JP7057339B2 - セグメント化ゲル複合材料およびこの複合材料から製造される剛性パネル - Google Patents
セグメント化ゲル複合材料およびこの複合材料から製造される剛性パネル Download PDFInfo
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- JP7057339B2 JP7057339B2 JP2019212817A JP2019212817A JP7057339B2 JP 7057339 B2 JP7057339 B2 JP 7057339B2 JP 2019212817 A JP2019212817 A JP 2019212817A JP 2019212817 A JP2019212817 A JP 2019212817A JP 7057339 B2 JP7057339 B2 JP 7057339B2
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Description
例1:下記例は、本発明によるセグメント化ゲル/繊維複合材料およびエアロゲル系剛性パネルの調製および性能を示す。カッティング深さが元の厚さの90%以上となることを目標としたカスタムメイドのカッティング・ジグと、万能ナイフまたは自動回転工具とを組み合わせて使用して、対向シートが一体化された商業的に入手可能なグラスウール不織布シートを正確に長手方向にセグメント化した。この方法を用いて、36”×8”(91.44cm×20.32cm)のセグメント化グラスウール・シートを、1”および2”(2.54cmおよび5.08cm)のセグメントの両方を有するように製造した。所要量の可溶性シリカ源(すなわち加水分解テトラエトキシシランおよびその誘導体を含むゾル)と縮合触媒である水性水酸化アンモニウムとを組合せ、水平/フラットな形態を成すグラスウール不織布シートに浸透させておいた。15分間のシネレシス後、ゲル/繊維複合材料を直径6”(15.24cm)のマンドレルに巻き付けた。このような複合材料の巻き取りは、セグメント・ギャップが巻き取り中にマンドレルとは反対に向くことを保証することによって行った。このようにすると、それぞれのセグメントに沿ってギャップが形成されるので、巻き応力が軽減された。次いで、円筒形状を成すゲル/繊維複合材料に所定の時間にわたってエ-ジングを施した。エ-ジングの際には、ロール型複合材料を水酸化アンモニウムの高温エタノール溶液、およびアルキル基とシリル基とを含有する疎水性物質(ヘキサメチルジシラザン)に曝露した。エ-ジング後、ロール型複合材料を円筒形圧力容器に移し、次いで超臨界CO2抽出を用いて乾燥させて溶媒を除去した。
なお、下記表において、「1”」は「2.54cm」、「2”」は「5.08cm」である。
以下に、本願発明に関連する発明の実施形態の例を記載する。
[実施形態1]
以下の工程を含む、セグメント化強化ゲル複合材料(composite)シートを製造する方法:
セグメント化繊維強化シートまたはセグメント化オープンセル発泡(foam)強化シートを含むセグメント化強化シートを与え(providing)、
該強化シートとゲル前駆体とを組合せ、
該組合せにおける前記前駆体をゲル化して、複合材料シートを形成し、
該複合材料シートを巻き取り(rolling);そして
該複合材料シートを乾燥させて、セグメント化強化ゲル複合材料シートを形成する。
[実施形態2]
前記乾燥された複合材料シートを巻出し、該複合材料シートの少なくとも1つの面に接着剤を塗布し、そして該複合材料シートを他の平面状の(planar)材料に取り付ける(attaching)工程を更に含む、実施形態1に記載の方法。
[実施形態3]
更に、以下の工程を含む、実施形態1に記載の方法:
