200415335 玖、發明說明： 【發明所屬之技術領域】 本各明有關例如為了進行脫脂處理等之陶瓷成形品之熱 處理方法和熱處理裝置。 【先前技術】 在陶资電子零件等的陶瓷成形品製造程序為在陶瓷粉末 中+加有機黏結劑、有機增塑劑等，在賦予流動性的狀態 下成形之成形程序。因此，必須具有在成形後將不需要的 有機黏結劑在燒結等高溫處理前除去（脫脂）的程序。 進仃此類脫脂時，為了避免陶瓷成形品產生裂紋、氣泡 或表層剥離等的不良情況，重要的是應控制其脫脂速度。 般’此類脫脂有兩種方法：使有機黏結劑等燃燒進行 脫脂和使有機黏結劑等蒸發燃燒進行脫脂。 在使有機黏結劑等燃燒進行脫脂時，已知有下列兩項技 術·根據脫脂速度，爐内的一氧化破發生量和氧氣成分比 例會有變化，按照爐内一氧化破發生量的管理而對燃燒溫 度和燃燒環境氣體進行控制，進而控制脫脂速度（如：參照 專利文獻1);按照爐内燃燒所必需的氧氣成分比例的管 理’而對燃燒溫度和燃燒環境氣體進行控制，從而控制脫 脂速度（如：參照專利文獻2)。 (專利文獻1) 特開平7-76132號（全部頁、全部圖） (專利文獻2) 特開平3-230090號（全部頁、全部圖） H6837 200415335 但是’在上述脫脂速度控制中，脫脂處理的初期在爐内 變化為-氧化碳之前’有機成分已開始揮發，或者是：哕 揮發的有機成分生成諸如醋酸H乙料的中間產物: 但是對於一氧化碳還沒有檢測到’有時就判斷為尚未進行 脫脂。這時，4 了促進脫脂，有可能對爐内溫度進行控制， 2之上升到比該狀態下用於脫脂的適當溫度還要高的高 /皿。右進行此控帝J，則脫脂將急速進彳，使黏結劑和增塑 劑從陶€成形品中迅速消失’從而有可能導致在該成形品 上產生裂紋等不良情況。 Q此，即使疋單純有關揮發和蒸發的有機成分也要正確 地進行該檢測。 、本叙明鑒於上述貫際情況為解決上述課題，提供了陶瓷 成形品之熱處理方法和熱處理裝置，使之能對熱處理過程 中從陶走成形品中揮發的有機成分確切地檢測，可以對陶 瓷成形品進行正確的熱處理，從而能提高優等品率。 【發明内容】 (1)本發明之第1種陶瓷成形品之熱處理方法，其特徵為具 有下列程序·在熱處理爐内對陶瓷成形品進行熱處理過程 中取出上逑熱處理爐内的環境氣體作為試樣，將該試樣 中的碳成分轉化為特定碳化物之轉化程序；檢測該轉化後 的特定碳化物在上述試樣中的成分比例之成分比例檢測程 序。 試樣中的碳成分是指主要是試樣中所包含的有機成分等 中的碳成分。將試樣中的碳成分轉化為碳化物是指，構成 200415335 主要作為各種有機化合物存在於試樣中的有機成分的碳， 如經使该妓芫全燃燒的過程，從而使碳成分絕大部分都化 學性地轉化為僅以特定碳化物形式存在之狀態。 由於本發明可藉由將伴隨熱處理所產生的有機成分中的 蛟成分轉化為特定的碳化物，檢測該特定碳化物在試樣中 的成分比例，根據該成分比例的檢測結果，對於從陶瓷成 形品中揮發和蒸發的有機成分，以高正確性對其數量和揮 叙速度等進行換算，所以能高精度地掌握實際的有機成分 從陶瓷成形品中的脫離狀況。 (2)本發明之第2種陶瓷成形品之熱處理方法，其特徵為具 有下列程序··在熱處理爐内對陶瓷成形品進行熱處理過程 中，取出上述熱處理爐内的環境氣體作為試樣，將該試樣 中的碳成分轉化為特定碳化物之轉化程彳；和檢測該轉化 後的特定碳化物在上述試樣中的成分比例之成》比例檢測 程序；和根據該成分比例的檢測結果，對上述熱處理爐内 的熱處理進行控制之控制程序。 本發明可藉由將伴隨熱處理所產生的有機成分中的碳成 分轉化為料的碳化物，檢測該特定碳化物在試樣中的成 分比例，根據該成分比例的檢測結果，冑於從陶竞成形品 中揮發和蒸發的有機成分，以高正輕對其數量和揮發速 度等進仃換算’因而能高精度地掌握實際的有機成分從陶 瓷成形品中的脫離狀況，同時根據該實際的有機成分從陶 资成形品中的脫離狀況，可對陶资成形品進行適當的熱處 理控制。 86837 200415335 本發明之第1及第2種陶瓷成形品之熱處理方法，上述特 定的碳化物較好是二氧化碳，同時上述轉化程序較好係使 上逑試樣完全燃燒使該試樣中的碳成分轉化為二氧化碳之 程序。這時，根據試樣中所包含的二氧化碳濃度的檢測結 不，可實現熱處理爐内的環境氣體中所含揮發的有機成分 量的換算，從而可精確、方便地檢測從熱處理爐内的陶瓷 成形Ρϋ揮發出來的有機成分量和其揮發速度等。 本發明之第2種陶瓷成形品熱處理方法，較妤上述控制程 序之熱處理控制為溫度控制。這時，藉溫度控制，能精確 地控制有關從陶瓷成形品中有機成分的脫離情況。 、本發明之第2種陶资成形品熱處理方法，較好上述控制程 序I熱處理控制為環境氣體成分比例的控制。這時，藉由 對環境氣體成分比例的控制，能精確地控制有關從陶瓷成 形品中有機成分的脫離情況。 、本發明之第2種陶资成形品熱處理方法，較好上述控制程 序係根據上述碳化物成分比例的檢測結果，對上述熱處理 進行反饋控制’使之逐步達到規定的碳化物成分比例。這 時’關於從陶彻品中有機成分的脫離情況能精確且應 答性良好地進行反饋控m能大量生產高質量的陶毫 成形品。 (3)本發明有關之第丨種陶资成形品之熱處理裝置，其特徵 是具有下列部分··對陶资成形品進行熱處理之熱處理爐； 以熱處理中的環境氣體為試樣’從該熱處理爐内取出，將 該試樣中的竣成分轉化為特定碳化物之轉化部；檢測在該 86837 200415335 轉化邵轉化後的特定碳化物在上述試樣中的成分比例之成 分比例檢測部。 本4月之陶瓷成形品熱處理裝置，可藉由將伴隨熱處理 所產生的有機成分中的碳成分轉化為特定之碳化物，檢測 S特疋妷化物在試樣中的成分比例，根據該成分比例的檢 測、、Ό果對於從陶瓷成形品中揮發和蒸發的有機成分，以 问正確性地對其數量和揮發速度等進行換算，從而能高精 度地掌握實際的有機成分從陶瓷成形品中的脫離狀況。 (4)本發明 < 第2種陶瓷成形品熱處理裝置，其特徵是具有 下歹j 4刀·對陶资成形品進行熱處理之熱處理爐；以熱處 理中的ί衣境氣體為試樣，從該熱處理爐内取出，將該試樣 中的故成刀轉化為特定竣化物之轉化部，·檢測在此轉化部 轉化後的特定碳化物在上述試樣中的成分比例之成分比例 松測4 ’和根據該成分比例檢測部的成分比例檢測結果， 對上逑熱處理爐内的熱處理進行控制之控制部。 本發明 < 陶瓷成形品之熱處理裝置，可藉由將伴隨熱處 理所產生的有機成分中的碳成分轉化為特定之碳化物，檢 測該特定碳化物在試樣中的成分比例，根據該成分比例的 檢測結果’對於從陶瓷成形品中揮發和蒸發的有機成分， 以南正確性地對其數量和揮發速度等進行換算，從而能高 精度地莩握實際的有機成分從陶瓷成形品中的脫離狀況， 同時根據孩脫離情況，可以對陶瓷成形品進行適當的熱處 理控制。 為了莩握Α處理中陶瓷成形品的脫脂狀況，對於測定陶 86837 -10 - 200415335 々成形P口重里的手段以往也有提案。但如果設置可實際運 作的上述重量測定手段，則會出現設備需大型化、成本提 向等問題，與此相對應，本發明的熱處理裝置具有實現設 備小型化等優點。 本發明的第1及第2種陶瓷成形品熱處理裝置，較好上述 特足的碳化物為二氧化碳，同時上述轉化部的結構可使上 述試樣完全燃燒，使該試樣中的碳成分轉化為二氧化唆。 k時’根據試樣中所包含的二氧化碳濃度的檢測結果，可 進行熱處理爐内的環境氣體中所含揮發的有機成分量的換 算，從而可精確、方便地檢測從熱處理爐内的陶瓷成形品 揮發出來的有機成分量和其揮發速度等。 本發明的第1及第2種陶瓷成形品之熱處理裝置，較好上 述轉化邵配置在上述熱處理爐的熱處理空間内。該情況 下和將轉化邵配置在熱處理爐的外部相比，熱處理空間 内的熱量可以作為預熱加以利用使有機成分轉化成二氧化 石反’可以節省用於該轉化的加熱處理之能源。而且，使試 樣從熱處理爐導向轉化部的結構等也可變得簡單。再者， 將轉化部設在外部時，在將試樣從熱處理空間移送到轉化 部的管道途中，由於環境氣體的溫度降低，使部分環境氣 骨豆有可说在該管道上結露，由於該結露情況的發生，二氧 化碳濃度的檢測精度也會降低。而轉化部等設置在高溫環 境下，可以避免上述結露的發生，可以高精度地進行二氧 化碳濃度的檢測。 本發明的第2種陶瓷成形品熱處理裝置，較好上述控制部 86837 -11 - 200415335 具有對熱處理的溫度進行控制的溫度控制手段。該情況 下，藉由溫度控制就能對於從陶瓷成形品中脫離的有機成 分高精度地進行控制。 本發明的罘2種陶瓷成形品熱處理裝置，較妤上述控制部 具有根據上述碳化物成分比例的檢測結果，對上述熱處理 進仃反饋，使之逐步達到規定的碳化物成分比例之控制手 段。孩情況下，根據環境氣體成分比例的控制，使之逐步 達到規定的碳化物成分比例，從而可高精度地控制從陶资 成形品中脫離的有機成分。 【實施方式】 以下’根據附圖所示的實施形態詳細說明本發明。 圖1至圖5，圖1是表示本發明實施形態的熱處理裝置的概 略說明圖，圖2是表示熱處理空間内的溫度和檢測的二氧化 奴濃度之間的關係圖，圖3是表示熱處理經過時間内的熱處 理空間内的溫度及環境氣體中二氧化碳濃度之關係圖，圖4 是表示熱處理經過時間内的二氧化碳濃度的控制曲線並據 此&制熱處理芝間的溫度關係圖’圖5是表示熱處理程序的 流程圖。 茶照圖1，表示例如用於對層疊陶瓷電容等的陶资成形品 進行脫脂處理的熱處理裝置。 該熱處理裝置可具有連續式熱處理爐，也可具有間歇式 熱處理爐。這裏對於具有間歇式熱處理爐的裝置加以說 明。參照圖1，熱處理裝置1的結構具有下列裝置、部件： 間歇式熱處理爐2 ;從該熱處理爐2的熱處理空間3取出環境 86837 -12 - 200415335 氣體為試樣而使試樣中的有機成分等中的碳成分轉化為二 氧化碳的轉化部，即環境氣體燃燒裝置4 ;從在環境氣體燃 燒裝置4中轉化為二氧化碳狀態的試樣並檢測二氧化碳濃 度的成分比例之檢測部，即氣體濃度計5 ;根據由該氣體濃 度計5檢測的二氧化碳的濃度，對熱處理空間3内的溫度進 行控制的控制部，即控制裝置6。 熱處理爐2係由在上下、前後、左右幾乎全方位包圍熱處 理空間3之絕熱壁7所構成。在該熱處理空間3内，將可堆積 許多個層疊陶瓷電容的匣8，以上下堆積多數段的狀態設置 於爐床的台面9上。在熱處理空間3内，配備有作為加熱手 段的加熱器10，同時配備有用於檢測爐内溫度的溫度感測 益11。在熱處理空間3内，環境氣體可藉由匣8循環（圖J中 環境氣體的循環形式是用空白箭頭表示的一例），也可以設 置送風扇等的環境氣體循環裝置。而且還可設置圖中未: 出的、例如對熱處理空間内供給空氣等的新鮮環境氣體的 環境氣體供給裝置。 二境氣體燃燒裝置4是在進行熱處理時，每隔規定時間 (例如H)分鐘）以熱處㈣間3内的環魏體為試樣， 迢取出規定量，用圖中去- ^ 工#女w H中未π的加熱器使該試樣加熱，從 而使有機成分等辦燒的裝$ 、凡的裝且。在環境氣體燃燒裝置4中，今 燃燒的溫度是1000t，Μ 中^ 触愀掉世盟 燃燒的時間約為1秒鐘。作為環境氣 月庄火·、粍I置4的燃燒加埶手 、 哭，也可莽士严㈣ μ段’並不限足是電加熱的加埶 。口也了猎由氣體加熱進行，氣體 二 等不和環境“混合的間接η 燃科氣體 間接加熱。此外’燃燒時的加孰溫 86837 -13 - 200415335 度及時間也並不限於上述。藉由該燃燒處理，燃燒後的試 樣一氧化碳濃度判明為1 0 〇 ppm以下，在上述燃燒條件下有 機成分中的碳成分幾乎完全轉化為二氧化碳。 在環境氣體燃燒裝置4中經燃燒處理的試樣氣體，通過管 道供給到氣體濃度計5，由氣體濃度計5所具備的紅外線式 二氧化碳濃度計測定作為試樣氣體中的二氧化碳濃度的二 氧化碳濃度。該測定結果的二氧化碳濃度信息轉化為電信 號，傳送到控制裝置6。 控制裝置6，根據由氣體濃度計5輸入的二氧化碳的濃度 信息，與藉由預實驗等繪製的溫度控制曲線（參照圖2)相比 較’再與溫度感測器11的檢測溫度相比較，對輸向加熱器 的電力進行控制，使熱處理空間3内的溫度達到與該溫度控 制曲線下的二氧化碳濃度相對應的最佳溫度。或者是控制 裝置6，根據由氣體濃度計5輸入的二氧化碳的濃度信息， 與藉由預實驗等繪製的二氧化碳濃度控制曲線（參照圖句相 比較，再根據溫度控制曲線與來自溫度感測器丨丨的檢測溫 度相比較，對輸向加熱器的電㈣行控帝】，成為使熱處理 空間3内的二氧化碳濃度達到與該二氧化碳濃度控制曲線 下的二氧化碳濃度相對應的最佳溫度。關於上述控制後文 將再加以說明。