JPH032660A - Method and apparatus for measuring amount of moisture in sintered ceramic body - Google Patents
Method and apparatus for measuring amount of moisture in sintered ceramic bodyInfo
- Publication number
- JPH032660A JPH032660A JP13615989A JP13615989A JPH032660A JP H032660 A JPH032660 A JP H032660A JP 13615989 A JP13615989 A JP 13615989A JP 13615989 A JP13615989 A JP 13615989A JP H032660 A JPH032660 A JP H032660A
- Authority
- JP
- Japan
- Prior art keywords
- moisture
- sintered body
- ceramic sintered
- tube
- amount
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000919 ceramic Substances 0.000 title claims description 41
- 238000000034 method Methods 0.000 title description 21
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000004448 titration Methods 0.000 claims description 10
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 9
- 230000008016 vaporization Effects 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 2
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 abstract description 18
- 238000005259 measurement Methods 0.000 abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 9
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 7
- 230000006378 damage Effects 0.000 abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000004308 accommodation Effects 0.000 description 4
- 230000001066 destructive effect Effects 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000005443 coulometric titration Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical class I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- RPMPQTVHEJVLCR-UHFFFAOYSA-N pentaaluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3] RPMPQTVHEJVLCR-UHFFFAOYSA-N 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 238000003221 volumetric titration Methods 0.000 description 2
- CVOFKRWYWCSDMA-UHFFFAOYSA-N 2-chloro-n-(2,6-diethylphenyl)-n-(methoxymethyl)acetamide;2,6-dinitro-n,n-dipropyl-4-(trifluoromethyl)aniline Chemical compound CCC1=CC=CC(CC)=C1N(COC)C(=O)CCl.CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O CVOFKRWYWCSDMA-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はセラミック焼結体の水分量の測定方法及びその
装置に関し、特に吸湿性セラミック焼結体の水分量の測
定方法およびその装置に関するものである。Detailed Description of the Invention (Industrial Application Field) The present invention relates to a method and apparatus for measuring the moisture content of a hygroscopic ceramic sintered body, and more particularly to a method and apparatus for measuring the moisture content of a hygroscopic ceramic sintered body. It is.
（従来の技術及びその問題点）
セラミック焼結体は、種々の素材を押出成形、乾式加圧
成形、加熱成形、鋳込み成形等によって成形し、これを
加熱処理して焼成することで製造される。こうしたセラ
ミック焼結体は、最終製品として、また部品として使用
される。(Prior art and its problems) Ceramic sintered bodies are manufactured by molding various materials by extrusion molding, dry pressure molding, heat molding, casting molding, etc., and then heat-treating and firing the molded material. . Such ceramic sintered bodies are used as final products and parts.
かかるセラミック焼結体、特に吸湿性セラミック焼結体
において、焼成後に大気中に曝露しておくと、大気中の
水分の吸着により表面から吸湿が進行し、特性が劣化し
たりクラックが生成することがある。このようにセラミ
ック焼結体に吸湿が起ると品質が低下するので、セラミ
ック焼結体の水分量を測定することが品質管理上要求さ
れる。If such a ceramic sintered body, especially a hygroscopic ceramic sintered body, is exposed to the atmosphere after firing, moisture absorption will progress from the surface due to adsorption of moisture in the atmosphere, resulting in deterioration of properties and generation of cracks. There is. As described above, when a ceramic sintered body absorbs moisture, its quality deteriorates, so it is required for quality control to measure the moisture content of the ceramic sintered body.
しかも、製品を破壊、粉砕して検査するのではなく、生
産ラインから出てきた製品を非破壊で検査、管理する必
要がある。破壊して検査するのでは、製品が無駄になり
、定期的にサンプリングを行うと大変なロスとなるから
である。Furthermore, instead of inspecting products by destroying or pulverizing them, it is necessary to non-destructively inspect and manage the products coming out of the production line. This is because if the product is destroyed and inspected, the product will be wasted, and if sampling is performed periodically, it will result in a huge loss.
