TW201527553A - 肥粒鐵燒結體、肥粒鐵燒結板及肥粒鐵燒結薄片 - Google Patents
肥粒鐵燒結體、肥粒鐵燒結板及肥粒鐵燒結薄片 Download PDFInfo
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Abstract
本發明之技術課題在於提供μ’高、μ”低、更且μ’之溫度變化小、肥粒鐵的微細構造為緻密之肥粒鐵燒結薄片。本發明係關於具有由以氧化物換算為47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO所成之組成的肥粒鐵燒結板,其係含有0.2~1.4wt%的SnO2與0.005~0.03wt%的S,密度為5.05~5.30g/cm3者作為特徵之肥粒鐵燒結體、肥粒鐵燒結板,及在該肥粒鐵燒結板之表面設置溝,更且設置黏著層及/或保護層者作為特徵之肥粒鐵燒結薄片。
Description
本發明提供肥粒鐵燒結體、肥粒鐵燒結板及在該肥粒鐵燒結板之表面上設有黏著層及/或保護層之肥粒鐵燒結薄片。
於行動電話、智慧型手機等之通信機器中,如NFC(近距離無線通信)或結算系統上,搭載有使用平面狀線圈天線可將資訊予以通訊聯絡的系統。該天線由於係接近電路基板或電池等之包含金屬的零件而配置,那樣子通訊聯絡感度係顯著降低。因此,為了提高通訊聯絡感度,在該天線與包含金屬的零件之間配置肥粒鐵燒結薄片。
於此等之系統中,為了提高其通訊聯絡感度,有揭示藉由在Ni-Zn-Cu肥粒鐵中添加CoO來控制肥粒鐵燒結薄片的導磁率之技術(專利文獻1、2)。
另一方面,於電感器零件之領域中,有揭示藉由添加SnO2、Co氧化物、Bi氧化物,而得到導磁率的溫度特性優異,且高密度之電感器零件之方法(專利文獻3)。又,有揭示藉由使肥粒鐵中的S與Cl之含量成為特定內,而
抑制Ag朝肥粒鐵中的擴散之方法(專利文獻4)。另外,已知使用含有SnO2的肥粒鐵於電感器(專利文獻5)。
專利文獻1:特開2005-340759號公報
專利文獻2:特開2013-133263號公報
專利文獻3:特開2002-255637號公報
專利文獻4:特開平5-258937號公報
專利文獻5:特開2002-124408號公報
由於通信機器之小型化、高機能化,要求進一步提高平面狀線圈天線的通訊聯絡感度,因此,必須藉由增大肥粒鐵燒結薄片的導磁率之實數部(μ’),而增大天線之電感。另一方面,於肥粒鐵燒結薄片中,在通訊聯絡頻率的13.56MHz中,有若μ’變大則導磁率的虛數部(μ”)所表示之損失變大之性質,該損失係使天線的通訊聯絡感度降低。因此,要求儘可能地μ”小、μ’大之肥粒鐵燒結薄片。
專利文獻1中,揭示添加CoO之技術,惟μ’低,在通訊聯絡感度的提高上不充分。
專利文獻2中,提案含有Co,具有由粒成長進行中的結晶粒子與空孔所成之微細構造的肥粒鐵燒結薄片,惟由於具有空孔,故在製造過程中於操作之際有容易破裂之
缺點。因為,為了不易破裂,必須提高燒結密度,去除空孔。
專利文獻3中,不考慮使S存在於肥粒鐵中。專利文獻4中為了控制內部導體中的Ag之擴散,而控制S成分及Cl成分之含量,惟不含Sn,μ’之溫度變化大。專利文獻5記載之肥粒鐵係不含Co,為μ”大者。
又,肥粒鐵燒結薄片多為併入攜帶式機器中,於室外使用。因此,為了使天線的特性對於外部氣體溫度的變化呈現安定,必須減少導磁率對於溫度的變化。
因此,本發明之技術課題在於提供燒結密度高、μ’大、μ”小、更且μ’之溫度變化小之肥粒鐵燒結薄片。
前述技術的課題係可藉由如以下的本發明達成。
即,本發明係肥粒鐵燒結體,其特徵係具有由以氧化物換算為47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO所成之組成的肥粒鐵燒結體,其係含有0.2~1.4wt%的SnO2與0.005~0.03wt%的S(本發明1)。