200415335 Description of the invention: [Technical field to which the invention belongs] The present invention relates to a heat treatment method and a heat treatment device for a ceramic molded product, such as a degreasing treatment. [Prior art] The manufacturing process of ceramic molded products such as ceramics and electronic parts is a molding process in which ceramic powder is added with an organic binder, an organic plasticizer, etc., and fluidized. Therefore, it is necessary to have a procedure for removing (degreasing) unnecessary organic binders after molding before high-temperature processing such as sintering. When such degreasing is performed, it is important to control the degreasing speed in order to avoid defects such as cracks, bubbles, and peeling of the ceramic molded product. Generally, there are two methods of this type of degreasing: degreasing by burning an organic binder and the like and degreasing by evaporation and burning an organic binder and the like. When degreasing by burning organic binders, the following two techniques are known: Depending on the degreasing rate, the amount of monoxide breakdown and the proportion of oxygen components in the furnace will change. Control the combustion temperature and the combustion environment gas, and then control the degreasing speed (eg, refer to Patent Document 1); control the combustion temperature and the combustion environment gas according to the management of the proportion of oxygen components necessary for combustion in the furnace, thereby controlling the degreasing Speed (for example, refer to Patent Document 2). (Patent Document 1) JP-A No. 7-76132 (all pages, all drawings) (Patent Document 2) JP-A 3-230090 (all pages, all drawings) H6837 200415335 However, in the above degreasing speed control, Initially, before the furnace changes to -carbon oxide, the organic components have begun to volatilize, or the volatilized organic components have formed intermediate products such as acetic acid and ethyl acetate: but carbon monoxide has not been detected yet. Skim. At this time, the degreasing is promoted, and it is possible to control the temperature in the furnace, and the temperature rises to a higher temperature than the appropriate temperature for degreasing in this state. If you execute this control J on the right, degreasing will rapidly advance, causing the adhesive and plasticizer to disappear from the ceramic molded product quickly ', which may cause defects such as cracks in the molded product. Q: This test must be performed correctly even if the organic components are only related to volatilization and evaporation. In view of the above-mentioned circumstances, in order to solve the above-mentioned problems, a heat treatment method and a heat treatment device for ceramic formed products are provided, which can accurately detect the organic components volatilized from the ceramic formed products during the heat treatment. The molded product is heat-treated correctly to improve the quality of the product. [Summary of the invention] (1) The first method for heat treatment of a ceramic formed article according to the present invention is characterized by having the following procedures: During the heat treatment of a ceramic formed article in a heat treatment furnace, take out the ambient gas in the upper heat treatment furnace as a test Then, a conversion program for converting a carbon component in the sample into a specific carbide; and a component ratio detection program for detecting a component ratio of the converted specific carbide in the sample. The carbon component in the sample refers to the carbon component mainly in organic components and the like contained in the sample. The conversion of the carbon component in the sample into carbide refers to the carbon that constitutes the organic component of 200415335 which is mainly present in the sample as various organic compounds. If the prostitutes are completely burned, the majority of the carbon component is made. Both are chemically converted to a state where they exist only in the form of a specific carbide. Since the present invention can convert the rhenium component in the organic component generated by the heat treatment to a specific carbide, the component ratio of the specific carbide in the sample can be detected, and according to the detection result of the component ratio, the ceramic molding The amount of volatilized and evaporated organic components in the product is converted with high accuracy, such as the quantity and volatility speed, so it is possible to accurately grasp the actual organic component's detachment from the ceramic molded product. (2) The second method for heat-treating a ceramic formed article according to the present invention is characterized by having the following procedures: During the heat treatment of the ceramic formed article in the heat-treating furnace, the ambient gas in the heat-treating furnace is taken as a sample, and The conversion process of the carbon component in the sample into a specific carbide; and detecting the ratio of the component ratio of the converted specific carbide in the sample, the proportion detection procedure; and according to the detection result of the component ratio, A control program for controlling the heat treatment in the heat treatment furnace. The present invention can detect the component ratio of the specific carbide in the sample by converting the carbon component in the organic component generated by the heat treatment into the carbide of the material. According to the detection result of the component ratio, The volatilized and evaporated organic components in the molded product are converted into their quantity and volatilization rate with a high degree of lightness. Therefore, it is possible to accurately grasp the actual organic component release from the ceramic molded product. The detachment of the components from the ceramic material can be controlled by appropriate heat treatment of the ceramic material. 