JPS63105977A - Method for forming thin film - Google Patents
Method for forming thin filmInfo
- Publication number
- JPS63105977A JPS63105977A JP61249543A JP24954386A JPS63105977A JP S63105977 A JPS63105977 A JP S63105977A JP 61249543 A JP61249543 A JP 61249543A JP 24954386 A JP24954386 A JP 24954386A JP S63105977 A JPS63105977 A JP S63105977A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- substrate
- small holes
- apertures
- packing material
- 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.)
- Granted
Links
- 239000010409 thin film Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 239000005373 porous glass Substances 0.000 claims abstract description 17
- 239000011148 porous material Substances 0.000 claims description 23
- 239000000945 filler Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 238000002844 melting Methods 0.000 abstract description 7
- 230000008018 melting Effects 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 229910045601 alloy Inorganic materials 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 5
- 239000012188 paraffin wax Substances 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 4
- 238000001704 evaporation Methods 0.000 abstract description 3
- 238000007747 plating Methods 0.000 abstract description 3
- 238000004544 sputter deposition Methods 0.000 abstract description 3
- 229920002472 Starch Polymers 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 abstract description 2
- 239000008107 starch Substances 0.000 abstract description 2
- 235000019698 starch Nutrition 0.000 abstract description 2
- 239000012808 vapor phase Substances 0.000 abstract description 2
- 238000012856 packing Methods 0.000 abstract 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 16
- 239000011521 glass Substances 0.000 description 10
- 239000012071 phase Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 4
- 238000005191 phase separation Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229940057995 liquid paraffin Drugs 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 150000001298 alcohols Chemical group 0.000 description 2
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011900 installation process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000005295 porous vycor glass Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006268 silicone film Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/0213—Silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0072—Inorganic membrane manufacture by deposition from the gaseous phase, e.g. sputtering, CVD, PVD
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0069—Inorganic membrane manufacture by deposition from the liquid phase, e.g. electrochemical deposition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/08—Specific temperatures applied
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/08—Specific temperatures applied
- B01D2323/081—Heating
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Surface Treatment Of Glass (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
［発明の目的］
（産業上の利用分野）
本発明は多孔質体表面開孔部を覆って薄膜を形成させる
方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Application Field) The present invention relates to a method of forming a thin film covering the pores on the surface of a porous body.
（従来の技術）
Ｐｄ膜、Ｎｉ膜、シリコーンゴム膜、ポリイミド膜等の
薄膜は水素分離、酸素富化等の各種用途に使用される。(Prior Art) Thin films such as Pd films, Ni films, silicone rubber films, and polyimide films are used for various purposes such as hydrogen separation and oxygen enrichment.
従来法にあっては、予め所定厚みの薄膜を製造し、この
薄膜を支持枠等で支持して使用する。薄膜には、このよ
うな枠体への取付方法。In the conventional method, a thin film having a predetermined thickness is manufactured in advance, and this thin film is supported by a support frame or the like for use. For thin films, there is a method for attaching them to the frame like this.
支持方法に耐えるだけの機械的強度を附与する必要があ
り、あまり薄い膜を使用すると枠体への取付工程或は使
用中に破損し易い。又薄膜の厚みには製造工程上の制約
もあり、あまり厚みの小さいものは実用化されていない
。It is necessary to provide mechanical strength sufficient to withstand the supporting method, and if a too thin membrane is used, it is likely to be damaged during the installation process to the frame or during use. Furthermore, there are restrictions on the thickness of the thin film due to the manufacturing process, and thin films have not been put into practical use.
薄膜を支持枠で支持して使用する場合、支持枠開孔部の
ディメンションが小さい程、厚みの小さい膜を使用する
ことが可能となる筈である。又支持枠開孔部を覆って直
接薄膜を形成させることができれば、薄膜を枠体に取付
ける際の破損も生ずることかなく、薄い膜を使用するこ
とか可能となる理である。しかし乍ら、このような技術
的命題を解決する方法は知られておらず、膜厚が大きく
なると性能が低下する場合ても、止むを得ず、厚い膜を
使用せざるを得なかった。When using a thin film supported by a support frame, the smaller the dimension of the support frame aperture, the smaller the thickness of the membrane can be used. Furthermore, if a thin film can be directly formed to cover the support frame opening, it will be possible to use a thin film without causing damage when attaching the thin film to the frame. However, there is no known method to solve such a technical problem, and even if the performance deteriorates as the film thickness increases, thick films have been unavoidably used.
