TWI803653B - 負熱膨脹材及其製造方法、以及複合材料 - Google Patents
負熱膨脹材及其製造方法、以及複合材料 Download PDFInfo
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- TWI803653B TWI803653B TW108121954A TW108121954A TWI803653B TW I803653 B TWI803653 B TW I803653B TW 108121954 A TW108121954 A TW 108121954A TW 108121954 A TW108121954 A TW 108121954A TW I803653 B TWI803653 B TW I803653B
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Abstract
一種負熱膨脹材，其特徵在於：包含含有Al原子的磷酸鎢酸鋯，熱膨脹係數為-2.0×10-6
/K～-3.3×10-6
/K。根據本發明，可提供一種具有各種熱膨脹係數的包含磷酸鎢酸鋯的負熱膨脹材、及其工業上有利的製造方法。
Description
本發明是有關於一種相對於溫度上昇而收縮的負熱膨脹材及其製造方法、以及包含該負熱膨脹材的複合材料。
大多物質若溫度上昇，則長度或體積藉由熱膨脹而增大。相對於此，亦已知有加溫時體積反而變小的顯示出負熱膨脹的材料(以下亦有時稱為「負熱膨脹材」)。已知顯示出負熱膨脹的材料與其他材料一起使用，可抑制由溫度變化引起的材料的熱膨脹的變化。
作為顯示出負熱膨脹的材料，例如已知有β-鋰霞石、鎢酸鋯(ZrW2O8)、磷酸鎢酸鋯(Zr2WO4(PO4)2)、ZnxCd1-x(CN)2、錳氮化物、鉍．鎳．鐵氧化物等。
磷酸鎢酸鋯的線膨脹係數於0℃~400℃的溫度範圍下為-3.4ppm/K~-3.0ppm/K，負熱膨脹性大，藉由與顯示出正熱膨脹的材料(以下亦有時稱為「正熱膨脹材」)併用，可製造低熱膨脹的材料(例如，參照專利文獻1~專利文獻2及非專利文獻1)。
本發明者等人先前亦提出一種作為負熱膨脹材而有用
的磷酸鎢酸鋯(專利文獻3~專利文獻4)。
[現有技術文獻]
[專利文獻]
[專利文獻1]日本專利特開2005-35840號公報
[專利文獻2]日本專利特開2015-10006號公報
[專利文獻3]日本專利特開2015-199000號公報
[專利文獻4]日本專利第6190023號公報
[專利文獻5]日本專利第6105140號公報
[非專利文獻]
[非專利文獻1]「材料研究通報(Materials Research Bulletin)」、44 (2009)、2045-2049.
負熱膨脹材是與正熱膨脹材併用而使用，根據與併用的正熱膨脹材的相容性或用途等，要求開發出具有各種熱膨脹係數的負熱膨脹材。
因此，本發明的目的在於提供一種具有各種熱膨脹係數的包含磷酸鎢酸鋯的負熱膨脹材、其工業上有利的製造方法以及包含該負熱膨脹材的複合材料。
本發明者等人鑑於所述實際情況，反覆進行了努力研究，結果發現如下內容：若於磷酸鎢酸鋯中含有例如Mg原子等副
成分元素，則有與未添加的情況相比而後述的熱膨脹係數變小的傾向，但磷酸鎢酸鋯中含有Al原子時，與Mg原子等副成分元素不同，有與未添加的情況相比而後述的熱膨脹係數變大的傾向，且根據Al的含量，可於特定的範圍內使熱膨脹係數變化，從而完成了本發明。
即，本發明(1)提供一種負熱膨脹材，其特徵在於：包含含有Al原子的磷酸鎢酸鋯，熱膨脹係數為-2.0×10-6/K~-3.3×10-6/K。
另外，本發明(2)提供如(1)所述的負熱膨脹材，其特徵在於：負熱膨脹材中的Al原子的含量為100質量ppm~6000質量ppm。
另外，本發明(3)提供如(1)或(2)所述的負熱膨脹材，其特徵在於：含有選自由Mg、Zn、Cu、Fe、Cr、Mn、Ni、V、Li、B、Na、K、F、Cl、Br、I、Ca、Sr、Ba、Ti、Hf、Nb、Sb、Te、Ga、Ge、La、Ce、Nd、Sm、Eu、Tb、Dy及Ho所組成的群組中的一種以上的副成分元素。
