JP7491691B2 - 電磁波吸収粒子分散体、電磁波吸収合わせ透明基材 - Google Patents
電磁波吸収粒子分散体、電磁波吸収合わせ透明基材 Download PDFInfo
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- JP7491691B2 JP7491691B2 JP2019535089A JP2019535089A JP7491691B2 JP 7491691 B2 JP7491691 B2 JP 7491691B2 JP 2019535089 A JP2019535089 A JP 2019535089A JP 2019535089 A JP2019535089 A JP 2019535089A JP 7491691 B2 JP7491691 B2 JP 7491691B2
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Description
少なくとも電磁波吸収粒子と熱可塑性樹脂とを含み、
前記電磁波吸収粒子は酸素欠損を有する六方晶のタングステンブロンズを含み、
前記タングステンブロンズは、一般式:MxWO3-y(ただし、元素Mは少なくともK、Rb、Csから選択された1種類以上を含み、0.15≦x≦0.327、0.242≦y≦0.46)で表され、
前記電磁波吸収粒子中の酸素空孔濃度NVが1.17×1021cm-3以上8.0×1021cm-3以下であり、
六方晶の前記タングステンブロンズの格子定数a、cである、aM-HTB(Å)、cM-HTB(Å)は、
格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、
点A(7.406,7.614)、点B(7.372,7.564)、点C(7.393,7.504)、及び点D(7.423,7.554)を結んだ四角形ABCDの領域内に位置する点(aM、cM)と、以下の式(1)、(2)の関係を有する電磁波吸収粒子分散体を提供する。
aM-HTB=aM±0.0084・・・(1)
cM-HTB=cM±0.0184・・・(2)
本実施形態では、電磁波吸収粒子の一構成例について説明する。
そして、係るタングステンブロンズは、一般式:MxWO3-y(ただし、元素Mは少なくともK、Rb、Csから選択された1種類以上を含み、0.15≦x≦0.33、0<y≦0.46)で表され、酸素空孔濃度NVを4.3×1014cm-3以上8.0×1021cm-3以下とすることができる。
そして、係るタングステンブロンズは、一般式:MxWO3-yで表され、酸素空孔濃度(酸素空孔密度)NVを4.3×1014cm-3以上とすることができる。
c(Å)=-3.436a(Å)+33.062・・・(A)
また、Jahn-Teller歪みが大きい時は近似直線の右下側へ、小さい時は左上側へ移動する。
aM-HTB=aM±0.0084・・・(1)
cM-HTB=cM±0.0184・・・(2)
このように、本実施形態の電磁波遮蔽粒子が含有するタングステンブロンズの格子定数が所定の範囲内あることで、元素M、及び酸素欠損が原子の配列のレベルで所定の範囲内にあることを意味していることになる。このため、日射透過率を抑制しつつも、波長が850nmの近赤外線の透過特性に優れた電磁波吸収粒子とすることができ、好ましい。
六方晶のタングステンブロンズの格子定数a、cである、aM-HTB(Å)、cM-HTB(Å)は、格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、cCs=-3.436aCs+33.062の直線上に位置する点(aCs、cCs)と、以下の式(3)、(4)の関係を有することが好ましい。
aM-HTB=aCs±0.0084・・・(3)
cM-HTB=cCs±0.0184・・・(4)
なお、日射透過率を抑制しつつ、波長が850nmの近赤外線の透過率を特に高めるため、cCsは、7.576≦cCs≦7.610を満たすことがより好ましい。
六方晶のタングステンブロンズの格子定数a、cである、aM-HTB(Å)、cM-HTB(Å)は、格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、cRb=-3.344aRb+32.265の直線上に位置する点(aRb、cRb)と、以下の式(5)、(6)の関係を有することが好ましい。
cM-HTB=cRb±0.0184・・・(6)
なお、日射透過率を抑制しつつ、波長が850nmの近赤外線の透過率を特に高めるため、cRbは、7.517≦cRb≦7.580を満たすことがより好ましい。
六方晶のタングステンブロンズの格子定数a、cである、aM-HTB(Å)、cM-HTB(Å)は、格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、cK=-2.9391aK+29.227の直線上に位置する点(aK、cK)と、以下の式(7)、(8)の関係を有することが好ましい。