86837 200415335 The heat treatment method for the first and second ceramic molded products of the present invention, the specific carbide is preferably carbon dioxide, and the conversion procedure is preferably to completely burn the upper sample to make the carbon component in the sample Process for conversion to carbon dioxide. At this time, according to the detection of the carbon dioxide concentration contained in the sample, the conversion of the amount of volatile organic components contained in the ambient gas in the heat treatment furnace can be achieved, so that the ceramic molding from the heat treatment furnace can be accurately and conveniently detected. The amount of volatilized organic components and its volatilization rate. According to the second method for heat-treating a ceramic formed product of the present invention, the temperature control is performed as compared with the heat-treatment control of the above control program. At this time, by controlling the temperature, it is possible to accurately control the separation of organic components from the ceramic molded product. 2. In the second method for heat-treating a ceramic molded product according to the present invention, it is preferable that the above-mentioned control procedure I is performed for controlling the heat treatment to control the proportion of the ambient gas component. At this time, by controlling the proportion of the ambient gas components, it is possible to accurately control the detachment of the organic components from the ceramic shaped article. 2. In the second heat treatment method for ceramic shaped products according to the present invention, it is preferable that the control program is based on the detection result of the carbide component ratio, and performs feedback control on the heat treatment to gradually reach a predetermined carbide component ratio. At this time, it is possible to accurately and responsively control the detachment of the organic component from the pottery product, and it is possible to mass-produce a high-quality pottery molded product. (3) The first type of ceramic material heat treatment device according to the present invention is characterized by having the following parts: a heat treatment furnace for heat treating ceramic material; using the ambient gas in the heat treatment as a sample 'from the heat treatment Take it out of the furnace, and convert the finished component in the sample into a specific carbide conversion unit; a component ratio detection unit that detects the component ratio of the specific carbide after conversion in the 86837 200415335 conversion. The ceramic molding product heat treatment device in April can convert the carbon component in the organic component generated by the heat treatment into a specific carbide, and detect the composition ratio of the S special compound in the sample. According to the composition ratio, For the detection of organic components that are volatilized and evaporated from ceramic molded products, the quantity and volatilization rate of the organic components that are evaporated from the ceramic molded products can be accurately converted, so that the actual organic components can be accurately grasped from the ceramic molded products. Out of condition. (4) The present invention < The second type of ceramic shaped product heat treatment device is characterized in that it has a heat treatment furnace for heat treatment of ceramic shaped products; Take it out of the heat treatment furnace, convert the old knife in the sample into the conversion part of the specific finished compound, and check the component ratio of the component ratio of the specific carbide after conversion in the conversion part. 'And a control section that controls the heat treatment in the upper heat treatment furnace based on the component ratio detection result of the component ratio detection section. The heat treatment device of the ceramic molded article of the present invention can convert the carbon component in the organic component generated by the heat treatment into a specific carbide, and detect the component ratio of the specific carbide in the sample. According to the component ratio, Test result 'For the organic components that are volatilized and evaporated from the ceramic molded product, the quantity and volatilization rate of the organic components that have been volatilized by Nannan can be accurately converted, so that the actual organic components can be accurately separated from the ceramic molded product. At the same time, it is possible to perform appropriate heat treatment control on the ceramic molded product according to the situation of child separation. In order to grasp the degreasing status of ceramic molded products during the A treatment, a method for measuring the pothole weight of ceramic 86837 -10-200415335 was also proposed in the past. However, if the above-mentioned weight measurement means which can be practically operated is provided, problems such as the need to increase the size of the equipment and the increase in cost will arise. Corresponding to this, the heat treatment device of the present invention has advantages such as miniaturization of the equipment. In the first and second types of ceramic