另外，本發明(4)提供如(1)至(3)中任一項所述的負熱膨脹材，其特徵在於：布厄特(Brunauer-Emmett-Teller，BET)比表面積為0.1m2/g~30m2/g。
另外，本發明(5)提供如(1)至(4)中任一項所述的負熱膨脹材，其特徵在於：平均粒徑為0.1μm~50μm。
另外，本發明(6)提供一種負熱膨脹材的製造方法，
具有：第1步驟，將W源、Zr源、P源、Al源混合而製備含有W源、Zr源、P源、Al源的漿料；第2步驟，對該漿料進行噴霧乾燥而獲得反應前驅物；以及第3步驟，對該反應前驅物進行煅燒而獲得含Al的磷酸鎢酸鋯，所述負熱膨脹材的製造方法的特徵在於：於該第1步驟中，以Al原子的含量相對於進行該第3步驟而獲得的含Al的磷酸鎢酸鋯而成為100質量ppm~6000質量ppm的方式，於該漿料中混合Al源。
另外，本發明(7)提供如(6)所述的負熱膨脹材的製造方法，其特徵在於：於所述第1步驟中，於所述漿料中進而混合具有選自由Mg、Zn、Cu、Fe、Cr、Mn、Ni、V、Li、B、Na、K、F、Cl、Br、I、Ca、Sr、Ba、Ti、Hf、Nb、Sb、Te、Ga、Ge、La、Ce、Nd、Sm、Eu、Tb、Dy及Ho所組成的群組中的一種或兩種以上的副成分元素的化合物的一種或兩種以上。
另外，本發明(8)提供如(6)或(7)所述的負熱膨脹材的製造方法，其特徵在於：所述Al源為硝酸鋁。
另外，本發明(9)提供一種複合材料，其特徵在於：包含如(1)至(5)中任一項所述的負熱膨脹材與正熱膨脹材。
另外，本發明(10)提供如(9)所述的複合材料，其特徵在於：所述正熱膨脹材為選自金屬、合金、玻璃、陶瓷、橡膠及樹脂中的至少一種。
根據本發明，可提供一種具有熱膨脹係數為-2.0×10-6/K~-3.3×10-6/K的各種熱膨脹係數的包含磷酸鎢酸鋯的負熱膨脹材。另外，根據本發明的製造方法，可以工業上有利的方法提供該負熱膨脹材。
圖1是實施例1中獲得的負熱膨脹材的X射線繞射圖。
圖2是實施例1中獲得的負熱膨脹材的SEM照片。
本發明的負熱膨脹材為如下的負熱膨脹材，其特徵在於：包含含有Al原子的磷酸鎢酸鋯，熱膨脹係數為-2.0×10-6/K~-3.3×10-6/K。
本發明的負熱膨脹材是使磷酸鎢酸鋯中含有Al原子而成者。而且，於本發明的負熱膨脹材中，Al原子固溶於磷酸鎢酸鋯中而存在。
本發明的負熱膨脹材的磷酸鎢酸鋯、即含有Al原子的磷酸鎢酸鋯基本上是由下述通式(1)所表示。
Zrx(WO4)y(PO4)z (1)
(式中，x為1.7≦x≦2.3，較佳為1.8≦x≦2.1，y為0.8≦y≦1.2，較佳為0.9≦y≦1.1，z為1.7≦z≦2.3，較佳為1.8≦z≦2.1)
本發明的負熱膨脹材中的Al原子的含量相對於負熱膨脹材整體、即含有Al原子並視需要含有副成分元素的磷酸鎢酸
鋯，為100質量ppm~6000質量ppm，較佳為1000質量ppm~5000質量ppm，特佳為1500質量ppm~5000質量ppm。於本發明的負熱膨脹材中，隨著Al原子的含量增加，熱膨脹係數有變大的傾向。於本發明的負熱膨脹材中，若Al原子的含量未滿所述範圍，則Al原子的添加效果不足，另一方面，若超過所述範圍，則並非為實用範圍的熱膨脹係數，負熱膨脹的特性受損。於本發明中，就使負熱膨脹材具有良好的負熱膨脹特性的觀點而言，Al原子的含量相對於負熱膨脹材整體而設為100質量ppm~6000質量ppm，較佳設為1000質量ppm~5000質量ppm，特佳設為1500質量ppm~5000質量ppm。再者，於本發明中，關於所述Al原子的含量，於負熱膨脹材不含有副成分元素的情況下，是指相對於含有Al原子的磷酸鎢酸鋯的含有比例，另外，於負熱膨脹材含有副成分元素的情況下，是指相對於含有Al原子及副成分元素的磷酸鎢酸鋯的含有比例。
本發明的負熱膨脹材的磷酸鎢酸鋯可以提高相對於正熱膨脹材的分散性或填充性為目的而含有副成分元素。作為副成分元素，可列舉：Mg、Zn、Cu、Fe、Cr、Mn、Ni、V、Li、B、Na、K、F、Cl、Br、I、Ca、Sr、Ba、Ti、Hf、Nb、Sb、Te、Ga、Ge、La、Ce、Nd、Sm、Eu、Tb、Dy及Ho，該些副成分元素可為一種，亦可為兩種以上。於該些副成分元素中，就相對於正熱膨脹材的分散性或填充特性變高的方面而言，較佳為Mg及/或V，就與Al的相容性佳的方面而言，特佳為Mg。再者，所謂副成分