（発明が解決しようとする問題点）
本発明は従来技術が有していた前述の問題点を解決し、
従来知られていなかった枠体の開孔部を覆って直接薄膜
を形成する方法を新規に提供することを目的とするもの
である。(Problems to be Solved by the Invention) The present invention solves the aforementioned problems that the prior art had,
The object of the present invention is to provide a new method of directly forming a thin film to cover the apertures of a frame, which has not been known in the past.
［発明の構成］
（問題点を解決するための手段）
本発明は前述の問題点を解決すべくなされたものであり
、表面に開孔する多数の小孔を有する基体の該小孔開孔
部に充填材を充填し、次いで基体表面に薄膜を被着せし
めた後充填材を除去することを特徴とする多孔質体表面
開孔部を覆って薄膜を形成させる方法を提供するもので
ある。[Structure of the Invention] (Means for Solving the Problems) The present invention has been made to solve the above-mentioned problems. The present invention provides a method for forming a thin film covering the openings on the surface of a porous body, the method comprising: filling the porous body with a filler, then depositing the thin film on the surface of the substrate, and then removing the filler. .
本発明においては、表面に開孔する多数の小孔を有する
多孔質体を使用する。このような多孔質体としては／１
ｆＬｔＣｈ等のセラミックス微粒の焼結体、金属微粒の
焼結体、多孔質硝子が例示されるか、多孔質硝子を使用
するのが好ましい。In the present invention, a porous body having a large number of small pores on its surface is used. For such a porous body, /1
Examples include a sintered body of fine ceramic particles such as fLtCh, a sintered body of fine metal particles, and porous glass, and it is preferable to use porous glass.
多孔質硝子としてはバイコール硝子、或はＳｉＯ□４５
〜７０ ｗｔ％、 Ｂ２０．８”’−３０ｗｔ％。As the porous glass, Vycor glass or SiO□45
~70 wt%, B20.8''-30 wt%.
ＣａＯ３〜２５ｗｔ％、 Ａｎ Ｊ−３５〜１５ ｗ
ｔ％。CaO3~25wt%, An J-35~15w
t%.
Ｎａ、０３〜８％、に２０１〜５％、 Ｎａ２Ｏ＋に
２０４〜１３ｗｔ％、 Ｍｇ００〜８ｗｔ％なる組成を
有する硝子（以下硝子Ａという）又はＳｉＯ□４５〜７
０ｗｔ％、 Ｂ２０．８〜３０ｗｔ％、 Ｃａ０８〜
２５ｗｔ％。Glass (hereinafter referred to as glass A) or SiO□45-7 having a composition of Na, 03-8%, 201-5%, Na2O+ 204-13wt%, and Mg 00-8wt%.
0wt%, B20.8~30wt%, Ca08~
25wt%.
Ａｌ２Ｏ，５〜１５％なる組成を有する硝子（以下硝子
Ｂという）を熱処理してＢ２０． 、 ＣａＯを主体と
する相を分相せしめ、この相を溶解除去することによっ
て得られる多孔質硝子（以下、多孔質硝子Ａ又はＢと呼
ぶ）が特に適当である。Glass having a composition of 5 to 15% Al2O (hereinafter referred to as glass B) is heat-treated to obtain B20. A porous glass (hereinafter referred to as porous glass A or B) obtained by phase-separating a phase mainly composed of CaO and dissolving and removing this phase is particularly suitable.
上述した組成を有する硝子Ａ又はＢの上記成分のうちＳ
ｉＯ□は分相、除去工程によって得られる多孔硝子の骨
格を形成するための基幹成分であり、 ＡＭ 、０．は
補助成分として得られた多孔硝子の脆さを減少させる作
用を有する。ＢｚＯ：＋は一方において多孔硝子の骨格
を形成する補助成分として機能するが、他方ＣａＯと協
同して、熱処理によって微少な分相を生成する作用を有
する。そしてこのようにして生成したＣａｂ、 Ｂ２
０：ｌを主成分とする分相を溶解除去することによって
多孔質硝子が形成される。Among the above components of glass A or B having the above composition, S
iO□ is a basic component for forming the framework of porous glass obtained by the phase separation and removal process, and AM, 0. has the effect of reducing the brittleness of the porous glass obtained as an auxiliary component. On the one hand, BzO:+ functions as an auxiliary component that forms the framework of the porous glass, but on the other hand, in cooperation with CaO, it has the effect of producing minute phase separation by heat treatment. And the Cab generated in this way, B2
Porous glass is formed by dissolving and removing the separated phase mainly composed of 0:l.