molded product heat treatment apparatuses of the present invention, it is preferable that the special carbide is carbon dioxide, and the structure of the conversion section can completely burn the sample, and convert the carbon component in the sample into Thorium dioxide. At time k, the amount of volatile organic components contained in the ambient gas in the heat treatment furnace can be converted based on the detection result of the carbon dioxide concentration contained in the sample, so that the ceramic molded product from the heat treatment furnace can be accurately and conveniently detected. The amount of volatilized organic components and its volatilization rate. It is preferable that the heat treatment apparatuses of the first and second ceramic molded articles of the present invention are disposed in the heat treatment space of the heat treatment furnace. In this case, the heat in the heat treatment space can be used as preheating and the organic component is converted into the dioxide reaction, as compared with disposing the reformer outside the heat treatment furnace, and energy for heat treatment for the conversion can be saved. Furthermore, the structure and the like for guiding the test sample from the heat treatment furnace to the conversion section can be simplified. Furthermore, when the conversion unit is provided externally, during the process of transferring the sample from the heat treatment space to the pipeline of the conversion unit, due to the decrease in the temperature of the ambient gas, some environmental gas bone beans may be said to have dew on the pipeline. When condensation occurs, the detection accuracy of the carbon dioxide concentration is also reduced. The conversion unit and the like are installed in a high-temperature environment, which can prevent the above-mentioned condensation from occurring, and can detect the carbon dioxide concentration with high accuracy. In the second ceramic shaped product heat treatment device of the present invention, it is preferable that the control unit 86837 -11-200415335 has a temperature control means for controlling the temperature of the heat treatment. In this case, it is possible to accurately control the organic components separated from the ceramic molded product by temperature control. According to the two types of ceramic shaped product heat treatment apparatuses of the present invention, the control unit has a control means for feeding back the heat treatment based on the detection result of the carbide component ratio to gradually reach a predetermined carbide component ratio. In some cases, according to the control of the composition ratio of the ambient gas, it is gradually brought to a predetermined carbide composition ratio, so that the organic components separated from the ceramic molded product can be controlled with high accuracy. [Embodiment] Hereinafter, the present invention will be described in detail based on an embodiment shown in the drawings. 1 to 5, FIG. 1 is a schematic explanatory diagram showing a heat treatment apparatus according to an embodiment of the present invention, FIG. 2 is a diagram showing a relationship between a temperature in a heat treatment space and a detected concentration of slave dioxide, and FIG. 3 is a diagram showing a heat treatment process Figure 4 shows the relationship between the temperature in the heat treatment space and the carbon dioxide concentration in the ambient gas over time. Figure 4 shows the control curve of the carbon dioxide concentration during the heat treatment elapsed time. Flow chart of heat treatment procedure. Fig. 1 shows a heat treatment apparatus for degreasing a ceramic molded article such as a laminated ceramic capacitor. The heat treatment apparatus may include a continuous heat treatment furnace or a batch heat treatment furnace. Here, an apparatus having a batch type heat treatment furnace will be described. Referring to FIG. 1, the structure of the heat treatment device 1 includes the following devices and components: an intermittent heat treatment furnace 2; taking out the environment 86837 -12-200415335 from the heat treatment space 3 of the heat treatment furnace 2 to make organic components in the sample, etc. The carbon component in the carbon dioxide conversion unit, that is, the ambient gas combustion device 4; from the ambient gas combustion device 4 into the carbon dioxide state of the sample and the detection portion of the carbon dioxide concentration of the detection unit, namely the gas concentration meter 5; Based on the concentration of carbon dioxide detected by the gas concentration meter 5, a control unit 6 that controls the temperature in the heat treatment space 3 is a control unit 6. The heat-treating furnace 2 is composed of heat-insulating walls 7 that surround the heat-treating space 3 almost vertically in all directions. In this heat-treating space 3, a plurality of cassettes 8 for stacking ceramic capacitors are stacked, and a plurality of stages are stacked on the table 9 of the hearth. In the heat treatment space 3, a heater 10 as a heating means is provided, and a temperature sensing benefit 11 for detecting the temperature in the furnace is also provided. In the heat treatment space 3, the ambient gas may be circulated by the cassette 8 (the circulation form of the ambient gas in FIG. J is an example indicated by a blank arrow), and an ambient gas circulation device such as a fan may be provided. Furthermore, an environmental gas