元素，表示於含有Al原子的磷酸鎢酸鋯中含有500ppm以上的Al、Zr、W、P及O以外的所有元素。
於本發明的負熱膨脹材含有副成分元素的情況下，本發明的負熱膨脹材中的副成分元素的合計含量相對於負熱膨脹材整體、即含有Al原子及副成分元素的磷酸鎢酸鋯，較佳為0.1質量%~3質量%，特佳為0.2質量%~2質量%。藉由本發明的負熱膨脹材中的副成分元素的含量處於所述範圍，成為具有優異的負熱膨脹性且分散性及填充性優異者。再者，關於本發明的負熱膨脹材中的副成分元素的合計含量，於本發明的負熱膨脹材僅含有一種副成分元素的情況下，表示該一種副成分元素的含量，另外，於本發明的負熱膨脹材含有兩種以上的副成分元素的情況下，表示該些兩種以上的副成分元素的含量的合計量。
本發明的負熱膨脹材為包含磷酸鎢酸鋯的負熱膨脹材，於熱膨脹係數方面具有特徵。再者，本發明中熱膨脹係數是藉由以下的順序求出。首先，將負熱膨脹材試樣0.5g與黏合劑樹脂0.05g混合，全部填充至3mm×20mm的模具中，繼而使用手動壓力機於2 t的壓力下進行成形而製成成形體。將該成形體於電爐中以1100℃於大氣環境中煅燒2小時，從而獲得陶瓷成形體。對於所獲得的陶瓷成形體而言，使用熱機械測定裝置並於氮氣環境中，以負荷10g、溫度50℃~250℃的形式測定熱膨脹係數。作為熱機械測定裝置，例如可使用日本耐馳(NETZSCH JAPAN)製造的TMA4000SE。
本發明的負熱膨脹材的熱膨脹係數為-2.0×10-6/K~-3.3×10-6/K，較佳為-2.2×10-6/K~-3.1×10-6/K，特佳為-2.2×10-6/K~-3.0×10-6/K。包含先前的磷酸鎢酸鋯及含有副成分元素的磷酸鎢酸鋯的負熱膨脹材的熱膨脹係數大致為-3.0×10-6/K~-3.3×10-6/K，但本發明的負熱膨脹材根據Al原子的含量，先前的磷酸鎢酸鋯及含有副成分元素的磷酸鎢酸鋯的熱膨脹係數可以所述範圍進行調整。
本發明的負熱膨脹材的BET比表面積並無特別限制，但較佳為0.1m2/g~50m2/g，特佳為0.1m2/g~20m2/g。藉由負熱膨脹材的BET比表面積處於所述範圍，於將負熱膨脹材用作樹脂或玻璃等填料時處理變容易。
本發明的負熱膨脹材的平均粒徑並無特別限制，以利用掃描式電子顯微鏡觀察法而求出的平均粒徑計，較佳為0.1μm~50μm，特佳為0.5μm~30μm。藉由負熱膨脹材的平均粒徑處於所述範圍，於將負熱膨脹材用作樹脂或玻璃等填料時處理變容易。
本發明的負熱膨脹材的粒子形狀並無特別限制，例如亦可為球狀、粒狀、板狀、鱗片狀、晶須狀、棒狀、絲狀、破碎狀。
本發明的負熱膨脹材可利用以下敘述的本發明的磷酸鎢酸鋯的製造方法來較佳地製造。
本發明的磷酸鎢酸鋯的製造方法為負熱膨脹材的製造方法，具有：第1步驟，將W源、Zr源、P源、Al源混合而製備含有W源、Zr源、P源、Al源的漿料；第2步驟，對該漿料進行
噴霧乾燥而獲得反應前驅物；以及第3步驟，對該反應前驅物進行煅燒而獲得含Al的磷酸鎢酸鋯，所述負熱膨脹材的製造方法的特徵在於：於該第1步驟中，以Al原子的含量相對於進行該第3步驟而獲得的含Al的磷酸鎢酸鋯而成為100質量ppm~6000質量ppm的方式，於該漿料中混合Al源。
本發明的磷酸鎢酸鋯的製造方法具有：第1步驟，將W源、Zr源、P源、Al源混合而製備含有W源、Zr源、P源、Al源的漿料；第2步驟，對漿料進行噴霧乾燥而獲得反應前驅物；以及第3步驟，對反應前驅物進行煅燒而獲得含Al的磷酸鎢酸鋯。
本發明的磷酸鎢酸鋯的製造方法的第1步驟為將W源、Zr源、P源、Al源混合而製備含有W源、Zr源、P源、Al源的水性漿料的步驟。亦即，於第1步驟中，使W源、Zr源、P源及Al源分散於水溶媒中來製備於水溶媒中分散有W源、Zr源、P源及Al源的水性漿料。
第1步驟的W源為具有W原子的化合物。作為W源，較佳為不溶或難溶於水的化合物，例如可列舉：三氧化鎢、鎢酸銨、氯化鎢等。
第1步驟的Zr源為具有Zr原子的化合物。作為Zr源，可列舉氫氧化鋯及/或碳酸鋯等。碳酸鋯可為鹼性鹽，亦可為氨或鈉、鉀等的複鹽(double salt)。