即,本發明係肥粒鐵燒結板,其特徵係具有由以氧化物換算為47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO所成之組成的肥粒鐵燒結板,其係含有0.2~1.4wt%的SnO2與0.005~0.03wt%的S(本發明2)。
即,本發明係肥粒鐵燒結板,其特徵為具有由以氧化物換算為47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO所成之組成的肥粒鐵燒結板,其係含有0.2~1.4wt%的SnO2與0.005~0.03wt%的S,密度為5.05~5.30g/cm3(本發明3)。
又,本發明係肥粒鐵燒結薄片,其係在本發明2或3記載之肥粒鐵燒結板的一側之表面上設有黏著層,在相反側之表面上設有保護層者(本發明4)。
另外,本發明係肥粒鐵燒結薄片,其係在本發明2或3記載之肥粒鐵燒結板之兩面上設有黏著層者(本發明5)。
還有,本發明係肥粒鐵燒結薄片,其係在本發明2或3記載之肥粒鐵燒結板之兩面上設有保護層者(本發明6)。
又,本發明係肥粒鐵燒結薄片,其係於本發明4~6中任一項記載之肥粒鐵燒結薄片中,在肥粒鐵燒結板的至少一側之表面上形成有至少1個溝(本發明7)。
另外,本發明係肥粒鐵燒結薄片,其係於本發明4~6中任一項記載之肥粒鐵燒結薄片中,肥粒鐵燒結板被分割成小片狀(本發明8)。
本發明之肥粒鐵燒結體、肥粒鐵燒結板及肥粒鐵燒結
薄片,由於μ’大、μ”小、更且μ’之溫度變化小,而成為適合在NFC等的系統中使通訊聯絡感度提高且安定之構件。
圖1係顯示實施例1所得之肥粒鐵燒結板的微細構造之掃描型電子顯微鏡照片。
圖2係顯示比較例1所得之肥粒鐵燒結板的微細構造之掃描型電子顯微鏡照片。
如以上更詳細地說明本發明之構成。
本發明之肥粒鐵燒結體及肥粒鐵燒結板之組成係以氧化物換算為47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO,合計為100mol%。對於其,進一步含有0.2~1.4wt%的SnO2與0.005~0.03wt%的S。即,為Fe2O3、NiO、ZnO、CuO、CoO所成之肥粒鐵與SnO2和S之混合物。
本發明之肥粒鐵燒結體及肥粒鐵燒結板中的Fe2O3之組成,係於未達47.5mol%時,μ’變小。超過49.8mol%時,變無法燒結。更佳的Fe2O3之組成為48~49.5mol%。
本發明之肥粒鐵燒結體及肥粒鐵燒結板中的NiO之組
成,係於未達13.5mol%時,μ”變大。超過19.5mol%,μ’變小。更佳的NiO之組成為14.5~18.5mol%。
本發明之肥粒鐵燒結體及肥粒鐵燒結板中的ZnO之組成,係於未達21mol%時,μ’變小。超過27mol%,μ”變大。更佳的ZnO之組成為22~26mol%。
本發明之肥粒鐵燒結體及肥粒鐵燒結板中的CuO之組成,係於未達7.5mol%時,變無法燒結。超過12.5mol%時,CuO析出,μ’變小。更佳的CuO之組成為8.5~11.5mol%。
本發明之肥粒鐵燒結體及肥粒鐵燒結板中的CoO之組成,係於未達0.2mol%時,μ”變大。超過0.8mol%時,μ’變小,而且μ’之溫度變化大。更佳的CoO之組成為0.2~0.7mol%。
本發明之肥粒鐵燒結體及肥粒鐵燒結板中的SnO2之含量,係於未達0.2wt%時,μ’之溫度變化大。超過1.4wt%時,μ’變小。更佳的SnO2之含量為0.2~1.3wt%。
本發明之肥粒鐵燒結體及肥粒鐵燒結板中的S之含量,係於未達0.005wt%時,燒結性變差,μ’變小。超過0.03wt%時,μ’之溫度變化與μ”變大。更佳的S之含量為0.007~0.025wt%。
