TWI652335B - Insulation material and manufacturing method thereof - Google Patents

Insulation material and manufacturing method thereof Download PDF

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Publication number
TWI652335B
TWI652335B TW102141271A TW102141271A TWI652335B TW I652335 B TWI652335 B TW I652335B TW 102141271 A TW102141271 A TW 102141271A TW 102141271 A TW102141271 A TW 102141271A TW I652335 B TWI652335 B TW I652335B
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Taiwan
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weight
heat insulating
fiber
insulating material
particles
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TW102141271A
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English (en)
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TW201435068A (zh
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坂倉正年
大貫寿文
福代壮二郎
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日商霓佳斯股份有限公司
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    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
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    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
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Abstract

一種絕熱材料，其係由燒結下述原料而得，該原料係包含：平均粒徑100nm以下之氧化鋁粒子52~93重量%，與由二氧化矽粒子、矽石、滑石、富鋁紅柱石、氮化矽、矽石煙、矽灰石、膨潤土、高嶺土、海泡石及雲母粒子中所選出之1種以上之結晶轉變抑制材1~45重量%，與輻射散射材料0~40重量%，與纖維1~20重量%。

Description

絕熱材料及其製造方法
本發明係關於絕熱材料及其製造方法，尤其是關於提高絕熱材料的耐熱性。
以往已知有由包含二氧化矽粒子或氧化鋁粒子、輻射散射材料、補強纖維之加壓成形體所構成之絕熱材料(例如專利文獻1)。由二氧化矽粒子所構成之絕熱材料，於超過1100℃的環境使用時，收縮變大，故追求於超過1100℃的溫度具有耐熱性之絕熱材料。進而，期望具備與包含二氧化矽粒子之絕熱材料同等之強度、熱傳導率。
[先前技術文獻] [專利文獻]
[專利文獻1]日本特開2012-149658號公報
本發明係鑑於上述課題而完成者，將提供一種提高於高溫之耐熱性之絕熱材料及其製造方法作為其目 的之一。
為了解決上述課題，本發明者們，並非二氧化矽粒子而是使用氧化鋁粒子。然而，即使為將氧化鋁粒子作為主體之絕熱材料，比起二氧化矽粒子作為主體之絕熱材料，雖耐熱性優異，但超過1150℃時收縮變大，耐熱性不充分。本發明者們，發現收縮的一個原因是氧化鋁之剛玉(Corundum)化(結晶轉變)，探求可抑制剛玉化率之化合物，而完成本發明。