（発明が解決しようとする課題）
本発明の課題は、セラミンク焼結体に吸着した水分の量
を、非破壊で精度良く測定できるようなセラミック焼結
体の水分量の測定方法及びその装置を提供することであ
る。(Problems to be Solved by the Invention) An object of the present invention is to provide a method and apparatus for measuring the amount of moisture in a ceramic sintered body that can non-destructively and accurately measure the amount of moisture adsorbed in the ceramic sintered body. It is to provide.
（課題を解決するための手段）
本発明は、セラミック焼結体を非破壊で好ましくは２０
０°Ｃ以上、更に好ましくは４００°Ｃ以上で加熱して
これに吸着した水分を気化させ、気化した水分をカール
フィッシャー試薬を用いて滴定し、前記水分の量を算出
する、セラミック焼結体の水分量の測定方法に係わるも
のである。(Means for Solving the Problems) The present invention provides a non-destructive ceramic sintered body, preferably
A ceramic sintered body that is heated at 0°C or higher, more preferably 400°C or higher to vaporize the moisture adsorbed thereon, and titrates the vaporized moisture using a Karl Fischer reagent to calculate the amount of moisture. This relates to a method for measuring the moisture content of.
また、本発明は、セラミック焼結体を非破壊で収容する
予備収容部と；この予備収容部内に乾燥雰囲気を送って
前記予備収容部内の気体を前記乾燥雰囲気で置換する手
段と；前記予備収容部に収容されたセラミックス成形体
を加熱部へと移送する移送手段と；前記加熱部に収容さ
れた前記セラミックス成形体を加熱してこれに吸着した
水分を気化させる加熱手段と；気化した水分をカールフ
ィッシャー試薬を用いて滴定し、前記吸着水分の量を定
量するための滴定部と；気化した水分を前記滴定部に移
送する手段と
を有するセラミック焼結体の水分量の測定装置に係わる
ものである。The present invention also provides a pre-accommodating section for non-destructively accommodating a ceramic sintered body; a means for sending a dry atmosphere into the pre-accommodating section to replace gas in the pre-accommodating section with the dry atmosphere; a transfer means for transferring the ceramic molded body accommodated in the heating section to the heating section; a heating means for heating the ceramic molded body housed in the heating section to vaporize moisture adsorbed thereto; An apparatus for measuring the amount of water in a ceramic sintered body, comprising a titration section for determining the amount of adsorbed water by titrating using a Karl Fischer reagent; and means for transferring vaporized water to the titration section. It is.
（実施例） 第１図は水分測定装置の全体の概略図である。(Example) FIG. 1 is a schematic diagram of the entire moisture measuring device.
セラミックス焼成体を加熱するだめの電気炉１は、温度
、窒素流量の制御装置２３上に取り付けられている。電
気炉１の一方の側面には吹込管１８が設けられ、吹込管
１８の先端が滴定装置２１に連結されている。この上に
は三方コック付乾燥管１７が設けられている。The electric furnace 1 for heating the ceramic fired body is mounted on a temperature and nitrogen flow rate control device 23. A blowing pipe 18 is provided on one side of the electric furnace 1 , and the tip of the blowing pipe 18 is connected to a titration device 21 . A drying tube 17 with a three-way cock is provided above this.
電気炉１の他方の側面には、耐熱ガラス製の長尺予備収
容管２０が取り付けられ、予備収容管固定金具２により
固定されている。長尺予備収容管２０の先端には押出棒
栓４が取り付けられ、押出棒５が長尺予備収容管２０内
に往復動可能に挿通される。A long preliminary accommodation tube 20 made of heat-resistant glass is attached to the other side of the electric furnace 1 and fixed by a preliminary accommodation tube fixing fitting 2 . A push-out rod stopper 4 is attached to the tip of the long preliminary storage tube 20, and a push-out rod 5 is inserted into the long preliminary storage tube 20 so as to be able to reciprocate.
押出棒５の先端には搬送具２５が取り付けられ、搬送具
２５上に例えばβ″−アルミナ袋管等のセラミック焼結
体が載置されている。A conveyor 25 is attached to the tip of the extrusion rod 5, and a ceramic sintered body such as a β''-alumina bag tube is placed on the conveyor 25.
