TWI758008B - Porous substrate structure and manufacturing method thereof - Google Patents
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- TWI758008B TWI758008B TW109143994A TW109143994A TWI758008B TW I758008 B TWI758008 B TW I758008B TW 109143994 A TW109143994 A TW 109143994A TW 109143994 A TW109143994 A TW 109143994A TW I758008 B TWI758008 B TW I758008B
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Abstract
Description
本揭露是有關於一種多孔基材結構及其製造方法。The present disclosure relates to a porous substrate structure and a manufacturing method thereof.
由於鈀膜在氫氣質傳上的特殊性,因此目前大多將鈀膜形成於多孔基材的表面上進行濾氫處理。藉由氫分子在鈀膜的表面解離並穿透膜層,可將氫分子和其他氣體分子分離。一般來說,採用鈀膜的厚度來作為濾氫性能的指標。也就是說,為了增加鈀膜的氫氣滲透率,必須降低鈀膜的厚度,且必須使膜層的缺陷盡可能地減少以提高鈀膜的緻密度。Due to the particularity of palladium membranes in the transmission of hydrogen gas, palladium membranes are mostly formed on the surface of porous substrates for hydrogen filtration treatment. By dissociating hydrogen molecules on the surface of the palladium membrane and penetrating the membrane layer, hydrogen molecules can be separated from other gas molecules. In general, the thickness of the palladium membrane is used as an indicator of the hydrogen filtration performance. That is to say, in order to increase the hydrogen permeability of the palladium film, the thickness of the palladium film must be reduced, and the defects of the film layer must be reduced as much as possible to improve the density of the palladium film.
此外,藉由對多孔基材的表面進行修飾(例如形成修飾層),可減少具有所需緻密度的鈀膜厚度。然而,若多孔基材上修飾層厚度過大,可能造成修飾層附著力不足而自多孔基材剝離的問題。In addition, by modifying the surface of the porous substrate (eg, forming a modified layer), the thickness of the palladium film with the desired density can be reduced. However, if the thickness of the modified layer on the porous substrate is too large, the problem of insufficient adhesion of the modified layer and peeling from the porous substrate may occur.
本揭露提供一種多孔基材結構,其中基材與修飾層(雙金屬氧化物層)之間設置有陽極氧化鋁層。The present disclosure provides a porous substrate structure, wherein an anodized aluminum oxide layer is disposed between the substrate and the modification layer (bimetal oxide layer).
本揭露提供一種多孔基材結構的製造方法,其中陽極氧化鋁層形成於基材與修飾層(雙金屬氧化物層)之間。The present disclosure provides a method for manufacturing a porous substrate structure, wherein an anodic aluminum oxide layer is formed between the substrate and a modification layer (a double metal oxide layer).
本揭露的多孔基材結構包括基材、陽極氧化鋁層以及雙金屬氧化物層。所述基材具有多個孔洞。所述陽極氧化鋁層設置於所述基材上。所述雙金屬氧化物層設置於所述陽極氧化鋁層上。The porous substrate structure of the present disclosure includes a substrate, an anodized aluminum oxide layer, and a bimetallic oxide layer. The substrate has a plurality of holes. The anodic aluminum oxide layer is disposed on the substrate. The double metal oxide layer is disposed on the anodized aluminum oxide layer.
本揭露的多孔基材結構的製造方法包括以下步驟。於基材上形成陽極氧化鋁層,其中所述基材具有多個孔洞。於所述陽極氧化鋁層上形成雙金屬氧化物層。The manufacturing method of the porous substrate structure of the present disclosure includes the following steps. An anodized aluminum oxide layer is formed on a substrate, wherein the substrate has a plurality of pores. A bimetallic oxide layer is formed on the anodic aluminum oxide layer.
為讓本揭露的上述特徵和優點能更明顯易懂,下文特舉實施例,並配合附圖作詳細說明如下。In order to make the above-mentioned features and advantages of the present disclosure more obvious and easy to understand, the following embodiments are given and described in detail with reference to the accompanying drawings as follows.
下文列舉實施例並配合所附圖來進行詳細地說明,但所提供的實施例並非用以限制本揭露所涵蓋的範圍。此外,附圖僅以說明為目的,並未依照原尺寸作圖。為了方便理解,在下述說明中相同的元件將以相同的符號標示來說明。The following examples are described in detail with the accompanying drawings, but the provided examples are not intended to limit the scope of the present disclosure. In addition, the drawings are for illustrative purposes only, and are not drawn in full scale. In order to facilitate understanding, the same elements will be described with the same symbols in the following description.