根據本發明，提供以下之絕熱材料及其製造方法。
1.一種絕熱材料，其係由燒結下述原料而得，該原料係包含：平均粒徑100nm以下之氧化鋁粒子52~93重量%，與由二氧化矽粒子、矽石、滑石、富鋁紅柱石、氮化矽、矽石煙、矽灰石、膨潤土、高嶺土、海泡石及雲母粒子所選出之1種以上之結晶轉變抑制材1~45重量%，與輻射散射材料0~40重量%，與纖維1~20重量%。
2.如1記載之絕熱材料，其中，前述氧化鋁粒子、前述結晶轉變抑制材、前述纖維，與前述輻射散射材料的合計為95重量%以上。
3.如1或2記載之絕熱材料，其中，前述結晶轉變抑制材為平均粒徑100nm以下之二氧化矽粒子。
4.如1~3中任一項記載之絕熱材料，其係包含：前述氧化鋁粒子60~80重量%，與 前述結晶轉變抑制材4~10重量%，與前述輻射散射材料10~30重量%，與前述纖維2~10重量%。
5.如1~4中任一項記載之絕熱材料，其中，前述輻射散射材料為由碳化矽、氧化鋯、矽酸鋯、二氧化鈦、氧化鐵、氧化鉻、硫化鋅及鈦酸鋇所構成之群中所選出之1種以上。
6.如1~5中任一項記載之絕熱材料，其中，前述纖維為由玻璃纖維、二氧化矽-氧化鋁纖維、二氧化矽-氧化鋁-氧化鎂纖維、二氧化矽纖維、氧化鋁纖維、氧化鋯纖維、生體溶解性無機纖維、岩棉及玄武岩纖維所構成之群中所選出之1種以上。
7.一種如1記載之絕熱材料的製造方法，其係具備：將平均粒徑100nm以下之氧化鋁粒子、由二氧化矽粒子、矽石、滑石、富鋁紅柱石、氮化矽、矽石煙、矽灰石、膨潤土、高嶺土、海泡石及雲母粒子所選出之1種以上之結晶轉變抑制材及纖維，與任意之輻射散射材料混合而得到混合物之步驟、將前述混合物加壓成形而得到加壓成形體之步驟，與將前述加壓成形體燒結之步驟。
8.如7之記載絕熱材料的製造方法，其中，前述燒結步驟之加熱溫度為超過1000℃。
根據本發明，可提供一種提高於高溫之耐熱性之絕熱材料及其製造方法。
本發明之絕熱材料係包含氧化鋁粒子、氧化鋁之剛玉化的抑制材(稱為結晶轉變抑制材或轉移抑制材)及纖維。
氧化鋁粒子係包含將α-氧化鋁(剛玉)以外之氧化鋁(Al2O3)作為主成分之粒子(例如該氧化鋁包含95重量%以上之粒子)，若為作為絕熱材料之原料使用者則無特別限制。尚且，此氧化鋁粒子可為未包含α-氧化鋁(例如在XRD測定中，並未檢出剛玉之峰值)。
氧化鋁粒子，例如一次粒子之平均粒徑為100m以下。氧化鋁粒子之一次粒子的平均粒徑可為50nm以下，亦可為30nm以下。氧化鋁粒子之一次粒子的平均粒徑之下限值，雖並未特別限定，但例如為2nm以上。
平均粒徑對於無規約100個粒子，以透過型電子顯微鏡(Transmission Electron Microscope；TEM)或場致發射掃描電子顯微鏡(Field Emission Scanning Electron Microscope；FE-SEM)觀察粒子徑而求得。
氧化鋁粒子係例如以氣相法所製造者及/或以濕式法所製造者。亦即，氧化鋁粒子例如可為以氣相法所製造之乾式氧化鋁粒子，可為濕式法所製造之濕式氧化鋁粒子。更具體而言，氧化鋁粒子係例如以氣相法所製造之煙燻氧化鋁粒子。
結晶轉變抑制材係由二氧化矽粒子、矽石、 滑石、富鋁紅柱石、氮化矽、矽石煙、矽灰石、膨潤土、高嶺土、海泡石、雲母粒子中所選出之1種以上使用。較佳為二氧化矽粒子，更佳為平均粒徑100nm以下之二氧化矽粒子。
二氧化矽粒子之一次粒子的平均粒徑可為50nm以下，亦可為30nm以下。二氧化矽粒子之一次粒子的平均粒徑之下限值雖未特別限制，但例如為2nm以上。
二氧化矽粒子係例如以氣相法所製造者及/或濕式法所製造者。亦即，二氧化矽粒子例如可為氣相法所製造之乾式二氧化矽粒子，可為濕式法所製造之濕式二氧化矽粒子。更具體而言，二氧化矽粒子係例如以氣相法所製造之煙燻二氧化矽粒子。
絕熱材料之原料所包含氧化鋁粒子的量，若為實現所期望特性的範圍則並未特別限制。絕熱材料係包含例如52~93重量%、53~92重量%、56~90重量%，較佳為60~80重量%，更佳為65~75重量%之氧化鋁粒子。