制御装置２３において、７は電源ランプ、８は電源スイ
・ンチ、１０は窒素ガスの流量を示す流量計、１１はニ
ードル弁、１２はレベル・アジャスター、１３は温度偏
差指示計、１５は電気炉１内の加熱温度を設定するため
の温度設定ダイヤルである。In the control device 23, 7 is a power lamp, 8 is a power switch, 10 is a flow meter that indicates the flow rate of nitrogen gas, 11 is a needle valve, 12 is a level adjuster, 13 is a temperature deviation indicator, and 15 is an electric furnace. This is a temperature setting dial for setting the heating temperature within 1.
次に、第１図の水分測定装置による測定例について述べ
る。Next, an example of measurement using the moisture measuring device shown in FIG. 1 will be described.
（ａ）試料
本例においては、セラミック焼結体２２としてβ−−ア
ルミナ袋管の水分量を測定した。これは、はぼ試験管状
の焼結体である。(a) Sample In this example, the moisture content of a β-alumina bag tube as the ceramic sintered body 22 was measured. This is a sintered body in the shape of a test tube.
（ｂ）測定試料の調製
の、 び 法
β″−Ａｊ２ｚＯｉ袋管を電気炉にて８００°ＣＸ３時
間熱処理し、吸着水の除去を行った。その後、電気炉内
で５００°Ｃまで冷却し、乾燥剤としてＰ２Ｏ，を用い
且つＮ２ガスをフローさせたガラス製デシケータ−中へ
試料を移し、室温まで冷却した。(b) Preparation of measurement sample Method β''-Aj2zOi bag tube was heat-treated at 800°C for 3 hours in an electric furnace to remove adsorbed water. Thereafter, it was cooled to 500°C in an electric furnace. The sample was transferred into a glass dessicator using P2O as a desiccant and flowing N2 gas, and cooled to room temperature.
の び ′ の 法恒温恒温器
５０°Ｃ１６０％Ｒ，Ｈの条件にて所定時間、試料を曝
露し、水分の吸着を行った。水分吸着後の試料はシリカ
ゲルを入れたプラスチック製密封容器中で保管した。The sample was exposed for a predetermined period of time in a constant temperature incubator at 50°C, 160% R, and H to adsorb moisture. The sample after water adsorption was stored in a sealed plastic container containing silica gel.
（ｃ）測定手順
β″−アルミナ袋管を搬送具２５に載置し、これを長尺
予備収容管２０内に収容する。次いで、三方コック付連
結管６を通して乾燥した窒素ガスを矢印Ａのように流し
、長尺予備収容管の大気を窒素ガスに入れ換える。次い
で、押出棒５を矢印Ｂのように動作させてβ″−アルミ
ナ袋管を電気炉１内に収容し、８００°Ｃで２０分間加
熱し、β−−アルミナ袋管に吸着した水分を気化させる
。なおこの間Ｎ２ガスを試料投入前から測定終了時まで
連続的に流通する。(c) Measurement procedure β'' - Place the alumina bag tube on the carrier 25 and store it in the long preliminary storage tube 20.Next, dry nitrogen gas is fed through the connecting tube 6 with a three-way cock in the direction of arrow A. The atmosphere in the long preliminary storage tube is replaced with nitrogen gas. Next, the push rod 5 is moved in the direction of arrow B to house the β''-alumina bag tube in the electric furnace 1, and the tube is heated at 800°C. Heat for 20 minutes to vaporize the moisture adsorbed on the β--alumina bag tube. During this time, N2 gas is continuously passed from before the sample is introduced until the end of the measurement.
この滴定装置２１内では、カールフィッシャー試薬を用
いる公知の滴定法を実行し、気化水分量を算出する。In this titration device 21, a known titration method using a Karl Fischer reagent is executed to calculate the amount of vaporized water.
具体的には、化学量論的に水１分子がカールフィッシャ
ー試薬中のヨウ素１分子と反応することを利用している
。Specifically, it utilizes the fact that one molecule of water stoichiometrically reacts with one molecule of iodine in the Karl Fischer reagent.
