JP2007513447A - ポリマー認証方法、認証可能ポリマー、認証可能ポリマー及び認証可能製品の製造方法、並びにそれで製造される製品 - Google Patents
ポリマー認証方法、認証可能ポリマー、認証可能ポリマー及び認証可能製品の製造方法、並びにそれで製造される製品 Download PDFInfo
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Abstract
【選択図】 図1
Description
次に、例示的であって限定的ではない図面について説明する。
実験用として熱安定性有機蛍光物質(Lumogen F Red 300、BASF社、ドイツ)を使用した。この特定の蛍光物質は、約578nmに位置する最大吸収、約615nmに位置する蛍光発光、及び90%を超える蛍光収率を有している。この蛍光物質をトレーサーレベル(最終製品中で約1ppm)で配合するため、それをまずポリカーボネート中に配合して蛍光物質含有量0.005pphのマスターバッチ(Lumogen F−300 MB)を形成した。熱変色性物質は、ポリカーボネート中で化学的に安定であると共に、このエンシニアリングポリマーの加工条件を維持できるように選択した。この実施例のためには、レギオランダムポリ(3−オクタデシルチオフェン)(ロードアイランド大学(キングストン、米国ロードアイランド州)から入手できるP3ODTロット#YW1202)を選択した。この熱変色性物質は、室温では赤色であり、熱変色転移温度を超えると赤みがかった黄色に変わる。この物質は65℃で熱変色転移を示すといわれているが、実際の実験によれば、迅速な熱変色を受けるためにP3ODTは実際には約100℃の温度(ヒーターの表面温度)を要求することが実証されている。
ポリマー製品の分析用の実験装置を図1に示す。ポリマー製品の蛍光測定は、熱源2としての小形532nmレーザー(Nanolase社、フランス)及びポータブル分光蛍光計4を用いて行った。分光蛍光計4(Ocean Optics,Inc.、ダニーディン、米国フロリダ州、モデルST2000)には、200μmのスリット、400nmのブレーズ波長を有すると共に30%を超える効率で250〜800nmのスペクトル範囲をカバーする600本/mmの回折格子、及び線形CCDアレイ検出器が備わっていた。レーザー2からの光は、「シックス・アラウンド・ワン」二分岐型光ファイバー反射プローブ8(Ocean Optics,Inc.、モデルR400−7−UV/VIS)の2つのアームの一方である第一の光ファイバーアーム6に集束させた。光ファイバープローブ8の共通端8を表面12への垂線に対して0又は45度の角度で試料10の近くに配置した場合、試料10からの発光が捕集された。プローブ8の第二の光ファイバーアーム12は分光計4に結合した。若干の実験では、ロングパス光学フィルター14により、分光計4への励起光の入射を阻止できる。捕集されたスペクトルの処理は、KaleidaGraph(Synergy Software社、レディング、米国ペンシルヴェニア州)を用いてコンピューター16上で行った。
図2は、実施例1で製造したポリマー製品に関し、製品が室温(低温)及び100℃(高温)にある場合に図1の実験装置で測定した蛍光スペクトルの差を示すものである。図2は、室温(低温)にある場合及び約100℃(高温)に加熱した場合について、532nmの励起波長での試料MWB0703031−2〜−5の蛍光発光プロフィルを示している。熱変色性標識(0.05pphのP3ODT)のみを含む試料MWB0703031−2は、試料温度を約100℃に上昇させた場合に蛍光スペクトルの顕著な変化を示す。蛍光発光が増加するばかりでなく、ピーク位置が約650nmから約590nmにシフトする。有機蛍光物質(1ppmのBASF社製Lumogen F−300)のみを含む試料MWB0703031−3は、「低温」状態と「高温」状態との間で蛍光発光特性の変化を示さない。それに比べて、同じ有機蛍光物質を増幅化合物として熱変色性化合物と共に添加した場合(試料MWB0703031−4及びMWB0703031−5の場合)には、第一の温度と認証温度との間(即ち、「低温」状態と「高温」状態との間)で蛍光発光スペクトルが顕著に変化する。認証温度の「高温」状態での発光は、試料MWB0703031−2(熱変色性化合物のみ)に比べ、約590nmに極大を有する一層はっきりしたピーク(即ち、強度が大きく幅の狭いピーク)を示す。これは、蛍光物質と熱変色性化合物との間の相乗効果を例示している。認証プロセス中における蛍光発光の差はNIR吸収剤の存在でほとんど影響されないことに注意されたい。その結果、NIR吸収剤及び(さらに詳しくは)その吸収特性を使用して、レーザーのような外部NIR光源で誘起される内部熱パルスを生み出すことができる。