本發明之肥粒鐵燒結板之密度未達5.05g/cm3時,由於其微細構造中發生數μm以下的空孔,成為不均勻的微細構造,操作時容易破裂。由於肥粒鐵之理論密度為5.30g/cm3左右,本發明中之密度上限為5.30g/cm3。如本
發明,肥粒鐵燒結板之密度若為5.05~5.30g/cm3之範圍,則在微細構造中不發生空孔,由於得到緻密的微細構造,操作時不易破裂而生產性提高。為了使肥粒鐵燒結板之密度成為上述範圍,可藉由使各構成成分的比率成為上述範圍內,同時控制燒結溫度而實現。
本發明之肥粒鐵燒結板之厚度較佳為0.01~0.7mm,更佳為0.02~0.7mm。
可在本發明之肥粒鐵燒結板的至少一側之表面上設置黏著層。黏著層之厚度較佳為0.001~0.1mm。
可在本發明之肥粒鐵燒結板的至少一側之表面上設置保護層。保護層之厚度較佳為0.001~0.1mm。
本發明之肥粒鐵燒結薄片的μ”(在25℃)較佳為90~180,更佳為100~170。
本發明之肥粒鐵燒結薄片的μ”(在25℃)較佳為0.05~5,更佳為0.1~4.5。
本發明之肥粒鐵燒結薄片的μ’之溫度變化(在85℃的導磁率之實數部μ’85與μ’25之差相對於在25℃的導磁率之實數部μ’25之比((μ’85-μ’25)/μ’25))較佳為5~30%,更佳為5~25%。
作為本發明中之黏著層,可舉出雙面黏著帶。作為雙面黏著帶,並沒有特別的限制,可使用眾所周知的雙面黏著帶。又,作為黏著層,亦可為在肥粒鐵燒結板之單面上依順序層合有黏著層、彎曲性且伸縮性的薄膜或薄片、黏著層及脫模薄片者。
藉由設置本發明中之保護層,可對於將肥粒鐵燒結板分割時的掉粉,提高可靠性及耐久性。作為該保護層,只要是使肥粒鐵燒結薄片彎曲時不斷裂之伸縮樹脂,則沒有特別的限制,可例示PET薄膜等。
本發明之肥粒鐵燒結薄片,係為了密接於經彎曲的部分而貼附,可為以在肥粒鐵燒結板的至少一側之表面上設置的至少1個溝作為起點,將肥粒鐵燒結板可分割地構成。前述溝係可為連續,也可斷續地形成,而且亦可藉由形成多數的微小凹部,作為溝之替代。溝係截面宜為U字型或V字型。
本發明之肥粒鐵燒結薄片,係為了密接於經彎曲的部分而貼附,及為了在使用時防止破裂,較佳為預先將肥粒鐵燒結板分割成小片狀。例如,可為以在肥粒鐵燒結板的至少一側之表面上設置的至少1個溝作為起點,將肥粒鐵燒結板分割,或不形成溝而將肥粒鐵燒結板分割成小片狀之方法的任一者。
肥粒鐵燒結板係藉由溝而劃分成任意大小三角形、四邊形、多角形或彼等之組合。例如,三角形、四邊形、多角形的1邊之長度通常為1~12mm,於被附著物的接著面為曲面時,較佳在1mm以上,其曲率半徑的1/3以下,更佳在1mm以上為1/4以下。形成溝時,在溝以外的地方不會破裂成不定形,平面係不用說,可密接或實質地密接於圓柱狀的側曲面及有一些凹凸的面。
形成於肥粒鐵燒結板中的溝之開口部的寬度,一般較
佳為250μm以下,更佳為1~150μm。開口部的寬度超過250μm時,肥粒鐵燒結板的導磁率之降低會變大而不宜。
又,溝的深度通常為肥粒鐵燒結板之厚度的1/20~3/5。
再者,厚度為0.01mm~0.2mm的薄肥粒鐵燒結板時,溝的深度較佳為肥粒鐵燒結板之厚度的1/20~1/4,更佳為1/20~1/6。
其次,說明本發明的肥粒鐵燒結板及肥粒鐵燒結薄片之製造方法。
首先,肥粒鐵粉末係可藉由將構成肥粒鐵的各元素之氧化物、碳酸鹽、氫氧化物、草酸鹽等之原料以指定之組成比例混合,使所得之原料混合物、或各元素沈澱在水溶液中而得的沈澱物,於大氣中在700~900℃之溫度範圍進行1~20小時初步燒成後,粉碎而得。此時,於製造肥粒鐵的原料混合物中,進一步混合SnO2,由於即使初步燒成SnO2也不是肥粒鐵的構成要素,故較佳為預先將SnO2混合於製造肥粒鐵的原料混合物中。或者,可進行初步燒成,於所製造的Ni-Zn-Cu-Co肥粒鐵中添加SnO2,粉碎混合而成為混合粉末,或進行初步燒成、粉碎,於所製造的Ni-Zn-Cu-Co肥粒鐵粉末中添加SnO2而成為混合粉末。
