JPH02306088A - Freeze drying vessel - Google Patents

Freeze drying vessel

Info

Publication number
JPH02306088A
JPH02306088A JP12525889A JP12525889A JPH02306088A JP H02306088 A JPH02306088 A JP H02306088A JP 12525889 A JP12525889 A JP 12525889A JP 12525889 A JP12525889 A JP 12525889A JP H02306088 A JPH02306088 A JP H02306088A
Authority
JP
Japan
Prior art keywords
particles
frozen
heat
vessel
freeze
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
Application number
JP12525889A
Other languages
Japanese (ja)
Inventor
Ginji Umada
馬田 銀二
Shigenori Aoki
重憲 青木
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujitsu Ltd
Original Assignee
Fujitsu Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Fujitsu Ltd filed Critical Fujitsu Ltd
Priority to JP12525889A priority Critical patent/JPH02306088A/en
Publication of JPH02306088A publication Critical patent/JPH02306088A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To uniformly sublimate solvent of all frozen particles in a short period of time by transferring heat also to the frozen particles of an upper layer via protrusions provided on the bottom of a vessel simultaneously upon transferring of heat to the frozen particles of a lower layer when many frozen particles are filled in the vessel, and heated in a reduced pressure chamber to sublimate the solvent. CONSTITUTION:Ceramic powder made of aluminum sulfate and zirconia and water are mixed. The mixture liquid is injected from a nozzle 11 into liquid nitrogen 9 while agitating the nitrogen 9 in a tank 8 by an agitator 10 to be momentarily frozen to be solidified in particles having 1-5mm of diameter. A vessel 4 in which many frozen particles 6 are filled is placed on a heat transfer plate 7 in which a heater 15 is buried, and introduced into a reduced pressure chamber 16. Then the chamber 16 is evacuated by a rotary pump 18, reduced under pressure to approx. 0.1Torr, the heater 15 is then energized to heat a freeze drying vessel via the plate 7. The heat is transferred to the bottom of the vessel 4 to conduct the particles 6 with protrusions 5 to the particles 6 of an upper layer, thereby completing uniformly covered ceramic particles.

Description

【発明の詳細な説明】 (概 要〕 凍結乾燥用容器に関し、更に詳しく言えば、セラミック
粉末と金属化合物の水溶液との混合液を凍結して粒状に
固めたものを多数個入れ、これらを減圧状態で加熱して
溶媒のみを昇華させるための凍結乾燥用容器に関し、 短時間に溶媒のみを昇華させることのできる凍結乾燥用
容器をf!供することを目的とし、容器内部の底面に複
数の突起部を有することを含み構成する。
[Detailed Description of the Invention] (Summary) Regarding a freeze-drying container, to be more specific, a large number of frozen and solidified granules of a mixture of ceramic powder and an aqueous solution of a metal compound are placed in the container, and the containers are dried under reduced pressure. Concerning freeze-drying containers for sublimating only the solvent by heating in It consists of having a section.

〔産業上の利用分野〕[Industrial application field]

凍結乾燥用容器に関し、更に詳しく言えば、セラミック
粉末と金属化合物の水溶液との混合液を凍結して粒状に
固めたものを多数個入れ、これらを減圧状態で加熱して
溶媒のみを4華させるための凍結乾燥用容器に関する。
Regarding the freeze-drying container, in more detail, a large number of frozen and solidified granular mixtures of ceramic powder and an aqueous solution of metal compounds are placed in the container, and these are heated under reduced pressure to dissolve only the solvent. Container for freeze-drying.

半導体装置の絶縁用下地基板として、安価で、加工の容
易なセラミックガラス基板が用いられている。このセラ
ミックガラス基板には補強材としてジルコニアなどのセ
ラミック粒子が充填される。
Ceramic glass substrates, which are inexpensive and easy to process, are used as insulating base substrates for semiconductor devices. This ceramic glass substrate is filled with ceramic particles such as zirconia as a reinforcing material.

しかし、ガラスの焼結時の加熱処理による温度上昇でガ
ラス材とセラミック粒子とが反応し、別の反応生成物が
生じる。このため、補強効果が弱まるという不都合があ
る。
However, the glass material and ceramic particles react with each other due to the temperature increase caused by the heat treatment during glass sintering, producing other reaction products. Therefore, there is a disadvantage that the reinforcing effect is weakened.