supply device not shown in the figure, for example, supplying fresh environmental gas such as air to the heat treatment space, can be provided. When performing the heat treatment, the two-state gas combustion device 4 takes the ring-shaped body in the hot room 3 as a sample every predetermined time (for example, H) minutes, and takes out a predetermined amount, and uses the figure to go-^ 工 # A female heater in female WH heats the sample, so that organic components and the like are burned. In the ambient gas combustion device 4, the temperature of the current combustion is 1000t, and the time for M to touch the World Union is about 1 second. As an environmental ambience, the burning of the fire and the 粍 I set 4 to increase hands, crying, but also reckless strict section μ section ’is not limited to the addition of electric heating. Mouth hunting is carried out by gas heating, indirect heating of the second-class gas that does not mix with the environment, and indirect heating of fuel gas. In addition, the heating temperature during combustion is 86837 -13-200415335, and the time is not limited to the above. By In this combustion treatment, the carbon monoxide concentration of the sample after combustion was determined to be 100 ppm or less, and the carbon component in the organic component was almost completely converted to carbon dioxide under the above-mentioned combustion conditions. The sample gas subjected to the combustion treatment in the ambient gas combustion device 4 It is supplied to the gas concentration meter 5 through a pipe, and the infrared carbon dioxide concentration meter provided in the gas concentration meter 5 measures the carbon dioxide concentration as the carbon dioxide concentration in the sample gas. The carbon dioxide concentration information of the measurement result is converted into an electric signal and transmitted to Control device 6. The control device 6 compares the detected temperature of the temperature sensor 11 with the temperature control curve (see FIG. 2) drawn by a preliminary experiment or the like based on the carbon dioxide concentration information input from the gas concentration meter 5. In comparison, the power to the heater is controlled so that the temperature in the heat treatment space 3 reaches The optimum temperature corresponding to the carbon dioxide concentration under the temperature control curve. Alternatively, the control device 6 uses the carbon dioxide concentration information input from the gas concentration meter 5 and the carbon dioxide concentration control curve (see the figure) drawn through preliminary experiments and the like. In comparison, according to the temperature control curve and the detected temperature from the temperature sensor, the electric power to the heater is controlled to make the carbon dioxide concentration in the heat treatment space 3 reach the carbon dioxide concentration control. The optimum temperature corresponding to the carbon dioxide concentration under the curve. The above control will be described later.
，，，τ王〜阿瓦；电各的P 成形品進行脫脂處理時，作為控制目標溫度控制曲㈣ 氧化碳濃度控制曲線的繪製程序，按照圖3加以說明。 對於所希望的層疊㈣電容的n成n 86837 -14- 200415335 脫脂處理生產實際產品時的脫脂程序同樣 π丨」^的狀怨，將該陶 瓷成形品的工件收藏於熱處理爐2内的匣卡 ' 接者，按照 預先適當設定的溫度曲線開始進行敎虚 J…、&理芝間3内的溫度 控制。圖3中’橫座標表示經過時間，原點 T u 屌點為開始脫脂埶處 理，縱座標表示將揮發的有機成分中的碳成分換算為二氧 化碳後的二氧化碳濃度以及熱處理空間内的環境氣體溫 度。這時的溫度曲線如圖3中用細線所示，溫度控制在初始 的單位時間裏溫度上升率設定成比過去被認為自陶瓷成形 品中有機成分的脫離速度過快而產生缺陷之溫度上升速率 低之速率，經過規定時間後，提高該溫度上升率的升溫， 然後經過規定時間後進行保持恒定溫度的設定。按照該溫 度曲線控制溫度時，每隔規定時間（例如10分鐘）取出熱處理 芝間3内的環境氣體作為試樣，用氣體濃度計$測定環境氣 體燃燒裝置4中完全燃燒的試樣。根據該測定所得到的二氧 化碳濃度在圖3中用粗線表示。如此可得到如圖2所示的脫 脂程序的溫度和在此溫度下使從陶瓷成形品脫離的有機成 分中的碳成分轉化為二氧化碳濃度之間的關係。此外，根 據預先設定的溫度曲線進行溫度控制時，按照所得到的脫 月曰程序的一氧化碳濃度變動情況，纟會製如圖4中用粗線所示 之實際生產產品時從脫脂程序脫脂處理開始時的二氧化碳 濃度控制曲線。該曲線的繪製可以用計算機自動繪製，也 可以用手工操作。如上所述，利用熱處理裝置1對於陶瓷成 形品進行脫脂處理包含下述程序：對於熱處理爐内的環境 氣體經過燃燒等方式轉化為特定的碳化物、該實施形態是 86837 -15 - 200415335 轉化為二氧化硬的程序；檢測該碳化物在試樣中的成分比 明j ^ &序1^種&處理万法相當^中請專利^圍第1項之發 按照如上述所得到的溫度控制曲線及二氧化碳濃度的於 制曲線，對於控制脫脂程序熱處理的熱處理方法，根據圖 2圖4及圖5的流程加以說明。 對於所希望的層疊陶走電容的n成形品進行脫脂處理 的脫脂處理溫度，和網：往Ρ、左胎 將伴ik脫知處理從陶瓷成形品脫離的 有機成分中的碳成分轉化為二氧化碳時該：氧化竣在環境 氣體中的濃度關係的控制曲線之一例如圖2所示。在圖2 t，橫座標為熱處理空間内的環境氣體溫度，縱座標為二 氧化碳濃度。在圖2中又用虛線例示以往的控制曲線。本發 明實施形態的控制曲線在圖2中用實線表示。以往的場人為 對應於熱處理爐内環境氣體中的：氧化碳濃度的控制曲 線°以往’大致在12(TC〜· t之間的環境氣體溫度時，實 際上是處於有機成分從陶走成形品中揮發的狀態，但是由 於沒有檢測到，所以在該沒有㈣出之環境氣體溫度下， 無法對從陶毫成形品脫離的有機成分進行控制。本實施形 態中，將過去沒有檢測到的揮發有機成分正確地以二氧化 碳的成分比例進行檢測，所以根據檢測的二氧化碳濃度， 可對適當抑制熱處理溫度進行控制。 該控制過程如同圖4所示。圖4中，橫座標表示經過時間， 原點為脫脂熱處理開始，點，縱座標表示揮發的有機成分中 的峻成分換算為二氧化碳後的該二氧化碳濃度及熱處理空 86837 -16 - 200415335 間内的環境氣體溫度。圖4中，粗線表示從脫脂程序開始時 點起的經過時間的二氧化碳濃度控制曲線，細線表示按照 該二氧化碳濃度的控制曲線和圖2所示的溫度控制曲線進 行溫度控制時的熱處理空間3内的溫度變化狀況。脫脂程序 的初期，按預先設定的每單位時間的溫度上升率使熱處理 空間3内升溫，然後按照二氧化碳濃度的控制曲線進行溫度 控制。對於進行該溫度控制時的熱處理空間3内的溫度，如 圖4所π，當二氧化碳控制曲線的二氧化碳濃度為時， 扣規足的/皿度上升率升溫，在控制曲線的二氧化碳濃度以 比較緩慢的恒定增加率增加的區域，描緣在該恒定增加率 下二乳化碳濃度增加的軌跡，將從實際的試樣所得到的二 乳化碳濃度和該軌跡上的二氧化碳濃度相比較，對從實際 的試樣所得到的二氧化碳濃度進行反饋控制，使其偏差變 小二同樣，從經過規定時間後的二氧化碳濃度起，以高於 以前的二氧化碳濃度增加率的預先設定的增加率描緣二氧 化碳濃度增加的軌跡，將從實際的試樣所得到的二氧化碳 濃度和該軌跡上的二氧化碳濃度相比較，對從實際的試樣 所得到的二氧化碳濃度進行反饋控制，使其偏差變小。而 且，經過規定時間後控制曲線的二氧化碳濃度為急速降低 的過程。在該過程中，對保持預先蚊的溫度進行控制， 再經過歧時間後，溫度控制停止，進行冷卻處理。 如上所述，由於本發明在對陶资成形品進行脫脂的熱處 理程序中，對於該程序初期的有機成分的揮發和_， 將熱處理空間中的環境氣體取出作為試樣，測定該試樣中 86837 -17- 200415335 有機成分幾乎全部轉化為二氧化碳後該二氧化碳濃度，根 據該測定結果，進行熱處理空間的溫度控制，所以能避免 脫脂不適當地急速進行等的不良情況。因此，脫脂處理後 的陶瓷:成形品中伴隨脫脂處理所產生的不良產品與過去相 比要低。 按照圖5的流程對於上述熱處理程序進行說明。使加熱器 10溫度上升、開始熱處理，然後每隔規定時間，用控制裝 置6讀取由氣體濃度計5測得的二氧化碳濃度作為現時點的 控制對象氣體濃度及由溫度測感器丨丨所得到的熱處理空間 3内的溫度（參照圖5的步騾S1)。接著，判斷該讀取的溫度 是否在預先設定的控制實際進行狀態的控制對象溫度範^ 内（參照圖5的步驟S2)，如在該範圍内，以由該時點的二氧 化竣濃度控制曲線所設定的二氧化碳濃度為目標進行設定 (參照圖5的步驟S3)。根據實測的二氧化碳濃度和目標二 氧化碳濃度之間的偏差，計算用於溫度控制的加熱:器： 出’使該偏差變小（參照圖5的步驟S4)，根據該計算結: 制力:熱器的輸出（參照圖5的步驟s5)。