特別地,鐵元素之供給源的氧化鐵,較佳為將在水溶液中由硫酸鐵與氫氧化鈉所得之沈澱物予以燒成而得的氧化鐵。該氧化鐵由於以硫酸鐵作為原料,故包含未被水洗等去除的S,其含量係可在製造過程中適宜調整。又,以
該氧化鐵為原料的肥粒鐵粉末係必然地包含S。
將所得之肥粒鐵粉末與黏結劑樹脂混合後,可藉由粉末壓縮成形法、射出成形法、輥軋法、壓出法等,將肥粒鐵板成形,視需要地脫脂處理後,進行燒結處理而製造肥粒鐵燒結板。又,將肥粒鐵粉末與黏結劑樹脂和溶劑混合後,可藉由刮刀等塗佈在薄膜或薄片上而得到生胚薄片(green sheet),視需要地脫脂處理後,將所得之生胚薄片予以燒結處理而製造肥粒鐵燒結板。再者,亦可於層合複數片的所得之生胚薄片後,進行燒結。
視需要地,於肥粒鐵燒結板中形成溝時,可在肥粒鐵板之成形中、成形後或燒結處理後,形成溝。例如,以粉末壓縮成形法或射出成形法進行成形時,較佳為在成形中形成,以輥軋法或壓出法進行成形時,較佳為在成形後且燒結前形成,經由生胚薄片來製造燒結肥粒鐵板時,較佳為形成於生胚薄片。
脫脂處理通常以150~500℃之溫度進行。燒結溫度通常為850~970℃,較佳為860~960℃。燒結時間通常為30~180分鐘,較佳為30~120分鐘。燒結溫度未達850℃時,粒子的燒結係變困難,所得之燒結肥粒鐵板的強度係不充分,μ’亦變低。又,燒結溫度若超過970℃,則粒子進行成長,由於μ’之溫度變化與μ”變大而不宜。燒結時間未達30分鐘時,粒子之燒結係變困難,所得之燒結肥粒鐵板的強度係不充分,μ’亦變低。又,由於燒結時間為180分鐘則粒子之燒結係充分進行,故不需要加長
超過180分鐘。
本發明中,藉由使各構成成分的比率成為指定之範圍內,同時控制燒結溫度,而可製造具有所欲特性(導磁率μ’、μ”及μ’之溫度變化率、密度)的肥粒鐵燒結體。
其次,對於所得之肥粒鐵燒結板之表面,視需要地設置黏著材層,例如雙面黏著帶。黏著材層係可形成在肥粒鐵燒結板的單面或兩面。
又,對於所得的肥粒鐵燒結板之表面,視需要地設置保護層。黏著材層係可形成在肥粒鐵燒結板的單面或兩面。保護層之形成,係藉由將構成保護層的樹脂之薄膜或薄片,視需要地經由接著劑而接著於燒結肥粒鐵板之表面,或藉由將含有構成保護層的樹脂之塗料塗佈在燒結肥粒鐵板之表面上而進行。藉由形成保護層,可防止肥粒鐵燒結板之掉粉。
另外,於本發明中,可在肥粒鐵燒結板的一側之表面上形成黏著層,在另一側之表面上形成保護層。
於沿著溝分割肥粒鐵燒結板時,可在形成黏著層及/或保護層後,藉由輥來分割。
本發明中最重要之點,係由特定組成所成的肥粒鐵燒結體、肥粒鐵燒結板或肥粒鐵燒結薄片為μ’高、μ”低、更且μ’之溫度變化小的事實。藉由此等,因天線的電感變大,其損失變小,而可提高通訊聯絡感度。再者,由於μ’
之溫度變化小,於室外之使用中,因外部氣體溫度之變化所造成的電感之變化小,故可安定地通訊聯絡。又,本發明之肥粒鐵燒結板由於其密度高,具有緻密的微細構造,故在操作時不易破裂,可提高生產性。
本發明之代表的實施形態係如以下。
肥粒鐵燒結板之組成係使用螢光X射線分析裝置3530(理學電機工業(股)製)與碳‧硫分析裝置EMIA-920V2((股)堀場製作所製)進行測定。
肥粒鐵燒結板之密度係自以游標卡尺與測微計所測定的外部尺寸與重量,經由計算而求得。
肥粒鐵燒結板及肥粒鐵燒結薄片之厚度係用測微計測定。
肥粒鐵燒結薄片之μ’與μ”,係使用阻抗/材料分析器E4991A(AGILIGENT科技(股)製),於13.56MHz之頻率,測定經衝壓成外徑20mm、內徑10mm的環。
