Csl 材料 堇青石I 堇青石 堇青石 堇青石 |堇青石I 堇青石 L堇青石 堇青石| 堇青石 堇青石 堇青石 堇青石 堇青石 實施例1〇 實施例11 賨施例12 實施例13 j 實施例14 實施例15 實施例16 實施例17 實施例18 實施例19 比較例6 比較例7 |比較例8 1 coCDtx) so ffi劍 Md ” 剡ff(:tH) (3)&amp;^M+ (O^N)rEs}嫲 #Anti-reactivity 〇〇〇〇〇〇〇〇〇〇 ◎ 〇〇 &lt;] &lt; 1 fWtA broken) \ 1 ^ S '〇〇〇〇〇〇〇〇〇〇 ◎ 〇 &lt; 1 XX surface layer construction method Plating Spray Plating Sputtering Plating &lt; H ^ Spraying Plating I Plating 1 Plating Plating Beryllium Material Chromium Oxide Chromium Oxide Chromium Oxide Chromium Oxide Chromium zirconia intermediate layer —._ .. _ί Construction method Spraying spraying i Spraying 1 Spraying spraying spraying Spraying spraying spraying Spraying spraying spraying material 1 i Alumina | Alumina Alumina (50%) + Al-rich Andalusite (50%) | Alumina (15%) + mullite (85%) Alumina (50%) + mullite (50%) Alumina (15%) + mullite (85 %) Alumina alumina alumina i Alumina and zirconia eutectic alumina alumina alumina matrix material impurities (%) Total 1 CO CSI CSI r— ί 〇〇〇〇〇〇〇 〇 〇 CD 〇〇〇CO 〇00 LO Other d 〇CO 〇00 〇CO 〇〇〇〇 CO ο 〇〇〇〇CO 〇 CO 〇05 〇r— (r—ί bu 1 A * + B * ① T—Η 00 〇 inch 0 inch C? Inch 〇 inch 0 inch ο inch 0 inch ο inch d Γ—Η ⑦ cn〇τ— &lt; inch 〇〇 〇CO 〇00 〇CO d 〇〇ό CO d CO ό 〇0 ο co ο ⑦ d ο t ^ inch r— d inch 〇－1 〇T &quot; 1 〇 1-1 〇〇11 〇1— ^ 〇τ— ^ 〇 r— ^ 〇 CM T— <1 Bu Csl material cordierite I cordierite cordierite cordierite | cordierite I cordierite L cordierite cordierite | cordierite Bluestone Cordierite Cordierite Cordierite Cordierite Cordierite Example 10 Example 11 Example 12 Example 13 j Example 14 Example 15 Example 16 Example 17 Example 18 Example 19 Comparative Example 6 Comparative Example 7 | Comparison Example 8 1 coCDtx) so ffi sword Md ”剡 ff (: tH) (3) &amp; ^ M + (O ^ N) rEs} 嫲 #

543051 五、發明說明（17) (評價） 如表3所示，可以知道使用雜質總量占質量2 t Γ且作為主要雜質的氧化鐵（FeA )、氧化 (NaJ )及氧化鉀（1〇 )占質量2%以上的堇青石 的，成失具，抗剝離性和抗反應性都不夠，:別 質量多時，結果基體材料與中間層的 使用雜質總量占質量2.5%以下，= 氧化鐵（Fe2〇3 )、氧化鈉（Na2〇 ) ’( 2%以下的堇青石基體材料的燒成失具乳彳 反應性都良好，中間層分別使用氣化鋁、：：鋁 柱石的混合物以及氧化鋁和氧化锆 s _ 等離子體喷鑛法或者嘴塗法形成，心3 = 過水穩定化等離子體噴链法或者嘴 使用 後好的性能。特別是，在表層通過二‘ 1 = 抗剝離性和抗反應性獲得優良結果。、=f形成的 成的層與通過水穩定化等離子體噴，通過 2的細小氣孔，這種氣孔能夠吸層 ^表面上看通過喷塗法形成的表層 ^脹， (實施例20〜25，比較例9、丨〇 ) 、、、恥脹小的 通過實施例20〜25，比較例9、1〇， 行評價。實施例2〇,是在與實施 :作的基體材料的表面上，以氧化鋁為原料 成中間層，然後以氧化錯為原料通過水穩定化 鍍法形成表層，製成燒成夾具。中間層和表声的 • 5%以 鋼 基體材料 是如果雜 生剝離。 要雜質的 )占質量 離性和抗 和富銘紅 水穩定化 氧化錯通 能夠發揮 情況下， 噴塗法形 比較含有 因此認為 原因。 