每隔規定時間反復: 上㈣，按照規定的二氧化碳濃度控制曲線進行控制 脫脂結束的時點（參照圖5的步驟s6)結束熱處理程序。 16本發明者藉由實際進行上述熱處理，對於具有3.2mmx ' mX1.8 _尺寸的^層叠陶资電容進行脫脂虚理如 對於同種的陶瓷電容按昭 5里和 Α照過去的万法進行脫脂處理，兩去 的利離（分層剝離）發生率如表丨所示。 兩者 86837 -18 - 200415335 [表1 ] 剝離的發生率（n= loooo) 過去例 實施例 剝離的發生率（°/〇) 0.5 0 對於本發明方法和過去方法分別檢查1〇〇〇〇個，檢查有無 發生剥離，結果過去方法剝離發生率為〇 5%。而本發明方 法為0 %。 對於和上述不同的實施形態參照圖6簡單加以說明。與上 迟貫施形恐相同構成的就省略說明，圖中的符號對於和上 述實施形態相同構成的也標上相同符號。在該不同的實施 形態中，將作為轉化部的環境氣體燃燒裝置14設置在熱處 里爐2的熱處理玄間3内。在該環境氣體燃燒裝置14中，設 置有圖中未示出之使自熱處理空間3得到的環境氣體作為 4樣予以燃燒的加熱器。而i，由於環境氣體燃燒裝置μ 配置在熱處理空間3㈣高溫環境下，所以環境氣體的試樣 可以不揭露地取樣，因此這時還可抑制由於揭露而產生的 本發明不限定於上述實施形態，還可以有各種變形。 〇):於從熱處理中的環境氣體取出的試樣，將其有機成 分寺中的碳成分轉化為二氧化碳在上述實施形態中已說 明，但即使是二氧化碳之外的碳化物，也可進行成分比 例分析’而且只要該轉化能大致完全進行的話，並 疋於二氧化碳。 ⑺對於從熱處理中的環境氣體取出的試樣，將其有機成 86837 •19- 200415335 分等中的碳成分轉化為二氧化碳，本發明是藉由試樣的 燃燒來完成該轉換的以已明示，至於該轉化手段，可 以採用藉燃燒之外的化學變化將有機成分等的碳成分轉 化為—氧化^^的手段。 (3) 上述各實施形態展示了在採用熱處理的脫脂程序中， 將從陶瓷成形品脫離的有機成分轉化為二氧化碳，並根 據該二氧化碳濃度進行熱處理溫度控制的情況。但是， 不僅是溫度控制，也可以與控制供給至熱處理空間的環 境氣體之量之手段組合進行控制。即是：藉由新鮮環境 氣體的供給等來控制有機成分揮發等的從陶瓷成形品中 有機成分脫離的難易程度。此外，也可以進行環境氣體 供給量的控制’而不進行溫度控制。 (4) 在上述各實施形態中，作為陶瓷成形品明示為層疊陶 资電容，但作為本發明之陶瓷成形品並不限於此，也能 適用於其他各種陶瓷成形品。 如上所述，若按照本發明，則藉由將伴隨熱處理所產生 的有機成为中的峡成分轉化為特定的碳化物，檢測該特定 灰化物在試樣中的成分比例，根據該成分比例的檢測結 果，對於從陶瓷成形品中揮發和蒸發的有機成分，可以高 正確性地對其數量和揮發速度等進行換算，從而能高精度 地掌握實際的有機成分從陶瓷成形品中的脫離狀況。 【圖式簡單說明】 圖1表示本發明實施形態的熱處理裝置的概略說明圖。 圖2表示熱處理空間内的溫度和檢測的二氧化碳濃度之 86837 -20 - 200415335 間的關係圖。 圖3表示熱處理經過時間下的熱處理空間内的溫度及環 境氣體中二氧化碳濃度之關係圖。 圖4表示熱處理經過時間下的二氧化碳濃度的控制曲線 和按此控制的熱處理空間的溫度關係圖。 圖5簡單表示本發明實施形態的熱處理程序的流程圖。 圖6表示本發明其他實施形態的熱處理裝置的概略說明 圖。 【圖式代表符號說明】 2 3 4 5 6 7 8 9 10 11 熱處理裝置 熱處理爐 熱處理空間 環境氣體的燃燒裝置（轉化裝置） 氣體濃度計（成分比例檢測部） 控制裝置 斷熱壁 匣 爐床台面 加熱器 溫度感測器 86837， 王 ， τ 王 ～ 阿瓦 ； When the P-shaped products of each electric component are subjected to degreasing treatment, the drawing procedure of the control curve of the carbon dioxide concentration control curve as the control target temperature will be described with reference to FIG. 3. Regarding the desired n-to-n ratio of the stacked capacitors 86837 -14- 200415335, the degreasing procedure when producing the actual product is the same as described above, and the workpiece of the ceramic molded product is stored in a cassette in the heat treatment furnace 2 'Then, start the temperature control in the imaginary J ..., & Richiba 3 according to the temperature curve appropriately set in advance. In Figure 3, the horizontal axis represents the elapsed time, the origin Tu is the degreasing process, and the vertical axis represents the carbon dioxide concentration after the carbon component in the volatilized organic component is converted to carbon dioxide, and the temperature of the ambient gas in the heat treatment space. The temperature curve at this time is shown by a thin line in FIG. 3. In the initial unit time of temperature control, the temperature rise rate is set to be lower than the temperature rise rate of the organic component in the ceramic molded product that was considered to be too fast in the past to produce defects. After a predetermined time has elapsed, the temperature is increased at the rate of temperature increase, and then a constant temperature is set after the predetermined time has elapsed. When the temperature is controlled according to the temperature curve, the ambient gas in the heat treatment Shiba 3 is taken out as a sample every predetermined time (for example, 10 minutes), and the completely burned sample in the ambient gas combustion device 4 is measured with a gas concentration meter. The carbon dioxide concentration obtained by this measurement is indicated by a thick line in FIG. 3. In this way, the relationship between the temperature of the degreasing process shown in FIG. 2 and the conversion of the carbon component in the organic component separated from the ceramic molded product to the carbon dioxide concentration at this temperature can be obtained. In addition, when temperature control is performed according to a preset temperature curve, in accordance with the obtained carbon monoxide concentration fluctuations of the obtained month-to-month program, the actual production of the product as indicated by the thick line in FIG. 4 starts from the degreasing program. Control curve of carbon dioxide concentration at time. The curve can be drawn automatically by a computer or manually. As described above, the degreasing treatment of the ceramic molded product by the heat treatment device 1 includes the following procedures: The ambient gas in the heat treatment furnace is converted into a specific carbide through combustion or the like. In this embodiment, 86837 -15-200415335 is converted into two Procedure for oxidizing hard; detecting the composition ratio of the carbide in the sample. ^ &Amp; order 1 ^ species & processing is equivalent ^ in the patent ^ enumeration of the first item according to the temperature control as obtained above The curve and the carbon dioxide concentration production curve will be described with reference to the flowcharts of FIG. 2, FIG. 4, and FIG. 5 for the heat treatment method for controlling the heat treatment of the degreasing process. Degreasing temperature for degreasing the n-shaped product of the desired laminated ceramic capacitor, and the net: when carbon components in the organic components detached from the ceramic molded product with the deik treatment are converted to carbon dioxide to P and the left tire This: One example of the control curve of the concentration relationship of the oxidation in the ambient gas is shown in FIG. 2. In Fig. 2 t, the horizontal coordinate is the ambient gas temperature in the heat