關於本文中所提到「包含」、「包括」、「具有」等的用語均為開放性的用語,也就是指「包含但不限於」。The terms "including", "including", "having", etc. mentioned in this article are all open-ended terms, that is, "including but not limited to".
此外,在本文中,由「一數值至另一數值」表示的範圍是一種避免在說明書中逐一列舉所述範圍中的所有數值的概要性表示方式。因此,某一特定數值範圍的記載涵蓋了所述數值範圍內的任意數值,以及涵蓋由所述數值範圍內的任意數值界定出的較小數值範圍。Also, herein, a range represented by "one value to another value" is a general representation that avoids listing all the values in the range in the specification. Thus, the recitation of a particular numerical range includes any number within that numerical range as well as any smaller numerical range bounded by any number within that numerical range.
另外,文中所提到「上」、「下」等的方向性用語,僅是用以參考圖式的方向,並非用以限制本揭露。In addition, directional terms such as "upper" and "lower" mentioned in the text are only used to refer to the direction of the drawings, and are not used to limit the present disclosure.
圖1A至圖1D為本揭露的實施例的多孔基材結構的製造流程剖面示意圖。本揭露的實施例的多孔基材結構允許氣體穿透,以應用於例如分離氣體等的氣體處理(例如濾氫處理)。1A to 1D are schematic cross-sectional views of the manufacturing process of the porous substrate structure according to an embodiment of the disclosure. The porous substrate structures of embodiments of the present disclosure allow gas penetration for applications in gas treatment (eg, hydrogen filtration) such as separation of gases.
首先,請參照圖1A,提供基材100。在本實施例中,基材100的材料為多孔不鏽鋼,但本揭露不限於此。在其他實施例中,基材100的材料可為多孔陶瓷。基材100具有多個孔洞100a,以供氣體穿透。孔洞100a的孔徑例如介於1μm至30 μm之間。基材100可為管狀基材或片狀基材,本揭露不對此進行限定。First, referring to FIG. 1A , a
接著,視實際需求,可於孔洞100a中填入填充粒子102。如此一來,當孔洞100a的孔徑相對較大時,將填充粒子102填充於孔洞100a中可使孔洞100a的孔徑縮小,可避免後續形成於基材100上的膜層陷入孔洞100a中,造成膜層的表面不平整或孔洞100a堵塞的問題。此外,將填充粒子102填充於孔洞100a中可改善孔洞100a的孔徑不均一的問題。Then, according to actual requirements, filling
填充粒子102的材料例如為氧化鋁、氧化矽、氧化鈣、氧化鈰、氧化鈦、氧化鉻、氧化錳、氧化鐵、氧化鎳、氧化銅、氧化鋅、氧化鋯或上述之組合。在填充粒子102不會將孔洞100a填滿的前提下,本揭露不對填充粒子102的粒徑進行限定。The material of the
另外,當孔洞100a的孔徑相對較小時,由於後續形成於基材100上的膜層不容易陷入孔洞100a中,因此可不需要將填充粒子102填充於孔洞100a中。In addition, when the pore size of the
接著,請參照圖1B,於基材100上形成鋁層104。鋁層104的厚度例如不超過3 μm。鋁層104的形成方法例如是真空蒸鍍或無電鍍。Next, referring to FIG. 1B , an
然後,請參照圖1C,對鋁層104進行陽極處理,以形成陽極氧化鋁(anodic aluminum oxide,AAO)層106。在所述陽極處理之後,所形成的陽極氧化鋁層106中具有多個穿透陽極氧化鋁層106的孔洞106a,且這些孔洞106a暴露出基材100以及孔洞100a。以供氣體穿透。在本揭露的實施例中,由於鋁層104的厚度例如不超過3 μm,因此在進行陽極處理而形成陽極氧化鋁層106之後,孔洞106a能夠穿透陽極氧化鋁層106。當鋁層104的厚度超過3 μm時,所形成的孔洞106a無法穿透陽極氧化鋁層106。如此一來,氣體將無法穿透陽極氧化鋁層106以及基材100。Then, referring to FIG. 1C , the