絕熱材料之原料所包含結晶轉變抑制材的量，若為實現所期望特性的範圍則並未特別限制。絕熱材料所佔有之轉移抑制材的量，例如為0.5~45重量%，較佳為1~35重量%，更佳為2~25重量%，再更佳為3~10重量%。結晶轉變抑制材的量過少時，恐有無法充分發揮效果之虞。結晶轉變抑制材的量過多時，恐有收縮變大 或是降低絕熱性之虞。使用二氧化矽粒子時，最佳的量為5~8重量%。
又，本發明所使用之轉移抑制材，雖包含二氧化矽元素，但相對於Al之Si的比，Si/Al可調整至發揮本發明效果的範圍。例如可成為0.008~1.0、0.01~0.9或0.02~0.8。
絕熱材料較佳為包含無機纖維作為纖維。纖維若為可補強成形體者則無特別限制。尚，於本發明未包含有機纖維。本發明之絕熱材料因為係以高溫製造或使用，而導致有機纖維被燒毀而消失。
無機纖維係例如由玻璃纖維、二氧化矽-氧化鋁纖維、二氧化矽-氧化鋁-氧化鎂纖維、二氧化矽纖維、氧化鋁纖維、氧化鋯纖維、生體溶解性無機纖維、岩棉及玄武岩纖維所構成之群中所選出之1種以上。較佳為二氧化矽-氧化鋁-氧化鎂纖維、氧化鋁纖維。
作為生體溶解性纖維，可例示SiO2、Al2O3與ZrO2的合計為50~82重量%、CaO與MgO的合計為18~50重量%之組成的無機纖維。又，亦可例示SiO2為50~82重量%、CaO與MgO的合計為10~43重量%之組成的無機纖維。
纖維之平均纖維長，例如可為0.5mm以上、20mm以下，為1mm以上、10mm以下。纖維之平均纖維徑，例如可為1μm以上、20μm以下，為2μm以上、15μm以下。
纖維之量，例如為1~20重量%，較佳為1.5~10重量%，更佳為2~9重量%。
又，絕熱材料可包含輻射散射材料。輻射散射材料若為藉由輻射可減低傳熱則無特別限制。輻射散射材料係例如由碳化矽、氧化鋯、矽酸鋯、二氧化鈦、氧化鐵、氧化鉻、硫化鋅、鈦酸鋇所構成之群中所選出之1種以上。
輻射散射材料之平均粒徑，例如可為1μm以上、50μm以下，為1μm以上、20μm以下。輻射散射材料以遠紅外線反射性者為佳，例如相對於1μm以上波長的光，以比折射率為1.25以上者為佳。
輻射散射材料的量係例如1~40重量%，較佳為5~35重量%，更佳為10~30重量%。
又，絕熱材料可進一步包含其他金屬氧化物粒子，亦可未包含。
又，絕熱材料可不包含結合劑(例如水玻璃接著劑等之無機結合劑，或樹脂等之有機結合劑)。
絕熱材料之原料係可將氧化鋁粒子、結晶轉變抑制材、纖維、輻射散射材料之合計成為95重量%以上、98重量%以上，或99重量%以上。又，可包含不可避免之不純物，可為100重量%。
本發明之絕熱材料係藉由包含氧化鋁粒子、轉移抑制材等之混合粉體進行成形而得到。更具體而言，將包含上述成分之經調製之混合粉體填充特定之成形型， 藉由乾式沖壓成形，對應該成形型來製造形狀之乾式加壓成形體。
成形體的形狀雖並未特別限制，但例如為木板狀、板狀或圓筒狀。進行乾式沖壓成形之溫度，雖並未特別限制，但例如可於0℃以上、100℃以下之溫度進行，亦可於0℃以上、50℃以下之溫度進行。
如此進行所得到之成形體，可直接使用作為絕熱材料，或作為絕熱材料之一部分(與其他絕熱材料組合)。成形體作為絕熱材料之一部分使用時，該絕熱材料，例如可具有該成形體、與耐熱性與該成形體不同之1個以上之其他絕緣構件。亦即，此時，絕熱材料係例如可具有成形體、與層合於該成形體之高溫側、耐熱性更高之絕緣構件，及/或層合於該成形體之低溫側、更便宜且耐熱性更低之絕緣構件。
又，本發明之方法係將混合粉體例如以700℃以上之溫度加熱。混合粉體之加熱可於成形體之成形前進行，可於成形體之成形後進行。
加熱溫度較佳為超過900℃且1300℃以下，更佳為1000~1200℃、再更佳為1050~1150℃。
於此，本發明之發明者們，對於提昇包含氧化鋁粒子之成形體的耐熱性之技術的手段，進行重複銳意檢討的結果，獨自發現未包含轉移抑制材之該成形體，於超過1100℃之溫度進行加熱時，相對於其耐熱性或絕熱性等特性受損，包含轉移抑制材之該成形體，即使於超過 1100℃之溫度進行加熱，效果性維持其特性。
更具體而言，本發明之發明者們，首先將包含氧化鋁粒子之未包含轉移抑制材之成形體於超過1100℃之溫度進行加熱時，引起剛玉(corundum)之生成(結晶之轉移)，且與該成形體於1100℃以下之溫度進行加熱時相比較，發現顯著產生細孔容積之減少及比表面積之減少。
