JP7346116B2 - 粉体及び固体組成物 - Google Patents
粉体及び固体組成物 Download PDFInfo
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- JP7346116B2 JP7346116B2 JP2019130484A JP2019130484A JP7346116B2 JP 7346116 B2 JP7346116 B2 JP 7346116B2 JP 2019130484 A JP2019130484 A JP 2019130484A JP 2019130484 A JP2019130484 A JP 2019130484A JP 7346116 B2 JP7346116 B2 JP 7346116B2
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Description
要件1:-200℃~1200℃における少なくとも一つの温度T1で|dA(T)/dT|が10ppm/℃以上を満たす。
Aは(前記粉体中の結晶のa軸(短軸)の格子定数)/(前記粉体中の結晶のc軸(長軸)の格子定数)であり、各前記格子定数は前記粉体のX線回折測定から得られる。
要件2:レーザー回折散乱法により得られる体積基準累積粒子径分布曲線における、累積頻度が50%となる粒子径D50、累積頻度が10%となる粒子径D10、及び累積頻度が90%となる粒子径D90が、下記条件(I)及び(II)を満たす。
(I)D50に対するD10の比(D10/D50)が、0.05以上0.45以下である。
(II)D90が、0.5μm以上70μm以下である。
本発明に係る粉体は、以下の要件1及び要件2を満たす。
Aは(前記粉体中の結晶のa軸(短軸)の格子定数)/(前記粉体中の結晶のc軸(長軸)の格子定数)であり、各前記格子定数は前記粉体のX線回折測定から得られる。
(I)D50に対するD10の比(D10/D50)が、0.05以上0.45以下である。
(II)D90が、0.5μm以上70μm以下である。
ここで、本明細書においては、|dA(T)/dT|は、以下の式により定義される。
|dA(T)/dT|=|A(T+50)-A(T)|/50 …(D)
前処理として、粉体1重量部に対して水を99重量部加えて希釈し、超音波洗浄機により超音波処理を行う。超音波処理時間は10分間とする。超音波洗浄機としては、日本精機製作所製のNS200-6Uを用いることができる。超音波の周波数としては、28kHz程度で実施する。
測定はレーザー回折散乱法により、体積基準の粒子径分布を測定する。例えば、Malvern Instruments Ltd. 製 レーザー回折式粒度分布測定装置 Mastersizer 2000を用いることができる。
粉体がTi2O3粉である場合、Ti2O3粒子の屈折率を2.40として測定することができる。
本明細書では、体積基準累積粒子径分布曲線において、累積頻度を粒子径の小さい方から計算して、累積頻度が10%となる粒子径をD10、累積頻度が50%となる粒子径をD50、累積頻度が90%となる粒子径をD90とする。
上述のように、本実施形態に係る粉体において、D10/D50は、0.05以上0.45以下である必要がある。D10/D50は、0.10以上であることが好ましく、0.20以上であることがより好ましい。D10/D50は、0.44以下であることが好ましく、0.43以下であることがより好ましい。D10/D50が、このような範囲であると、熱膨張抑制特性が向上する。D10/D50が0.05以上であると、樹脂などのマトリックス材料に混合した際の均一分散性を保ち易い。
BET比表面積の測定方法を以下に示す。
前処理として窒素雰囲気中で200℃、30分間乾燥した後、測定を実施する。測定法としてはBET流動法を用いる。測定条件としては、窒素ガス及びヘリウムガスの混合ガスを用いる。混合ガス中の窒素ガスの割合は30体積%とし、混合ガス中のヘリウムガスの割合は70体積%で実施する。測定装置としては、例えばBET比表面積測定装置 Macsorb HM-1201(マウンテック社製)を用いることができる。
本実施形態に係る固体組成物は、本実施形態に係る粉体と第一の材料とを含む。
第一の材料としては、特に限定はされないが、樹脂、アルカリ金属珪酸塩、セラミックス、金属などを挙げることができる。第一の材料は、上記の粉体同士を結合させるバインダ材料、又は、上記の粉体を分散状態で保持するマトリクス材料であることができる。
セラミックスは、耐熱性を高くできるので好ましい。放電プラズマ焼結などによって焼結体を作ることができる。
