JP2016513369A - グラフェンを含む熱電材料およびデバイス - Google Patents
グラフェンを含む熱電材料およびデバイス Download PDFInfo
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- JP2016513369A JP2016513369A JP2015557516A JP2015557516A JP2016513369A JP 2016513369 A JP2016513369 A JP 2016513369A JP 2015557516 A JP2015557516 A JP 2015557516A JP 2015557516 A JP2015557516 A JP 2015557516A JP 2016513369 A JP2016513369 A JP 2016513369A
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Abstract
Description
を用いて算出される。特定の用途に応じて、約0.5を超えるZTまたは約0.2を超えるZTでも許容される。ZT値、電力密度、および熱電力などの特性は、経験的に決定することが出来ず、熱伝導率および導電率と同様に、特定材料の固有の特徴である。
I.低温材料(最高でおよそ200℃まで):室温付近用途用および冷却用で、通常、アンチモン、テルル、スズまたはセレンと組み合わせたビスマス合金をベースとしている。このような材料のピークZTは、約0.8〜1.1の範囲で、p型が最大値を達成する。このような材料は、冷却用途におよび低温廃熱回収に有効であるが、そのような低い作動温度を使用する用途に限定され、かつ毒性の希元素を含有する。
II.中温材料(最高でおよそ600℃まで):鉛、スズおよびテルルの合金。このような材料のピークZTは、0.6〜0.8において最適化される。このような材料は、現在、遠隔地での熱電発電に使用されている。このような材料には、幅広い用途が見出せていない。なぜなら、それら材料は、600℃未満に限られ、かつ400℃付近で最適化されるからである。
III.高温材料(最高でおよそ800℃まで):シリコンおよびゲルマニウムの合金。このような材料は、自動車の排気熱電発電装置のプロトタイプで使用されてきたが、このような材料には、特に、p型には、ダイヤモンド構造の格子熱伝導率が高いことでZTがかなり低いという難点がある。
金属酸化物材料と、
グラフェンまたは修飾グラフェンと
を含む、熱電コンポジット材料が提供される。
少なくとも1つの熱電ユニットがp型ユニットであり、かつ少なくとも1つの熱電ユニットがn型ユニットであり、両方の熱電ユニットが互いに電気的に接触しており、少なくとも1つの熱電ユニットが、金属酸化物材料(例えば、n型熱電金属酸化物材料またはp型熱電金属酸化物材料)と、グラフェンまたは修飾グラフェンとを含む、熱電デバイスが提供される。
少なくとも1つの熱電ユニットがp型ユニットであり、かつ少なくとも1つの熱電ユニットがn型ユニットであり、両方の熱電ユニットが互いに電気的に接触しており、少なくとも1つの熱電ユニットが第1の態様の熱電コンポジット材料を含む、熱電デバイスを提供し得る。
熱電材料が、
金属酸化物材料(例えば、n型熱電金属酸化物材料またはp型熱電金属酸化物材料)と、
グラフェンまたは修飾グラフェンと
を含み、前記方法が、
金属酸化物材料(例えば、n型熱電金属酸化物材料またはp型熱電金属酸化物材料)とグラフェンまたは修飾グラフェンとを合わせるステップを、含む方法が提供される。
1.ランダムに分布するグラフェンを含有するコンポジットの場合、浸透閾値より低いグラフェン濃度を使用すること、
2.グラフェンを非ランダムに配置すること、
3.熱電にグラフェンをコーティングすること、
が挙げられる。
RTGシステム:放射性同位体ベース電力源を使用して、火星探査機「キュリオシティー」を含めて、この26回のミッションに対して動力を供給してきた。ボイジャーミッションは、数百W級の(MHW)RTGを使用していた。MHW−RTGは、312のシリコンゲルマニウム(SiGe)熱電対を使用していた。本発明の熱電コンポジットは、このような用途の使用にも適用され得るだろう。