發明的燒 相同方式 喷塗法形 離子體噴 形成與實543051 V. Description of the invention (17) (Evaluation) As shown in Table 3, it can be known that iron oxide (FeA), oxidation (NaJ), and potassium oxide (10), which are the main impurities, occupying 2 t Γ of the total amount of impurities, are used as the main impurities. Cordierite, which accounts for more than 2% of the mass, has insufficient forming resistance, insufficient peel resistance and resistance to reaction. When the mass is different, the total amount of impurities used in the base material and the intermediate layer accounts for less than 2.5% of the mass, = iron oxide (Fe2O3), sodium oxide (Na2O) '(less than 2% of cordierite base material has good sintering reactivity after firing, and the intermediate layer uses gasified aluminum, a mixture of betalite, and oxidation Aluminum and zirconium oxide s _ formed by plasma blasting method or nozzle coating method, core 3 = water-stabilized plasma spray chain method or nozzle with good performance after use. In particular, the surface layer passes two '1 = peel resistance Excellent results were obtained with anti-reaction. The layer formed by f and sprayed with water-stabilized plasma passed through 2 small pores. Such pores can absorb the layer. ^ The surface layer formed by spraying method is swelled on the surface. (Examples 20 to 25, Comparative Examples 9, 丨 〇) The small swelling was evaluated according to Examples 20 to 25, Comparative Examples 9, and 10. Example 20 is an intermediate layer made of alumina as a raw material on the surface of the substrate material used in the implementation. Then, the surface layer is formed by the water-stabilizing plating method using oxidation error as a raw material, and the firing jig is made. The intermediate layer and the surface sound • 5% of the steel base material is mixed if it is peeled off. The impurities) account for mass separation and In the case that anti-fuming red water stabilizing oxidation misconnection can be exerted, the spray method is more likely to contain the reason. Invention of the same way, spray method, plasma spray, formation and implementation

第20頁 543051 五、發明說明（18) 施例1 0〜1 9相同方式完成。比較例9、1 0是在與實施例4、5 相同方式製作的基體材料的表面上，通過與實施例2 0〜2 5 相同方式形成中間層和表層，製成燒成夾具。中間層和表 層的膜厚均為1 0 0微米（// m)。根據實施例2 0〜2 5以及比較 例9、1 0對抗剝離性和抗反應性的評價結果在表4中示出。 抗剝離性和抗反應性的評價以與實施例1 0〜1 9同樣方式進 行。Page 20 543051 V. Description of the invention (18) Examples 10 to 19 are completed in the same manner. In Comparative Examples 9 and 10, an intermediate layer and a surface layer were formed on the surface of the base material produced in the same manner as in Examples 4 and 5 to form a firing jig in the same manner as in Examples 2 to 25. The film thickness of the intermediate layer and the surface layer is 100 micrometers (// m). Table 4 shows the evaluation results of anti-peeling and anti-reaction properties according to Examples 20 to 25 and Comparative Examples 9 and 10. Evaluation of peel resistance and reaction resistance was performed in the same manner as in Examples 10 to 19.