aM-HTB=aK±0.0084・・・(7)
cM-HTB=cK±0.0184・・・(8)
なお、日射透過率を抑制しつつ、波長が850nmの近赤外線の透過率を特に高めるため、cKは、7.504≦cK≦7.564を満たすことが好ましい。
[電磁波吸収粒子の製造方法]
本実施形態では、電磁波吸収粒子の製造方法の一構成例について説明する。
(1)還元性ガス気流中合成法
本実施形態の電磁波吸収粒子の製造方法として、例えば還元性ガス気流中合成法を用いることができる。この場合、本実施形態の電磁波吸収粒子の製造方法は、元素M(ただし、前記元素Mは少なくともK、Rb、Csから選択された1種類以上を含む)、及びWを含み、
元素Mと、Wとの原子数比M/Wがx(0.15≦x≦0.33)である原料混合物を、還元性気体の気流中、400℃以上650℃以下の固相反応温度で加熱して固相反応させる加熱工程を有することができる。
0.165M2CO3+H2WO4+(0.165+y)H2
→0.165CO2↑+(1.165+y)H2O↑+M0.33WO3―y
均質化工程では、加熱工程の固相反応温度よりも高温、例えば700℃以上900℃以下で熱処理を行うことができる。均質化工程は、例えば窒素や、アルゴン等の不活性ガス雰囲気下で実施できる。
(2)固相還元反応法
また、本実施形態の電磁波吸収粒子は、固相還元反応法により製造することもできる。
(x/2)M2WO4+(1-2x/3)WO3+(x/6)W=MxWO3
しかし、酸素の化学量論比(stoichiometry)は原料間の固相反応によって実現されるはずであるが、通常は酸素欠損が導入され、MxWO3―yが生成される。この理由は原料の1つであるM2CO3、M2WO4にある。M2CO3や、M2WO4は室温で秤量中に吸湿して潮解する傾向を持つ。このまま固相反応させると、大気中の湿度に応じて混入した水分が蒸発して還元剤として作用する為、酸素欠損を持つMxWO3―yが生成される。
(3)タングステンブロンズを酸化処理または還元処理する方法
本実施形態の電磁波吸収粒子の製造方法として、タングステンブロンズを酸化性気体を用いて酸化処理する方法や、還元性気体を用いて還元処理する方法も挙げられる。
[電磁波吸収粒子分散体]
次に、本実施形態では、電磁波吸収粒子分散体の一構成例について説明する。
そして、係るタングステンブロンズは、一般式:MxWO3-y(ただし、元素Mは少なくともK、Rb、Csから選択された1種類以上を含み、0.15≦x≦0.33、0<y≦0.46)で表され、電磁波吸収粒子中の酸素空孔濃度NVを4.3×1014cm-3以上8.0×1021cm-3以下とすることができる。
[電磁波吸収粒子分散体の製造方法]
本実施形態では、電磁波吸収粒子分散体の製造方法の一構成例について説明する。
(1)マスターバッチの製造方法
マスターバッチは、電磁波吸収粒子を含有するペレット状の電磁波吸収粒子分散体であり、例えば電磁波吸収粒子、または以下に説明する電磁波吸収粒子分散粉と、樹脂とから製造することができる。
(2)シート形状、ボード形状またはフィルム形状の電磁波吸収粒子分散体の製造方法
電磁波吸収粒子分散粉、またはマスターバッチを透明樹脂中へ均一に混合することにより、シート形状、ボード形状またはフィルム形状の電磁波吸収粒子分散体を製造できる。
[電磁波吸収合わせ透明基材]
本実施形態では電磁波吸収合わせ透明基材の一構成例について説明する。
(化学分析)
得られた電磁波吸収粒子の化学分析は、Csについては原子吸光分析(AAS)、WについてはICP発光分光分析(ICP-OES)により行った。また、Oについては軽元素分析装置(LECO社製 型式:ON-836)を用いて、Heガス中で試料を融解し、ルツボのカーボンと反応したCOガスをIR吸収分光法で定量する方法で分析した。化学分析は、各成分について3回測定して標準偏差を求めた。
(X線回折測定)
X線回折測定はSpectris社のX'Pert-PRO/MPD装置でCu-Kα線を用いて粉末XRD測定することで実施した。
(可視光線透過率、日射透過率、波長が850nmの近赤外線の透過率)
電磁波吸収粒子分散体および電磁波吸収合わせ透明基材の可視光線透過率、日射透過率、及び波長が850nmの近赤外線の透過率は、ISO 9050及びJIS R 3106に準拠して測定を行った。具体的には、日立製作所(株)製の分光光度計U-4100を用いて透過率を測定し、太陽光のスペクトルに応じた係数を乗じて算出した。透過率の測定に当たっては波長300nm以上2100nm以下の範囲について、5nm間隔で測定を行っている。測定手順については以下の実施例1で詳述する。
(平均粒径)