第1步驟的P源為具有P原子的化合物。作為P源，較佳為磷酸。
第1步驟的Al源為具有Al原子的化合物。作為Al源，例如可列舉：硝酸鋁、硫酸鋁、磷酸氫鋁(aluminium biphosphate)、乳酸鋁等，該些中的硝酸鋁就廉價且工業上容易獲取，且容易獲得具有良好的負熱膨脹特性的負熱膨脹材的方面而言較佳。
第1步驟中的漿料的製備方法只要獲得將各原料均勻分散而成的漿料，則並無特別限制，就容易製備將各原料均勻分散而成的水性漿料的方面而言，較佳為首先製備均勻分散有W源的水性漿料，於其中混合P源及Zr源，繼而混合Al源。另外，漿料的製備中視需要可利用介質磨機對漿料進行濕式粉碎處理。作為介質磨機，較佳為珠磨機、球磨機、塗料振盪器、磨碎機及砂磨機。濕式粉碎處理的運轉條件或珠粒的種類及大小可根據裝置尺寸或處理量適當選擇。
關於第1步驟中的漿料的製備，就更有效地進行使用介質磨機的濕式粉碎處理的觀點而言，亦可於漿料中混合分散劑。作為於漿料中混合的分散劑，可列舉各種界面活性劑、聚羧酸銨鹽等。就分散效果變高的方面而言，漿料中的分散劑的濃度較佳為0.01質量%~10質量%，特佳為0.1質量%~5質量%。
關於第1步驟中的漿料的製備，於進行使用介質磨機的濕式粉碎處理的情況下，進行濕式粉碎處理直至利用雷射繞射．散射法而求出的固體成分的平均粒徑較佳為2μm以下，進而佳為1μm以下，特佳為0.1μm以上且0.5μm以下。就獲得反應性更優異的反應前驅物的方面而言，較佳為進行濕式粉碎處理直至固體
成分的平均粒徑成為所述範圍為止。
關於第1步驟中的P源向漿料中的混合量，漿料中的P源的P原子相對於W源的W原子的原子換算的莫耳比(P/W)較佳為1.7~2.3，特佳為1.9~2.1。就獲得反應性優異的反應前驅物的方面而言，較佳為漿料中的P源的P原子相對於W源的W原子的原子換算的莫耳比(P/W)處於所述範圍。
關於第1步驟中的Zr源向漿料中的混合量，漿料中的Zr源的Zr原子相對於W源的W原子的原子換算的莫耳比(Zr/W)較佳為1.7~2.3，特佳為1.9~2.1。就獲得反應性優異的反應前驅物的方面而言，較佳為漿料中的Zr源的Zr原子相對於W源的W原子的原子換算的莫耳比(Zr/W)處於所述範圍。
於第1步驟中，以Al原子的含量相對於經過第3步驟而獲得的含Al的磷酸鎢酸鋯而成為100質量ppm~6000質量ppm、較佳成為1000質量ppm~5000質量ppm、特佳成為1500質量ppm~5000質量ppm的方式，於漿料中混合Al源。於本發明中，隨著磷酸鎢酸鋯中的Al原子的含量增加，負熱膨脹材的熱膨脹係數有變大的傾向。若漿料中的Al原子的含量未滿所述範圍，則Al原子於負熱膨脹材中的添加效果不足，另外，若超過所述範圍，則負熱膨脹材並非為實用範圍的熱膨脹係數，負熱膨脹的特性受損。再者，於本發明中，所謂經過第3步驟而獲得的含Al的磷酸鎢酸鋯，於負熱膨脹材不含有副成分元素的情況下，為經過第3步驟而獲得的含有Al原子的磷酸鎢酸鋯，於負熱膨脹材
含有副成分元素的情況下，為含有Al原子及副成分元素的磷酸鎢酸鋯。另外，經過第3步驟而獲得的含Al的磷酸鎢酸鋯的生成量是根據於第1步驟中混合至漿料中的W源、Zr源、P源、Al源、以及視需要混合的具有副成分元素的化合物的混合量來算出。
漿料濃度、即漿料中的固體成分含量較佳為5質量%~50質量%，特佳為10質量%~30質量%。藉由漿料濃度處於所述範圍，成為操作性與處理容易的黏度。
作為第1步驟的形態例，可列舉第1步驟(1)：藉由使用磷酸作為P源，使用氫氧化鋯及碳酸鋯作為Zr源，磷酸與Zr源於漿料中進行反應，獲得均勻分散有W源與包含P及Zr的無定形化合物的中間漿料(A)，繼而於該中間漿料(A)中混合Al源，藉此獲得漿料(1)。就獲得具有優異的反應性的反應前驅物的方面而言，較佳為將進行第1步驟(1)而獲得的漿料(1)用於第2步驟。
關於第1步驟(1)的中間漿料(A)的製備，使磷酸與Zr源反應的溫度較佳為5℃~100℃，特佳為20℃~90℃，使磷酸與Zr源反應的時間較佳為0.5小時以上。
另外，關於中間漿料(A)的製備，就進一步提高均勻性、獲得反應性高的反應前驅物的方面而言，較佳為進而利用介質磨機對中間漿料(A)進行濕式粉碎處理。作為介質磨機，較佳為珠磨機、球磨機、塗料振盪器、磨碎機及砂磨機。濕式粉碎處理的運轉條件或珠粒的種類及大小可根據裝置尺寸或處理量來適
