JP6871257B2 - セラミックおよび複合材料の低温焼結 - Google Patents
セラミックおよび複合材料の低温焼結 Download PDFInfo
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- JP6871257B2 JP6871257B2 JP2018536075A JP2018536075A JP6871257B2 JP 6871257 B2 JP6871257 B2 JP 6871257B2 JP 2018536075 A JP2018536075 A JP 2018536075A JP 2018536075 A JP2018536075 A JP 2018536075A JP 6871257 B2 JP6871257 B2 JP 6871257B2
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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Description
本出願は、2015年9月29日出願の米国仮特許出願第62/234,389号明細書および2016年6月13日出願の米国仮特許出願第62/349,444号明細書の利益を主張し、これらの両方の開示全体は、ここをもって参照により本明細書に組み込まれる。
本発明は、National Science Foundationが認可した助成金番号第IIP1361571号を受けて、政府の支援によってなされた。政府は、本発明に一定の権利を有する。
ZnO以外のすべての粉末を、ピペットを使用して4〜25wt%までの脱イオン水と混合した。ZnOを、0.5〜5.0M酢酸(約2〜4までのpH値)という濃度の水性酢酸溶媒と混合した。乳鉢および乳棒を用いて撹拌した後、湿潤させた粉末を、80〜570MPaまでの一軸圧力下において120℃で鋼ダイによってホットプレスして、高密度なペレット(12.7mmの直径および1〜5mmまでの高さ)に変えた。ダイを120℃で1時間超予備加熱した。最後に、ペレットを120℃のオーブン内に6時間入れて、残留水の可能性をなくした。
すべての乾いた粉末を、低圧(30〜70MPaまで)下において室温でプレス加工して、柔らかいペレットに変えた。次いで、ペレットを、多湿雰囲気(脱イオン水の加熱によって生成した水蒸気または湿度室)下に10〜360分置いた。湿潤させたペレットを、80〜570MPaまでの一軸圧力下において120℃で鋼ダイによってホットプレスして、高密度なペレットに変えた。ダイを120℃で1時間超予備加熱した。最後に、ペレットを120℃のオーブン内に6時間入れて、残留水の可能性をなくした。
(1−x)LM−xPTFE粉末の調製
微粉を得るために、Li2MoO4(Alfa Aesar、99%)を、乳鉢を用いて粉砕し、次いで、エタノール中で48時間ボールミル粉砕した。乾燥させた後、Li2MoO4粉末を、次の組成に従ったPTFE(Howard Piano Industries)と混合した:(1−x)LM−xPTFE(x=0、10、40、50、60、70vol%)。混合物をエタノール中で24時間ボールミル粉砕し、続いて、85℃で乾燥させた。
化学量論量のLi2CO3(Alfa Aesar、99%)、Al2O3(Tape Casting Warehouse, Inc.)、GeO2(Alfa Aesar、99.98%)およびNH4H2PO4(Alfa Aesar、98%)を24時間ボールミル粉砕し、空気中において750℃で30分か焼し、24時間再度ボールミル粉砕した。微粉砕された粉末を、カバー付きアルミナるつぼ内に入れ、空気中において1380℃で1時間溶融させた後、スプラットクエンチした。スプラットクエンチされたガラスを、450℃で3.75時間アニーリングし、空気中において825℃で8時間結晶化させた。ガラス−セラミック粉末を、74μmメッシュによってふるい分けした。
最初に、V2O5粉末(Sigma Aldrich、98%)を脱イオン水中に分散させ、次いで、釣り合い(x=0、0.8、1.6、3.2、14.9、27vol%)がとれるようにPEDOT:PSS溶液(Sigma Aldrich、高伝導度グレード、H2O中3〜4%)と混合した。混合物を室温で4時間撹拌し、120℃で乾燥させた。