平均粒径は、透過型電子顕微鏡(FEI Company製TECNAI G2 F20)を用いて測定した粒度分布から求めた。
[実施例1]
原料として炭酸セシウム(Cs2CO3)水溶液とタングステン酸(H2WO4)をCs/W=0.33となるように、秤量、混合、混練して原料混合物を調製した。
[実施例2~実施例7]
加熱工程における550℃での保持時間を表1に示した時間に変更した点以外は、実施例1と同様の手順で電磁波吸収粒子である粉末を作製し、続いてこれら粉末に対して実施例1と同様に、化学分析、XRDパターンの測定と、該XRDパターンを用いたリートベルト解析を行なった。
[実施例8~実施例10]
原料混合物を調製する際、実施例8~10では、それぞれCs/W=0.30、0.25、0.20となるように、原料を秤量、混合、混練した。また、加熱工程においてN2ガスをキャリアーとした0.7vol%H2ガス気流下で加熱を行った。以上の点以外は、実施例4と同様にして電磁波吸収粒子を調製、評価を行った。
[実施例11]
無水の三酸化タングステン(WO3)とタングステン酸セシウム(Cs2WO4)、及びW単体(金属)粉を原子数比でCs/W=0.33、O/W=3.00となるように合計30gを秤量、混合した。
[実施例12]
無水の三酸化タングステン(WO3)とタングステン酸セシウム(Cs2WO4)及びW単体(金属)粉を原子数比でCs/W=0.33、O/W=2.95となるように合計30gを秤量、混合した。秤量時に、Cs2WO4は大気中の湿度を拾って薬包紙にシミを作ったが、なるべく手早く秤量して混合し、カーボンボートに薄く広げて真空焼成炉に入れ、750℃で3日間加熱保持した(加熱・還元工程)。
[実施例13]
無水の三酸化タングステン(WO3)とタングステン酸セシウム(Cs2WO4)及びW単体(金属)粉を原子数比でCs/W=0.33、O/W=3.00となるように合計30gを秤量、混合した。
[実施例14]
無水の三酸化タングステン(WO3)とタングステン酸セシウム(Cs2WO4)及びW単体(金属)粉を原子数比でCs/W=0.33、O/W=3.00となるように合計30gを秤量、混合した。
[実施例15]
無水の三酸化タングステン(WO3)とタングステン酸セシウム(Cs2WO4)及びW単体(金属)粉を原子数比でCs/W=0.33、O/W=3.00となるように合計30gを秤量、混合した。
[実施例16]
実施例1で作製したフル還元状態の青色の電磁波吸収粒子Cs0.325WO2.542を、アルミナボートに入れて、酸化性気体の雰囲気である大気中、500℃、30分アニールを行った(アニール工程)。
[実施例17]
原料として炭酸ルビジウム(Rb2CO3)水溶液とタングステン酸(H2WO4)をRb/W=0.33となる割合で秤量、混合、混練し、原料混合物を調製した。
[実施例18]
原料として炭酸カリウム(K2CO3)水溶液と、タングステン酸(H2WO4)をK/W=0.25となる割合で、秤量、混合、混練し、原料混合物を調製した。
[実施例19]
原料として炭酸セシウム(Cs2CO3)水溶液と炭酸ルビジウム(Rb2CO3)水溶液とタングステン酸(H2WO4)をCs/W=0.13、Rb/W=0.20となる割合で、秤量、混合、混練し、原料混合物を調製した。
[実施例20]
熱可塑性樹脂であるアクリル樹脂の粉末に対して、製造される電磁波吸収シート(2.0mm厚)の可視光線領域での透過率の最大値が89.7%となるように(すべて500nm付近で最大値を取った)、実施例1で作製した所定量の電磁波吸収粒子分散粉を添加し、電磁波吸収シートの製造用組成物を調製した。
[実施例21]
熱可塑性樹脂であるポリビニルブチラール樹脂の粉末に対して、可塑剤のトリエチレングリコール-ジ-2-エチルブチレ-トを添加し、ポリビニルブチラール樹脂と可塑剤との重量比が[ポリビニルブチラール樹脂/可塑剤]=100/40となるように調製した混合物を作製した。この混合物に対して、製造される電磁波吸収合わせ透明基材の可視光線領域での透過率の最大値が89.7%となるように(すべて500nm付近で最大値を取った)、実施例1で作製した所定量の電磁波吸収粒子分散粉を添加し、電磁波吸収フィルムの製造用組成物を調製した。
この製造用組成物を3本ロールのミキサーを用いて70℃で30分練り込み混合し、混合物とした。当該混合物を、型押出機で180℃に昇温して厚み1mm程度にフィルム化してロールに巻き取ることで、実施例21に係る電磁波吸収フィルムを作製した。
なお、実施例1と比較した際に良好な近赤外線遮蔽効果が得られるとともに波長が850nmの近赤外線の透過率が低下したのは、合わせ基材の作製に用いた無機クリアガラス板自体が持つ近赤外吸収に起因するものである。
Claims (14)
- 少なくとも電磁波吸収粒子と熱可塑性樹脂とを含み、
前記電磁波吸収粒子は酸素欠損を有する六方晶のタングステンブロンズを含み、
