TWI659006B - 介電陶瓷組成物 - Google Patents
介電陶瓷組成物 Download PDFInfo
- Publication number
- TWI659006B TWI659006B TW107104646A TW107104646A TWI659006B TW I659006 B TWI659006 B TW I659006B TW 107104646 A TW107104646 A TW 107104646A TW 107104646 A TW107104646 A TW 107104646A TW I659006 B TWI659006 B TW I659006B
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- Prior art keywords
- ceramic composition
- inorganic component
- dielectric ceramic
- dielectric
- atomic
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- 239000000203 mixture Substances 0.000 title claims abstract description 44
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 28
- 239000006104 solid solution Substances 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims description 26
- 229910020068 MgAl Inorganic materials 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 description 18
- 239000000047 product Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- 238000001354 calcination Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- 238000010894 electron beam technology Methods 0.000 description 6
- 229910004283 SiO 4 Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000010344 co-firing Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000006112 glass ceramic composition Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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Abstract
一種介電陶瓷組成物，包括具有三方複三正方錐面晶體結構的第一無機成分、具有六八面體晶體結構的第二無機成分以及所述三方複三正方錐面晶體結構與所述六八面體晶體結構的固溶體部，其形成於所述第一無機成分與所述第二無機成分之間。
Description
本發明是有關於一種在微波頻率下有低介電常數（Dk）和低介電損耗的介電陶瓷組成物。
在第五代無線通訊網路（Fifth Generation or 5G wireless communications networks）中毫米波（millimeter-wave, MMW）已經開發出來，用以支持快速移動大量數據。