反応式： 水分＋ヨウ素＋ＳＯ□十塩基＋メタノール→
塩基・ヨウ化水素塩＋塩基・水素メチル硫酸塩
滴定方式は容量滴定方式でも電量滴定方式でもよい。容
量滴定方式では、ヨウ素、二酸化硫黄、塩基を含むカー
ルフィッシャー試薬で滴定し、この試薬の消費量から水
分量を算出する。Reaction formula: Moisture + iodine + SO□ ten bases + methanol →
The base/hydrogen iodide salt + base/hydrogen methyl sulfate titration method may be a volumetric titration method or a coulometric titration method. In the volumetric titration method, titration is performed using a Karl Fischer reagent containing iodine, sulfur dioxide, and a base, and the water content is calculated from the consumption amount of this reagent.
電量滴定方式では、ヨウ化物、二酸化硫黄、塩基、メタ
ノールなどを含む電解液を滴定容器の中で電気分解し、
ヨウ素を発生させ、内部的にカールフィッシャー試薬を
作りながら終点まで滴定する。終点までに要した電気量
から、ファラデーの法則により、水分量を算出する。In the coulometric titration method, an electrolytic solution containing iodide, sulfur dioxide, base, methanol, etc. is electrolyzed in a titration vessel.
Generate iodine and titrate to the end point while internally creating Karl Fischer reagent. The amount of water is calculated from the amount of electricity required to reach the end point using Faraday's law.
（ｄ）恒温恒温条件（５０°Ｃ，６０％）曝露試料の重
量変化と水分測定結果
上記（ｂ）のように、熱処理した直後、所定時間曝露し
たβ−−アルミナ管（径１５Ｘ１５０ ｍｍ）につき、
重量変化を測定し、かつ上記（ｃ）のようにして水分量
を測定した。この結果を表１に示す。(d) Weight change and moisture measurement results of samples exposed to constant temperature and constant temperature conditions (50°C, 60%) As shown in (b) above, for a β-alumina tube (diameter 15 x 150 mm) exposed for a specified time immediately after heat treatment. ,
The weight change was measured, and the moisture content was measured as in (c) above. The results are shown in Table 1.
５０°Ｃ５６０χＲ，Ｉ（曝露条件での曝露時間と水分
吸湿量の関係
また、第２図は曝露時間と水分吸湿量との関係を示すグ
ラフであり、第３図は曝露後の重量増加量と水分検出量
との関係を示すグラフである。50°C560χR,I (Relationship between exposure time and amount of moisture absorbed under exposure conditions. Figure 2 is a graph showing the relationship between exposure time and amount of moisture absorbed, and Figure 3 is a graph showing the relationship between the amount of weight increase and the amount of moisture absorbed after exposure. It is a graph showing the relationship with the detected amount of moisture.
次に、上記測定例の検討結果等について述べる。Next, the study results of the above measurement examples will be described.
（ａ）カールフィッシャー法によりベータアルミナ管中
の水分測定は非破壊で可能である。(a) Moisture content in beta alumina tubes can be measured non-destructively using the Karl Fischer method.
このように、非破壊で水分量を測定できるのは、焼成に
よりベータアルミナ管の組織内部の水分は除去されてお
り１表面から吸湿が進行するという独特の性質によるも
のである。例えば、鉄鉱石等は組織内部に付着水、結晶
水を含んでいるため、粉砕することが必須であり、非破
壊で試験することは考えられない。本発明はこの点で特
異であると言える。The reason why the moisture content can be measured non-destructively in this way is due to the unique property that moisture inside the structure of the beta alumina tube is removed by firing and moisture absorption progresses from one surface. For example, since iron ore and the like contain adhering water and crystallized water inside their structures, it is essential to crush them, and it is unthinkable to test them non-destructively. The present invention can be said to be unique in this respect.
本発明の測定方法を用いれば、非破壊でベータアルミナ
管のセラミック焼結体の水分量を簡単、短時間に検査で
きるので、より有効に品質管理を行なえる。By using the measuring method of the present invention, the water content of a ceramic sintered body of a beta alumina tube can be easily and quickly tested non-destructively, so quality control can be carried out more effectively.