於此，本發明之發明者們，對於抑制在如此之高溫下的成形體之劣化之技術性手段，進行重複銳意檢討的結果，發現藉由混合氧化鋁粒子與轉移抑制材而使用經調製之混合粉體，由該混合粉體之乾式沖壓成形所得到之成形體，即使於超過1100℃之溫度進行加熱，效果性抑制剛玉之生成，或細孔容積及比表面積的減少，即使在高溫(例如、1200℃)亦顯示小的加熱線收縮率。
雖藉由添加轉移抑制材於氧化鋁粒子，防止因為於超過1100℃之溫度的加熱造成之成形體的劣化之機制，尚未明朗，作為其一，被認為係例如氧化鋁與轉移抑制材進行反應而生成複合化合物，此係抑制氧化鋁的結晶轉變(剛玉之生成)。
又，在本發明之方法，藉由將包含氧化鋁粒子與轉移抑制材之混合粉體於上述之加熱溫度進行加熱，可將上述鋁及轉移抑制材之反應物或轉移抑制材，形成於該氧化鋁粒子的表面。此時，在氧化鋁粒子的表面，鋁及轉移抑制材之反應物或轉移抑制材可進行如被膜般之機能。
本發明之絕熱材料具有優異之絕熱性。例如在絕熱材料之1000℃之熱傳導率為0.20W/(m．K)以下、0.15W/(m．K)以下、0.13W/(m．K)以下、0.10W/(m．K)以下，或0.04W/(m．K)以下。又，例如在絕熱材料之25℃之熱傳導率為0.045W/(m．K)以下，或0.040W/(m．K)以下。
將絕熱材料於1200℃加熱24小時時之加熱線收縮率，較佳為15%以下。更佳為10%以下、8%以下、6%以下，或5%以下。加熱線收縮率根據加熱前成形體的長度(X)及於1200℃下加熱24小時後之該成形體的長度(Y)，由以下之式所算出：加熱線收縮率(%)={(X-Y)/X}×100。
由絕熱材料之BET法之比表面積為20m2/g以上，或30m2/g以上。由絕熱材料之BJH法所測定之細孔容積為0.3cm3/g以上，或0.5cm3/g以上。絕熱材料之容積密度雖並未特別限制，但例如可為100~800kg/m3，或200~500kg/m3。
本發明之絕熱材料係利用其優異之耐熱性，可於高溫所要求耐熱性之環境使用。亦即，本發明之絕熱材料，例如可作為於要求超過1100℃(例如1200℃以上)之耐熱性的環境所使用之絕熱材料(例如最高使用溫度超過1100℃(例如1200℃以上)之絕熱材料)使用。
[實施例]
以下雖對於本發明之實施例進行說明，但本發明並非被限制於此等實施例。
實施例1 [絕熱材料之製造]
氧化鋁粒子係成形之包含表1~4所示之轉移抑制材及S2纖維(二氧化矽-氧化鋁-氧化鎂纖維、AGY公司製)之混合粉末，來製造成形體。作為氧化鋁粒子，使用一次粒子之平均粒徑約13nm之氧化鋁粒子(煙燻氧化鋁粒子、日本Aerosil股份有限公司製)。摻合量係將氧化鋁粒子與轉移抑制材摻合成95重量%，S2纖維為5重量%。將轉移抑制材之摻合量表示於表1~4。
具體而言，係將氧化鋁粒子、轉移抑制材、纖維投入混合裝置，藉由進行乾式混合，來調製混合粉末。
其次，將此混合粉末填充於特定之脫氣機構所附屬之成形型。而且，經製造之乾式加壓成形體的容積密度以成為270kg/m3之方式調節沖壓壓力，進行乾式沖壓成形。然後，將經成形之板狀乾式加壓成形體從模型中取出。
進而燒成乾式加壓成形體。亦即，將乾式加壓成形體於1200℃下加熱24小時。
[絕熱材料之評估]
根據在加熱之前後所測定之乾式加壓成形體的長度變化，算出於1200℃下加熱24小時時之該乾式加壓成形體 的加熱線收縮率。亦即，從各乾式加壓成形體，製作長100mm、寬30mm、厚度15mm之板狀試驗體。其次，將此試驗體於1200℃電爐中加熱特定時間。尚且，至1200℃為止的昇溫速度為200℃/小時。進而，測定加熱後之試驗體的長度。而且，由以下之式算出加熱線收縮率。
加熱線收縮率(%)={(X-Y)/X}×100(式中，X為加熱前之試驗體的長度(mm)，Y為加熱後之該試驗體的長度(mm))。
又，對於加熱後之乾式加壓成形體進行XRD測定，測定剛玉化強度。
將測定結果表示於表1~4。
比較例1
除了使用未包含轉移抑制材，包含氧化鋁粒子95重量%與纖維5重量%之混合粉末之外，其他與實施例1以相同方式進行，製造絕熱材料，進行評估。將結果表示於表5。
實施例2 [絕熱材料之製造]