當訊號頻率進入毫米波範圍時，毫米波的輻射損耗會非常高，限制了5G應用的覆蓋範圍。一種解決方案是降低RF模組中封裝基板的介電常數和介電損耗。在MMW通訊的情況下，封裝基板的介電常數較佳是小於4＠10GHz。
近來，一種為了降低介電常數的方法是在陶瓷材料中添加玻璃，以製造用於封裝基板的玻璃陶瓷材料。然而，用於玻璃陶瓷材料的成核劑可能會阻礙介電損耗降低。而且，由於玻璃陶瓷材料具有玻璃成分，無法改善熱傳導效率。因此，有必要開發具有低介電常數和低介電損耗的介電陶瓷組成物。
本發明提供一種介電陶瓷組成物，包括成分具有三方複三正方錐面晶體結構的第一無機成分、具有六八面體晶體結構的第二無機成分以及三方複三正方錐面晶體結構與六八面體晶體結構的固溶體部，其形成於第一無機成分與第二無機成分之間。
在本發明的一實施例中，上述的第一無機成分包括Mg4
Nb2
O9
。
在本發明的一實施例中，上述的第二無機成分包括MgAl2
O4
、Mg2
SiO4
、Mg2
TiO4
、Zn2
TiO4
、β-SiO2
或Zn2
VO4
。
在本發明的一實施例中，上述的介電陶瓷組成物中的第一無機成分的含量為25原子%~50原子%。
在本發明的一實施例中，上述的介電陶瓷組成物中的第二無機成分的含量為25原子%~50原子%。
在本發明的一實施例中，上述的介電陶瓷組成物還可包括玻璃成分。
在本發明的一實施例中，上述的介電陶瓷組成物中的玻璃成分的含量為30重量%以下。
本發明提供另一種介電陶瓷組成物，包括第一無機成分、第二無機成分以及形成於第一無機成分與第二無機成分之間的固溶體部。所述第一無機成分包括Mg4
Nb2
O9
，且所述第二無機成分包括MgAl2
O4
、Mg2
SiO4
、Mg2
TiO4
、Zn2
TiO4
、β-SiO2
或Zn2
VO4
。
在本發明的另一實施例中，上述的介電陶瓷組成物中的第一無機成分的含量為25原子%~50原子%。
在本發明的另一實施例中，上述的介電陶瓷組成物中的第二無機成分的含量為25原子%~50原子%。
在本發明的另一實施例中，上述的介電陶瓷組成物還可包括玻璃成分。
在本發明的另一實施例中，上述的介電陶瓷組成物中的玻璃成分的含量為30重量%以下。
為讓本發明的上述特徵能更明顯易懂，下文特舉實施例，並配合所附圖式作詳細說明如下。
現在將參照圖式來更完整地描述本發明的實施例。然而，仍可使用多種不同形式來實施本發明，因此圖式與以下實施例只是為了使本發明的概念更為清楚與完整，而不是用以限制本發明的範圍。
在本發明的第一實施例中，介電陶瓷組成物包括具有三方複三正方錐面晶體結構的第一無機成分、具有六八面體晶體結構的第二無機成分以及在第一無機成分與第二無機成分之間形成的三方複三正方錐面晶體結構與六八面體晶體結構的固溶體部。
在本文中所述的「三方複三正方錐面晶體結構」（trigonal ditrigonal pyramidal crystal structure）是指三方晶系系統（trigonal system）中的複三正方錐面晶族的結構；亦即，三方晶系系統具有位於同一平面上的三軸，分別為a軸、b軸、c軸，且a=b≠c，即a、b兩軸比c軸短或比c軸長。
在本文中所述的「六八面體晶體結構」（hexoctahedral crystal structure）是指立方晶系（cubic system）中的六八面體晶族的結構。在晶體學中，六方晶體為六大晶系的其中之一。
在本文中所述的「固溶體」（solid solution）是指兩種成分的固態溶液，其中一種成分與溶質相似，另一種成分與溶劑相似。因此，在本文中所述的固溶體部是指在兩個成分之間形成的部分，其中一個成分的晶體結構添加另一個成分仍保持不變。
在本發明的第一實施例中，第一無機成分例如是Mg4
Nb2
O9
。
在本發明的第一實施例中，第二無機成分例如是MgAl2
O4
、Mg2
SiO4
、Mg2
TiO4
、Zn2
TiO4
、β-SiO2
或Zn2
VO4
。
在本發明的第一實施例中，介電陶瓷組成物中的第一無機成分的含量例如是25原子%~50原子%，且第二無機成分的含量例如是25原子%~50原子%。