此外,在進行陽極處理之後,鋁層104轉變為具有平整的表面以及高孔隙率的陽極氧化鋁層106。因此,陽極氧化鋁層106可作為基材100的修飾層,以提高後續形成於其上的膜層的平整度。在本實施例中,當孔洞100a的孔徑相對較大時,由於有填充粒子102填充於孔洞100a中而避免了鋁層104陷入孔洞100a中,因此鋁層104可具有平整的表面且不會造成孔洞100a堵塞。如此一來,所形成的陽極氧化鋁層106可具有更高的表面平整度,且氣體可有效地穿透陽極氧化鋁層106以及基材100。Furthermore, after anodizing, the
接著,請參照圖1D,於陽極氧化鋁層106上形成雙金屬氧化物層108,以形成本揭露的實施例的多孔基材結構10。雙金屬氧化物層108中具有孔洞108a,以供氣體穿透。在本揭露的實施例中,雙金屬氧化物層108的材料包含雙金屬氧化物。在一實施例中,雙金屬氧化物可例如為鋰鋁氧化物。此外,在一些實施例中,雙金屬氧化物可為層狀雙金屬氧化物,其可由式1表示,
[M
II 1-xM
III x]O
y式1
其中M
II為Mg
2+、Zn
2+、Fe
2+、Ni
2+、Co
2+、Cu
2+或Li
+,M
III為Al
3+、Cr
3+、Fe
3+或Sc
3+,x介於0.2至0.33之間,y介於0.7至2之間。此外,在本揭露的實施例中,雙金屬氧化物層108的形成方法例如先於陽極氧化鋁層106上形成雙金屬氫氧化物(layered double hydroxide,LDH)層(未繪示)。然後,對雙金屬氫氧化物層進行鍛燒處理,以得到雙金屬氧化物層。在陽極氧化鋁層106上形成雙金屬氫氧化物層的方法可例如為化學鍍、熱浸鍍、物理蒸鍍、化學蒸鍍、共沉法或水熱法,但不限定。雙金屬氫氧化物為雙金屬氧化物的前驅物,可經由高溫處理(例如鍛燒)轉化為雙金屬氧化物。此外,鍛燒處理的溫度約為300
oC至500
oC。
Next, referring to FIG. 1D , a double
在本揭露的實施例中,雙金屬氧化物層108的厚度小於3 μm。詳細地說,由於基材100上形成有陽極氧化鋁層106,因此可用較薄之雙金屬氧化物層即達到修飾效果,因而提高雙金屬氧化物層108在基材100上的附著力。如此一來,雙金屬氧化物層108的厚度可降低至小於3 μm,以避免為了提高表面平整度而厚度過大造成附著力不足,進而導致雙金屬氧化物層108剝離的問題。當雙金屬氧化物層的厚度降低,亦可提升氣體的通過量。In an embodiment of the present disclosure, the thickness of the double
此外,由於陽極氧化鋁層106具有平整的表面,因此形成於陽極氧化鋁層106上的雙金屬氧化物層108也可具有平整的表面。如此一來,雙金屬氧化物層108可作為基材100的修飾層,且使得後續所形成的膜層具有較少的缺陷而有較高的緻密度。In addition, since the anodized
在本揭露的實施例中,多孔基材結構10包括具有孔洞100a的基材100、具有孔洞106a的陽極氧化鋁層106以及具有孔洞108a的雙金屬氧化物層108。因此,多孔基材結構10可允許氣體穿透,以應用於例如分離氣體等的氣體處理(例如濾氫處理)。以下對多孔基材結構10的結構與氣體穿透特性作進一步的說明。In an embodiment of the present disclosure, the
實施例:Example:
在多孔不鏽鋼管材(PSS,Pall Accusep filter, P/N: 7CC6L465236235SC02)表面的孔洞內填入氧化鋁粒子,其中氧化鋁粒子的平均粒徑為10 µm。接著,將填有氧化鋁粒子的不鏽鋼管管材置入真空蒸鍍機中進行表面蒸鍍。於腔體內的靶台上放置1 g鋁錠,以真空幫浦將腔體壓力抽至1×10 -4torr以下,開始旋轉待蒸鍍的不鏽鋼管材並加熱靶台,使其表面形成極薄(小於3 µm)的鋁層。接著,將鍍有鋁層的不鏽鋼管管材進行陽極處理,得到表面披覆有陽極氧化鋁層的不鏽鋼管管材。 The pores on the surface of the porous stainless steel pipe (PSS, Pall Accusep filter, P/N: 7CC6L465236235SC02) were filled with alumina particles, wherein the average particle size of the alumina particles was 10 µm. Next, the stainless steel pipe material filled with alumina particles was placed in a vacuum evaporation machine for surface evaporation. Place 1 g aluminum ingot on the target table in the chamber, pump the chamber pressure to below 1×10 -4 torr with a vacuum pump, start to rotate the stainless steel pipe to be evaporated and heat the target table to make the surface extremely thin (less than 3 µm) aluminum layer. Next, the stainless steel pipe material plated with the aluminum layer is anodized to obtain a stainless steel pipe material coated with an anodized aluminum layer on the surface.