図3は、実施例1で製造した材料MWB0703031−4を加熱した際における蛍光強度増加の可逆性を実証している。試料MWB0703031−4をヒートガンからの相次ぐ短い熱パルスに暴露しながら、動的蛍光測定を行った。
図4は、実施例1で製造した試料MWB0703031−4の加熱中に測定した吸収特性の変化を示している。図4の第一のグラフ(左)は、温度を「低温」から「高温」に上昇させた場合の吸収スペクトルの変化を示している。図4の第二のグラフ(右)は、535nmでの吸光度変化を示している。
図6は、熱パルス後の蛍光発光の変化を例示している。実施例1で製造した試料MWB0703031−4の蛍光減衰度が加熱後の時間の関数として示されている。実施例3の実験装置を使用した。これは、2つの試料状態(「高温」及び「低温」)間における蛍光発光の変化の監視ばかりでなく、加熱後の蛍光減衰度のような動的パラメーターの分析によっても確認を行うのが可能であることを示している。かかる減衰特性は、通例、熱パルスの強度及び持続時間並びに熱変色性物質の添加量及びポリマー母材の性質に依存する。このような理由で、確認プロセス中に減衰特性を使用することは一層確実な認証を可能にする。
Claims (14)
- 試験ポリマーが認証可能ポリマーであることを認証する方法であって、認証可能ポリマーが基板ポリマーと熱変色性化合物とを含んでおり、熱変色性化合物が第一の温度及び認証波長で第一の信号を有するとともに、認証温度及び認証波長で第二の信号を有し、第一の信号と第二の信号とが異なり、認証温度が第一の温度より高い温度であり、当該方法が、
試験ポリマーの一部分を認証温度に上昇させて加熱部分を生み出すのに十分な刺激に試験ポリマーを暴露し、
認証波長で試験ポリマーの加熱部分の試験信号を測定し、
試験信号が認証可能ポリマーの認証信号と実質的に同じであれば試験ポリマーが認証可能ポリマーであると認証する
ことを含んでなる方法。 - 試験信号を測定する段階がさらに、反射、発光、蛍光又はルミネセンスの1以上を測定することを含む、請求項1記載の方法。
- 熱変色性化合物が、認証可能ポリマーを基準にして約1重量%未満の量で認証可能ポリマー中に存在する、請求項1記載の方法。
- 熱変色性化合物が、認証可能ポリマーを基準にして0.005重量%以上の量で認証可能ポリマー中に存在する、請求項1記載の方法。
- 熱変色性化合物が、目視で検出できる熱変色応答を与えない量で認証可能ポリマー中に存在する、請求項1記載の方法。
- 試験信号が、蛍光の強度、蛍光ピークの形状、蛍光ピークの位置、経時的な又は熱源除去後の蛍光の持続時間又は減衰度、2以上の異なる波長での蛍光強度の比、及びこれらの組合せの1以上である、請求項1記載の方法。
- 認証可能ポリマーがさらに増幅化合物を含み、増幅化合物の結果として認証可能ポリマーの認証信号が熱変色性化合物の第二の信号より大きい、請求項1記載の方法。
- 基板ポリマー、及び
第一の温度及び認証波長で第一の信号を有すると共に、認証温度及び認証波長で第二の信号を有する熱変色性化合物であって、第一及び第二の信号は異なっており、認証温度は第一の温度より高い熱変色性化合物
を含んでなる認証可能ポリマーであって、
熱変色性化合物は認証可能ポリマーの重量を基準にして約0.001〜約0.50重量%の量で認証可能ポリマー中に存在する、認証可能ポリマー。 - 熱変色性化合物が認証可能ポリマーの重量を基準にして約0.005〜約0.4重量%の量で存在する、請求項8記載の認証可能ポリマー。
- 認証可能ポリマーがさらに増幅化合物を含み、増幅化合物の結果として認証可能ポリマーの認証信号が熱変色性化合物の第二の信号より大きい、請求項8記載の認証可能ポリマー。
- 認証可能ポリマーの製造方法であって、
基板ポリマー及び熱変色性化合物を合体させて認証可能ポリマーを製造することを含んでなり、熱変色性化合物が認証可能ポリマーの重量を基準にして約0.001〜約0.50重量%の量で導入される、方法。 - 認証可能製品の製造方法であって、
請求項30記載の認証可能ポリマーを用意し、
認証可能ポリマーから認証可能製品を形成する
ことを含んでなる方法。 - 請求項12記載の方法で製造される認証可能製品。
- 光ディスクである、請求項13記載の認証可能製品。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/723,625 US7094364B2 (en) | 2003-11-26 | 2003-11-26 | Method of authenticating polymers, authenticatable polymers, methods of making authenticatable polymers and authenticatable articles, and articles made there from |