treatment space, and the vertical coordinate is the carbon dioxide concentration. In FIG. 2, a conventional control curve is illustrated by a dotted line. The control curve of the embodiment of the present invention is shown by a solid line in FIG. 2. The conventional field artificially corresponds to the control curve of the concentration of carbon oxide in the ambient gas in the heat treatment furnace. In the past, when the ambient gas temperature was approximately 12 (TC ~ · t), the organic components were actually formed from ceramics. The state of volatilization, but it is not detected, so it is impossible to control the organic components detached from the ceramic molded product at the temperature of the ambient gas that is not scavenged. In this embodiment, the volatile organics that have not been detected in the past are not detected. The components are accurately detected by the proportion of carbon dioxide, so the heat treatment temperature can be controlled appropriately according to the detected carbon dioxide concentration. The control process is shown in Figure 4. In Figure 4, the horizontal axis represents the elapsed time and the origin is degreasing. The heat treatment starts, and the ordinate indicates the concentration of carbon dioxide converted from carbon dioxide in the volatilized organic component and the ambient gas temperature in the heat treatment space between 86837 -16-200415335. In Figure 4, the thick line indicates the start of the degreasing process. The control curve of the carbon dioxide concentration of the elapsed time from the point in time. The control curve of the concentration of carbon oxide and the temperature control curve shown in Fig. 2 during the temperature control of the heat treatment space 3. In the initial stage of the degreasing program, the heat treatment space 3 is set at a predetermined temperature rise rate per unit time. The temperature is raised, and then the temperature is controlled according to the control curve of carbon dioxide concentration. For the temperature in the heat treatment space 3 when performing the temperature control, as shown in FIG. 4, when the carbon dioxide concentration of the carbon dioxide control curve is The rise rate rises, and in the area where the carbon dioxide concentration of the control curve increases at a relatively slow and constant increase rate, the trajectory of the increase in the di-emulsified carbon concentration at the constant increase rate is traced, and the di-emulsified carbon concentration obtained from the actual sample is traced. Compared with the carbon dioxide concentration on this trajectory, feedback control is performed on the carbon dioxide concentration obtained from the actual sample to make the deviation smaller. Similarly, the carbon dioxide concentration after a predetermined time is higher than the previous carbon dioxide concentration. The increase rate of the pre-set increase rate traces the increase in carbon dioxide concentration The trajectory compares the carbon dioxide concentration obtained from the actual sample with the carbon dioxide concentration on the trajectory, and feedback-controls the carbon dioxide concentration obtained from the actual sample to make the deviation smaller. Moreover, after a predetermined time elapses, The carbon dioxide concentration of the control curve is a process of rapid decrease. In this process, the temperature of the mosquito is maintained in advance, and after a lapse of time, the temperature control is stopped and the cooling process is performed. As described above, since the invention is In the heat treatment program for degreasing the molded product, the volatilization of organic components and _ at the beginning of the program were performed by taking the ambient gas in the heat treatment space as a sample, and measuring 86837 -17- 200415335 almost all organic components in the sample were converted to carbon dioxide. This carbon dioxide concentration is then used to control the temperature of the heat treatment space based on the measurement results, so that problems such as improper and rapid degreasing can be avoided. As a result, ceramics and molded products with degreasing treatment have a lower number of defective products associated with degreasing treatment than in the past. The above-mentioned heat treatment procedure will be described in accordance with the flowchart of FIG. 5. The temperature of the heater 10 is increased, and the heat treatment is started. Then, at a predetermined time, the control device 6 reads the carbon dioxide concentration measured by the gas concentration meter 5 as the control target gas concentration at the current point and obtained by the temperature sensor. Temperature in the heat treatment space 3 (see step S1 in FIG. 5). Next, it is determined whether the read temperature is within a preset control target temperature range of the actual control state (refer to step S2 in FIG. 5). If it is within this range, the control curve of the concentration at the time point is completed The set carbon dioxide concentration is set as a target (see step S3 in FIG. 5). Based on the difference between the measured carbon dioxide concentration and the target carbon dioxide concentration, calculate the heating control used for temperature control: Out 'to make the deviation smaller (refer to step S4 in Fig. 5), according to this calculation: Braking force: Heater (Refer to step s5 in FIG. 5). Repeat every predetermined time: The upper part is controlled according to a predetermined carbon dioxide concentration control curve. At the end of degreasing (refer to step s6 in FIG. 5), the heat treatment program is ended. 