將AlLi介金屬化合物(以AlLi介金屬化合物的總重量計,Li的含量約為18 wt.%至21 wt.%)粉末置入1000 mL的純水中,導入氮氣且曝氣攪拌,使大部分的AlLi介金屬化合物粉末與水反應而溶解。接著,過濾雜質,以得到澄清且含有Li +及Al 3+的鹼性溶液(pH值約為11.0至12.3)。 The AlLi intermetallic compound (based on the total weight of the AlLi intermetallic compound, the Li content is about 18 wt.% to 21 wt.%) powder is placed in 1000 mL of pure water, and nitrogen is introduced and aerated and stirred to make the large Part of the AlLi intermetallic compound powder reacts with water and dissolves. Next, the impurities were filtered to obtain a clear alkaline solution containing Li + and Al 3+ (pH about 11.0 to 12.3).
將表面披覆有陽極氧化鋁層的不鏽鋼管管材浸置於含有Li +及Al 3+的鹼性溶液中約2小時後進行乾燥,使得連續相的層狀含有鋰的鋁氫氧化物層披覆於陽極氧化鋁層上。接著,在500℃下對不鏽鋼管管材進行鍛燒兩小時,在陽極氧化鋁層上形成層狀鋰鋁氧化物層,其中鋰鋁氧化物層的厚度約為2.9 μm,得到本實施例的多孔基材結構。 The surface of the stainless steel pipe coated with anodized aluminum layer was immersed in an alkaline solution containing Li + and Al 3 + for about 2 hours, and then dried, so that the continuous phase layered aluminum hydroxide layer containing lithium was covered. Overlaid on the anodized aluminum layer. Next, the stainless steel pipe was calcined at 500° C. for two hours to form a layered lithium-aluminum oxide layer on the anodic aluminum oxide layer, wherein the thickness of the lithium-aluminum oxide layer was about 2.9 μm. Substrate structure.
比較例Comparative example
除了未形成陽極氧化鋁層之外,以與實施例相同的方式形成多孔基材結構,其中鋰鋁氧化物層的厚度約為6.4 μm。A porous substrate structure was formed in the same manner as in the Example except that the anodic aluminum oxide layer was not formed, wherein the thickness of the lithium aluminum oxide layer was about 6.4 μm.
圖2A為比較例的多孔基材結構截面影像圖。圖2B為本揭露的實施例的多孔基材結構截面影像圖。由圖2A與圖2B可清楚看出,當雙金屬氧化物層與基材之間設置有陽極氧化鋁層時,雙金屬氧化物層可在符合所需平整度(表面上的最大落差為2.8 μm)的條件下具有較薄的厚度,且因此可有效地避免修飾層(雙金屬氧化物層)自基材剝離。FIG. 2A is a cross-sectional image of a porous substrate structure of a comparative example. FIG. 2B is a cross-sectional image view of a porous substrate structure according to an embodiment of the disclosure. It can be clearly seen from FIG. 2A and FIG. 2B that when an anodized aluminum oxide layer is arranged between the double metal oxide layer and the substrate, the double metal oxide layer can meet the required flatness (the maximum drop on the surface is 2.8). μm) has a thinner thickness, and thus can effectively prevent the modification layer (double metal oxide layer) from peeling off the substrate.
此外,將本揭露的實施例的多孔基材結構與比較例的多孔基材結構(金屬氧化物層直接形成於基材上)進行氣體穿透率測試,結果如表1所示。In addition, the porous substrate structure of the embodiment of the present disclosure and the porous substrate structure of the comparative example (the metal oxide layer is directly formed on the substrate) were tested for gas permeability, and the results are shown in Table 1.