BiTeおよび方コバルト鉱(Skutteridite)ベース熱電材料は自動車用途に使用されてきた。5%の変換効率および1ガロンあたり1マイルの燃費を達成することが目的である。最大排気ガス流量は約450℃〜600℃にある。
電子基板パッケージ:マルチコアプロセッサは、熱流束を消費する十分な手段を有さない場合、最大300℃までの中程度の温度範囲で作動する、安定で安全な熱電機器を、空冷または液冷アプローチと組み合わせて、システムにおける性能の継続性に適用することができる。
[実施例]
チタン酸ストロンチウム(以下、STO)セラミックを、標準混合酸化物法を用いて製造する。過剰の、あらゆる吸湿性粉末を、炉中、適切な温度で乾燥し、続いて行う秤量に影響するあらゆる水塊を除去する。炭酸ストロンチウムおよび二酸化チタンの粉末を、次いで化学量論比で秤量し、混合するためプラスチックボトルに入れる。ドープしたSTOについては、ストロンチウム、チタン、または双方の適切なモル含量を除去し、かつ、1:1:1の比率で添加した、所望量のドーパント、8mmのジルコニアボールおよびプロパン−2−オールで置き換え、湿式磨砕プロセス用のスラリーを作製する。ボトルは密封し、18時間、振動磨砕器にしっかりと取り付ける。磨砕の後、スラリーを、プロパン−2−オールが完全に蒸発するまで、オーブンで乾燥する。
カルシウムコバルタイト(以下、CCO)セラミックを、溶液から当該金属を析出することにより製造する。硝酸カルシウムおよび硝酸コバルトを化学量論比で秤量し、次いでマグネチックスタラーを使用して、1g:10mlの比でともに蒸留水に溶解させる。セラミックをドープする場合、カルシウム、コバルト、または双方の適切なモル含量を除去し、かつ、所望量のドーパントで置き換える。この溶液を,次いで、滴下漏斗に移す。適量の0.1M水酸化ナトリウムを、ビーカーに加える。そのNaOH溶液をマグネチックスタラーで攪拌し、スタラーで生じた渦のはじに金属溶液を滴下添加する。反応が生じるように、この溶液はpH13以上に維持しなければならない。
水性酸化グラフェン溶液を、The Real Graphene Oxide Revealed: Stripping the
Oxidative Debris from the Graphene-like Sheets (Rourke et al, Angewandte Chemie International Edition, 50(14), 3173-3177, 2011) に記載の、修正Hummer経路を用いて作製する。この例では、塩基洗浄は適用されず、したがって酸化グラフェンは水に可溶のままである。実施例1に記載の手順に従い、Ca(NO3)2、Co(NO3)2・6H2O、La(NO3)3・6H2Oおよびクエン酸を、最終セラミック炭素コンポジットに炭素5wt%が充填しているように、適切な比率でこの酸化グラフェン溶液に、次いで加える。か焼温度を500セ氏温度まで減じ、続いて不活性雰囲気下800セ氏温度で高温焼き鈍しを行うことを除いて、実施例1に記載の手順の残りに従う。
NMPのグラフェンフレーク溶液を、グラファイトをNMP中で、24時間超音波処理し、次いで10000rpmで遠心分離し、上澄みを保存することにより、調製する。任意の上記例で作製されたセラミック粒子をグラフェン溶液に混合し、1:5の質量比で炭素:酸化物粒子を得る。このNMPを蒸発除去し、結果として得られた粉末をペレットにプレスする。場合により、ポリビニルアルコールまたはPVDFなどのバインダーを添加して、プレスした粉末とともに保持してもよい。このペレットを、不活性雰囲気中、400セ氏温度で焼結することもできる。
一般手順3に記載のように水性酸化グラフェン溶液を調製する。このようなグラフェンフレークは負の電荷を有する。別のビーカーで、前に記載した任意の方法でセラミック粒子を調製し、正に荷電している表面活性剤を用いて水に分散させる。