高密度な複合材料を低温焼結方法によって調製した。(1−x)LM−xPTFEの場合、適量の脱イオン水(6〜12wt%まで)をLi2MoO4およびPTFEの混合物に添加し、乳鉢および乳棒を用いて均一に混合した。この後、湿潤させた粉末を、350MPaの一軸圧力下において120℃で15〜20分プレス加工して、高密度な試料に変えた。(1−x)LAGP−x(PVDF−HFP)の場合、30〜39vol%までの脱イオン水をLAGPに添加し、乳鉢および乳棒によって均一化した。LAGPおよびPVDF−HFP(Arkema、Kynar Powerflex LBG)を、液体窒素中に渦巻きを発生させることによって混合し、400MPaの一軸圧力下において120℃で1時間プレス加工した。(1−x)V2O5−xPEDOT:PSSの場合、湿潤を脱イオン水(11〜17wt%まで)によって実施し、高密度なセラミック−ポリマー複合材料を、350MPaの一軸圧力下において120℃で20〜30分プレス加工した。
低温焼結後の複合材料の相純度および組成を、X線回折(PANalytical Empyrean)によって決定した。エネルギー分散型分光計(EDS)付きの環境制御走査型電子顕微鏡(ESEM、FEI、Quanta200)を使用して、低温焼結試料の断面における微細構造および元素分布を分析した。バルク密度を、質量/幾何形状体積比およびアルキメデス法によって測定した。(1−x)LM−xPTFEのマイクロ波誘電特性(誘電率およびQ×f値)を、ベクトルネットワークアナライザー(Anritsu37369D)を用いて、TE011モードにより、Hakki−Coleman方法を使用して確認した。TE01δ遮へい空洞法を使用して、ネットワークアナライザー、反響する円筒形の空洞および温度室(Delta9023、Delta Design、Poway、CA)を用いて、共振周波数(TCF)値の温度係数を、次のように計算して得た:TCF=(f85−f25)/(f25(85−25))106ppm ℃−1、式中、f25およびf85が、それぞれ25℃および85℃における共振周波数だった。弾性率およびせん断弾性率の測定を、ASTM規格E494−05に基づいた音速法によって実施した。Liイオン伝導性(1−x)LAGP−x(PVDF−HFP)複合材料を対象にしてインピーダンス測定を実施するために、100nmの厚さのAu電極を、ペレット面上にスパッタリングした。ペレットを、Arグローブボックスの内部で25℃の1M LiPF6 EC−DMC(50:50vol%)(BASF Selectilyte LP30)中に浸し、過剰な液体をふき取った後、インピーダンス分光法(Solartron Ametek ModuLab)のために空気密セル内に装入した。液体の取込みは、5〜10wt%まで(10〜12μLまで)だった。(1−x)V2O5−xPEDOT:PSS上のDC導電性を測定するために、ディスクを、10×2×1mmの寸法を有する棒材になるように切断した。棒材の研磨後、Pt電極を堆積させ、Agワイヤーを、Agエポキシ(Epo−tek H20E)と共に取り付けた。4端子法を使用して、Keithley2700Integraシリーズのデジタルマルチメーターによって、DC導電性を測定した。
使用前にエタノール中で48〜100時間ボールミル粉砕したリチウム酸化モリブデン粉末(99+%、Alfa Aesar、Ward Hill、MA)を使用して、セラミックインクを調製した。自転公転式ミキサー(AR250、Thinky USA、Laguna Hills、CA)内において、樹脂が溶媒中に完全に溶解するまで、QPAC40(ポリ(プロピレンカーボネート))樹脂(Empower Materials、New Castle、DE)を、エチレングリコールジアセテート(97%、Alfa Aesar、Ward Hill、MA)と、それぞれ15wt%および85wt%の量で混合することによって、印刷用溶剤を製造した。インクを配合するために、それぞれ66.1wt%、22.0wt%、11.0wt%および0.9wt%の量のLi2MoO4、印刷用溶剤、さらなるエチレングリコールジアセテートおよびブチルベンジルフタレートS−160(Tape Casting Warehouse、Morrisville、PA)を配合し、自転公転式ミキサー内で均一化した。