氣體穿透率測試:Gas Penetration Test:
將待量測的多孔基材結構置於測試腔體中,然後將氮氣通入測試腔體,並由壓力計來監控壓力數值。使用流量計來量測從測試腔體的開口端流出的氮氣,並計算在特定壓力下的氮氣通量。The porous substrate structure to be measured is placed in the test chamber, then nitrogen gas is passed into the test chamber, and the pressure value is monitored by a pressure gauge. A flow meter was used to measure the nitrogen flow from the open end of the test chamber and to calculate the nitrogen flux at a specific pressure.
表1
由圖2A、圖2B與表1可以清楚看出,在本揭露的實施例中,由於多孔基材與修飾層(雙金屬氧化物層)之間設置有陽極氧化鋁層,因此修飾層(雙金屬氧化物層)在具有相同平整度的條件下可具有較薄的厚度,且同時具有較高的氣體通量,亦即本揭露的實施例的多孔基材結構可具有較高的氣體滲透率。It can be clearly seen from FIG. 2A , FIG. 2B and Table 1 that in the embodiments of the present disclosure, since an anodized aluminum oxide layer is disposed between the porous substrate and the modification layer (dual metal oxide layer), the modification layer (dual metal oxide layer) The metal oxide layer) can have a thinner thickness under the condition of the same flatness, and at the same time have a higher gas flux, that is, the porous substrate structure of the embodiment of the present disclosure can have a higher gas permeability .
雖然本揭露已以實施例揭露如上,然其並非用以限定本揭露,任何所屬技術領域中具有通常知識者,在不脫離本揭露的精神和範圍內,當可作些許的更動與潤飾,故本揭露的保護範圍當視所附的申請專利範圍所界定者為準。Although the present disclosure has been disclosed above with examples, it is not intended to limit the present disclosure. Anyone with ordinary knowledge in the technical field may make some changes and modifications without departing from the spirit and scope of the present disclosure. The scope of protection of the present disclosure shall be determined by the scope of the appended patent application.
10:多孔基材結構
100:基材
100a、106a、108a:孔洞
102:填充粒子
104:鋁層
106:陽極氧化鋁層
108:雙金屬氧化物層
10: Porous substrate structure
100:
圖1A至圖1D為本揭露的實施例的多孔基材結構的製造流程剖面示意圖。 圖2A為雙金屬氧化物層直接形成於基材上的多孔基材結構的截面影像圖。 圖2B為本揭露的實施例的多孔基材結構的截面影像圖。 1A to 1D are schematic cross-sectional views of the manufacturing process of the porous substrate structure according to an embodiment of the disclosure. 2A is a cross-sectional image of a porous substrate structure in which a double metal oxide layer is directly formed on the substrate. 2B is a cross-sectional image view of the porous substrate structure of the disclosed embodiment.
10:多孔基材結構 10: Porous substrate structure
100:基材 100: Substrate
100a、106a、108a:孔洞 100a, 106a, 108a: holes
102:填充粒子 102: Fill Particles
106:陽極氧化鋁層 106: Anodized aluminum layer
108:雙金屬氧化物層 108: Double metal oxide layer
Claims (13)
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TW200927275A (en) * | 2007-12-21 | 2009-07-01 | Ind Tech Res Inst | Hydrogen filtration membrane structure and manufacturing method thereof |
TW201326461A (en) * | 2011-12-30 | 2013-07-01 | Ind Tech Res Inst | Method for modifying porous substrate and modified porous substrate |
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US5393325A (en) * | 1990-08-10 | 1995-02-28 | Bend Research, Inc. | Composite hydrogen separation metal membrane |
JPH1085568A (en) * | 1996-09-10 | 1998-04-07 | Tonen Corp | Gas separator |
JP2000189772A (en) * | 1998-12-24 | 2000-07-11 | Kyocera Corp | Separation filter of hydrogen gas and its production |
WO2003076050A1 (en) * | 2002-03-05 | 2003-09-18 | Eltron Research, Inc. | Hydrogen transport membranes |
US7018446B2 (en) * | 2003-09-24 | 2006-03-28 | Siemens Westinghouse Power Corporation | Metal gas separation membrane |
US20100219079A1 (en) * | 2006-05-07 | 2010-09-02 | Synkera Technologies, Inc. | Methods for making membranes based on anodic aluminum oxide structures |
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