（ｂ）第３図の結果から、重量変化と水分検出量との間
には比例関係があり、高温多湿環境下での重量変化が吸
着水分によるものであることが分る。(b) From the results in FIG. 3, it can be seen that there is a proportional relationship between the weight change and the detected amount of moisture, and that the weight change in a high temperature and humid environment is due to adsorbed moisture.
（ｃ）長尺予備収容管２０にベータアルミナ袋管を非破
壊で収容し、窒素ガスを送り込んで湿った雰囲気を置換
しているので、湿った外気の水分をカールフィッシャー
試薬により検出することを防止できる。(c) Since the beta alumina bag tube is non-destructively housed in the long preliminary storage tube 20 and the humid atmosphere is replaced by nitrogen gas, it is possible to detect moisture in the humid outside air using Karl Fischer reagent. It can be prevented.
従来、カールフィッシャー法による水分測定装置におい
ては、例えば、鉄鉱石用に二連の加熱室を設けたものが
ある。しかし、これは一つ目の加熱室で付着水を気化し
、二つ目の加熱室で結晶水を気化するためのものに過ぎ
ない。Conventionally, moisture measuring devices using the Karl Fischer method include devices equipped with two heating chambers for iron ore, for example. However, this is only for vaporizing adhering water in the first heating chamber and vaporizing water of crystallization in the second heating chamber.
従って、ベータアルミナ袋管を予備収容管２０に非破壊
で収容し、この中の雰囲気を置換することで、本実施例
に述べた水分量測定方法を実用化できたのである。固体
試料を粉砕し、またペレットとして水分量を測定する従
来の装置では、上記のようにベータアルミナ袋管を非破
壊で収容することはもともと不可能であり、かつ不必要
だったのである。Therefore, by non-destructively housing the beta-alumina bag tube in the preliminary storage tube 20 and replacing the atmosphere therein, the water content measuring method described in this embodiment could be put to practical use. With conventional equipment that crushes a solid sample and measures the moisture content in the form of pellets, it was originally impossible and unnecessary to accommodate the beta-alumina bag tube in a non-destructive manner as described above.
（ｄ）上記のように、非破壊でベータアルミナ管の水分
量測定が実現したことで、以下の効果が得られる。(d) As described above, the following effects can be obtained by non-destructively measuring the moisture content of beta alumina tubes.
（ｉ）ベータアルミナ管を粉砕したり、一部を測定試料
として切り出す必要がないので、製品が無駄にならず、
定期的にサンプリングをし、水分量を測定しても、何ら
ロスは生じない。(i) There is no need to crush the beta alumina tube or cut out a portion as a measurement sample, so the product is not wasted.
Even if you sample regularly and measure the moisture content, no loss will occur.
（ｉｉ）ベータアルミナ管を粉砕したり、一部を切り出
す方法では、粉砕時、切り出し時に新たな表面に水が吸
着されるので、水分量が真の値より増加し、正確な値が
得られない。本例では、非破壊で測定し、破壊にともな
う新たな表面を生じないので、正確な値が得られる。(ii) In the method of crushing or cutting out a portion of the beta alumina tube, water is adsorbed on the new surface during crushing and cutting, so the moisture content increases from the true value and accurate values cannot be obtained. do not have. In this example, since the measurement is performed non-destructively and no new surface is created due to destruction, accurate values can be obtained.
（ｉｉｉ） ベータアルミナ管の一部を粉砕し、又は
測定試料として切り出す方法では、測定試料としてベー
タアルミナ管の一部のみを選定することになる。しかし
、現実の試料では、局所的に水分吸着量のバラツキが存
在するため、上記（ｉｉ）とも相まって正確な値は得ら
れない。本例では、目的とするベータアルミナ管製品自
体について水分量測定を行うので２局所的なバラツキに
よる影響は受けない。(iii) In the method of crushing a portion of the beta alumina tube or cutting it out as a measurement sample, only a portion of the beta alumina tube is selected as the measurement sample. However, in actual samples, since there are local variations in the amount of water adsorption, combined with the above (ii), accurate values cannot be obtained. In this example, since the moisture content is measured for the target beta-alumina tube product itself, it is not affected by two local variations.