當選擇。
於第1步驟(1)中，繼而於中間漿料(A)中混合Al源，視需要實施攪拌等混合處理，使Al源分散於漿料中而獲得漿料(1)。
於第1步驟中，至第1步驟完成為止的期間，可向漿料中進一步混合具有選自由Mg、Zn、Cu、Fe、Cr、Mn、Ni、V、Li、B、Na、K、F、Cl、Br、I、Ca、Sr、Ba、Ti、Hf、Nb、Sb、Te、Ga、Ge、La、Ce、Nd、Sm、Eu、Tb、Dy及Ho所組成的群組中的一種或兩種以上的副成分元素的化合物的一種或兩種以上。
作為副成分元素，可列舉：Mg、Zn、Cu、Fe、Cr、Mn、Ni、V、Li、B、Na、K、F、Cl、Br、I、Ca、Sr、Ba、Ti、Hf、Nb、Sb、Te、Ga、Ge、La、Ce、Nd、Sm、Eu、Tb、Dy及Ho等。而且，作為具有副成分元素的化合物，可列舉：具有副成分元素的氧化物、氫氧化物、碳酸鹽、有機酸鹽、銨鹽、硝酸鹽、磷酸鹽、硫酸鹽、氯化物、溴化物、碘化物等。具有副成分元素的化合物可為單獨一種，亦可為兩種以上的組合。
關於第1步驟，於在漿料中混合具有副成分元素的化合物的情況下，為具有副成分元素的化合物向漿料中的混合量，但以副成分元素的原子換算的含量相對於經過第3步驟而獲得的含Al的磷酸鎢酸鋯、即含有Al原子及副成分元素的磷酸鎢酸鋯而較佳為0.1質量%~3質量%、特佳為0.2質量%~2質量%的方式，
於漿料中混合具有副成分元素的化合物。就負熱膨脹材成為具有優異的負熱膨脹性、分散性及填充性優異者的方面而言，較佳為具有副成分元素的化合物向漿料中的混合量處於所述範圍。
本發明的負熱膨脹材的製造方法的第2步驟是對第1步驟中獲得的漿料進行噴霧乾燥而獲得反應前驅物的步驟。
由於藉由噴霧乾燥進行乾燥處理時，可獲得原料粒子密集堵塞的狀態的造粒物，故進一步更容易獲得X射線繞射為單相的含有Al原子的磷酸鎢酸鋯。
關於噴霧乾燥法，藉由規定手段使漿料霧化，並使藉此產生的微細的液滴乾燥，藉此獲得反應前驅物。於漿料的霧化時例如有使用旋轉圓盤的方法與使用壓力噴嘴的方法。於第2步驟中亦可使用任一方法。
關於噴霧乾燥法，經霧化的液滴的大小並無特別限定，但較佳為1μm~40μm，特佳為5μm~30μm。漿料向噴霧乾燥裝置的供給量較佳為考慮該觀點來決定。
再者，於噴霧乾燥裝置中用於乾燥的熱風的溫度為100℃~270℃，較佳為150℃~230℃時防止粉體的吸濕且粉體的回收變容易，就所述方面而言較佳。
第2步驟中獲得的反應前驅物為含有生成磷酸鎢酸鋯的原料成分的W、P及Zr、Al、以及進而視需要含有的副成分元素的造粒粒子。就成為反應性優異的反應前驅物的方面而言，反應前驅物較佳為至少包含磷酸與Zr源於漿料中反應而生成的含有P
與Zr的無定形的化合物。再者，於使用磷酸作為P源、使用氫氧化鋯及碳酸鋯作為Zr源的情況下，已知磷酸與Zr源反應，生成包含P與Zr的無定形的化合物(例如，參照日本專利第6105140號公報、日本專利第6190023號公報等)。
第3步驟為藉由對反應前驅物進行煅燒而獲得目標負熱膨脹材的步驟。
關於第3步驟，對反應前驅物進行煅燒的煅燒溫度為900℃~1300℃。若反應前驅物的煅燒溫度未滿所述範圍，則有殘存有未反應的氧化物等，難以獲得X射線繞射為單相的含Al的磷酸鎢酸鋯的傾向，另外，若超過所述範圍，則有形成粒子彼此固結而成的狀態的塊而難以獲得粉末的傾向。
關於第3步驟，對反應前驅物進行煅燒的煅燒時間並無特別限制，進行充分的時間反應直至生成X射線繞射為單相的含Al的磷酸鎢酸鋯。關於第3步驟，大多情況下，以煅燒時間為1小時以上、較佳為2小時~20小時來生成具有希望滿足的各種物性的含Al的磷酸鎢酸鋯。另外，關於第3步驟，對反應前驅物進行煅燒的煅燒環境並無特別限制，亦可為惰性氣體環境下、真空環境下、氧化性氣體環境下、大氣中的任一種。
於第3步驟中，可進行一次煅燒，亦可根據需要進行多次。或者，於第3步驟中，出於使粉體特性均勻的目的，亦可將一次煅燒者粉碎，繼而再次進行煅燒。
關於第3步驟，於煅燒後適宜加以冷卻，視需要進行粉
碎、破碎、分級等，從而獲得作為目標的X射線繞射為單相的含Al的磷酸鎢酸鋯。