Ｂ２Ｏ３は上述の説明からも首肯しつるように小孔の大
きさを決定する重要な因子であり、分相中に移行して除
去されるＢ２０：Ｉ量、或は逆に多孔硝子中に残存する
８２ｏｚ 量は、小孔の径の均一性と密接な関係を有す
ることか判明した。As can be seen from the above explanation, B2O3 is an important factor that determines the size of the pores, and the amount of B20:I transferred and removed during phase separation, or conversely, the amount of B20:I remaining in the porous glass. It has been found that the amount of 82 oz is closely related to the uniformity of the pore diameter.
上記成分を前述の範囲内に保つことにより好適な多孔質
体をうることができる。A suitable porous body can be obtained by keeping the above components within the above ranges.
硝子Ａ、Ｂを所定形状に成型した後熱処理してＣａＯ１
Ｂ２Ｏ３を主体とする相（以下ＣａＯ１Ｂ２Ｏ３相とい
う）を分相せしめる。加熱処理温度が高い程、又熱処理
時間が長い程ＣａＯ１Ｂ２０３相は大きくなり、従って
得られる多孔硝子の小孔の径は大きくなる傾向を有し、
熱処理条件を選択することによって小孔の径を４０〜１
００，０００人の範囲所望の値とすることができる。こ
のようにして得られた多孔質硝子は、小孔の径は均一で
あり、本発明の目的を達成するのに極めて好適なもので
ある。Glasses A and B are molded into a predetermined shape and then heat treated to form CaO1
A phase mainly composed of B2O3 (hereinafter referred to as CaO1B2O3 phase) is phase-separated. The higher the heat treatment temperature and the longer the heat treatment time, the larger the CaO1B203 phase becomes, and therefore the diameter of the small pores of the resulting porous glass tends to become larger.
By selecting the heat treatment conditions, the diameter of the small pores can be adjusted from 40 to 1
00,000 can be any desired value. The porous glass thus obtained has small pores of uniform diameter and is extremely suitable for achieving the object of the present invention.
加熱処理を行った硝子をＨＣＩ 、 Ｈ，ＳＯ，、ＨＮ
Ｏ。The heat-treated glass is HCI, H, SO,, HN
O.
等の酸中に浸漬してＣａＯ１Ｂ２０３相を溶解除去する
。なお酸処理を行なうに先立ち、ＩＦ温溶液短時間その
表面をエツチング処理するのが望ましい。etc. to dissolve and remove the CaO1B203 phase. Note that prior to the acid treatment, it is desirable to etch the surface using an IF warm solution for a short time.
前述したように熱処理の条件によって、得られる多孔硝
子の小孔の径を制御することができるが、小孔の径は多
孔質硝子中に残存するＢ２Ｏ３の量に応じて変化するこ
と及びこのＢ２Ｏ３の量は熱処理、酸処理の条件によっ
て左右されることが判明した。モしてＢ２Ｏ３が望まし
く ０．５ ｗｔ％以上残存するようこれらの条件を定
めることにより特に好適な結果の得られることが判明し
た。As mentioned above, the diameter of the small pores in the resulting porous glass can be controlled by the conditions of heat treatment, but the diameter of the small pores changes depending on the amount of B2O3 remaining in the porous glass, and this B2O3 It has been found that the amount of is influenced by the conditions of heat treatment and acid treatment. It has been found that particularly favorable results can be obtained by setting these conditions so that B2O3 desirably remains in an amount of 0.5 wt% or more.
望ましい処理条件は次の通りである。Desirable processing conditions are as follows.