（ｉｖ ）ベータアルミナ管を粉砕したり、一部を切り
出す手間がかからない。(iv) There is no need to pulverize the beta alumina tube or cut out a portion of it.
上述の実施例は種々変更できる。The embodiments described above can be modified in various ways.
例えば、被測定物の材質は、ベータアルミナ以外でもよ
く、吸湿性セラミックスにはすべて有効であり、種々の
導電性セラミックス、機能性セラミックス、磁気シール
ド用等に用いられる超電導セラミックス等であってもよ
い。これらの形状は、板状、円筒状、線状、コイル状等
種々変化させてよい。For example, the material to be measured may be other than beta alumina, which is effective for all hygroscopic ceramics, and may also be various conductive ceramics, functional ceramics, superconducting ceramics used for magnetic shielding, etc. . These shapes may be changed into various shapes such as a plate shape, a cylindrical shape, a line shape, and a coil shape.
電気炉等に送り込む乾燥雰囲気は、窒素ガスだけでなく
、例えばアルゴン等も使用できる。As the drying atmosphere sent into the electric furnace or the like, not only nitrogen gas but also, for example, argon or the like can be used.
また、予備収容部内におけるセラミックス焼成体の移送
方法も変更してよく、予備収容部の形状等も変更してよ
い。Furthermore, the method of transferring the fired ceramic body within the pre-accommodating section may be changed, and the shape of the pre-accommodating section may also be changed.
吸着水除去のための熱処理条件としては２００°Ｃ以上
特に４００°Ｃ以上が好ましく、時間は１０分以上保持
することが好ましい。The heat treatment conditions for removing adsorbed water are preferably 200°C or higher, particularly 400°C or higher, and the heat treatment is preferably maintained for 10 minutes or longer.
（発明の効果）
本発明に係わるセラミック焼結体の水分量の測定方法に
よれば、セラミック焼結体を非破壊で加熱し水分を気化
させているので、破壊した場合と異なり、セラミック製
品が無駄とならない。また、非破壊なので、破壊により
生じた新たな表面に水が吸着されることもなく、かつ局
所的な水分吸着量のバラツキの影響も受けず、セラミッ
ク焼結体の水分量をそのまま正確に測定できる。しかも
、破壊のための手間もかからない。(Effects of the Invention) According to the method for measuring the moisture content of a ceramic sintered body according to the present invention, the ceramic sintered body is heated non-destructively to vaporize the moisture, so unlike when the ceramic sintered body is destroyed, the ceramic product is It won't go to waste. In addition, since it is non-destructive, water will not be adsorbed to the new surface created by destruction, and it will not be affected by local variations in the amount of water adsorption, allowing accurate measurement of the water content of the ceramic sintered body. can. Moreover, it does not take much effort to destroy it.
しかも、非破壊で加熱して、吸着水分を気化させ、これ
をカールフィッシャー試薬を用いて滴定しているので極
めて正確で精度の高い測定が可能となる。しかも、セラ
ミック焼結体が表面から吸湿が進行するという特異性を
利用したものであり、焼結体であるから組織内部には水
分がほとんどない。従って、非破壊で加熱することで含
有水分を速やかに、かつ完全に気化させうるのであり、
これにより高精度の測定を初めて実現できる。Furthermore, since the adsorbed moisture is vaporized by non-destructive heating and titrated using Karl Fischer reagent, extremely accurate and highly accurate measurements are possible. Furthermore, this method takes advantage of the unique property of a ceramic sintered body that moisture absorption progresses from the surface, and since it is a sintered body, there is almost no moisture inside the structure. Therefore, by heating non-destructively, the contained moisture can be quickly and completely vaporized.
This makes it possible to achieve highly accurate measurements for the first time.
本発明に係わるセラミック焼結体の水分量の測定装置に
よれば、セラミック焼結体を非破壊で予備収容部内に収
容し、この予備収容部内の気体を乾燥雰囲気で置換し、
その後セラミック焼結体を加熱部に移送し、加熱して水
分を気化させている。According to the apparatus for measuring the moisture content of a ceramic sintered body according to the present invention, the ceramic sintered body is non-destructively accommodated in the pre-accommodation part, the gas in the pre-accommodation part is replaced with a dry atmosphere,
Thereafter, the ceramic sintered body is transferred to a heating section and heated to vaporize moisture.