少なくとも2つの主要な(major)面および複数のセグメント化断面を備える実施形態1の乾燥された複合材料シートを与え、
前記複合材料の少なくとも1つの面に接着剤を塗布し;そして
前記複合材料を他の乾燥されたゲル複合材料シートに取り付ける。
[実施形態4]
前記セグメント化強化シートに、対向する(facing)層またはシートが取り付けられている、実施形態1~3のいずれか1項に記載の方法。
[実施形態5]
前記対向層が繊維を含む、実施形態4に記載の方法。
[実施形態6]
前記セグメント化強化シートが、不連続な繊維を含む繊維強化シートを含む、実施形態1~5のいずれか1項に記載の方法。
[実施形態7]
更に、二酸化チタン、酸化鉄、カーボンブラック、グラファイト、水酸化アルミニウム、リン酸塩、ホウ酸塩、金属ケイ酸塩、メタロセン、モリブデン酸塩、スズ酸塩、水酸化物、炭酸塩、酸化亜鉛、酸化アルミニウム、酸化アンチモン、マグネシウム亜鉛ブレンド、マグネシウム亜鉛アンチモンブレンド、炭化ケイ素、ケイ化モリブデン、酸化マンガン、鉄チタン酸化物、ケイ酸ジルコニウム、酸化ジルコニウム、酸化鉄(II)、酸化鉄(III)、二酸化マンガン、鉄チタン酸化物(イルメナイト)、酸化クロム、およびこれらの組み合わせからなる群から選択された添加剤を組み込む(incorporating)工程を含む、実施形態1~6のいずれか1項に記載の方法。
[実施形態8]
前記セグメント化強化シートが繊維強化シートを含む前記方法であって;該方法が、前記繊維強化シートの繊維に少なくとも1種のバインダーを加える工程か、または少なくとも1種のバインダーを含む繊維強化シートを使用する工程を含む、実施形態1~7のいずれか1項に記載の方法。
[実施形態9]
前記セグメント化強化シートの少なくとも1つのセグメントが剛性である、実施形態1~3のいずれか1項に記載の方法。
[実施形態10]
前記ゲル前駆体が、ジルコニア、イットリア、ハフニア、アルミナ、チタニア、セリア、シリカ、ポリアクリレート、ポリスチレン、ポリアクリロニトリル、ポリウレタン、ポリイミド、ポリフルフラールアルコール、フェノールフルフリルアルコール、メラミンホルムアルデヒド、レゾルシノールホルムアルデヒド、クレゾールホルムアルデヒド、フェノールホルムアルデヒド、ポリビニルアルコールジアルデヒド、ポリシアヌレート、ポリアクリルアミド、種々のエポキシ、寒天、およびアガロース、およびこれらの組み合わせからなる群から選択された材料を含む、実施形態1~9のいずれか1項に記載の方法。
[実施形態11]
前記セグメント化強化シートが、鉱物ウール、グラスウール、繊維ガラス、ポリエステル、ポリオレフィンテレフタレート、ポリ(エチレン)ナフタレート、ポリカーボネート、およびレーヨン、ナイロン、綿系ライクラ(DuPont製)、炭素系繊維、炭素繊維のための前駆体、ポリアクリロニトリル(PAN)、酸化PAN、非炭化(uncarbonized)熱処理PAN、繊維ガラス系材料、Sガラス、901ガラス、902ガラス、475ガラス、Eガラス、シリカ系繊維、石英、quartzel(Saint-Gobain製)、Qフェルト(Johns Manville製)、Saffil(Saffil製)、Durablanket(Unifrax製)、ポリアラミド繊維、Kevlar(DuPont製),Nomex(DuPont製),Sontera(DuPont製)、Conex(Taijin製)、ポリオレフィン、Tyvek(DuPont製)、Dyneema(DSM製)、Spectra(Honeywell製)、ポリプロピレン繊維、Typar(DuPont製)、Xavan(DuPont製)、フルオロポリマー、PTFE、Teflon(DuPont製), Goretex(GORE製)、炭化ケイ素繊維、Nicalon(COI Ceramics製)、セラミック繊維、Nextel(3M製)、アクリルポリマー、ウール、絹、麻、皮革、スエードの繊維、PBO-Zylon繊維(Tyobo製)、液晶材料、Vectan(Hoechst製)、Cambrelle繊維(DuPont製)、ポリウレタン、ポリアミド、木質繊維、ホウ素、アルミニウム、鉄、ステンレス鋼繊維、熱可塑性材料、PEEK、PES、PEI、PEK、PPS、およびこれらの組み合わせからなる群から選択された材料を含む繊維強化シートを含む、実施形態1~10のいずれか1項に記載の方法。