この対策として、セラミック粒子の表面をアルミナ膜で
均一に被覆してガラス材とセラミック粒子との反応を防
止することが必要になる。
As a countermeasure to this problem, it is necessary to uniformly coat the surfaces of the ceramic particles with an alumina film to prevent the reaction between the glass material and the ceramic particles.

凍結乾燥法はこのようなセラミック粒子を作成すること
ができる方法の−っである。
Freeze-drying is one method by which such ceramic particles can be made.

〔従来の技術] 第3図、第4図及び第5図は凍結乾燥法によりセラミッ
ク粒子の表面を硫酸アルミニウムの膜で均一に被覆する
方法を説明する図で、セラミック粒子の表面をアルミナ
膜で均一に被覆するための前段の工程にあたる。
[Prior Art] Figures 3, 4, and 5 are diagrams illustrating a method for uniformly coating the surfaces of ceramic particles with an aluminum sulfate film by freeze-drying. This is the first step to ensure uniform coating.

まず、第3図に示すように、硫酸アルミニウムの水溶液
にセラミック粉末を混入した混合液を液体窒素9巾に滴
下し、瞬間的に凍結して粒状に固化する。このとき、硫
酸アルミニウムは当初液状であったので、セラミック粒
子の間にすきまなく入り込むことができ、このためセラ
ミック粒子の表面を均一に被覆することができる。
First, as shown in FIG. 3, a mixture of ceramic powder mixed into an aqueous solution of aluminum sulfate is dropped into a 9-width area of liquid nitrogen, and is instantly frozen and solidified into particles. At this time, since the aluminum sulfate was initially in a liquid state, it could enter between the ceramic particles without any gaps, and therefore the surfaces of the ceramic particles could be coated uniformly.

次いで、この凍結粒6を第5図に示すステンレス製の凍
結乾燥用容器に入れる。その後、第4図に示すように、
ヒータI5の埋込まれた熱伝達板7にこの容器1を載せ
て減圧室16内に入れた後、減圧室16内を排気して減
圧する。
Next, the frozen particles 6 are placed in a stainless steel freeze-drying container shown in FIG. After that, as shown in Figure 4,
After this container 1 is placed on the heat transfer plate 7 in which the heater I5 is embedded and placed in the decompression chamber 16, the inside of the decompression chamber 16 is evacuated and the pressure is reduced.

次に、凍結乾燥用容器1をヒータ15により加熱すると
、容器l内の凍結粒6に含まれる水分のみが昇華する。
Next, when the freeze-drying container 1 is heated by the heater 15, only the water contained in the frozen particles 6 in the container 1 sublimates.

その結果、硫酸アルミニウムが表面に均一に被覆された
セラミック粒子の固形物が完成する。
As a result, a solid body of ceramic particles whose surfaces are uniformly coated with aluminum sulfate is completed.

その後、この固形物を1200 ’Cの酸素雰囲気中で
加熱することにより、硫酸アルミニウムの硫酸が蒸発す
るとともにアルミニウムが酸化され、セラミック粒子の
表面はアルミナ膜によって均一に被覆されることになる
Thereafter, by heating this solid material in an oxygen atmosphere at 1200'C, the sulfuric acid in aluminum sulfate is evaporated and the aluminum is oxidized, so that the surfaces of the ceramic particles are uniformly coated with an alumina film.

[発明が解決しようとする課題] ところで、凍結乾燥用容器Iに入れた凍結粒6を減圧室
16内で加熱して、凍結粒6に金主れる水分を昇華させ
るとき、次のような問題が起こる。
[Problems to be Solved by the Invention] By the way, when the frozen grains 6 placed in the freeze-drying container I are heated in the decompression chamber 16 to sublimate the water contained in the frozen grains 6, the following problems occur. happens.

即ち、減圧室16内でヒータ15により凍結粒6を加熱
する場合、熱は主に凍結乾燥用容器1の底部を伝導する
。このため、凍結乾燥用容器1の底部に接していない上
の方の凍結粒6には熱がなかなか伝わらず、下の方の粒
子に比べて水分の昇華が遅くなる。従って、すべての凍
結粒6の水分を昇華させるには長時間を要するという問
題がある。
That is, when the frozen grains 6 are heated by the heater 15 in the reduced pressure chamber 16, the heat is mainly conducted through the bottom of the freeze-drying container 1. For this reason, heat is not easily transferred to the upper frozen particles 6 that are not in contact with the bottom of the freeze-drying container 1, and sublimation of water is slower than in the lower particles. Therefore, there is a problem in that it takes a long time to sublimate the water in all the frozen particles 6.