進行本發明的負熱膨脹材的製造方法而獲得的負熱膨脹材為X射線繞射為單相的含Al的磷酸鎢酸鋯。再者，進行本發明的負熱膨脹材的製造方法而獲得的負熱膨脹材於不使用具有副成分元素的化合物的情況下，為含有Al原子的磷酸鎢酸鋯，於使用具有副成分元素的化合物的情況下，為含有Al原子及副成分元素的磷酸鎢酸鋯。
如以上般，於本發明的負熱膨脹材的製造方法中，經過第1步驟至第3步驟而獲得負熱膨脹材。
進行本發明的負熱膨脹材的製造方法而獲得的負熱膨脹材的平均粒徑以藉由掃描式電子顯微鏡觀察來求出的平均粒徑計，較佳為0.1μm~50μm，特佳為0.5μm~30μm，且負熱膨脹材的BET比表面積較佳為0.1m2/g~50m2/g，更佳為0.1m2/g~20m2/g。藉由負熱膨脹材的平均粒徑及BET比表面積處於所述範圍，於將負熱膨脹材用作針對樹脂或玻璃等的填料用途時，處理變容易，就所述方面而言較佳。
進行本發明的負熱膨脹材的製造方法而獲得的負熱膨脹材的熱膨脹係數以利用所述方法來求出的熱膨脹係數計，為-2.0×10-6/K~-3.3×10-6/K，較佳為-2.2×10-6/K~-3.0×10-6/K。而且，於本發明的負熱膨脹材的製造方法中，藉由以所述範圍調節於第1步驟中混合的Al源的量，可將負熱膨脹材的熱膨脹係數調節為所
述範圍。
本發明的負熱膨脹材被用作粉體或膏。於將本發明的負熱膨脹材用作膏的情況下，可與黏性低的液狀樹脂混合，以膏的狀態使用本發明的負熱膨脹材。或者，亦可使本發明的負熱膨脹材分散於黏性低的液狀樹脂中，進而視需要含有黏合劑、焊劑材及分散劑等，以膏的狀態使用本發明的負熱膨脹材。
另外，出於改良本發明的負熱膨脹材於樹脂或橡膠等中的分散性的目的，可利用矽烷偶合劑對本發明的負熱膨脹材進行表面處理而加以使用。
將本發明的負熱膨脹材與正熱膨脹材併用而可用作複合材料。
本發明的複合材料為以包含所述本發明的負熱膨脹材與正熱膨脹材為特徵的複合材料。
本發明的複合材料中，作為與本發明的負熱膨脹材併用的正熱膨脹材，可使用各種有機化合物或無機化合物。作為用作正熱膨脹材的有機化合物或無機化合物，並無特別限定。作為用作正熱膨脹材的有機化合物，例如可列舉：橡膠、聚烯烴、聚環烯烴、聚苯乙烯、ABS、聚丙烯酸酯、聚苯硫醚、苯酚樹脂、聚醯胺樹脂、聚醯亞胺樹脂、環氧樹脂、矽酮樹脂、聚碳酸酯樹脂、聚乙烯樹脂、聚丙烯樹脂、聚對苯二甲酸乙二酯樹脂(PET樹脂)及聚氯乙烯樹脂等。另外，作為用作正熱膨脹材的無機化合物，例如可列舉：二氧化矽、石墨、藍寶石、各種玻璃材料、混凝土
材料、各種陶瓷材料等。該些中，正熱膨脹材較佳為選自金屬、合金、玻璃、陶瓷、橡膠及樹脂中的至少一種。
作為本發明的複合材料中的本發明的負熱膨脹材的含量，可採用該領域中一般的含量。可根據本發明的複合材料的用途或要求性能來選擇本發明的負熱膨脹材的含量。
本發明的複合材料中，藉由適宜選擇本發明的負熱膨脹材與其他化合物的調配比率，能夠實現負熱膨脹率、零熱膨脹率或低熱膨脹率。於本發明的負熱膨脹材中，藉由使磷酸鎢酸鋯含有Al原子，能夠於-2.0×10-6/K~-3.3×10-6/K的寬廣範圍調節熱膨脹係數，因此使用本發明的負熱膨脹材的本發明的複合材料藉由選擇本發明的負熱膨脹材的含量及正熱膨脹材的種類而容易調節熱膨脹率。
本發明的複合材料特別適合用作密封材料、電子零件的密封材料等。
[實施例]
以下，藉由實施例對本發明進行說明，但本發明並不限定於該些實施例。
(實施例1)
<第1步驟>
將市售的三氧化鎢(WO3；平均粒徑1.2μm)15質量份放入燒杯中，進而添加純水150質量份，於室溫(25℃)下攪拌60分鐘來製備包含三氧化鎢的9質量%漿料。繼而，向該漿料中以漿料
中的Zr：W：P的莫耳比成為2：1：2的方式添加氫氧化鋯、85質量%磷酸水溶液及氫氧化鎂，進而添加0.35質量份的氫氧化鎂，並於室溫(25℃)下攪拌60分鐘。
繼而，投入1.3質量份的作為分散劑的聚羧酸銨鹽，攪拌漿料，同時供給至投入有直徑0.5mm的氧化鋯珠的介質攪拌型珠磨機，來進行濕式粉碎。利用雷射繞射．散射法而求出的濕式粉碎後的漿料中的固體成分的平均粒徑為0.3μm。
繼而，向濕式粉碎後的漿料中添加硝酸鋁．九水合物2.8質量份，於室溫(25℃)下攪拌60分鐘來獲得原料漿料。
<第2步驟>