[実施形態12]
前記接着剤が、カリウム水ガラス、ナトリウム水ガラス、セメント、およびアルカリ活性化アルミノケイ酸塩、ポリエチレン、カプトン、ポリウレタン、ポリエステル、天然ゴム、合成ゴム、ハイパロン、プラスチックアロイ、PTFE、ポリビニルハロゲン化物、ポリエステル、ネオプレン、アクリル、ニトリル、EPDM、EP、バイトン(viton)、ビニル、ビニルアセテート、エチレンビニルアセテート、スチレン、スチレンアクリレート、スチレンブタジエン、ポリビニルアルコール、ポリビニルクロリド、アクリルアミド、フェノール、およびこれらの組み合わせからなる群から選択される、実施形態2~11のいずれか1項に記載の方法。
[実施形態13]
前記乾燥ゲル複合材料シートの熱伝導率が、周囲条件で25mW/mK未満である、実施形態1~12のいずれか1項に記載の方法。
[実施形態14]
前記複合シートの巻き取りが、前記セグメントの間に形成されたギャップが前記ロールの軸とは反対に向くように行われる、実施形態1~13のいずれか1項に記載の方法。
[実施形態15]
セグメント化繊維強化シートまたはセグメント化オープンセル発泡体強化シートを含むセグメント化強化シートを含むセグメント化強化ゲル複合材料シートであって;該ゲルが、セグメント化強化シートの少なくとも1つのセグメント内で繊維または発泡(foam)にわたって連続しており、そして、少なくとも2つの隣接セグメント間に、該ゲルおよび繊維または該オープンセル発泡体の両方に不連続性が形成された状態で、少なくとも1つのギャップが存在している、セグメント化強化ゲル複合材料シート。
[実施形態16]
二酸化チタン、酸化鉄、カーボンブラック、グラファイト、水酸化アルミニウム、リン酸塩、ホウ酸塩、金属ケイ酸塩、メタロセン、モリブデン酸塩、スズ酸塩、炭酸塩、酸化亜鉛、酸化アルミニウム、酸化アンチモン、マグネシウム亜鉛ブレンド、マグネシウム亜鉛アンチモンブレンド、炭化ケイ素、ケイ化モリブデン、酸化マンガン、鉄チタン酸化物、ケイ酸ジルコニウム、酸化ジルコニウム、酸化鉄(II)、酸化鉄(III)、鉄チタン酸化物(イルメナイト)、酸化クロム、およびこれらの組み合わせからなる群から選択された充填剤を更に含む、実施形態15に記載のセグメント化強化ゲル複合材料シート。
[実施形態17]
前記繊維中に少なくとも1種のバインダーを含むセグメント化繊維強化シートを含む、実施形態15~16のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態18]
前記セグメント化強化シートに、対向する層またはシートが取り付けられている、実施形態15~17のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態19]
前記対向する層が繊維を含む、実施形態18に記載のセグメント化強化ゲル複合材料シート。
[実施形態20]
前記セグメント化強化シートが、不連続な繊維を含む繊維強化シートを含む、実施形態15~19のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態21]