この対策として、凍結乾燥用容器1に入れる凍結粒6の
数を少なくすると、処理回数が増え、手間がかかるとい
う問題がある。
As a countermeasure to this problem, if the number of frozen grains 6 placed in the freeze-drying container 1 is reduced, there is a problem in that the number of times of processing increases and it takes time and effort.

更に、上から光等を照射して輻射熱を利用する方法では
、逆に、下の方の凍結粒6の水分の昇華が遅くなり、そ
の結果すべての凍結粒6の水分を昇華させるのに長時間
を要することになる。
Furthermore, in the method of using radiant heat by irradiating light or the like from above, on the contrary, the sublimation of the water in the lower frozen grains 6 is delayed, and as a result, it takes a long time to sublimate the water in all the frozen grains 6. It will take time.

本発明は、かかる従来の問題点に鑑みてなされたもので
、短時間に溶媒のみを昇華させることのできる凍結乾燥
用容器を提供することを目的とするものである。
The present invention was made in view of such conventional problems, and an object of the present invention is to provide a freeze-drying container that can sublimate only the solvent in a short time.

〔課題を解決するための手段〕[Means to solve the problem]

上記課題は、第1図の本発明の実施例の凍結乾燥用容器
を示す斜視図に示すように、容器4内部の底面に複数の
突起部5を有することを特徴とする凍結乾燥用容器によ
って解決される。
The above problem can be solved by a freeze-drying container characterized by having a plurality of protrusions 5 on the bottom surface inside the container 4, as shown in the perspective view of the freeze-drying container according to the embodiment of the present invention in FIG. resolved.

〔作 用〕[For production]

即ち、本発明の凍結乾燥用容器においては、容器4内部
の底面に複数の突起部5を備えている。
That is, in the freeze-drying container of the present invention, a plurality of protrusions 5 are provided on the bottom surface inside the container 4.

このため、第2図に示すように、容器4内に固体粒子と
溶媒とを混合して固化させた凍結粒6を多数人れて容器
4底部を加熱した場合、熱は底部から直接下層の凍結粒
6に伝わるだけでなく、突起部5を伝導して上層の凍結
粒6にも均等に伝わるので、短時間にすべての凍結粒6
に含まれる溶媒を昇華させることができる。
Therefore, as shown in Fig. 2, when a large number of frozen particles 6 made by mixing solid particles and a solvent are placed in the container 4 and the bottom of the container 4 is heated, the heat is directly transferred from the bottom to the lower layer. It is transmitted not only to the frozen grains 6, but also to the frozen grains 6 in the upper layer through the protrusion 5, so that all the frozen grains 6 are transmitted in a short time.
It is possible to sublimate the solvent contained in the

〔実施例] 次に、図を参照しながら本発明の実施例について説明す
る。
[Example] Next, an example of the present invention will be described with reference to the drawings.

第1図は、本発明の実施例の凍結乾燥用容器を示す斜視
図である。
FIG. 1 is a perspective view showing a freeze-drying container according to an embodiment of the present invention.

同回において、4は幅30cm、奥行40cm、高さ4
C11のステンにスからなる凍結乾燥用容器、5は該容
Rif4の底面に縦、横それぞれ10mmの間隔で設け
られた直径10m高さ3olIII!1のステンレスか
らなる多数の突起部である。
In the same episode, 4 has a width of 30 cm, a depth of 40 cm, and a height of 4.
A freeze-drying container 5 made of C11 stainless steel is installed on the bottom of the container Rif4 at intervals of 10 mm both vertically and horizontally, and has a diameter of 10 m and a height of 3olIII! These are a large number of protrusions made of stainless steel.

次に、この凍結乾燥用容器4を用いた凍結乾燥法につい
て第1図〜第4図を参照しながら説明する。図では、凍
結乾燥法により、硫酸アルミニウムが表面に均一に被覆
されたセラミック粒子の固形物を作成する場合について
示しである。
Next, a freeze-drying method using this freeze-drying container 4 will be explained with reference to FIGS. 1 to 4. The figure shows a case where a solid material of ceramic particles whose surfaces are uniformly coated with aluminum sulfate is prepared by a freeze-drying method.

まず、硫酸アルミニウム100gとジルコニアからなる
セラミック粉末100gと水1000gとを混合させる
First, 100 g of aluminum sulfate, 100 g of ceramic powder made of zirconia, and 1000 g of water are mixed.