従って、前記気体中の湿気を検出することはなく、正確
な水分量測定が可能となり、本発明の方法を良好に遂行
できる。Therefore, there is no need to detect moisture in the gas, making it possible to accurately measure the amount of moisture, allowing the method of the present invention to be carried out satisfactorily.
第１図は水分測定装置の全体の概略図、第２図は曝露時
間と水分吸湿量の関係を示すグラフ、
第３図はＩＩ１％露後の重量増加量と水分検出量との関
係を示すグラフである。
第２図
榎露時聞ｔ“（Ｓｅｃ）”Figure 1 is a schematic diagram of the entire moisture measuring device, Figure 2 is a graph showing the relationship between exposure time and moisture absorption, and Figure 3 is a graph showing the relationship between weight increase after II 1% dew and the amount of moisture detected. It is a graph. Figure 2 Enokiro Jimon t “(Sec)”
Claims (1)
た水分を気化させ、気化した水分をカールフィッシャー
試薬を用いて滴定し、前記水分量を定量する、セラミッ
ク焼結体の水分量の測定方法。 ２、セラミック焼結体を非破壊で収容する予備収容部と
；この予備収容部内に乾燥雰囲気を送って前記予備収容
部内の気体を前記乾燥雰囲気で置換する手段と；前記予
備収容部に収容されたセラミック焼結体を加熱部へと移
送する移送手段と；前記加熱部に収容された前記セラミ
ック焼結体を加熱してこれに吸着した水分を気化させる
加熱手段と；気化した水分をカールフィッシャー試薬を
用いて滴定し、前記水分量を定量するための滴定部と；
気化した水分を前記滴定部に移送する手段と を有するセラミック焼結体の水分量の測定装置。[Claims] 1. A ceramic sintered body that non-destructively heats a ceramic sintered body to vaporize the moisture adsorbed thereto, and titrates the vaporized moisture using a Karl Fischer reagent to quantify the amount of moisture. How to measure the water content of solid bodies. 2. A pre-accommodating part for non-destructively accommodating the ceramic sintered body; means for sending a dry atmosphere into the pre-accommodating part to replace the gas in the pre-accommodating part with the dry atmosphere; a transfer means for transferring the ceramic sintered body to a heating section; a heating means for heating the ceramic sintered body housed in the heating section and vaporizing moisture adsorbed thereon; a titration unit for titrating using a reagent to determine the amount of water;
A device for measuring the amount of water in a ceramic sintered body, comprising means for transferring vaporized water to the titration section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13615989A JPH032660A (en) | 1989-05-31 | 1989-05-31 | Method and apparatus for measuring amount of moisture in sintered ceramic body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13615989A JPH032660A (en) | 1989-05-31 | 1989-05-31 | Method and apparatus for measuring amount of moisture in sintered ceramic body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH032660A true JPH032660A (en) | 1991-01-09 |
Family
ID=15168697
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13615989A Pending JPH032660A (en) | 1989-05-31 | 1989-05-31 | Method and apparatus for measuring amount of moisture in sintered ceramic body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH032660A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1993002351A1 (en) * | 1991-07-16 | 1993-02-04 | Tadahiro Ohmi | Method of and device for measuring water content |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61247955A (en) * | 1985-04-26 | 1986-11-05 | Mitsubishi Chem Ind Ltd | Electrolyte for karl fischer coulometric titration |
-
1989
- 1989-05-31 JP JP13615989A patent/JPH032660A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61247955A (en) * | 1985-04-26 | 1986-11-05 | Mitsubishi Chem Ind Ltd | Electrolyte for karl fischer coulometric titration |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1993002351A1 (en) * | 1991-07-16 | 1993-02-04 | Tadahiro Ohmi | Method of and device for measuring water content |
| US5504009A (en) * | 1991-07-16 | 1996-04-02 | Tadahiro Ohmi | Method of and device for measuring water content |
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