於表6所示之摻合量(重量%)，將包含氧化鋁粒子、二氧化矽粒子(轉移抑制材)、鋯石(輻射散射材料)及S2纖維之混合粉末，以與實施例1相同方式成形來製造成形體。作為二氧化矽粒子，係使用一次粒子之平均粒徑約12nm之二氧化矽粒子(煙燻二氧化矽粒子，德山股份有限公司製)。
進而，將所得到之成形體於1100℃下加熱24小時。
[絕熱材料之評估]
與實施例1相同方式進行，算出在1200℃下加熱48小時、120小時及192小時時之加熱線收縮率(%)。將結果表示於表7。
實驗例
使用未包含轉移抑制材，包含氧化鋁粒子100重量%之粉末材料(由氧化鋁粒子所構成之粉末材料)。亦即，將此粉末材料於800℃~1200℃之範圍內的5種溫度下(800℃、1000℃、1100℃、1150℃或1200℃)加熱24小時。
對於於不同溫度下加熱之5種粉末材料，與未加熱之粉末材料的各種，進行細孔容積及比表面積之測定、與XRD測定。
尚，比表面積係由BET法測定。細孔容積係由BJH法測定。亦即，使用藉由將加熱後之乾式加壓成形體作為試驗體之氣體吸著法，取得表示相對壓與吸著量的相關關係之脫附等溫線，由該脫附等溫線求得乾式加壓成形體之細孔徑，由該細孔徑算出該乾式加壓成形體之細孔容積。
其結果，對於未經加熱之粉末材料及於800℃~1100℃下經加熱之粉末材料，比表面積為100~119(m2/g)，細孔容積為0.51~0.70(cm3/g)，未檢出在XRD圖之剛玉的峰值。
對於此，對於在1150℃下經加熱之粉末材料，比表面積為69(m2/g)，細孔容積為0.49(cm3/g)，僅檢出在XRD圖之剛玉的峰值。
進而，對於在1200℃下經加熱之粉末材料，比表面積為13(m2/g)，細孔容積為0.05(cm3/g)，僅檢出在XRD圖之剛玉。
亦即，由氧化鋁粒子所構成之粉末材料，藉由於超過1100℃之溫度下加熱，確認未損害其特性的同時，於如此特性的劣化顯示關係剛玉之生成(結晶轉變)的可能性。
於上述雖部分詳細說明本發明之實施形態及/或實施例，但該領域具有通常知識者，實質上並未脫離從本發明之新教示及效果，於此等例示之實施形態及/或實施例加入許多變更係容易。據此，此等多數之變更為本發明之範圍所包含。
將此說明書所記載之文獻及成為本案之巴黎優先基礎的日本申請說明書之內容全部援用於此。

Claims (8)

  1. 一種絕熱材料，其係由燒結下述原料而得，該原料係包含：平均粒徑100nm以下之氧化鋁粒子52~93重量%，與由二氧化矽粒子、矽石、滑石、富鋁紅柱石、氮化矽、矽石煙、矽灰石、膨潤土、高嶺土、海泡石及雲母粒子所選出之1種以上之結晶轉變抑制材1~45重量%，與氧化鋯的輻射散射材料0~40重量%，與纖維1~20重量%，於1200℃加熱24小時時之加熱線收縮率15%以下，即使於要求超過1200℃之耐熱性的環境亦可使用。
  2. 如請求項1之絕熱材料，其中，在前述原料之前述氧化鋁粒子、前述結晶轉變抑制材、前述纖維，與前述輻射散射材料的合計為95重量%以上。
  3. 如請求項1或2之絕熱材料，其中，前述結晶轉變抑制材為平均粒徑100nm以下之二氧化矽粒子。
  4. 如請求項1或2之絕熱材料，其係包含：前述氧化鋁粒子60~80重量%，與前述結晶轉變抑制材4~10重量%，與前述輻射散射材料10~30重量%，與前述纖維2~10重量%。
  5. 如請求項1或2之絕熱材料，其中，於1200℃加熱24小時時之加熱線收縮率5%以下。
  6. 如請求項1或2之絕熱材料，其中，前述纖維為由玻璃纖維、二氧化矽-氧化鋁纖維、二氧化矽-氧化鋁-氧化 鎂纖維、二氧化矽纖維、氧化鋁纖維、氧化鋯纖維、生體溶解性無機纖維、岩棉及玄武岩纖維所構成之群中所選出之1種以上。
  7. 一種如請求項1之絕熱材料的製造方法，其係具備：將平均粒徑100nm以下之氧化鋁粒子、由二氧化矽粒子、矽石、滑石、富鋁紅柱石、氮化矽、矽石煙、矽灰石、膨潤土、高嶺土、海泡石及雲母粒子所選出之1種以上之結晶轉變抑制材及纖維，與任意之氧化鋯輻射散射材料混合而得到混合物之步驟、將前述混合物加壓成形而得到加壓成形體之步驟，與將前述加壓成形體燒結之步驟。
  8. 如請求項7之絕熱材料的製造方法，其中，前述燒結步驟之加熱溫度為超過1000℃。
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