加熱温度 ６００〜８５０℃
加熱時間 ２〜４８ｈｒ、望ましくは１２〜２４ｈｒ酸
の種類 Ｈｅ文、Ｈ，３０，、ＨＮＯ：１酸の濃度 ０
．０１〜２．ＯＮ、望ましくは０．１〜１、ＯＮ
処理時間 ２〜２０ｈｒ、望ましくは４〜１６ｈｒ温
度 ５０〜９５℃、望ましくは８０〜９０°Ｃ本発明
においては、所定形状に形成した多孔質体を基体として
使用する。このような基体は例えば所定形状に成型した
原料硝子に分相処理、溶解処理を施こすことによって得
ることができる。Heating temperature: 600-850°C Heating time: 2-48 hr, preferably 12-24 hr Type of acid: He, H, 30, HNO: 1 Concentration of acid: 0
．． 01-2. ON, preferably 0.1 to 1, ON Treatment time 2 to 20 hr, preferably 4 to 16 hr Temperature
Temperature: 50 to 95°C, preferably 80 to 90°C In the present invention, a porous body formed into a predetermined shape is used as a substrate. Such a substrate can be obtained, for example, by subjecting raw material glass molded into a predetermined shape to phase separation treatment and dissolution treatment.
基体の小孔開孔部に充填材を充填し、小孔を閉塞し、こ
の状態で基体表面に薄膜を被着せしめることにより、基
体開孔部を覆って薄膜を形成させ、次いて充填材を除去
することにより、多孔質伸開孔部を支持枠とした薄膜を
形成させることができる。多孔質体の開口部の大きさは
極めて小さく直径４０〜ｔｏｏ、ｏｏｏ人程度とするこ
とができ、薄膜はこの開孔部を覆って直接形成されるの
で、本発明の方法によるときは、０．５ル程度の薄膜を
破損の恐れなく製造、使用することが可能となった。Filling material is filled into the small pores of the substrate to close the small pores, and in this state, a thin film is applied to the surface of the substrate to form a thin film covering the openings of the substrate. By removing , it is possible to form a thin film using the porous expanded pores as a support frame. The size of the opening in the porous body is extremely small and can be approximately 40 to 40 mm in diameter, and the thin film is formed directly covering this opening, so when using the method of the present invention, It has become possible to manufacture and use thin films of approximately .5 µm without fear of damage.
充填材としてはパラフィン、低融点合金。Paraffin and low melting point alloys are used as fillers.
ＣＭＣ（カルボキシメチルセルローズ）、Ｗ粉等を用い
ることができる。これらの充填材は溶融或は溶解して液
状として使用し、小孔中に充填した後、冷却或は溶媒の
蒸発等の手段により望ましくは固化せしめる。CMC (carboxymethyl cellulose), W powder, etc. can be used. These fillers are melted or dissolved and used in a liquid state, and after being filled into the small holes, they are desirably solidified by means such as cooling or evaporation of the solvent.
小孔に充填する手段に特に限定はないか、基体の一方の
側を減圧状態として、上記のような充填材を含む液体を
基体の組方の側に接触させて吸引する方法、或は基体を
容器中に収納し、容器を真空源と接続して基体の小孔中
に含まれる空気を充分脱気し、次いで容器中に充填材を
含む液体を注入する等の方法を用いることがてきる。There are no particular limitations on the means for filling the small pores, or there may be a method in which one side of the substrate is under reduced pressure and a liquid containing the filler as described above is brought into contact with the assembled side of the substrate and suctioned, or It is possible to use a method such as storing the filler in a container, connecting the container to a vacuum source to sufficiently degas the air contained in the small pores of the substrate, and then injecting a liquid containing the filler into the container. Ru.
小孔を閉塞した基体上に薄膜を形成させる。この際基体
の開孔部以外の表面部分に耐着している充填材は、予め
充分除去するのが適当である。A thin film is formed on the substrate with the small pores closed. At this time, it is appropriate to sufficiently remove the filler that has adhered to the surface of the substrate other than the openings in advance.