第21頁 543051 五、發明說明（19) 表4Page 21 543051 V. Description of the invention (19) Table 4

抗反 應性 〇◎◎〇〇〇 ◎〇 抗剝 離性 〇◎◎◎◎◎ ◎ ◎ 腫5 懈 施工方法 鑕鑛鑛鸛鑕鑕 噴鍍 噴鍍 義 ^R -ϋΠΙ -ijn φ -^Ό. -ϋΐΐ &lt;m &lt;m &lt;m &lt;m &lt;m &lt;m 碱碱碱_ _减 氧化锆 氧化鉻 中間層 施工方法 剡剡鐦剡剡剡 噴塗 噴塗 1 5g SS SS §g Si gg 减减Jpf减腻减 氧化鋁 氧化鋁 雜質量(%) ϊίϊπ LO CD 卜 LO 运 00 O O C? 〇 ^ 〇 00 00 Ο 〇 &amp; 0. 3 0. 35 0. 4 0. 3 0. 35 0· 4 CO CO ο 〇 * 0. 2 0. 25 0. 3 0· 2 0. 3 0· 4 LO ΙΩ ο Ο 基體材來 義 &gt;^N 〇〇〇〇〇〇 r-H CO LO r—( 〇〇 LO Vw/ QD QQ an na QD QD &lt;m &lt;na &lt;na &lt;hs ^ ^ ^ ^ ^ ^ 喊减臧碱M喊 + + + + + + 屯K1啐啐啐啐 Dm: Hi: 歉 |r |r 細铺細械4λ!ι1 ·ώϋ 侧側侧侧侧侧 /*~Ν /-~Ν ο ο οο &lt;R Φ 链资 c5 c5 .iN (Ν γ-Η γ-Η &lt; &lt; •fee □π an &lt;m &lt;m |nffi |nffi έ A u u 賨施例20 實施例21 實施例22 賨施例23 實施例24 實施例25 比較例9 比較例10 S-班剡»”剡»(坊) (3)&amp;^碱+ (0#)¥&gt;«:? (0^0癱沒祕&lt;* 第22頁 543051 五、發明說明（20) (評價） 如表4所示，可以知道 :，而且作為主要雜質的氧化鐵';二〇量占f量2. 5%以 及氧化鉀（κ2〇)占質量2 2 3 )、氧化鈉 置5 0«/„以上的基體材料的燒成夾的董青石含量為質 結果都良好。在使用氧化鋁和富鋁έ二Η離性和抗反應性 的燒成夾具中，同樣抗剝離性二上石構成的基體材料 是’如同表2所示一 #， 几^性結果都良好。可 點。 材枓存在抗裂性不夠的缺 (實施例26〜29，比較例u、丨2) 實施例26、27以及比較例u 式製作的基體材料的表面上，使用f =貫施例卜3相同方 過水穩定化等離子體喷鑛法或者噴=5所示的材料，通 ’然後以氧化錯為原料通過水^ =成2層的中間層 喷塗法形成表|，製成燒成夹：：離子體喷鍍法或者 施例4〜9相同方式製作的基體材料的面例^、29與是在實 示的材料，通過與實施例26、27相1 ’使用如表5所 層，製成燒成夾具。比較例！ 2是在斑比^ =成中一間層和表 作的基體材料的表面上，使用如^、 乂例4相同方式製 ^。 成中間層和表層’製成燒成夾 而且，中間層通過水穩定化等離子 ，是在第一層喷鍍完成後直接換成第二;的二料2層 的表面上喷銀形成。另外，中間層通過；【：層Anti-reaction 〇 ◎ ◎ 〇〇〇 ◎ 〇 Peeling resistance ◎ ◎ ◎ ◎ ◎ ◎ swollen 5 施工 swollen construction method 锧 ore mine stork 锧 锧 spray coating spraying meaning ^ R -ϋΠΙ -ijn φ-^ Ό.- ϋΐΐ &lt; m &lt; m &lt; m &lt; m &lt; m &lt; m &lt; m &lt; m alkali alkali alkali _ _ minus zirconia chromium oxide intermediate layer construction method 剡 剡 鐦 剡 剡 剡 spray spray 1 5g SS SS §g Si gg minus Decrease Jpf Decrease Alumina Alumina Impurity (%) ϊίϊπ LO CD 卜 LO 运 00 OOC? 〇 ^ 〇00 00 〇 〇 & 0. 3 0. 35 0. 4 0. 3 0. 35 0 · 4 CO CO ο 〇 * 0. 2 0. 25 0. 3 0 · 2 0. 3 0 · 4 LO ΙΩ ο 〇 Base material meaning &gt; ^ N 〇〇〇〇〇〇〇rH CO LO r— (〇〇LO Vw / QD QQ an na QD QD &lt; m &lt; na &lt; na &lt; hs ^ ^ ^ ^ ^ ^ ^ Minus Zang alkali M shout + + + + + + Tun K1 啐 啐 啐 啐 Dm: Hi: sorry | r | r Fine shop 4λ! ι1 · FREE • fee □ π an &lt; m &lt; m | nffi | nffi A A uu Example 20 Example 21 Example 22 Example 23 Example 24 Example 25 Comparative Example 9 Comparison Example 10 S-Ban »» 剡 »(Fang) (3) & ^ alkali + (0 #) ¥ &gt;«:? (0 ^ 0 paralysis mystery &lt; * page 22 543051 V. Description of the invention ( 20) (Evaluation) As shown in Table 4, it can be known that: and iron oxide 'as the main impurity; the amount of 20 accounts for 2.5% of the amount of f and potassium oxide (κ2〇) accounts for the mass of 2 2 3), sodium oxide The cyanite content of the