更に、二酸化チタン、酸化鉄、カーボンブラック、グラファイト、水酸化アルミニウム、リン酸塩、ホウ酸塩、金属ケイ酸塩、メタロセン、モリブデン酸塩、スズ酸塩、水酸化物、炭酸塩、酸化亜鉛、酸化アルミニウム、酸化アンチモン、マグネシウム亜鉛ブレンド、マグネシウム亜鉛アンチモンブレンド、炭化ケイ素、ケイ化モリブデン、酸化マンガン、鉄チタン酸化物、ケイ酸ジルコニウム、酸化ジルコニウム、酸化鉄(II)、酸化鉄(III)、二酸化マンガン、鉄チタン酸化物(イルメナイト)、酸化クロム、およびこれらの組み合わせからなる群から選択された添加剤を含む、実施形態15~20のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態22]
前記セグメント化強化シートの少なくとも1つのセグメントが剛性である、実施形態15~21のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態23]
前記ゲル前駆体が、ジルコニア、イットリア、ハフニア、アルミナ、チタニア、セリア、シリカ、ポリアクリレート、ポリスチレン、ポリアクリロニトリル、ポリウレタン、ポリイミド、ポリフルフラールアルコール、フェノールフルフリルアルコール、メラミンホルムアルデヒド、レゾルシノールホルムアルデヒド、クレゾールホルムアルデヒド、フェノールホルムアルデヒド、ポリビニルアルコールジアルデヒド、ポリシアヌレート、ポリアクリルアミド、種々のエポキシ、寒天、およびアガロース、およびこれらの組み合わせからなる群から選択された材料を含む、実施形態15~22のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態24]
前記セグメント化強化シートが、鉱物ウール、グラスウール、繊維ガラス、ポリエステル、ポリオレフィンテレフタレート、ポリ(エチレン)ナフタレート、ポリカーボネート、およびレーヨン、ナイロン、綿系ライクラ(DuPont製)、炭素系繊維、炭素繊維のための前駆体、ポリアクリロニトリル(PAN)、酸化PAN、非炭化(uncarbonized)熱処理PAN、繊維ガラス系材料、Sガラス、901ガラス、902ガラス、475ガラス、Eガラス、シリカ系繊維、石英、quartzel(Saint-Gobain製)、Qフェルト(Johns Manville製)、Saffil(Saffil製)、Durablanket(Unifrax製)、ポリアラミド繊維、Kevlar (DuPont製), Nomex(DuPont製), Sontera (DuPont製)、Conex (Taijin製)、ポリオレフィン、Tyvek(DuPont製)、Dyneema(DSM製)、Spectra(Honeywell製)、ポリプロピレン繊維、Typar(DuPont製)、Xavan(DuPont製)、フルオロポリマー、PTFE、Teflon(DuPont製), Goretex(GORE製)、炭化ケイ素繊維、Nicalon(COI Ceramics製)、セラミック繊維、Nextel(3M製)、アクリルポリマー、ウール、絹、麻、皮革、スエードの繊維、PBO-Zylon繊維(Tyobo製)、液晶材料、Vectan(Hoechst製)、Cambrelle繊維(DuPont製)、ポリウレタン、ポリアミド、木質繊維、ホウ素、アルミニウム、鉄、ステンレス鋼繊維、熱可塑性材料、PEEK、PES、PEI、PEK、PPS、およびこれらの組み合わせからなる群から選択された材料を含む繊維強化シートを含む、実施形態15~23のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態25]
前記セグメント化強化ゲル複合材料シートの熱伝導率は周囲条件で25mW/mK未満である、実施形態15~24のいずれか1項に記載のセグメント化強化ゲル複合材料シート。
[実施形態26]
強化ゲル複合材料(composites)の少なくとも2つの層を含むパネルであって、少なくとも1つの層が、実施形態15~25のいずれか1項に記載のセグメント化強化ゲル複合材料シートを含む、パネル。
[実施形態27]