本実施形態の固体組成物は、第一の材料及び粉体以外のその他の成分を含んでいてもよい。例えば、触媒が挙げられる。触媒としては、特に限定はされないが、酸性化合物、アルカリ性化合物、有機金属化合物などが挙げられる。酸性化合物としては、塩酸、硫酸、硝酸、燐酸、燐酸、蟻酸、酢酸、蓚酸等の酸を用いることができる。アルカリ性化合物としては、水酸化アンモニウム、水酸化テトラメチルアンモニウム、水酸化テトラエチルアンモニウム等を用いることができる。有機金属化合物触媒としては、アルミニウム、ジルコニウム、スズ、チタン、亜鉛を含むもの等が挙げられる。
本実施形態に係る粉体の製造方法は特に限定はされないが、例えば、焼成等の処理により原料粉を準備した後、得られた粉体の粒子径分布を調整することにより製造できる。
粉砕工程は、例えば、ボールミル、遊星ボールミル、ビーズミル等で原料粉を粉砕する工程であることができる。
固体組成物の製造方法は特に制限されない。
結晶構造の解析として、粉末X線回折測定装置SmartLab(リガク社製)を用いて、下記の条件で温度を変えて粉体を粉末X線回折測定し、粉末X線回折図形を得た。得られた図形に基づいて、PDXL2(リガク社製)ソフトウェアを用い、最小二乗法による格子定数の精密化を行い、2つの格子定数、すなわち、a軸長、及び、c軸長を求めた。
測定装置: 粉末X線回折測定装置SmartLab(Rigaku製)
X線発生器: CuKα線源 電圧45kV、電流200mA
スリット: スリット幅2mm
スキャンステップ:0.02deg
スキャン範囲:5-80deg
スキャンスピード:10deg/min
X線検出器:一次元半導体検出器
測定雰囲気:Ar 100mL/min
試料台:専用のガラス基板SiO2製
比較例1の粉体について、25℃、100℃、150℃、200℃、250℃、300℃、350℃、及び、400℃でそれぞれX線回折測定を行った。その結果、比較例1の粉体はコランダム構造のTi2O3に帰属され、空間群はR-3cであった。上記各温度におけるa軸長、c軸長及びc軸長に対するa軸長の比(a軸長/c軸長)を表1にまとめる。また、a軸長/c軸長の温度Tとの関係、すなわちA(T)を図1に示す。
|dA(T)/dT|=|A(T+50)-A(T)|/50 … (D)
実施例1のT1=150℃におけるdA(T)/dT=(A(T+50)-A(T))/50は、-44ppm/℃であった。また、T1=150℃において、|dA(T)/dT|は、44ppm/℃であった。
実施例2のT1=150℃におけるdA(T)/dT=(A(T+50)-A(T))/50は、-42ppm/℃であった。また、T1=150℃において、|dA(T)/dT|は、42ppm/℃であった。
実施例3のT1=150℃におけるdA(T)/dT=(A(T+50)-A(T))/50は、-45ppm/℃であった。また、T1=150℃において、|dA(T)/dT|は、45ppm/℃であった。
実施例1~3、及び比較例1の結果から、後述の粉砕においてa軸長及びc軸長は大きく変化しないものと推定できる。このことより、比較例2の粉体のT1=150℃でのdA(T)/dT=(A(T+50)-A(T))/50は負であり、かつ、|dA(T)/dT|は少なくとも10ppm/℃以上であると推測される。
また、実施例1~3及び比較例2の粉体はいずれもコランダム構造のTi2O3に帰属され、空間群はR-3cであった。
以下の方法により粒子径分布について測定した。
前処理:粉体1重量部に対して水を99重量部加えて希釈し、超音波洗浄機により超音波処理を行った。超音波処理時間は10分間とし、超音波洗浄機としては、日本精機製作所製のNS200-6Uを用いた。超音波の周波数としては、約28kHzで実施した。
測定:レーザー回折散乱法により、体積基準の粒子径分布を測定した。
測定条件:Ti2O3粒子の屈折率を2.40とした。
測定装置:Malvern Instruments Ltd.製 レーザー回折式粒度分布測定装置 Mastersizer 2000
以下の方法により、BET比表面積を測定した。
前処理:窒素雰囲気中で200℃、30分間乾燥を行った。
測定:BET流動法により測定した。
測定条件:窒素ガス及びヘリウムガスの混合ガスを用いた。混合ガス中の窒素ガスの割合は30体積%であり、混合ガス中のヘリウムガスの割合は70体積%で実施した。
測定装置:BET比表面積測定装置 Macsorb HM-1201(マウンテック社製)
以下の方法により、熱膨張制御特性を評価した。
粉体を80重量部と、富士化学社製の一号珪酸ソーダを20重量部と、純水を10重量部添加し混合することで混合物を得た。
得られた混合物をポリテトラフルオロエチレン製の鋳型に入れ、以下の硬化プロファイルで硬化させた。