無次元数字「ZT」を、次式のように、ZTに影響する、いくつかのパラメーターを測定することで決定した。
グラフェンシートを調製するのに使用した手順は、次のとおりである。グラファイト(xGnp M−5)100mgを、まず、フェノールおよびメタノールの混合物(5:1の比率)5ml中で、約30分間超音波処理した。ヘキサデシルトリメチルアンモニウム臭化物(CTAB)10mgを添加し、結果として得られたグラファイトを、別途30分間超音波処理し、次いで、その混合物中に2日間浸漬放置した。その後、結果として得られたグラファイト/グラフェン混合物を、遠心分離で分離し、水およびメタノールの混合物(4:1の比率)100mlに移し、次いで、2時間撹拌した。最終的に、未洗浄剥離グラフェン(EG)分散液を、さらに使用するため室温で保存した(Lin et al.J Phys Chem C; 2013; 117; 17237-17244を参照のこと)。
0.1wt%のグラフェン(EG)/チタン酸ストロンチウム(STO100nm、Aldrich製)の調製が例として示されている。実施例7に記載のように製造したグラフェン10mgを含有する、剥離グラフェン分散液10mlを、0.5時間超音波処理した。同時に、STO10gを水100mlに加え、次いで0.5時間超音波処理した。その後に、グラフェン分散液およびSTO水分散液を、0.5時間撹拌し、次いで0.5時間超音波処理することにより互いに混合した。結果として得られた混合物を、攪拌を行わず放置し、均一に混合したグラフェン/STO粉末が、1時間で容器の底に析出した。上層の清水は除去した。残った、均一に混合した粉末を真空下60℃で2日間、乾燥した。次いで、乾燥粉末を、遊星ミル磨砕器で、10000rpmで3時間、磨砕した。結果として得られた粉末を、さらなる使用のために密封ボトルに保存した。
酸化グラフェンを、修正Hummers法(J. P. Rourke et al, Angew. Chem. 2011, 123, 3231-3235)で調製した。その方法は以下のとおりである。
酸化グラフェン(修飾グラフェン)からグラフェン熱電酸化物コンポジットを調製する方法の2つの例を示す。
1.熱電酸化物と酸化グラファイト(GO)を合わせ、次いで結果として得られた粉末をプレスし、適切な雰囲気下でペレットを焼結し、GOをグラフェンに分解させるが、それの酸化はさせない。
2.熱電酸化物の前駆物質と酸化グラファイト(GO)を合わせ、次いで結果として得られた粉末をプレスし、適切な雰囲気下でペレットを焼結し、GOをグラフェンに分解させるが、それの酸化はさせない。
チタン酸ストロンチウム(10g)を水(40g)に分散し、少なくとも1時間超音波処理した。これに、あらかじめ調製した、酸化グラフェンの分散液(1mg/ml)を加えた。次いで、混合物を少なくとも1時間超音波処理した。次いで、この混合物を凍結乾燥した後に、プレスし、適切な雰囲気下で焼結した。
チタン酸ストロンチウム酸化グラフェンコンポジットを、チタン酸ストロンチウムを製造するためのCalderone(Chem Mater 2006 (18) 1627-1633)の方法を変えて、作製した。
上記方法を用いて、次のコンポジットを作製した。
1および2wt%グラファイトナノ粒子を有するSrTiO3(STO)(比較例)。
0.05、0.1、0.6、1、2および5wt%剥離グラフェンを有するSrTiO3。
0.1、0.6、および1wt%剥離グラフェンを有するSr0.8La0.2/3Ti0.8Nb0.2O3(L2R)。
0.1、0.3、0.6、および1wt%剥離グラフェンを有するLa0.067Sr0.9TiO3(LSTO)(この試料はAr/5%H2雰囲気中1427℃で焼結した)。
Claims (20)
- 金属酸化物材料と、
前記金属酸化物材料全体にわたって分散されたグラフェンまたは修飾グラフェンと
を含む、熱電コンポジット材料。 - プリスチングラフェンを含む、請求項1に記載のコンポジット材料。
- 酸化グラフェンまたは部分酸化グラフェンを含む、請求項1に記載のコンポジット材料。