firing clip of the base material set above 50 «/„ is qualitatively good. In the firing jig using alumina and aluminum-rich diisocyanate and reaction resistance, the same peel resistance The base material made of Nisangite is' ## shown in Table 2. The results are good. It is acceptable. There is a lack of crack resistance in materials (Examples 26 to 29, Comparative Examples u, 2) On the surfaces of the substrate materials prepared in the methods of Examples 26 and 27 and Comparative Example u, the materials shown in f = the same way as in Example 3, the water-stabilized plasma blasting method, or the materials shown in FIG. 5 were used. Oxidation error is used as a raw material to form a table by water ^ = 2 layers of intermediate layer spraying method, and made into a firing clip :: surface examples of the base material produced in the same manner as in the ion spraying method or Examples 4 to 9 ^, 29 with yes Solid material is shown, as in Example 1 with 26 and 27 'as shown in Table 5 using the layer made of the firing jig. Comparative example! 2 is made on the surface of the base material of the spot ratio ^ = intermediate layer and the surface, using ^, 乂 Example 4 to make ^. The intermediate layer and the surface layer are made into a firing clip. Furthermore, the intermediate layer is formed by spraying silver on the surface of the second layer and the second layer directly after the first layer spraying is completed by water-stabilized plasma. In addition, the middle layer passes; [: layer

第23頁 543051 五、發明說明（21) 層，在第一層喷塗完成後，在8 0 °C下乾燥5小時去掉噴塗 層的水分，然後在第一層的表面上喷塗第二層的材料，燒 成第二層的表面。 又表層的形成與實施例1 0〜1 9相同方式完成。第一個 中間層的膜厚為5 0微米（// m )，第二個中間層的膜厚為1 0 0 微米（// m )，表層的膜厚為1 0 0微米（v m )。根據實施例 2 6〜2 9以及比較例1 1、1 2，評價抗剝離性、抗反應性的結 果在表5中示出。抗剝離性、抗反應性的評價以與實施例 1 0〜1 9同樣方式進行。Page 23, 543051 V. Description of the invention (21) After the first layer is sprayed, dry it at 80 ° C for 5 hours to remove the moisture from the sprayed layer, and then spray the second layer on the surface of the first layer The material is fired to the surface of the second layer. The formation of the surface layer was completed in the same manner as in Examples 10 to 19. The film thickness of the first intermediate layer is 50 micrometers (// m), the film thickness of the second intermediate layer is 100 micrometers (/ m), and the film thickness of the surface layer is 100 micrometers (vm). Table 5 shows the results of evaluating peel resistance and reaction resistance based on Examples 2 6 to 29 and Comparative Examples 1 and 12. Evaluation of peel resistance and reaction resistance was performed in the same manner as in Examples 10 to 19.

