JP2021510748A - 熱処理を使用して拡張された焼結ウィンドウを有するフルオロポリマー粉末及びそのレーザー焼結での使用 - Google Patents
熱処理を使用して拡張された焼結ウィンドウを有するフルオロポリマー粉末及びそのレーザー焼結での使用 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/141—Processes of additive manufacturing using only solid materials
- B29C64/153—Processes of additive manufacturing using only solid materials using layers of powder being selectively joined, e.g. by selective laser sintering or melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/124—Treatment for improving the free-flowing characteristics
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J3/00—Processes of treating or compounding macromolecular substances
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- C08J3/128—Polymer particles coated by inorganic and non-macromolecular organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
Description
−短鎖炭化水素、例えばエタン及びプロパン、
−エステル、例えば酢酸エチル及びマレイン酸ジエチル
−アルコール、カーボネート、ケトン、
−ハロカーボン及びハイドロハロカーボン、例えばクロロカーボン、ハイドロクロロカーボン、クロロフルオロカーボン及びハイドロクロロフルオロカーボン、
−有機溶媒(それらが乳化又は懸濁重合反応に添加される場合)から選択される。
a)特定の温度に加熱されたチャンバ内に維持された水平プレート上に本発明の組成物の粉末の薄層を堆積させる工程、
b)レーザーによって供給されるエネルギーを介して、例えば、物体の形状を保存し、この形状をスライスの形態で再現するコンピュータを使用して、物体に対応する幾何学形状に粉末層のさまざまな点で粉末粒子を溶融する工程、
c)粉末の1つの層の厚さに対応する値、例えば0.05〜2mm、一般に約0.1mmで水平プレートを下げる工程、
d)粉末の新しい層を堆積させる工程。この層は、粉末床温度(又は床温度)と称される温度にあり、
e)この新しい層を、物体のこの新しいスライスに対応する幾何学形状で、レーザーによって供給されるエネルギーによって溶融する工程、
f)物体全体が製造されるまで、工程c)、d)及びe)の手順を繰り返す工程、
g)物体の完全な製造の最後にアセンブリを冷却する工程、
h)製造された物体を、溶融されていない周囲の粉末から分離する工程を含む。
−熱可塑性フルオロポリマー粉末の弱凝集(ケーキング)開始温度の上昇、
−周囲温度及び焼結方法の温度での粉末の流動性の改善、
−タップ密度及び嵩密度の増加、
−焼結部品の特性の改善である。
PVDF:250Pa.sの230℃、100s−1で測定した溶融粘度を有する二フッ化ビニリデンホモポリマー。
PVDF粉末は、Netzch CUM150ミルを使用した2工程の低温粉砕によって調製された。最初の工程は、顆粒の低温予備粉砕からなっていた。この工程では、ミルに、5mmの直径を有するピンディスクが装備されている。ディスクの回転速度は14000pmに設定されている。次いで、このようにして得られた粉末を、同じであるが、ブラストローター及びミリングチャンバ内に100μmのグリッドを備えているNetzchミルで2回目の低温粉砕を行う。ローターの速度は12000rpm、5kg/hのスループットに設定されている。得られた粉末は、50μmのDV50を特徴とする粒径分布を有する。
粒径分布:粒径分布は、Malvern INSITEC Systemレーザー粒径分析器を使用してドライルートで測定した。
粉末の「嵩」密度は、以下の方法で測定された。250mlのメスシリンダに粉末を満たした。正確な体積及び質量が測定され、そこから密度が推定される。密度は、嵩密度の測定のために以前に満たされたシリンダに、一連の制御された垂直方向の衝撃(振幅、周波数)を与えることによって得られた。
機械的特性:
焼結試験片の機械的特性は、10kNロードセルを備えたZwick 3万能試験機を使用して測定した。変位は、光学式伸び計を使用して測定された。変位速度は5mm/分に設定した。
PVDFの分解は、GPCによるモル質量の測定及びゲル/不溶物の含有量の推定によって評価された。
機械を通過する前後のモル質量は、P600ポンプ、Wisp 717Plusインジェクタ及びWaters 2414 RID屈折計検出器を備えたWaters分析チェーンを使用して、GPCで測定された。カラムの温度は50℃に調整されている。分析するサンプルを、DMSO+0.1MのNaNO3に2g/lの濃度で、95℃で4時間かけて溶解する。次いで、直径25mm、気孔率0.45μmのACRODISC GHPポリプロピレンフィルタを使用して、溶液を濾過する。質量はPMMA相当として表される。不溶性画分は、屈折計の信号の強度を完全に可溶性のPVDFの強度と比較することによって推定される。
疎水性シリカは、粉末が漏斗のオリフィスを通って流れることを可能にする。この試験では、7秒の流動時間が非常に良好な流動性の兆候と見なされる。シリカがない場合、又は親水性シリカFA2を添加した場合、粉末は流動せず、流動性が低いため、そのまま焼結方法で使用できない。結果を表1に示す。