繼而，以2.4L/h的供給速度向設定為220℃的噴霧乾燥機中供給漿料，獲得至少含有包含P與Zr的無定形的化合物的反應前驅物。
<第3步驟>
繼而，以1050℃於大氣中對所獲得的反應前驅物進行2小時煅燒反應，從而獲得白色的煅燒品。利用研缽對煅燒品進行粉碎而獲得含有Al原子的磷酸鎢酸鋯粉末，將其作為負熱膨脹材試樣。
對所獲得的負熱膨脹材試樣進行X射線繞射分析，結果煅燒品為單相的Zr2(WO4)(PO4)2。
(實施例2)
於第1步驟中，將添加至濕式粉碎後的漿料中的硝酸鋁．九水合物設為1.1質量份，除此以外進行與實施例1相同的操作，獲得
含有Al原子的磷酸鎢酸鋯粉末，將其作為負熱膨脹材試樣。
對所獲得的負熱膨脹材試樣進行X射線繞射分析，結果煅燒品為單相的Zr2(WO4)(PO4)2。
(實施例3)
於第1步驟中，將添加至濕式粉碎後的漿料中的硝酸鋁．九水合物設為0.84質量份，除此以外進行與實施例1相同的操作，獲得含有Al原子的磷酸鎢酸鋯粉末，將其作為負熱膨脹材試樣。
對所獲得的負熱膨脹材試樣進行X射線繞射分析，結果煅燒品為單相的Zr2(WO4)(PO4)2。
(實施例4)
於第1步驟中，將添加至濕式粉碎後的漿料中的硝酸鋁．九水合物設為0.56質量份，除此以外進行與實施例1相同的操作，獲得含有Al原子的磷酸鎢酸鋯粉末，將其作為負熱膨脹材試樣。
對所獲得的負熱膨脹材試樣進行X射線繞射分析，結果煅燒品為單相的Zr2(WO4)(PO4)2。
(比較例1)
<第1步驟>
將市售的三氧化鎢(WO3；平均粒徑1.2μm)15質量份放入燒杯中，進而添加純水150質量份，於室溫(25℃)下攪拌60分鐘來製備包含三氧化鎢的9質量%漿料。繼而，向該漿料中以漿料中的Zr：W：P的莫耳比成為2：1：2的方式添加氫氧化鋯、85質量%磷酸水溶液及氫氧化鎂，進而添加0.35質量份的氫氧化鎂，
並於室溫(25℃)下攪拌60分鐘。
繼而，投入1.3質量份的作為分散劑的聚羧酸銨鹽，攪拌漿料，同時供給至投入有直徑0.5mm的氧化鋯珠的介質攪拌型珠磨機，來進行濕式粉碎。利用雷射繞射．散射法而求出的濕式粉碎後的漿料中的固體成分的平均粒徑為0.3μm。
<第2步驟>
繼而，以2.4L/h的供給速度向設定為220℃的噴霧乾燥機中供給漿料，獲得至少含有包含P與Zr的無定形的化合物的反應前驅物。
<第3步驟>
繼而，以1050℃於大氣中對所獲得的反應前驅物進行2小時煅燒反應，從而獲得白色的煅燒品。利用研缽對煅燒品進行粉碎而獲得磷酸鎢酸鋯粉末，將其作為負熱膨脹材試樣。
對所獲得的負熱膨脹材試樣進行X射線繞射分析，結果煅燒品為單相的Zr2(WO4)(PO4)2。
(比較例2)
於比較例1的第1步驟中，不向漿料中添加氫氧化鎂，除此以外進行與比較例1相同的操作，獲得白色的煅燒品。利用研缽對煅燒品進行粉碎而獲得磷酸鎢酸鋯粉末，將其作為負熱膨脹材試樣。
對所獲得的負熱膨脹材試樣進行X射線繞射分析，結果煅燒品為單相的Zr2(WO4)(PO4)2。
<物性評價>
對實施例及比較例中獲得的負熱膨脹材試樣測定平均粒徑、BET比表面積及熱膨脹係數。再者，平均粒徑及熱膨脹係數如下述般進行測定。將其結果示於表1中。另外，將實施例1中獲得的負熱膨脹材試樣的X射線繞射圖示於圖1，將SEM照片示於圖2。
(平均粒徑)
負熱膨脹材試樣的平均粒徑是根據掃描式電子顯微鏡觀察中以倍率400倍任意提取的50個以上的粒子的平均值來求出。
(線熱膨脹係數)
<陶瓷成型體的製作>
利用研缽將實施例及比較例中獲得的負熱膨脹材試樣0.5g與黏合劑(光譜摻合物44μm粉末(SpectroBlend 44μm Powder))0.05g混合5分鐘，並全部填充至3mm×20mm的模具中。繼而，使用手動壓力機於2 t的壓力下進行成型而製作粉末成型體。將獲得的粉末成型體於電爐中以1100℃於大氣環境中煅燒2小時，從而獲得磷酸鎢酸鋯的陶瓷成型體。
<熱膨脹係數的測定>
利用熱機械測定裝置(日本耐馳(NETZSCH JAPAN)製造的TMA4000SE)，來測定陶瓷成型體的線熱膨脹係數。測定條件設為氮氣環境、負荷10g、溫度範圍50℃~250℃。
[表1]
1)Al含量表示硝酸鋁中的Al原子相對於經過第3步驟而生成的含Al的磷酸鎢酸鋯整體的比例。