第24頁 543051 五、發明說明（22) ，價 評Page 24 543051 V. Description of the Invention (22)

1¾劫 〇 〇 ◎ 〇 &lt;3 ◎ &quot;Z=T&gt; rl-1_] ◎ 〇 ◎ ◎ X ◎ 剡 鑛 -0¾ 德 Η 響 # 螫 15 &lt;m 七11 &lt;m 材料 ¥ Ιί Μ , 〇 Ο 〇 L〇 Τ-Η 〇 Ο 〇 LO T—( Ο 〇 LO Τ-Η 〇 ο 〇 LO T-—( 〇 Ο 〇 LO r-H 〇 Ο 〇 LO 11 剡剡 镖鑲 鑛镲 鑲镖 镖镖 鑛鑛 1! 1¾ H S? 15 1 紙 铝 ^ SS ^ SS 运55 运58 •fe- §s §8^ SS安 SS这 |π田喊 徊扭勝 _减 {IDE U inffi减 |π扭减 3 LO _ * 寸 d 〇 CD 〇 〇 CD CO 00 〇 /-N /*N Ο 〇 基體材料 材料 氧化鋁（30% CO 4ϋ •fee SS 00 &lt;R η rH _ _ + 加扭 + 伽： _ Ο 卜 Ο SS !&gt;· 加扭 #Γ CQ &lt;H^ _ 舾 _ Ιί ① CNJ 00 CM Oi Cvl τ-Η r-H C\! 累 羣 羣 累 S 魏 舾 舰 AJ (,n 嫉&amp;,1 紙),SE-fr*iissi sc«_»”剡So (¾) 第25頁 543051 五、發明說明（23) 如表5所示，可以知道使用雜質總量占質量2. 5 %以 下，而且作為主要雜質的氧化鐵（Fe2 03 )、氧化鈉 (Na20 )及氧化鉀（K20 )占質量2%以下的堇青石基體材 料、中間層形成為兩層的燒成夾具，抗剝離性和抗反應性 結果都良好。中間層分別使用氧化鋁、富鋁紅柱石通過水 穩定化等離子體噴鍍法或者喷塗法形成，而且表層使用氧 化錯通過水穩定化等離子體喷鍍法或者喷塗法形成，也能 夠發揮很好的性能。 使用雜質總量占質量2. 5%以下，而且作為主要雜質的 氧化鐵（Fe203 )、氧化鈉（Na20 )及氧化鉀（Κ20 )占質量 2%以下的堇青石含量占質量50%以上的基體材料、中間層 - 形成為兩層的燒成夾具，同樣抗剝離性和抗反應性結果都 良好。 - 可以知道使用雜質總量占質量2. 5 %以上，而且作為主 要雜質的氧化鐵（Fe2 03 )、氧化鈉（Na20 )及氧化鉀 (K20 )占質量2%以上的堇青石基體材料、中間層形成為 兩層的燒成夾具，抗剝離性和抗反應性結果都不夠好。在 雜質總量占質量2. 5%以上，而且作為主要雜質的氧化鐵 (Fe2 03 )、氧化鈉（Na20 )及氧化鉀（K20 )占質量2%以上 · 情況下、即使中間層形成為兩層，也不能獲得良好特性。 而且，使用氧化I呂和富銘紅柱石構成的基體材料、中間層 形成為兩層的燒成夾具，抗剝離性和抗反應性結果都良好 。但是，如表2所示，這種基體材料存在抗裂性不夠的缺 點。1¾ 劫 〇〇 ◎ 〇 &lt; 3 ◎ &quot; Z = T &gt; rl-1_] ◎ 〇 ◎ ◎ X ◎ 剡 -0-0¾ 德 Η 响 # 螫 15 &lt; m VII 11 &lt; m materials ¥ Ιί Μ, 〇 〇 〇L〇Τ-Η 〇〇 〇LO T— (〇 〇LO Τ-Η 〇ο 〇LO T -— (〇〇 〇LO rH 〇〇 〇LO 11 1! 1¾ HS? 15 1 Paper aluminum ^ SS ^ SS Win 55 Win 58 • fe- §s §8 ^ SSAnn SSThis | π 田 called to win _ minus {IDE U inffi minus | π minus 3 LO _ * Inch d 〇CD 〇〇CD CO 00 〇 / -N / * N 〇 〇 Matrix material alumina (30% CO 4ϋ • fee SS 00 &lt; R η rH _ _ + twist + Gamma: _ Ο Ο 〇 SS! &## Twist # Γ CQ &lt; H ^ _ 舾 _ Ιί ① CNJ 00 CM Oi Cvl τ-Η rH C \! Swarm group S S Wei Weijian AJ (, n &&amp;, 1 paper) , SE-fr * iissi sc «_» "剡 So (¾) Page 25 543051 V. Description of the invention (23) As shown in 5, it can be known that the total amount of impurities used is less than 2.5% by mass, and