次に、第3図に示すように、槽8内の液体窒素9を攪拌
器10で攪拌しながら、この混合液をノズル11から液
体窒素9の中へi!1ffl噴出して瞬間的に凍結させ
、直径1〜5論の粒状に固化させる。
Next, as shown in FIG. 3, while stirring the liquid nitrogen 9 in the tank 8 with the stirrer 10, this liquid mixture is poured into the liquid nitrogen 9 through the nozzle 11. Squirt out 1 ffl and freeze instantly to solidify into particles with a diameter of 1 to 5 mm.

このとき硫酸アルミニウムは当初水に溶解して液状にな
っていたので、セラミック粒子の間にすきまなく入り込
んでおり、粒子の表面を均一に被覆することになる。こ
のようにして凍結粒6が作成される。
At this time, since the aluminum sulfate was initially dissolved in water and became liquid, it entered between the ceramic particles without any gaps, and the surfaces of the particles were uniformly coated. In this way, frozen grains 6 are created.

次いで、この凍結粒6を第1図に示す凍結乾燥用容器4
に多数人れる。このときC様子を第2図に示す。
Next, the frozen particles 6 are placed in a freeze-drying container 4 shown in FIG.
Many people will be there. The state of C at this time is shown in FIG.

次に、第4図に示すように、多数の凍結粒6が入った該
容器4をヒータ15の埋込まれた熱伝達板7上に代置し
、減圧室16内に入れる。
Next, as shown in FIG. 4, the container 4 containing a large number of frozen particles 6 is placed on a heat transfer plate 7 in which a heater 15 is embedded, and placed in a decompression chamber 16.

次いで、真空配管19を介して減圧室16と接続された
ロークリポンプ18で減圧室16内を排気し、該室内の
圧力を0. ITorr稈度に減圧した後、ヒータ15
に通電して発熱させ、熱伝達板7を介して凍結乾燥用容
器を加熱する。このとき、加熱温度を約30°Cに保持
する。すると、第2図に示すように、熱は容器4の底部
を伝導して、一部は直接凍結粒6に伝わり、他の一部は
各突起部5を伝導して上層の凍結粒6に伝わる。その結
果、全ての凍結粒6の水分はほぼ同時に、かつ短時間に
昇華して硫酸アルミニウムが表面に均一に被覆されたセ
ラミック粒子の固形物が完成する。
Next, the inside of the decompression chamber 16 is evacuated by the vacuum pump 18 connected to the decompression chamber 16 via the vacuum piping 19, and the pressure inside the chamber is reduced to 0. After reducing the pressure to ITorr, the heater 15
is energized to generate heat, and the freeze-drying container is heated via the heat transfer plate 7. At this time, the heating temperature is maintained at about 30°C. Then, as shown in FIG. 2, some of the heat is conducted through the bottom of the container 4 and is directly transferred to the frozen particles 6, while the other part is conducted through each protrusion 5 and transferred to the frozen particles 6 in the upper layer. Conveyed. As a result, the water content of all the frozen particles 6 sublimates almost simultaneously and in a short period of time, completing solid ceramic particles whose surfaces are uniformly coated with aluminum sulfate.

その後、この固形物を1200℃の酸素雰囲気中で加熱
することにより、硫酸は蒸発して除去されるとともに、
残ったアルミニウムは酸化されてセラミック粒子の表面
はアルミナ膜によって均一に被覆されることになる。
Thereafter, by heating this solid in an oxygen atmosphere at 1200°C, the sulfuric acid is evaporated and removed.
The remaining aluminum is oxidized and the surfaces of the ceramic particles are uniformly covered with an alumina film.

なお、コールドトラップ17は昇華した水分をトラップ
するために減圧室16とロークリポンプ18との間に真
空配管19を介して、接続されている。
Note that the cold trap 17 is connected via a vacuum pipe 19 between the decompression chamber 16 and the low-pressure pump 18 in order to trap sublimated moisture.

このように、本発明の実施例の凍結乾燥用容器4によれ
ば、短時間に全ての凍結粒6の水分を昇華できるのでス
ループットの向上を図ることができる。
As described above, according to the freeze-drying container 4 of the embodiment of the present invention, all of the water in the frozen particles 6 can be sublimated in a short time, so that throughput can be improved.