在本發明的另一實施例中，介電陶瓷組成物還可選擇性地包括玻璃成分。例如，所述介電陶瓷組成物中的玻璃成分的含量例如在30重量%以下。若玻璃成分的含量為30重量%以下，則介電陶瓷組成物的介電常數可進一步降低，同時可以維持其熱傳導效率在良好的程度。
在本發明的第二實施例中，介電陶瓷組成物包括第一無機成分、第二無機成分與形成於第一無機成分與第二無機成分之間的固溶體部。所述第一無機成分例如是Mg4
Nb2
O9
，且所述第二無機成分例如是MgAl2
O4
、Mg2
SiO4
、Mg2
TiO4
、Zn2
TiO4
、β-SiO2
或Zn2
VO4
。介電陶瓷組成物中的第一無機成分的含量例如是25原子%~50原子%，第二無機成分的含量例如是25原子%~50原子%。另外，在第二實施例中，介電陶瓷組成物還可包括玻璃成分。
以下為根據本發明的介電陶瓷組成物的製備方式。但是本發明並不侷限於此。
首先，提供兩種符合高對稱性的結晶相需求的原料。舉例來說，三方晶系系統中具有高度對稱性的複三正方錐面晶族(ditrigonal pyramidal class)（赫爾曼-莫甘符號:3m，Hermann-Maugin symbol: 3m）和複三方偏三角面晶族(ditrigonal scalahedral class)（赫爾曼-莫甘符號:，Hermann-Maugin symbol:）。因此，具有三方複三正方錐面晶體結構的材料如Mg4
Nb2
O9
可作為其中一種原料，另一種原料是具有三方複三方偏三角面晶體結構的材料如（Sr1-2x
Nax
Lax
）TiO3
（x ＜ 0.5）、AlBO3
、Al2
O3
或Ta2
O3
。
在1300 °C以上的預定溫度對所述兩種原料進行共燒。因為這兩種原料的晶相皆具有高度對稱性，所以共燒產物由於極性的抵銷而具有低介電常數，且由於高結晶性而具有低介電損耗。在共燒之前，可選擇性地在1250 °C以下的預定溫度進行鍛燒（calcination）。而在添加玻璃成分的情況下，所述玻璃成分應該添加到共燒產物中，且在低於1000 °C的溫度下進行低溫熱處理。
以下透過實驗例來更具體地描述本發明，然而，應知本發明的實驗例並不侷限於以下內容，且可以適當變化來實踐。
〈實驗例A-1〉
1. 製備Mg4
Nb2
O9
以下為兩種製備Mg4
Nb2
O9
的方法。
方法1. 利用過量的MgO來穩定Mg4
Nb2
O9
的相。其反應流程如下所示： 4MgO + Nb2
O5
→ (1-x)MgNb2
O6
+ (x)Mg4
Nb2
O9
(1) (1-x)MgNb2
O6
+ (x)Mg4
Nb2
O9
+ 4MgO → Mg4
Nb2
O9
+ xMgO (2)
最後，用稀硝酸進行酸洗。
方法2. 先形成MgNb2
O6
後加入MgO轉化成Mg4
Nb2
O9
。反應流程如下所示： MgO + Nb2
O5
→ MgNb2
O6
(3) MgNb2
O6
+ 3MgO → Mg4
Nb2
O9
(4)
實驗例A-1是利用方法2製備。具體而言，先將高純度的MgO和Nb2
O5
（MgO與Nb2
O5
的莫耳比為1:1）放入裝有酒精作為溶劑的研磨罐中，再用氧化鋯球進行球磨24小時。將混合過的漿料在80 °C乾燥，然後於高溫爐中以1050 °C鍛燒10小時，以形成中間產物MgNb2
O6
。之後，利用上述步驟的相同方法將MgNb2
O6
和MgO（MgNb2
O6
與MgO的莫耳比為1:3）混合後，將混合物在高溫爐中以1050 °C鍛燒10小時，以形成Mg4
Nb2
O9
。
2. 共燒
將Mg4
Nb2
O9
、MgO和Al2
O3
（Mg4
Nb2
O9
、MgO與Al2
O3
的莫耳比為3:1:1）放入裝有作為溶劑的酒精的研磨罐中，再用氧化鋯球進行球磨24小時。將混合的漿料以80 °C乾燥後，放入高溫爐中以1050°C鍛燒10小時，再以1350 °C燒結10小時。MgO的存在有助於降低燒結溫度。反應式（5）如下： Mg4
Nb2
O9
+ MgO + A12
O3
→ Mg4
Nb2
O9
+ MgAl2
O4
(5)