the iron oxide (Fe2 03), sodium oxide (Na20), and potassium oxide (K20) as the main impurities account for less than 2% by mass of the cordierite matrix. The material and the intermediate layer are formed into a two-layer firing jig, and the results of peel resistance and reaction resistance are good. The intermediate layer is formed by using alumina and mullite by water-stabilized plasma spraying method or spraying method, respectively. Moreover, the surface layer is formed by water-stabilized plasma spraying method or spraying method using oxidation faults, and can also perform very well. The total amount of impurities used is less than 2.5%, and iron oxide (Fe203) is used as the main impurity. , Sodium oxide (Na20) and potassium oxide (K20) account for less than 2% by mass of the cordierite content and more than 50% by mass of the base material, the intermediate layer-formed into a two-layer firing jig, the same peel resistance and reaction resistance The results are all good. -It can be known that the total amount of impurities used is more than 2.5%, and the iron oxide (Fe2 03), sodium oxide (Na20), and potassium oxide (K20), which are the main impurities, account for more than 2% of the mass of the cordierite base material, the intermediate The layers were formed into a two-layer firing jig, and the peel resistance and reaction resistance results were not good enough. When the total amount of impurities accounts for more than 2.5% by mass, and iron oxide (Fe2 03), sodium oxide (Na20), and potassium oxide (K20) as the main impurities account for more than 2% by mass, even if the intermediate layer is formed as two Layer, nor can it obtain good characteristics. In addition, using a base material composed of oxide I and Fuming andalusite and an intermediate layer formed into a two-layer firing jig, both the peel resistance and the reaction resistance were good. However, as shown in Table 2, this base material has a drawback that the crack resistance is insufficient.