薄膜の種類及び形成方法には特に限定はなく、形成方法
としては化学メッキ法、気相法、スパッタリング法、真
空蒸着法、塗布法等の公知の方法を、又薄膜としては金
属膜、セラミックス膜、プラスチック膜、ゴ゛ム膜、シ
リコーン膜等を例示することができ、０．５〜５０ＪＬ
程度の薄膜を形成させることができる。なお充填材は、
薄膜を形成する際、薄膜を形成すべき材料が、小孔中に
侵入するのを防止し、該材料を支持する作用を有するも
のであれば足り、必ずしも固体である必要はなく、流動
パラフィン、寒天、水銀、比較的粘稠な澱粉糊等を用い
ることも可能である。There are no particular limitations on the type and formation method of the thin film, and known methods such as chemical plating, vapor phase method, sputtering, vacuum evaporation, and coating methods may be used, and metal films and ceramic films may be used as the thin film. , plastic film, rubber film, silicone film, etc., and 0.5 to 50 JL
It is possible to form a thin film of approximately The filling material is
When forming a thin film, it is sufficient that the material to form the thin film has the function of preventing intrusion into the pores and supporting the material, and does not necessarily have to be a solid, such as liquid paraffin, It is also possible to use agar, mercury, relatively viscous starch paste, etc.
又成る種の液体も充填材として機能することが判明した
。例えば［Ｐｄ（ＮＨ：＋）４］ Ｃ１２を用いて化学
メッキ法によってＰｄ膜を形成させる際、低級アルコー
ルか有効に機能することか判明した。Other types of liquids have also been found to function as fillers. For example, it has been found that when a Pd film is formed by chemical plating using [Pd(NH:+)4]C12, lower alcohols function effectively.
その作用については明らかではないが、［Ｐｄ（ＮＨ：
＋）４１ Ｃ１２は低級アルコールに溶解性を有しない
ため、低級アルコールを充填した基体に［Ｐｄ（Ｎｔｌ
：＋） ４］ Ｃ交２溶液を接触せしめると、界面にお
いてｃ ｐｄ（Ｎｏ、）、】Ｃｘ ２が析出することも
一因と考えられる。Although its effect is not clear, [Pd(NH:
+)41 Since C12 has no solubility in lower alcohols, [Pd(Ntl
:+) 4] It is thought that one reason is that c pd(No, ), ]Cx 2 is precipitated at the interface when the C2 solution is brought into contact.
薄膜を形成させた後、充填材を除去する。除去手段に特
に限定はなく、加熱溶融蒸発、物理的又は化学的溶解或
は化学分解等の手段を例示することができる。例えばパ
ラフィン、低融点合金は加熱溶融、或は物理的又は化学
的溶解によって、澱粉質充填材は酵素を用いて分解する
ことにより除去することができる。After forming the thin film, the filler is removed. There is no particular limitation on the removal means, and examples include means such as heating melting and evaporation, physical or chemical dissolution, and chemical decomposition. For example, paraffin and low melting point alloys can be removed by heat melting or physical or chemical dissolution, and starchy fillers can be removed by decomposing them using enzymes.
本発明薄膜は各種用途に使用することかてきる。The thin film of the present invention can be used for various purposes.
例えば多孔質硝子を基体として用いてＰｄ膜を形成させ
、水素分離用媒体として用いることができる。又ＡＪ１
２０３粒焼結体を基体として用い、極めて微少な小孔を
有するセラミック薄膜を形成させ、或は金属膜を形成さ
せ、フィルターとして用いることもできる。For example, a Pd film can be formed using porous glass as a substrate and used as a hydrogen separation medium. Also AJ1
It is also possible to use the 203-grain sintered body as a substrate to form a ceramic thin film having extremely small pores, or to form a metal film and use it as a filter.
（作 用）
基体小孔開口部に充填された充填材が、基体表面に薄膜
を形成させる際の支持体として機能し、小孔開口部を覆
って簿膜が形成され、開口部が薄膜の支持枠として機能
する。(Function) The filler filled in the opening of the small pore of the substrate functions as a support when forming a thin film on the surface of the substrate, and a film is formed covering the opening of the small pore, and the opening becomes a part of the thin film. Acts as a support frame.
（実施例）
平均５．０（１（］λの多数の小孔を有する、Ａ！Ｑ、
Ｑ３焼結体よりなる板状体（厚み１ｏｎｎ、大きさ１０
ｃｍＸ １０ｃｍ）を基体として使用した。(Example) A!Q, having a large number of small holes with an average of 5.0(1(]λ)
A plate-shaped body made of Q3 sintered body (thickness 1 onn, size 10
cm×10 cm) was used as the substrate.