2)Mg含量表示氫氧化鎂中的Mg原子相對於經過第3步驟而生成的含Al的磷酸鎢酸鋯整體的比例。
根據表1的結果可知，由比較例1及比較例2而明確，磷酸鎢酸鋯的線膨脹係數藉由含有Mg而變小。相對於此，可知由比較例1與實施例1~實施例4而明確，藉由含有Al，磷酸鎢酸鋯的線膨脹係數變大，Mg與Al對負熱膨脹特性帶來的影響不同。另外，可知由實施例1~實施例4而明確，藉由使Al的含量發生變化，可調整磷酸鎢酸鋯的線膨脹係數。
(實施例4~實施例5及參考例1)
<環氧樹脂複合體的製作>
以相對於液狀環氧樹脂(三菱化學828EL)4g而成為表2所示的體積%(Vol%)的方式秤量實施例3中獲得的負熱膨脹材試樣，加入0.12g的硬化劑(四國化成的固唑(Curezol)2E4MZ)，利用混合機以旋轉速度2000rpm混合1分鐘而製成膏，並填充至1.5ml的微管(microtube)容器中。繼而，利用乾燥機旋轉同時於80℃下保持2小時，繼而於150℃下靜置0.5小時狀態下使其硬
化，從而獲得環氧樹脂複合體試樣。
將所獲得的環氧樹脂複合體試樣切斷，利用熱機械測定裝置(日本耐馳(NETZSCH JAPAN)製造的TMA4000SE)，於負荷50g、昇溫速度5℃/min下測定線膨脹，求出40℃~200℃的範圍的熱膨脹係數(CTE)。將其結果示於表2中。
另外，對於在環氧樹脂中不添加填料者(空白)及於環氧樹脂中添加二氧化矽填料(平均粒徑6.4μm：宇部日東公司製造、hipresica)者(參考例1)，亦進行相同的試驗，其結果亦一併記載於表2中。
可知，根據表2明確，與未添加(空白)相比，使本發明的負熱膨脹材含有於環氧樹脂中的環氧樹脂複合體的熱膨脹得到抑制，且調配有40Vol%者(實施例5)與配合有同量的二氧化矽者(參考例1)相比，熱膨脹得到抑制。
Claims (10)
- 一種負熱膨脹材，其特徵在於：包含含有Al原子的磷酸鎢酸鋯，X射線繞射為單相的含Al的磷酸鎢酸鋯，且熱膨脹係數為-2.0×10-6/K~-3.3×10-6/K。
- 如申請專利範圍第1項所述的負熱膨脹材，其中負熱膨脹材中的Al原子的含量為100質量ppm~6000質量ppm。
- 如申請專利範圍第1項或第2項所述的負熱膨脹材，含有選自由Mg、Zn、Cu、Fe、Cr、Mn、Ni、V、Li、B、Na、K、F、Cl、Br、I、Ca、Sr、Ba、Ti、Hf、Nb、Sb、Te、Ga、Ge、La、Ce、Nd、Sm、Eu、Tb、Dy及Ho所組成的群組中的一種以上的副成分元素。
- 如申請專利範圍第1項或第2項所述的負熱膨脹材，其中布厄特比表面積為0.1m2/g~30m2/g。
- 如申請專利範圍第1項或第2項所述的負熱膨脹材，其中平均粒徑為0.1μm~50μm。
- 一種負熱膨脹材的製造方法，具有：第1步驟，將W源、Zr源、P源、Al源混合而製備含有W源、Zr源、P源、Al源的漿料；第2步驟，對所述漿料進行噴霧乾燥而獲得反應前驅物；以及第3步驟，對所述反應前驅物進行煅燒而獲得含Al的磷酸鎢酸鋯，所述負熱膨脹材的製造方法的特徵在於：於所述第1步驟中，以Al原子的含量相對於進行所述第3步驟而獲得的所述含Al的磷酸鎢酸鋯而成為100質量ppm~6000 質量ppm的方式於所述漿料中混合Al源，且於所述第3步驟獲得的為X射線繞射為單相的所述含Al的磷酸鎢酸鋯。
- 如申請專利範圍第6項所述的負熱膨脹材的製造方法，於所述第1步驟中，於所述漿料中進而混合具有選自由Mg、Zn、Cu、Fe、Cr、Mn、Ni、V、Li、B、Na、K、F、Cl、Br、I、Ca、Sr、Ba、Ti、Hf、Nb、Sb、Te、Ga、Ge、La、Ce、Nd、Sm、Eu、Tb、Dy及Ho所組成的群組中的一種或兩種以上的副成分元素的化合物的一種或兩種以上。
- 如申請專利範圍第6項或第7項所述的負熱膨脹材的製造方法，其中所述Al源為硝酸鋁。
- 一種複合材料，其特徵在於：包含如申請專利範圍第1項至第5項中任一項所述的負熱膨脹材與正熱膨脹材。
- 如申請專利範圍第9項所述的複合材料，其中所述正熱膨脹材為選自金屬、合金、玻璃、陶瓷、橡膠及樹脂中的至少一種。
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