第26頁 543051Page 543 051

第27頁 543051 圖式簡單說明Page 543051 Illustration

第28頁Page 28

Claims (1)

543051 六、申請專利範圍 1. 一種用於電子元件的燒成夾具，用於把由陶瓷構成的 被燒成體裝載在上面，燒成該被燒成體製作電子元件，其 特徵在於： 由含有堇青石、或者堇青石和氧化銘和/或富銘紅柱 石的基體材料、至少為1層的中間層、和與上述被燒成體 反應性低的材料形成的表層構成。 2. 根據申請專利範圍第1項所述的用於電子元件的燒成夾 具，其特徵在於由含有雜質量占質量2. 5%以下的堇青石、 或者雜質量占質量2 · 5 %以下的堇青石和氧化銘和/或富銘 紅柱石的基體材料、至少為1層的中間層、和與上述被燒 成體反應性低的材料形成的表層組成。 3. 根據申請專利範圍第1或2項所述的用於電子元件的燒 成夾具，其特徵在於上述雜質中含有氧化鐵（Fe203 )，上 述堇青石中含有的氧化鐵（Fe203)量占質量1%以下。 4. 根據申請專利範圍第1或2項所述的用於電子元件的燒 成夾具，其特徵在於上述雜質含有氧化鐵（Fe2 03 )、氧化 鈉（Na20 )及氧化鉀（K20 )，上述堇青石中含有的氧化鐵 Fe〇〇f 氧化納（N a; 及氧化鉀（K20 )量占質量2%以 下 5.根據申請專利範圍第1或2項所述的用於電子元件的燒543051 VI. Application for patent scope 1. A firing jig for electronic components, for loading a fired body made of ceramics on it, and firing the fired body to make electronic components, characterized in that: The base material of cordierite, or cordierite, and oxidized and / or fuming andalusite, at least one intermediate layer, and a surface layer formed of a material having low reactivity with the fired body. 2. The firing jig for electronic components according to item 1 of the scope of the patent application, which is characterized by containing cordierite with an impurity amount of 2.5% or less, or an impurity amount of 2.5.5% or less. The base material of cordierite and oxidized and / or fused andalusite is composed of at least one intermediate layer and a surface layer formed of a material having low reactivity with the fired body. 3. The firing jig for electronic components according to item 1 or 2 of the scope of patent application, characterized in that the impurities contain iron oxide (Fe203), and the amount of iron oxide (Fe203) contained in the cordierite accounts for mass Less than 1%. 4. The firing jig for electronic components according to item 1 or 2 of the scope of the patent application, characterized in that the impurity contains iron oxide (Fe2 03), sodium oxide (Na20) and potassium oxide (K20), and the cord The amount of iron oxide FeO〇f sodium oxide (Na) and potassium oxide (K20) contained in the bluestone is 2% by mass or less. 5. The firing of electronic components according to item 1 or 2 of the scope of patent application. 第29頁 543051 六、申請專利範圍 成夾具，其特徵在於上述基體材料含有的上述堇青石占質 量5 0 %以上。 6. 根據申請專利範圍第1或2項所述的用於電子元件的燒 成夾具，其特徵在於上述中間層含有選自氧化銘、富銘紅 柱石、氧化銘和氧化結的共晶物、及氧化紹和富銘紅柱石 的混合物所構成的組中的一種以上，上述表層含有氧化 錯。 7. 根據申請專利範圍第1或2項所述的用於電子元件的燒 成夾具，其特徵在於上述中間層通過喷鍍法或者喷塗法形 成，上述表層通過喷鍍法或者喷塗法形成。 8. 根據申請專利範圍第7項所述的用於電子元件的燒成夾 具，其特徵在於上述喷鍍法是水穩定化等離子體喷鍍法。Page 29 543051 6. Scope of patent application The fixture is characterized in that the above-mentioned cordierite contained in the above-mentioned base material accounts for more than 50% of the mass. 6. The firing jig for electronic components according to item 1 or 2 of the scope of the patent application, wherein the intermediate layer contains a eutectic material selected from the group consisting of oxide oxide, Fuming andalusite, oxide oxide and oxide junction, And one or more of the group consisting of a mixture of oxide shao and Fuming andalusite, and the surface layer contains oxidation faults. 7. The firing jig for electronic components according to item 1 or 2 of the scope of the patent application, wherein the intermediate layer is formed by a spraying method or a spraying method, and the surface layer is formed by a spraying method or a spraying method. . 8. The firing jig for an electronic component according to item 7 of the scope of the patent application, wherein the thermal spraying method is a water-stabilized plasma spraying method. 第30頁Page 30