JP2015505807A - 二酸化チタンナノ粉末、チタネート、リチウムチタネートナノ粉末及びこれらの製造方法 - Google Patents
二酸化チタンナノ粉末、チタネート、リチウムチタネートナノ粉末及びこれらの製造方法 Download PDFInfo
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Abstract
Description
TiCl4+H2O[insufficient]→TiOCl2liquidsolidjelly+H2O[insufficient]→TiO2[metalstablestate]+HCl[liquid]+HCl[gas]+H2O
上記反応時、Ti3+イオンの濃度は1.5乃至4.3Mであり得る。
97%以上のTiCl4溶液500mlに蒸溜水3500mlを徐々に反応させて、Ti3+イオンの濃度が0.9Mになるように添加する。
上記実施例1で製造された二酸化チタンを用いて、10MのNaOHと反応させた後、多様な温度及び/または時間で反応させて、一方向性チタネートを製造した。
上記実施例2で製造された一方向性二酸化チタンナノチューブとLiOHを40乃至1200℃で熱処理してリチウムチタネートを製造した。
上記実施例3で製造されたリチウムチタネートを負極活物質とし、導電剤としてケッチェンブラック、バインダーとしてポリビニリデンフルオライド(polyvinylidene fluoride、PVdF)fmf90:2:8の重量比で混合し、これらを溶媒であるN−メチル−2−ピロリドン(NMP)と共に混合して負極スラリーを製造した。製造された負極スラリーを銅集電体の一面に塗布し、約130℃で2時間乾燥した後、1.4875cm2大きさの負極を製造した。
図1は実施例1による二酸化チタンナノ粉末の透過電子顕微鏡写真である。図1のように二酸化チタンの粒子が10nm乃至50nm程度の粒径を有していることが分かる。
図2は実施例1による二酸化チタンナノ粉末のXRDピークを示す。
図3は実施例2による一方向性チタネートの走査電子顕微鏡写真である。
図5は実施例2で反応条件を変化させながら製造したチタネートの走査電子顕微鏡写真である。図5に示されているように、水熱合成温度及び/または時間の変化によって、ナノワイヤー、ナノチューブ、ナノシートなど一方向性形態を自由に変化させることができるのを確認した。
図6は上記実施例4によるコイン型半電池の特性を評価したデータである。
Claims (15)
- 結晶相と非晶質相の中間形態である準結晶相を有する、二酸化チタンナノ粉末。
- 前記準結晶相のXRD主ピークは結晶相に比べてシフトされておりブロードニングされている、請求項1に記載の二酸化チタンナノ粉末。
- 前記準結晶相の半値幅(FWHM)が1.9乃至2.5の値を有する、請求項2に記載の二酸化チタンナノ粉末。
- 前記準結晶相のXRD主ピークはアナターゼ型結晶相の主ピークに比べてシフトされて2θ値が23°≦2θ≦26°である、請求項2に記載の二酸化チタンナノ粉末。
- 前記準結晶相のXRD主ピークはルチル型結晶相の主ピークに比べてシフトされて2θ値が26°≦2θ≦29°である、請求項2に記載の二酸化チタンナノ粉末。
- 前記粉末の平均粒度は150nm以下である、請求項1に記載の二酸化チタンナノ粉末。
- (a)TiCl4溶液と水を混合してゼリー形態のTiOCl2を準備する段階;及び
(b)前記ゼリー形態のTiOCl2と水を混合する水熱反応によって結晶相と非晶質相の中間形態である準結晶相を有する二酸化チタンナノ粉末を収得する段階;を含み、
前記(a)段階はTi3+イオン濃度が0.1乃至1.3Mになるように水の量を制御し、
前記(b)段階はTi3+イオン濃度が1.5乃至4.3Mになるように水の量を制御する、二酸化チタンナノ粉末の製造方法。 - 前記(b)段階の水熱反応は50乃至200℃の温度で加熱する、請求項7に記載の二酸化チタンナノ粉末の製造方法。
- 結晶相と非晶質相の中間形態である準結晶相を有する二酸化チタンナノ粉末とアルカリ溶液の反応によって製造されて一方向性を有する、チタネート。
- 前記一方向性チタネートはナノチューブ、ナノシート、ナノワイヤーまたはナノロッド形態である、請求項9に記載のチタネート。
- 請求項7に記載の方法によって製造された二酸化チタンナノ粉末をアルカリ水溶液5乃至25Mと反応させて一方向性チタネートを収得する、チタネートの製造方法。
- 前記アルカリ水溶液はLiOH、KOH、及びNaOHのうちの少なくとも一つを含む、請求項11に記載のチタネートの製造方法。
- 前記二酸化チタンナノ粉末と前記アルカリ水溶液の反応条件は80乃至350℃温度で6乃至20時間反応させることである、請求項11に記載のチタネートの製造方法。
- 請求項9に記載の一方向性チタネートと水酸化リチウム(LiOH)の反応によって製造された、リチウムチタネートナノ粉末。
- 請求項11に記載の方法によって製造されたチタネートと水酸化リチウム(LiOH)10乃至30molを反応させた後、これを400乃至1200℃で加熱する、リチウムチタネートナノ粉末の製造方法。
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KR10-2011-0145368 | 2011-12-29 | ||
KR1020110145368A KR101431693B1 (ko) | 2011-12-29 | 2011-12-29 | 이산화티타늄 나노분말, 타이타네이트, 리튬 타이타네이트 나노 분말 및 이들의 제조 방법 |
PCT/KR2012/011529 WO2013100608A1 (ko) | 2011-12-29 | 2012-12-27 | 이산화티타늄 나노분말, 타이타네이트, 리튬 타이타네이트 나노 분말 및 이들의 제조 방법 |
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CN105873853A (zh) * | 2013-09-16 | 2016-08-17 | 南洋理工大学 | 长形钛酸盐纳米管及其合成方法和用途 |
US20200095168A1 (en) * | 2018-09-21 | 2020-03-26 | Saint-Gobain Ceramics & Plastics, Inc. | High pore volume titanium dioxide ceramic materials and methods of making thereof |
CN109821525A (zh) * | 2019-03-28 | 2019-05-31 | 东北林业大学 | 一种负载生物质碳点缺陷二氧化钛光催化剂的制备方法 |
KR102199812B1 (ko) * | 2019-05-15 | 2021-01-07 | (주)다인스 | 습식 나노 분말 제조방법 |
CN112707726B (zh) * | 2020-02-24 | 2022-12-20 | 中国科学院深圳先进技术研究院 | 一种钛酸钡纳米粉体制备方法 |
CN111533163B (zh) * | 2020-05-20 | 2022-04-19 | 中国科学技术大学 | 一种锂离子电池负极用黑色钛酸锂材料及其制备方法以及应用 |
KR102438000B1 (ko) * | 2020-10-27 | 2022-08-29 | 한국세라믹기술원 | 자외선 차단제용 이산화티타늄 나노입자의 제조 방법 |
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KR20130076935A (ko) | 2013-07-09 |
AU2012360322B2 (en) | 2015-11-05 |
US9260316B2 (en) | 2016-02-16 |
US20140363368A1 (en) | 2014-12-11 |
AU2012360322A1 (en) | 2014-07-24 |
JP5877249B2 (ja) | 2016-03-02 |
KR101431693B1 (ko) | 2014-08-22 |
WO2013100608A1 (ko) | 2013-07-04 |
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