80℃まで15分で昇温、80℃で20分保持、その後、150℃まで20分で昇温、150℃で60分保持する。
さらに、その後320℃まで昇温させ10分保持し、降温する処理を行い、以上の工程から固体組成物を得た。
得られた固体組成物の熱線膨張係数を、以下の装置を用いて測定した。
測定装置:Thermo plus EVO2 TMAシリーズ Thermo plus 8310
温度領域:25℃-320℃とし、代表値として190-210℃における熱線膨張係数の値を算出した。
リファレンス固体:アルミナ
固体組成物の測定試料の典型的な大きさとしては、15mm×4mm×4mmとした。
15mm×4mm×4mmの固体組成物について、最長辺を試料長Lとして温度Tにおける試料長L(T)を測定した。30℃の試料長(L(30℃)に対する寸法変化率ΔL(T)/L(30℃)を下記式により算出した。
ΔL(T)/L(30℃)=(L(T)-L(30℃))/L(30℃)
190℃-210℃の温度範囲で、寸法変化率ΔL(T)/L(30℃)を求め、190℃-210℃における熱線膨張係数α(1/℃)を下記式により算出した。
α(1/℃)=(ΔL(210℃)-ΔL(190℃))/(L(30℃)×20℃)
以下の方法により、塗工性を評価した。
50重量部の粉体に対して富士化学社製の一号珪酸ソーダを50重量部加えて、混合物を作製した。得られた混合物を、100μmの深さの粒ゲージ(日本シーダースサービス社製)を用いて、基材に塗工した。塗工後の状態を目視で確認し、ゲージ目盛りの80~100μmの範囲でかすれがなかったものを「A」、ゲージ目盛りの80~100μmの範囲でかすれがあったものを「B」と判定した。塗工後の状態は、図2に示す。
Ti2O3粉(高純度化学社製、150μmPass、純度99.9%)を以下の条件でビーズミルにより粉砕して、粉体を得た。
粉砕条件:ビーズミルとして、アイメックス株式会社製のバッチ式レディーミル(RM B-08)を用いた。800cm3のベッセルを用い、1348rpm、周速5m/sの条件で粉砕をした。1mmの粒子径のZrO2ビーズを用い、水217g、ZrO2を613g、Ti2O3(高純度化学社製、150μmPass、24.9g)の割合で混合し、10分間粉砕した。得られた粉体の粒子径分布を図3に示す。体積基準累積粒子径分布曲線は、図3に示す粒子径分布を累積粒子径分布曲線に換算することにより得られる。
粉砕時間を20分としたこと以外は実施例1と同様の方法で、実施例2の粉体を作製した。
粉砕時間を40分としたこと以外は実施例1と同様の方法で、実施例3の粉体を作製した。得られた粉体の粒子径分布を図4に示す。体積基準累積粒子径分布曲線は、図4に示す粒子径分布を累積粒子径分布曲線に換算することにより得られる。
Ti2O3粉(高純度化学社製、150μmPass、純度99.9%)を比較例1の粉体とした。得られた粉体の粒子径分布を図5に示す。体積基準累積粒子径分布曲線は、図5に示す粒子径分布を累積粒子径分布曲線に換算することにより得られる。
粉砕時間を60分としたこと以外は実施例1と同様の方法で、比較例2の粉体を作製した。得られた粉体の粒子径分布を図6に示す。体積基準累積粒子径分布曲線は、図6に示す粒子径分布を累積粒子径分布曲線に換算することにより得られる。
Claims (5)
- チタンを含有する金属酸化物粉であり、以下の要件1及び要件2を満たす、粉体。
要件1:-200℃~1200℃における少なくとも一つの温度T1で|dA(T)/dT|が10ppm/℃以上を満たす。
Aは(前記粉体中の結晶のa軸(短軸)の格子定数)/(前記粉体中の結晶のc軸(長軸)の格子定数)であり、各前記格子定数は前記粉体のX線回折測定から得られる。
要件2:レーザー回折散乱法により得られる体積基準累積粒子径分布曲線における、累積頻度が50%となる粒子径D50、累積頻度が10%となる粒子径D10、及び累積頻度が90%となる粒子径D90が、下記条件(I)及び(II)を満たす。
(I)D50に対するD10の比(D10/D50)が、0.05以上0.45以下である。
(II)D90が、0.5μm以上70μm以下である。 - 前記チタンを含有する金属酸化物粉が、TiOx(x=1.30~1.66)粉である、請求項1に記載の粉体。
- D50が、0.5μm以上60μm以下である、請求項1又は2に記載の粉体。
- 請求項1~3のいずれか1項に記載の粉体と第一の材料とを含む、固体組成物。
- 前記第一の材料が、樹脂、アルカリ金属珪酸塩、セラミックス、及び、金属からなる群より選ばれる少なくとも1つである、請求項4に記載の固体組成物。
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