Claims (15)
- 焼結材料を調製するための方法であって、50μm未満の粒径を有する粒子形態の少なくとも1種の無機化合物を、前記無機化合物を部分的に溶解できる溶媒と合わせて、混合物を形成すること、ならびに圧力および熱を前記混合物に加えて、前記溶媒を蒸発させ、前記少なくとも1種の無機化合物を高密度化して、焼結材料を形成することを含み、前記加えられる熱が、前記溶媒の沸点を200℃以下で上回る温度であり、前記焼結材料を80%超の相対密度になるまで高密度化する、方法。
- 焼結複合材料を調製するための方法であって、粒子形態の少なくとも1種の無機化合物および少なくとも1種の他の物質を、前記無機化合物を部分的に溶解できる溶媒と合わせて、混合物を形成すること、ならびに圧力および熱を前記混合物に加えて、前記溶媒を蒸発させ、前記少なくとも1種の無機化合物を高密度化して、焼結複合材料を形成することを含み、前記加えられる熱が、前記溶媒の沸点を200℃以下で上回る温度であり、前記焼結材料を80%超の相対密度になるまで高密度化する、方法。
- 前記溶媒が、1種または複数の原料化合物を含む、請求項1に記載の方法。
- 基材上に焼結材料を調製するための方法であって、セラミックを基材上に堆積させ、続いて、前記堆積したセラミックを水性溶媒に曝露して、濡れた状態の堆積したセラミックを形成すること、ならびに圧力および熱を前記濡れた状態の堆積したセラミックに加えて、溶媒を蒸発させ、前記セラミックを前記基材上に焼結することを含み、前記加えられる熱が、200℃以下であり、前記加えられる圧力が、5,000MPa以下であり、前記セラミックが、85%以上の相対密度になるまで焼結される、方法。
- 前記焼結材料または複合材料が、180分未満の期間で少なくとも85%の相対密度を達成するか、前記焼結材料または複合材料が、60分以下の期間で少なくとも85%の相対密度を達成するか、または前記焼結材料または複合材料が、30分以下の期間で少なくとも90%の相対密度を達成する、請求項1から4のいずれか一項に記載の方法。
- 前記溶媒が、C1〜12アルコール、ケトン、エステルもしくは水または有機酸またはこれらの混合物のうちの1つまたは複数を含み、前記溶媒が、200℃未満の沸点を有する、請求項1から4のいずれか一項に記載の方法。
- 前記溶媒が、少なくとも50重量%の水を含む、請求項1から4のいずれか一項に記載の方法。
- 前記無機化合物またはセラミックおよび前記溶媒が、前記無機化合物またはセラミックを、前記溶媒の制御された相対雰囲気に曝露することによって合わせられる、請求項1、2または4に記載の方法。
- 前記加えられる熱が、250℃以下の温度である、請求項1から3のいずれか一項に記載の方法。
- 前記圧力が、一軸圧力である、請求項1から4のいずれか一項に記載の方法。
- 前記焼結材料または複合材料の相対密度が、90%超である、請求項1から4のいずれか一項に記載の方法。
- 前記少なくとも1種の無機化合物またはセラミックが、30μm未満の粒径を有する、請求項1から4のいずれか一項に記載の方法。
- 前記少なくとも1種の無機化合物またはセラミックを微粉砕した後、前記混合物を形成することをさらに含む、請求項1から4のいずれか一項に記載の方法。
- 前記混合物を2個以上の基材上に形成すること、および焼結無機化合物または複合材料によって前記2個以上の基材を積層することをさらに含む、請求項1から4のいずれか一項に記載の方法。
- 前記他の物質が、ポリマーである、請求項2に記載の方法。
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CN109133911A (zh) * | 2018-09-25 | 2019-01-04 | 桂林电子科技大学 | 一种超低温冷烧结ZnO基陶瓷的方法 |
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