- 前記金属酸化物材料が、好ましくはCa3CoO9、NaxCoO2、Bi2Sr2Co2Ox、SrTiO3、CaMnO3、およびZnOから選択され、ドーパントを含んでいても含んでいなくてもよい、請求項1から3のいずれか一項に記載のコンポジット材料。
- 前記金属酸化物材料が、ドーパントを含む、請求項1から4のいずれか一項に記載のコンポジット材料。
- 前記グラフェンまたは修飾グラフェンが浸透限界未満の量で存在する、請求項1から5のいずれか一項に記載のコンポジット材料。
- 前記グラフェンまたは修飾グラフェンが、前記コンポジットの0.05〜1wt%の量で存在する、請求項1から5のいずれか一項に記載のコンポジット材料。
- 前記熱電コンポジット材料が、n型熱電金属酸化物材料を含む、請求項1から7のいずれか一項に記載のコンポジット材料。
- 前記熱電コンポジット材料が、p型熱電金属酸化物材料を含む、請求項1から7のいずれか一項に記載のコンポジット材料。
- 2つ以上の熱電ユニットを含む熱電デバイスであって、
少なくとも1つの熱電ユニットがp型ユニットであり、かつ少なくとも1つの熱電ユニットがn型ユニットであり、前記両方の熱電ユニットが互いに電気的に接触しており、少なくとも1つの熱電ユニットが、
n型金属酸化物材料またはp型金属酸化物材料と、
グラフェンまたは修飾グラフェンと
を含む、熱電デバイス。 - 前記少なくとも1つのn型ユニットが、請求項8に記載のn型熱電金属酸化物コンポジット材料を含む、請求項10に記載のデバイス。
- 前記少なくとも1つのp型ユニットが、請求項9に記載のp型熱電金属酸化物コンポジット材料を含む、請求項10または請求項11に記載のデバイス。
- 熱電コンポジット材料を作製する方法であって、前記熱電材料が、
金属酸化物材料と、
グラフェンまたは修飾グラフェンと
を含み、前記方法が、前記金属酸化物材料と前記グラフェンまたは修飾グラフェンとを合わせるステップを含む、方法。 - 前記金属酸化物材料と前記グラフェンまたは修飾グラフェンとを合わせる前記ステップが、前記金属酸化物材料と前記グラフェンまたは修飾グラフェンとをスラリーで混合して、混合物を形成する、ステップを含む、請求項13に記載の方法。
- 液相剥離によりグラフェン得るステップをさらに含む、請求項14に記載の方法。
- 前記金属酸化物材料と前記グラフェンまたは修飾グラフェンとを合わせる前記ステップが、前記グラフェンまたは修飾グラフェンを前記金属酸化物材料の粒子上に堆積させ、前記粒子を磨砕しまたは粉砕して、混合物を形成する、ステップを含む、請求項13に記載の方法。
- 前記堆積が電着法である、請求項16に記載の方法。
- 前記堆積が化学蒸着法である、請求項16に記載の方法。
- 前記混合ステップ後に、前記混合物をプレスしてペレットを形成するステップをさらに含む、請求項14から18のいずれか一項に記載の方法。
- 前記ペレットを形成後に、前記ペレットを焼結するステップをさらに含む、請求項19に記載の方法。
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EP2956973B1 (en) | 2017-11-22 |
CN105122485A (zh) | 2015-12-02 |
EP2956973A1 (en) | 2015-12-23 |
GB201302556D0 (en) | 2013-03-27 |
JP6438894B2 (ja) | 2018-12-19 |
ES2660904T3 (es) | 2018-03-26 |
KR20150119271A (ko) | 2015-10-23 |
CN105122485B (zh) | 2018-06-29 |
US20150380625A1 (en) | 2015-12-31 |
US10950774B2 (en) | 2021-03-16 |
WO2014125292A1 (en) | 2014-08-21 |
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