〔発明の効果] 以上のように、本発明の凍結乾燥用容器によれば、該容
器内に多数の凍結粒を入れ、減圧室内で加熱して溶媒を
昇華させる際、下層の凍結粒に熱が伝わるのとほぼ同時
に容器底面に設けられた突起部を介して上層の凍結粒に
も熱が伝わるので、全ての凍結粒の溶媒を短時間に、か
つ均一に肩車させることができる。
[Effects of the Invention] As described above, according to the freeze-drying container of the present invention, when a large number of frozen grains are placed in the container and heated in a vacuum chamber to sublimate the solvent, heat is applied to the frozen grains in the lower layer. Almost at the same time as the heat is transferred, the heat is also transferred to the frozen particles in the upper layer via the protrusion provided on the bottom of the container, so that the solvent in all the frozen particles can be uniformly transferred in a short time.

これにより、スループントの向上を図ることができる。Thereby, throughput can be improved.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は、本発明の実施例の凍結乾燥用容器を示す斜視
図、 第2図は、本発明の実施例の凍結乾燥用容器の作用を説
明する断面図、 第3図は、凍結粒の作成方法を説明する図、第4図は、
凍結粒を乾燥する方法を説明する図、第5図は、従来例
の凍結乾燥用容器を嬌明畦44示す斜視図である。 第6図は、従来例の凍結乾燥用容器の問題点を説明する
断面図である。 (符号の説明) 1・・・凍結乾燥用容器、 4・・・凍結乾燥用容器(容器)、 5・・・突起部、 6・・・凍結粒、 7・・・熱伝達板、 8・・・槽、   ′ 9・・・液体窒素、 10・・・攪拌器、 11・・・ノズル、 I5・・・ヒータ、 16・・・減圧室、 l7・・・コールドトランプ、 18・・・ロータリーポンプ、 19・・・真空配管。
FIG. 1 is a perspective view showing a freeze-drying container according to an embodiment of the present invention, FIG. 2 is a cross-sectional view explaining the function of the freeze-drying container according to an embodiment of the present invention, and FIG. 3 is a frozen particle Figure 4 is a diagram explaining how to create the
FIG. 5, which is a diagram illustrating a method of drying frozen grains, is a perspective view showing a conventional freeze-drying container with a ridge 44. FIG. 6 is a sectional view illustrating problems with a conventional freeze-drying container. (Explanation of symbols) 1... Container for freeze-drying, 4... Container for freeze-drying (container), 5... Projection, 6... Frozen grains, 7... Heat transfer plate, 8. ... Tank, '9... Liquid nitrogen, 10... Stirrer, 11... Nozzle, I5... Heater, 16... Decompression chamber, l7... Cold Trump, 18... Rotary Pump, 19...vacuum piping.

Claims (1)

【特許請求の範囲】[Claims] 容器(4)内部の底面に複数の突起部(5)を有するこ
とを特徴とする凍結乾燥用容器。
A freeze-drying container characterized by having a plurality of protrusions (5) on the bottom surface inside the container (4).
JP12525889A 1989-05-18 1989-05-18 Freeze drying vessel Pending JPH02306088A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP12525889A JPH02306088A (en) 1989-05-18 1989-05-18 Freeze drying vessel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP12525889A JPH02306088A (en) 1989-05-18 1989-05-18 Freeze drying vessel

Publications (1)

Publication Number Publication Date
JPH02306088A true JPH02306088A (en) 1990-12-19

Family

ID=14905645

Family Applications (1)

Application Number Title Priority Date Filing Date
JP12525889A Pending JPH02306088A (en) 1989-05-18 1989-05-18 Freeze drying vessel

Country Status (1)

Country Link
JP (1) JPH02306088A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6684524B1 (en) * 1999-08-02 2004-02-03 Bayer Aktiengesellschaft Lyopohilization method
KR100889789B1 (en) * 2007-04-28 2009-03-20 한국기계연구원 Machine for Frozen Drying
JP2015092619A (en) * 2015-01-08 2015-05-14 東京エレクトロン株式会社 Substrate drying method and substrate processing apparatus
WO2022202938A1 (en) * 2021-03-26 2022-09-29 富士フイルム株式会社 Freeze-drying container

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6684524B1 (en) * 1999-08-02 2004-02-03 Bayer Aktiengesellschaft Lyopohilization method
KR100889789B1 (en) * 2007-04-28 2009-03-20 한국기계연구원 Machine for Frozen Drying
JP2015092619A (en) * 2015-01-08 2015-05-14 東京エレクトロン株式会社 Substrate drying method and substrate processing apparatus
WO2022202938A1 (en) * 2021-03-26 2022-09-29 富士フイルム株式会社 Freeze-drying container

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