對實驗例A-1的共燒產物進行X光繞射分析(XRD)，結果如圖1所示。從圖1可以得知，在Mg4
Nb2
O9
（標記為429）和MgAl2
O4
實際為共燒形成的產物，同時也發現少量殘餘未反應的MgO。
此外，檢測實驗例A-1的共燒產物的介電常數和介電損耗（Df），結果顯示於表1。所述的「介電損耗」是指介電材料種類的函數，通常由材料的耗散因子（dissipation factor，Df）來定義，較低的數值表示較低的介電損耗。
3. 計算理論介電常數
根據上述反應式（5），其理論Dk可由以下方程式（6）來計算。(6)
在方程式（6）中，ε1
表示Mg4
Nb2
O9
的介電常數（Dk =13.5），ε2
表示MgAl2
O4
的介電常數（Dk =8.8），ν表示體積分率，εmix
表示介電常數的最低理論值。理論Dk顯示於表1。
〈實驗例A-2、A-3、A-4、A-5〉
根據實驗例A-1的方法製備，不同之處在於改變了原料的莫耳比。莫耳比的改變量與結果顯示於表1。
〈實驗例B-1〉
根據實驗例A-1的方法製備，不同之處在於鍛燒溫度變為1150 °C。其介電性能的結果如表2所示。
〈實驗例B-2、B-3、B-4、B-5〉
根據實驗例B-1的方法製備，不同之處在於改變了原料的莫耳比。其介電性能的結果如表2所示。
〈實驗例C-1〉
根據實驗例A-1的方法製備，不同之處在於鍛燒溫度變為1250 °C。其介電性能的結果如表3所示。
〈實驗例C-2、C-3、C-4、C-5〉
根據實驗例C-1的方法製備，不同之處在於改變了原料的莫耳比。其介電性能的結果如表3所示。
〈實驗例D-1〉
根據實驗例A-1的方法製備，不同之處在於燒結溫度變為1500 °C。其介電性能的結果如表4所示。
〈實驗例D-2、D-3、D-4、D-5〉
根據實驗例D-1的方法製備，不同之處在於改變了原料的莫耳比。其介電性能的結果如表4所示。
〈實驗例E-1〉
根據實驗例B-1的方法製備，不同之處在於燒結溫度變為1500 °C。其介電性能的結果如表5所示。
〈實驗例E-2、E-3、E-4、E-5〉
根據實驗例E-1的方法製備，不同之處在於改變了原料的莫耳比。其介電性能的結果如表5所示。
〈實驗例F-1〉
根據實驗例C-1的方法製備，不同之處在於燒結溫度變為1500 °C。其介電性能的結果如表6所示。
〈實驗例F-2、F-3、F-4、F-5〉
根據實驗例F-1的方法製備，不同之處在於改變了原料的莫耳比。其介電性能的結果如表6所示。
表1
鍛燒溫度為1050 °C，燒結溫度為1350 °C。
表2
鍛燒溫度為1150 °C，燒結溫度為1350 °C。
表3
鍛燒溫度為1250 °C，燒結溫度為1350 °C。
表4
鍛燒溫度為1050 °C，燒結溫度為1500 °C。
表5
鍛燒溫度為1150 °C，燒結溫度為1500 °C。
表6
鍛燒溫度為1250 °C，燒結溫度為1500 °C。
從上表1至表6可以得知，根據本發明所有實驗例所檢測的實際介電常數都小於理論介電常數。換句話說，本發明的共燒產物具有低於期望值的介電常數。
〈實驗例G〉
根據實驗例A-1的方法製備，不同之處在於形成共燒產物後再添加玻璃成分。具體而言，在實驗例A-1所得到的粉末中添加玻璃粉末（SiO2
-MgO-CaO-ZnO），其中實驗例A-1的粉末與玻璃粉末的重量比為7:3。經球磨混合後，將混合物壓成圓柱狀試片，再放入高溫爐於850 °C中燒結1小時。在高頻下測量圓柱狀試片，以獲得介電常數為4.2（Dk=4.2）、介電損耗為0.003（Df=0.003）。因此，證明了添加玻璃成分能在低溫（＜900 °C）燒結的同時維持良好的電性能。
接著，對實驗例G進行掃描式電子顯微鏡(SEM)分析，得到圖2A和圖2B的SEM影像，其中圖2A是5,000倍的SEM影像、圖2B是2,500倍的SEM影像。
〈比較例A〉
將Mg4
Nb2
O9
、Al2
O3
和玻璃成分（Mg4
Nb2
O9
、Al2
O3