カリウム水ガラス、ナトリウム水ガラス、セメント、およびアルカリ活性化アルミノケイ酸塩、ポリエチレン、カプトン、ポリウレタン、ポリエステル、天然ゴム、合成ゴム、ハイパロン、プラスチックアロイ、PTFE、ポリビニルハロゲン化物、ポリエステル、ネオプレン、アクリル、ニトリル、EPDM、EP、バイトン(viton)、ビニル、ビニルアセテート、エチレンビニルアセテート、スチレン、スチレンアクリレート、スチレンブタジエン、ポリビニルアルコール、ポリビニルクロリド、アクリルアミド、フェノール、およびこれらの組み合わせからなる群から選択される接着剤を更に含む、実施形態26に記載のパネル。
Claims (24)
- 以下の工程:
セグメント化繊維強化シートまたはセグメント化オープンセル発泡体強化シートを含むセグメント化強化シートを与え(providing)、ここで前記セグメント化強化シートは長さ、幅および厚さを有し、かつ前記セグメント化強化シートは、対向シートに取り付けられた別々のセグメントを含み、前記別々のセグメントは、前記対向シートによってつなぎ合わされて、前記セグメント化強化シートの幅にわたって、前記厚さ方向を通してセグメント化されたセグメント化強化シートを形成しており;
前記セグメント化強化シートとゲル前駆体とを組合せ;
前記組合せにおける前記ゲル前駆体をゲル化して、強化ゲル複合材料シートを形成し;そして
前記強化ゲル複合材料シートを乾燥させて、強化エアロゲル複合材料シートを形成する;
を含む、強化エアロゲル複合材料(composite)シートを製造する方法。 - 更に、以下の工程を含む、請求項1に記載の方法:
少なくとも2つの主要な(major)面および複数のセグメント化断面を備える請求項1の強化エアロゲル複合材料シートを与え、
前記強化エアロゲル複合材料シートの少なくとも1つの主要な面に接着剤を塗布し;そして
前記強化エアロゲル複合材料シートを平面状の(planar)材料に取り付ける。 - 前記平面状の材料が第2の強化エアロゲル複合材料シートである、請求項2に記載の方法。
- 前記セグメント化強化シートに、対向する(facing)層または対向するシートが取り付けられている、請求項1~3のいずれか1項に記載の方法。
- 前記対向する層または対向するシートが繊維を含む、請求項4に記載の方法。
- 前記セグメント化強化シートが、不連続繊維と少なくとも1種のバインダーとを含むセグメント化繊維強化シートを含む、請求項1~5のいずれか1項に記載の方法。
- 前記ゲル前駆体がシリカゲル前駆体を含む、請求項1~6のいずれか1項に記載の方法。
- 前記接着剤が、カリウム水ガラス、ナトリウム水ガラス、セメント、およびアルカリ活性化アルミノケイ酸塩、ポリエチレン、カプトン、ポリウレタン、ポリエステル、天然ゴム、合成ゴム、ハイパロン、プラスチックアロイ、PTFE、ポリビニルハロゲン化物、ポリエステル、ネオプレン、アクリル、ニトリル、EPDM、EP、バイトン(viton)、ビニル、ビニルアセテート、エチレンビニルアセテート、スチレン、スチレンアクリレート、スチレンブタジエン、ポリビニルアルコール、ポリビニルクロリド、アクリルアミド、フェノール、およびこれらの組み合わせからなる群から選択される、請求項2または請求項3に記載の方法。
- 前記強化ゲル複合材料シートを乾燥工程前に巻き取って軸を有するロールを製造する工程をさらに含み、前記強化ゲル複合材料シートの巻き取りが、前記強化ゲル複合材料シートのセグメントの間に形成された任意のギャップが前記ロールの軸とは反対に向くように行われる、請求項1~8のいずれか1項に記載の方法。
- 前記強化エアロゲル複合材料シートの熱伝導率が、37.5℃及び周囲圧力下で25mW/mK未満である、請求項1~9のいずれか1項に記載の方法。