16 The inventor actually degreased the ^ laminated ceramic capacitors with a size of 3.2mmx 'mX1.8 _ by performing the above heat treatment, such as degreasing the same type of ceramic capacitors according to the previous method Treatment, the incidence of delamination (layer separation) is shown in Table 丨. Both 86837 -18-200415335 [Table 1] Incidence of peeling (n = loooo) Incidence of peeling in past examples (° / 〇) 0.5 0 For the method of the present invention and the past method, check 1,000 It was checked whether peeling occurred. As a result, the peeling rate of the conventional method was 05%. The method of the present invention is 0%. A different embodiment from the above will be briefly described with reference to FIG. 6. The description of the same configuration as that of the above-mentioned delayed application is omitted, and the symbols in the figure are marked with the same symbols for the same configuration as in the above embodiment. In this different embodiment, an ambient gas combustion device 14 serving as a conversion unit is installed in the heat treatment chamber 3 of the furnace 2 in a hot place. The ambient gas combustion device 14 is provided with a heater (not shown) that burns ambient gas obtained from the heat treatment space 3 as four samples. However, since the ambient gas combustion device μ is arranged in a heat treatment space at a high temperature environment, a sample of the ambient gas can be sampled without being exposed. Therefore, the present invention can also be prevented from being caused by the disclosure. There can be various deformations. 〇): In the sample taken from the ambient gas during heat treatment, the carbon component in the organic component is converted into carbon dioxide as described in the above embodiment, but even if it is a carbide other than carbon dioxide, the component ratio analysis can be performed 'And as long as the conversion can be carried out almost completely, it is limited to carbon dioxide. ⑺ For the sample taken from the ambient gas in the heat treatment, the carbon component in the organic fraction 86837 • 19- 200415335 is converted into carbon dioxide. The invention completes the conversion by the combustion of the sample. As for the conversion means, a means for converting a carbon component such as an organic component into -oxidizing by a chemical change other than combustion can be adopted. (3) In each of the above embodiments, in the degreasing process using heat treatment, the organic components separated from the ceramic molded product were converted into carbon dioxide, and the heat treatment temperature was controlled according to the carbon dioxide concentration. However, not only temperature control, but also control in combination with a means for controlling the amount of ambient gas supplied to the heat treatment space. In other words, it is possible to control the ease with which organic components are detached from the ceramic molded product, such as the volatilization of organic components, by the supply of fresh ambient gas and the like. It is also possible to perform the control of the supply amount of the ambient gas' without performing temperature control. (4) In each of the above embodiments, the ceramic molded product is explicitly described as a laminated ceramic capacitor, but the ceramic molded product of the present invention is not limited to this, and can be applied to various other ceramic molded products. As described above, according to the present invention, the component ratio of the specific ash in the sample is detected by converting the isthmus component in the organic compound generated by the heat treatment to a specific carbide, and based on the detection of the component ratio As a result, the amount of organic components volatilized and evaporated from the ceramic molded product can be converted with high accuracy, such as the number and volatilization rate, so that it is possible to accurately grasp the actual organic component release from the ceramic molded product. [Brief Description of the Drawings] FIG. 1 is a schematic explanatory diagram of a heat treatment apparatus according to an embodiment of the present invention. Figure 2 shows the relationship between the temperature in the heat treatment space and the detected carbon dioxide concentration between 86837-20 and 200415335. Fig. 3 is a graph showing the relationship between the temperature in the heat treatment space and the carbon dioxide concentration in the ambient gas under the heat treatment elapsed time. Fig. 4 is a graph showing the relationship between the control curve of the carbon dioxide concentration under the heat treatment elapsed time and the temperature of the heat treatment space controlled by this. Fig. 5 is a flowchart showing a heat treatment procedure in accordance with an embodiment of the present invention. Fig. 6 is a schematic explanatory view of a heat treatment apparatus according to another embodiment of the present invention. [Illustration of Symbols in the Drawings] 2 3 4 5 6 7 8 9 10 11 Heat Treatment Device Heat Treatment Furnace Heat Treatment Space Combustion Device (Conversion Device) Gas Concentration Meter (Composition Ratio Detector) Control Device Insulation Wall Furnace Table Top Heater temperature sensor 86837