與玻璃成分的重量比為7:7:6）利用球磨方式充分混合，其中玻璃成分與實驗例G相同。之後，將混合物壓成圓柱狀試片，放入高溫爐於850 °C中燒結1小時。在高頻下測量圓柱狀試片，以獲得介電常數為7.1（Dk=7.1）、介電損耗為0.008（Df=0.008）。比較例A的介電常數明顯高於實驗例G的介電常數。因此，證明了比較例A具有不良的電性能。
接著，對比較例A進行掃描式電子顯微鏡(SEM)分析，得到圖3的SEM影像。
藉由比較具有玻璃成分的實驗例G和比較例A，可以得知，實驗例G的實際介電常數小於比較例A的實際介電常數。此外，從圖3中可以得知，比較例A的玻璃成分是與Mg4
Nb2
O9
、Al2
O3
混合。
然而，圖4A和圖4B是對圖2A的選擇區域A以透射電子束分別進行繞射的[001]和[-111]軸繞射圖，兩個繞射點之間的距離可以透過下述公式（1）獲得。由此可以證明圖4A和圖4B中的Mg4
Nb2
O9
為六方晶系。
(1)
此外，圖5A和圖5B是對圖2B的選擇區域B以透射電子束分別進行繞射的[001]和[-111]軸繞射圖，兩個繞射點之間的距離可以透過下述公式(2)獲得。由此可以證明圖5A和圖5B中的MgAl2O4為立方晶系。
因此，從圖4A、圖4B、圖5A和圖5B可以得知，實驗例G的玻璃成分沒有與Mg4Nb2O9和MgAl2O4混合。
綜上所述，根據本發明，可得到在微波頻率下具有低介電常數與低介電損耗的介電陶瓷組成物。具體來說，本發明所得的介電陶瓷組成物具有低於理論值的介電常數。
雖然本發明已以實施例揭露如上，然其並非用以限定本發明，任何所屬技術領域中具有通常知識者，在不脫離本發明的精神和範圍內，當可作些許的更動與潤飾，故本發明的保護範圍當視後附的申請專利範圍所界定者為準。
A、B‧‧‧選擇區域
圖1是根據本發明的實驗例A-1的共燒產物的X光繞射分析(XRD)曲線圖。 圖2A是根據本發明的實驗例G的產物的5,000倍掃描式電子顯微(SEM)影像。 圖2B是根據本發明的實驗例G的產物的2,500倍SEM影像。 圖3是比較例A的產物的SEM影像。 圖4A是對圖2A的選擇區域A以透射電子束進行繞射的[001]軸繞射圖。 圖4B是對圖2A的選擇區域A以透射電子束進行繞射的[-111]軸繞射圖。 圖5A是對圖2B的選擇區域B以透射電子束進行繞射的[001]軸繞射圖。 圖5B是對圖2B的選擇區域B以透射電子束進行繞射的[-111]軸繞射圖。
Claims (8)
- 一種介電陶瓷組成物，包括：一第一無機成分，具有一三方複三正方錐面晶體結構，其中該介電陶瓷組成物中的該第一無機成分的含量為25原子%~50原子%；一第二無機成分，具有一六八面體晶體結構，其中該介電陶瓷組成物中的該第二無機成分的含量為25原子%~50原子%；以及一固溶體部，形成於該第一無機成分與該第二無機成分之間，其中該固溶體部為該三方複三正方錐面晶體結構與該六八面體晶體結構的固溶體。
- 如申請專利範圍第1項所述的介電陶瓷組成物，其中該第一無機成分包括Mg4Nb2O9。
- 如申請專利範圍第1項所述的介電陶瓷組成物，其中該第二無機成分包括MgAl2O4、Mg2TiO4、Zn2TiO4、β-SiO2或Zn2VO4。
- 如申請專利範圍第1項所述的介電陶瓷組成物，更包括一玻璃成分。
- 如申請專利範圍第4項所述的介電陶瓷組成物，其中該介電陶瓷組成物中的該玻璃成分的含量為30重量%以下。
- 一種介電陶瓷組成物，包括：一第一無機成分，包括Mg4Nb2O9，其中該介電陶瓷組成物中的該第一無機成分的含量為25~50原子%；一第二無機成分，包括MgAl2O4、Mg2TiO4、Zn2TiO4、六八面體晶體結構的β-SiO2或Zn2VO4，其中該介電陶瓷組成物中的該第二無機成分的含量為25~50原子%；以及一固溶體部，形成於該第一無機成分與該第二無機成分之間。
- 如申請專利範圍第6項所述的介電陶瓷組成物，更包括一玻璃成分。
- 如申請專利範圍第7項所述的介電陶瓷組成物，其中該介電陶瓷組成物中的該玻璃成分的含量為30重量%以下。
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