この基体を容器中に収納して脱気し、該容器中に流動パ
ラフィンを注入し、基体の開口部を流動パラフィンで充
填した。表面に付着したパラフィンを充分除去し、その
−面に銀鏡反応を利用し、厚さ２〜３ｗのＡｇ膜を形成
させ、次いで基体なで充分洗滌し、充填されたパラフィ
ンを除去することにより ＡＪ１２ｏｚ焼結体の開口部
を覆って厚さ２〜３用のＡｇ薄膜を形成させた。This substrate was placed in a container and degassed, and liquid paraffin was poured into the container to fill the opening of the substrate with liquid paraffin. By thoroughly removing the paraffin attached to the surface, forming an Ag film with a thickness of 2 to 3 w on the surface using a silver mirror reaction, and then thoroughly washing the base with the substrate to remove the filled paraffin, AJ12oz. A thin Ag film having a thickness of 2 to 3 was formed to cover the opening of the sintered body.
（実施例２）
平均４０人の多数の小孔を有するバイコール硝子よりな
る実施例１ど同一の大きさの板状体を基体として使用し
た。(Example 2) A plate-shaped body made of Vycor glass having a large number of pores of 40 on average and having the same size as in Example 1 was used as a substrate.
実施例１と同様の手段により開口部に低融点合金を充填
し、スパッタリング法により厚み０．５ルＡｕ膜を形成
させた。The opening was filled with a low melting point alloy by the same means as in Example 1, and a 0.5 μl thick Au film was formed by sputtering.
充填された合金な賄処理によって除去し、バイコール硝
子の開口部を覆って厚さｏ、ｓ ＪＬのＡｕ製薄膜を形
成させた。The filled alloy was removed by polishing, and a thin Au film having a thickness of o and sJL was formed covering the opening of the Vycor glass.
Claims (3)
開孔部に充填材を充填し、次いで基体表面に薄膜を被着
せしめた後充填材を除去することを特徴とする多孔質体
表面開孔部を覆って薄膜を形成させる方法。(1) A substrate having a large number of small pores on its surface is filled with a filler, and then a thin film is deposited on the surface of the substrate, and then the filler is removed. A method of forming a thin film covering the pores on the surface of a porous body.
許請求の範囲第１項記載の薄膜を形成させる方法。(2) The method for forming a thin film according to claim 1, wherein the porous body is porous glass.
とを特徴とする特許請求の範囲第１項又は第２項記載の
薄膜を形成させる方法。(3) The method for forming a thin film according to claim 1 or 2, characterized in that the size of the small pores is 40 to 100,000 Å.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61249543A JPS63105977A (en) | 1986-10-22 | 1986-10-22 | Method for forming thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61249543A JPS63105977A (en) | 1986-10-22 | 1986-10-22 | Method for forming thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63105977A true JPS63105977A (en) | 1988-05-11 |
| JPH0568553B2 JPH0568553B2 (en) | 1993-09-29 |
Family
ID=17194552
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61249543A Granted JPS63105977A (en) | 1986-10-22 | 1986-10-22 | Method for forming thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63105977A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007517655A (en) * | 2004-01-09 | 2007-07-05 | ビーピー ピー・エル・シー・ | Metal palladium composite membrane or alloy palladium composite membrane and method for producing the same |
| JP2008018387A (en) * | 2006-07-14 | 2008-01-31 | Ngk Insulators Ltd | Method for applying seed crystal to porous base material |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1208189B1 (en) | 1999-05-28 | 2004-10-06 | Cepheid | Device and method for analysing liquid samples |
| US9073053B2 (en) | 1999-05-28 | 2015-07-07 | Cepheid | Apparatus and method for cell disruption |
-
1986
- 1986-10-22 JP JP61249543A patent/JPS63105977A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007517655A (en) * | 2004-01-09 | 2007-07-05 | ビーピー ピー・エル・シー・ | Metal palladium composite membrane or alloy palladium composite membrane and method for producing the same |
| US8052775B2 (en) | 2004-01-09 | 2011-11-08 | Bp P.L.C. | Process for the preparation of a two-layer metal palladium or palladium alloy composite membrane |
| JP2008018387A (en) * | 2006-07-14 | 2008-01-31 | Ngk Insulators Ltd | Method for applying seed crystal to porous base material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0568553B2 (en) | 1993-09-29 |
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