- エアロゲルとセグメント化強化シートとを含む、強化エアロゲル複合材料シートであって、前記セグメント化強化シートはセグメント化繊維強化シートまたはセグメント化オープンセル発泡体強化シートを含み、ここで前記セグメント化強化シートは長さ、幅および厚さを有し、かつ前記セグメント化強化シートは、対向シートに取り付けられた別々のセグメントを含み、前記別々のセグメントは、前記対向シートによってつなぎ合わされて、前記セグメント化強化シートの幅にわたって、前記厚さ方向を通してセグメント化されたセグメント化強化シートを形成している、強化エアロゲル複合材料シート。
- 前記セグメント化強化シートに、対向する層または対向するシートが取り付けられている、請求項11に記載の強化エアロゲル複合材料シート。
- 前記対向する層又は対向するシートが繊維を含む、請求項12に記載の強化エアロゲル複合材料シート。
- 前記セグメント化強化シートが、不連続繊維と少なくとも1種のバインダーとを含む繊維強化シートを含む、請求項11に記載の強化エアロゲル複合材料シート。
- 前記エアロゲルが乾燥シリカゲルを含む、請求項11~14のいずれか1項に記載の強化エアロゲル複合材料シート。
- 前記強化エアロゲル複合材料シートの熱伝導率は37.5℃及び周囲圧力下で25mW/mK未満である、請求項11~15のいずれか1項に記載の強化エアロゲル複合材料シート。
- 二酸化チタン、酸化鉄、カーボンブラック、グラファイト、水酸化アルミニウム、リン酸塩、ホウ酸塩、金属ケイ酸塩、メタロセン、モリブデン酸塩、スズ酸塩、水酸化物、炭酸塩、酸化亜鉛、酸化アルミニウム、酸化アンチモン、マグネシウム亜鉛ブレンド、マグネシウム亜鉛アンチモンブレンド、炭化ケイ素、ケイ化モリブデン、酸化マンガン、鉄チタン酸化物、ケイ酸ジルコニウム、酸化ジルコニウム、酸化鉄(II)、酸化鉄(III)、二酸化マンガン、鉄チタン酸化物(イルメナイト)、酸化クロム、およびこれらの組み合わせからなる群から選択された充填剤をさらに含む、請求項11に記載の強化エアロゲル複合材料シート。
- 炭化ケイ素をさらに含む、請求項11に記載の強化エアロゲル複合材料シート。
- 前記セグメント化繊維強化シートが、繊維中に少なくとも1種のバインダーを含む、請求項11に記載の強化エアロゲル複合材料シート。
- 少なくとも2つの隣接セグメント間に、少なくとも1つのギャップが存在しており、前記少なくとも1つのギャップは、強化エアロゲル複合材料シートの幅方向に延在する、請求項11に記載の強化エアロゲル複合材料シート。
- 前記少なくとも1つのギャップが、少なくとも前記セグメント化強化シート内における不連続性を含む、請求項20に記載の強化エアロゲル複合材料シート。
- 少なくとも2つの隣接セグメント間に存在する前記少なくとも1つのギャップは、強化エアロゲル複合材料シートの幅方向全体に延在する、請求項20に記載の強化エアロゲル複合材料シート。
- 強化エアロゲル複合材料(composites)の少なくとも2つの層を含むパネルであって、少なくとも1つの層が、請求項11~22のいずれか1項に記載の強化エアロゲル複合材料シートを含む、パネル。
- カリウム水ガラス、ナトリウム水ガラス、セメント、およびアルカリ活性化アルミノケイ酸塩、ポリエチレン、カプトン、ポリウレタン、ポリエステル、天然ゴム、合成ゴム、ハイパロン、プラスチックアロイ、PTFE、ポリビニルハロゲン化物、ポリエステル、ネオプレン、アクリル、ニトリル、EPDM、EP、バイトン(viton)、ビニル、ビニルアセテート、エチレンビニルアセテート、スチレン、スチレンアクリレート、スチレンブタジエン、ポリビニルアルコール、ポリビニルクロリド、アクリルアミド、フェノール、およびこれらの組み合わせからなる群から選択される接着剤を更に含む、請求項23に記載のパネル。
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