ISO 527 1BA及び1Aタイプの引張試験片は、EOSのFormiga P100レーザー焼結機で焼結して製造された。機械の通過条件は次のとおりである。
−輪郭速度(contour speed)=1500mm/s
−ハッチング速度=2500mm/s
−「ビームオフセット」ハッチング=0.15mm
動作条件を以下の表2にまとめる。
シリカとの粉末の配合:0.2重量%のCab−o−sil TS610シリカを、急速ミキサを使用してPVDF粉末と混合する。
−150°Cで8時間
−155°Cで8時間
熱処理は、オーブンに入れられた容器に粉末を堆積させることにより静的に行われる。
Claims (16)
- 熱可塑性フルオロポリマー及び流動剤を含む粉末形態の組成物であって、前記組成物は、Tm−40℃〜Tm−5℃の範囲の温度で加熱が行われ、TmはDSCにより測定される熱可塑性ポリマーの溶融温度である、組成物。
- 熱処理を受けた粉末に対して行われる圧縮試験により測定して、2N未満、好ましくは1.5N未満の圧縮力を有する、請求項1に記載の組成物。
- 前記フルオロポリマーが、以下に列挙する少なくとも1つのモノマー:フッ化ビニル;フッ化ビニリデン;トリフルオロエチレン;クロロトリフルオロエチレン;1,2−ジフルオロエチレン;テトラフルオロエチレン;ヘキサフルオロプロピレン;パーフルオロ(アルキルビニル)エーテル、例えばパーフルオロ(メチルビニル)エーテル、パーフルオロ(エチルビニル)エーテル及びパーフルオロ(プロピルビニル)エーテル;パーフルオロ(1,3−ジオキソール);パーフルオロ(2,2−ジメチル−1,3−ジオキソール);式CF2=CFOCF2CF(CF3)OCF2CF2X(式中、Xは、SO2F、CO2H、CH2OH、CH2OCN又はCH2OPO3H)の生成物;式CF2=CFOCF2CF2SO2Fの生成物;式F(CF2)nCH2OCF=CF2(式中、nは1、2、3、4又は5である)の生成物;式R1CH2OCF=CF2(式中、R1は水素又はF(CF2)mであり、mは1、2、3又は4に等しい)の生成物;式R2OCF=CH2(式中、R2はF(CF2)pであり、pは1、2、3又は4である)の生成物;パーフルオロブチルエチレン(PFBE);3,3,3−トリフルオロプロペン及び2−トリフルオロメチル−3,3,3−トリフルオロ−1−プロペンを含むホモポリマー又はコポリマーである、請求項1及び2に記載の組成物。
- 前記フルオロポリマーが、フッ化ビニリデンから誘導される単位を含むポリマーであり、ポリフッ化ビニリデンホモポリマー並びに少なくとも50mol%、好ましくは少なくとも75mol%のフッ化ビニリデンから誘導される単位と、フッ化ビニル;トリフルオロエチレン;クロロトリフルオロエチレン;1,2−ジフルオロエチレン;テトラフルオロエチレン;ヘキサフルオロプロピレン;パーフルオロ(アルキルビニル)エーテル、例えばパーフルオロ(メチルビニル)エーテル、パーフルオロ(エチルビニル)エーテル及びパーフルオロ(プロピルビニル)エーテル;パーフルオロ(1,3−ジオキソール);パーフルオロ(2,2−ジメチル−1,3−ジオキソール)及びそれらの混合物から選択される少なくとも1つの他のコモノマーから誘導される残りの単位とを含むコポリマーから選択される、請求項1〜3のいずれか一項に記載の組成物。
- 前記フルオロポリマーが、エチレンとクロロトリフルオロエチレンとのコポリマー、エチレンとテトラフルオロエチレンとのコポリマー、ヘキサフルオロプロピレンとテトラフルオロエチレンとのコポリマー、テトラフルオロエチレンとパーフルオロ(アルキルビニル)エーテルのファミリーからのモノマーとのコポリマーから選択される、請求項1〜3のいずれか一項に記載の組成物。
- 前記フルオロポリマーが、標準のASTM D3825に従って232℃の温度及び100s−1の剪断速度で測定して、1600Pa.s以下、好ましくは1000Pa.s以下の粘度を有する、請求項1〜5のいずれか一項に記載の組成物。
- フルオロポリマー粉末が、100μm以下、好ましくは25〜80マイクロメートルのDv50で定義される粒径を有する、請求項1〜6のいずれか一項に記載の組成物。
- 前記フルオロポリマーが、5kDa〜200kDa、好ましくは5kDa〜150kDa、なおより好ましくは5kDa〜120kDaの範囲の数平均分子量を有する、請求項1〜7のいずれか一項に記載の組成物。
- 前記流動剤が、沈降シリカ、ヒュームドシリカ、ガラス質シリカ、焼成シリカ、ガラス質リン酸塩、ガラス質ホウ酸塩、ガラス質酸化物、アモルファスアルミナ、二酸化チタン、タルク、マイカ、カオリン、アタパルジャイト、ケイ酸カルシウム、アルミナ及びケイ酸マグネシウムから選択される、請求項1〜8のいずれか一項に記載の組成物。
- 前記流動剤が疎水性ヒュームドシリカである、請求項9に記載の組成物。
- 流動剤の重量割合が、前記組成物の総重量の0.01%〜5%、好ましくは0.025%〜1%である、請求項1〜10のいずれか一項に記載の組成物。
- フルオロポリマー及び流動剤からなる、請求項1〜11のいずれか一項に記載の組成物。
- さらに染料、着色用の顔料、赤外線吸収用の顔料、カーボンブラック、難燃性添加剤、ガラス繊維、炭素繊維、抗酸化安定剤、光安定剤、衝撃改質剤、帯電防止剤及び難燃剤から選択される1つ以上の添加剤を最大50重量%含む、請求項1〜11のいずれか一項に記載の組成物。
- 三次元物体を製造する方法であって、前記方法が、三次元物体を得るために、請求項1〜13のいずれか一項に記載の粉末形態の組成物をレーザー焼結することを含む、方法。
- 三次元レーザー焼結用の材料としての、請求項1〜13のいずれか一項に記載の組成物の使用。
- 請求項14に記載の方法により得られる三次元物体。
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