肥粒鐵燒結薄片的μ’之溫度變化△μ’,係以百分率表示在85℃的導磁率之實數部μ’85與μ’25之差相對於在25℃的導磁率之實數部μ’25之比((μ’85-μ’25)/μ’25)的值進行評價。
肥粒鐵燒結板之微細構造係使用S-4800型電場發射型掃描電子顯微鏡((股)日立高科技製),以8000倍的倍率觀察。
肥粒鐵之組成係以成為指定組成之方式,秤量各氧化物原料,使用球磨機進行20小時濕式混合後,將混合漿體予以過濾分離‧乾燥,而得到原料混合粉末。將該原料混合粉末在720℃燒成3小時,以球磨機粉碎所得之初步燒成物,得到本發明之Ni-Zn-Cu-Co肥粒鐵粉末。再者,S係來自於在製造原料Fe2O3時所使用的硫酸鐵。
對於所得之Ni-Zn-Cu-Co肥粒鐵粉末100重量份,添加作為結合材料的聚乙烯縮丁醛8重量份、作為可塑劑的苯二甲酸苄基正丁酯3重量份、作為溶劑的3甲基-3甲氧基-1丁醇50重量份後,充分混合而得到漿體。藉由刮刀式塗佈機,將該漿體塗佈於PET薄膜上而形成塗膜後,藉由乾燥而得到厚度120μm的生胚薄片。
在該生胚薄片之表面,使用刀尖為V字型的刀型,以3mm間隔形成格子狀的深度50μm之溝。
將所得之生胚薄片在400℃脫脂後,藉由在920℃燒結2小時,而得到肥粒鐵燒結板。該肥粒鐵燒結板之組成係Fe2O3為48.37mol%,NiO為16.95mol%,ZnO為23.43mol%,CuO為10.97mol%,CoO為0.28mol%,SnO2為0.40wt%,S為0.01wt%,厚度為98μm,密度為5.17g/cm3。再者,推斷S係以氧化物(SO2、SO3等)之形態存在。圖1中顯示該肥粒鐵燒結板之微細構造。根據該圖,該肥粒鐵燒結板之微細構造係無空孔而緻密者。
於所得之肥粒鐵燒結板的一側之表面上貼附PET薄膜,於另一側之表面上貼附雙面膠帶而得到肥粒鐵燒結薄片。厚度為118μm。
將所得之肥粒鐵燒結薄片分割後,在13.56MHz的μ’為148,μ”為2.8,△μ’為14%。
藉由與實施例1同樣之方法,得到肥粒鐵燒結板及肥粒鐵燒結薄片。表1中顯示此時的製造條件及所得之肥粒鐵燒結板及肥粒鐵燒結薄片的緒特性。
藉由與實施例1同樣之方法,得到肥粒鐵燒結板及肥粒鐵燒結薄片。表1中顯示此時的製造條件及所得之肥粒鐵燒結板及肥粒鐵燒結薄片的緒特性。圖2中顯示肥粒鐵燒結板之微細構造。如由此圖可明知,在該肥粒鐵燒結板之微細構造中,看到許多的空孔。
藉由與實施例1同樣之方法,得到肥粒鐵燒結板及肥粒鐵燒結薄片。表1中顯示此時的製造條件及所得之肥粒鐵燒結板及肥粒鐵燒結薄片的緒特性。
本發明之肥粒鐵燒結薄片由於μ’大、μ”小、更且μ’之溫度變化小,而可使天線的特性對於外部氣體溫度的變化呈現安定,可將本發明之肥粒鐵燒結薄片併入攜帶式機器中而使用。
Claims (6)
- 一種肥粒鐵燒結體,其特徵係具有由以氧化物換算為47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO所成之組成的肥粒鐵燒結體,其係進一步含有0.2~1.4wt%的SnO2與0.005~0.03wt%的S。
- 如請求項1之肥粒鐵燒結體,其中肥粒鐵燒結體係肥粒鐵燒結板。
- 如請求項2之肥粒鐵燒結板,其中肥粒鐵燒結板之密度為5.05~5.30g/cm3。
- 一種肥粒鐵燒結薄片,其係在如請求項2或3之肥粒鐵燒結板的一側之表面上設有黏著層或保護層,在相反側之表面上設有黏著層或保護層者。
- 如請求項4之肥粒鐵燒結薄片,其係在肥粒鐵燒結板的至少一側之表面上形成有至少1個溝。
- 如請求項4之肥粒鐵燒結薄片,其中肥粒鐵燒結板係被分割成小片狀。
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