前記タングステンブロンズは、一般式:MxWO3-y(ただし、元素Mは少なくともK、Rb、Csから選択された1種類以上を含み、0.15≦x≦0.327、0.242≦y≦0.46)で表され、
前記電磁波吸収粒子中の酸素空孔濃度NVが1.17×1021cm-3以上8.0×1021cm-3以下であり、
六方晶の前記タングステンブロンズの格子定数a、cである、aM-HTB(Å)、cM-HTB(Å)は、
格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、
点A(7.406,7.614)、点B(7.372,7.564)、点C(7.393,7.504)、及び点D(7.423,7.554)を結んだ四角形ABCDの領域内に位置する点(aM、cM)と、以下の式(1)、(2)の関係を有する電磁波吸収粒子分散体。
aM-HTB=aM±0.0084・・・(1)
cM-HTB=cM±0.0184・・・(2) - 前記元素Mは、添加元素としてNa、Tl、In、Li、Be、Mg、Ca、Sr、Ba、Al、Gaから選択された1種類以上をさらに含む請求項1に記載の電磁波吸収粒子分散体。
- 前記元素MがCsからなり、
六方晶の前記タングステンブロンズの格子定数a、cである、前記aM-HTB(Å)、前記cM-HTB(Å)は、
格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、
cCs=-3.436aCs+33.062の直線上に位置する点(aCs、cCs)と、以下の式(3)、(4)の関係を有する請求項1に記載の電磁波吸収粒子分散体。
aM-HTB=aCs±0.0084・・・(3)
cM-HTB=cCs±0.0184・・・(4) - 前記cCsは、
7.576≦cCs≦7.610を満たす、請求項3に記載の電磁波吸収粒子分散体。 - 前記元素MがRbからなり、
六方晶の前記タングステンブロンズの格子定数a、cである、前記aM-HTB(Å)、前記cM-HTB(Å)は、
格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、
cRb=-3.344aRb+32.265の直線上に位置する点(aRb、cRb)と、以下の式(5)、(6)の関係を有する請求項1に記載の電磁波吸収粒子分散体。
aM-HTB=aRb±0.0084・・・(5)
cM-HTB=cRb±0.0184・・・(6) - 前記cRbは、
7.517≦cRb≦7.580を満たす、請求項5に記載の電磁波吸収粒子分散体。 - 前記元素MがKからなり、
六方晶の前記タングステンブロンズの格子定数a、cである、前記aM-HTB(Å)、前記cM-HTB(Å)は、
格子定数a(Å)を横軸、格子定数c(Å)を縦軸にとり、座標位置が(格子定数a、格子定数c)で表される座標空間において、
cK=-2.9391aK+29.227の直線上に位置する点(aK、cK)と、以下の式(7)、(8)の関係を有する請求項1に記載の電磁波吸収粒子分散体。
aM-HTB=aK±0.0084・・・(7)
cM-HTB=cK±0.0184・・・(8) - 前記cKは、
7.504≦cK≦7.564を満たす、請求項7に記載の電磁波吸収粒子分散体。 - 六方晶の前記タングステンブロンズの結晶中に存在するWO6八面体において、[W原子から見てc軸方位に存在するO原子]から[中心のW原子]までの距離の、最小値に対する最大値の比が、1.00以上1.10以下である請求項1から8のいずれか一項に記載の電磁波吸収粒子分散体。
- 前記電磁波吸収粒子の平均粒径が0.1nm以上100nm以下である請求項1から請求項9のいずれか一項に記載の電磁波吸収粒子分散体。
- 前記熱可塑性樹脂が、ポリエチレンテレフタレート樹脂、ポリカーボネート樹脂、アクリル樹脂、スチレン樹脂、ポリアミド樹脂、ポリエチレン樹脂、塩化ビニル樹脂、オレフィン樹脂、エポキシ樹脂、ポリイミド樹脂、フッ素樹脂、エチレン・酢酸ビニル共重合体、ポリビニルアセタール樹脂という樹脂群から選択される1種の樹脂、
または、前記樹脂群から選択される2種以上の樹脂の混合物、
または、前記樹脂群から選択される2種以上の樹脂の共重合体、のいずれかである請求項1から10のいずれか一項に記載の電磁波吸収粒子分散体。 - 前記電磁波吸収粒子を、0.5質量%以上80.0質量%以下含む請求項1から11のいずれか一項に記載の電磁波吸収粒子分散体。
- 前記電磁波吸収粒子分散体が、シート形状、ボード形状、またはフィルム形状を有する請求項1から12のいずれか一項に記載の電磁波吸収粒子分散体。
- 複数枚の透明基材と、
請求項1から13のいずれか一項に記載の電磁波吸収粒子分散体とを有し、
前記電磁波吸収粒子分散体が、複数枚の前記透明基材間に配置されている電磁波吸収合わせ透明基材。
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