PCT/US2004/038667 WO2005055156A2 (en) | 2003-11-26 | 2004-11-18 | Method of authenticating polymers, authenticatable polymers, methods of making authenticatable polymers and authenticatable articles, and articles made there from |
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JP2007513447A true JP2007513447A (ja) | 2007-05-24 |
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Family Applications (1)
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US (1) | US7094364B2 (ja) |
EP (1) | EP1690235B1 (ja) |
JP (1) | JP2007513447A (ja) |
AT (1) | ATE553463T1 (ja) |
TW (1) | TW200538717A (ja) |
WO (1) | WO2005055156A2 (ja) |
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-
2003
- 2003-11-26 US US10/723,625 patent/US7094364B2/en not_active Expired - Fee Related
-
2004
- 2004-11-18 AT AT04817845T patent/ATE553463T1/de active
- 2004-11-18 WO PCT/US2004/038667 patent/WO2005055156A2/en not_active Application Discontinuation
- 2004-11-18 JP JP2006541364A patent/JP2007513447A/ja not_active Withdrawn
- 2004-11-18 EP EP20040817845 patent/EP1690235B1/en not_active Not-in-force
- 2004-11-26 TW TW93136615A patent/TW200538717A/zh unknown
Cited By (5)
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JP2009299003A (ja) * | 2008-05-13 | 2009-12-24 | Toyobo Co Ltd | 高次構造変化表示体およびそれを用いたポリマーの高次構造変化の検知方法 |
JP2009300985A (ja) * | 2008-05-13 | 2009-12-24 | Toyobo Co Ltd | 温度時間経歴を表示する製造工程チェックラベル |
JP2009300986A (ja) * | 2008-05-13 | 2009-12-24 | Toyobo Co Ltd | 温度時間経歴を表示する流通履歴表示ラベル |
JP2015505111A (ja) * | 2012-01-17 | 2015-02-16 | ハネウェル・インターナショナル・インコーポレーテッド | サーモグラフィ蛍光体を組み込む物品、ならびにそのような物品を認証するための方法および装置 |
Also Published As
Publication number | Publication date |
---|---|
EP1690235A2 (en) | 2006-08-16 |
WO2005055156A3 (en) | 2005-07-28 |
EP1690235B1 (en) | 2012-04-11 |
TW200538717A (en) | 2005-12-01 |
US20050109984A1 (en) | 2005-05-26 |
WO2005055156A2 (en) | 2005-06-16 |
US7094364B2 (en) | 2006-08-22 |
ATE553463T1 (de) | 2012-04-15 |
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