JP6472590B1 - 造形物及びその製造方法 - Google Patents
造形物及びその製造方法 Download PDFInfo
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- JP6472590B1 JP6472590B1 JP2018565071A JP2018565071A JP6472590B1 JP 6472590 B1 JP6472590 B1 JP 6472590B1 JP 2018565071 A JP2018565071 A JP 2018565071A JP 2018565071 A JP2018565071 A JP 2018565071A JP 6472590 B1 JP6472590 B1 JP 6472590B1
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- WUMSTCDLAYQDNO-UHFFFAOYSA-N triethoxy(hexyl)silane Chemical compound CCCCCC[Si](OCC)(OCC)OCC WUMSTCDLAYQDNO-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明の造形物を構成する樹脂組成物は、平均繊維長1μm〜300μm、且つ平均アスペクト比3〜200である無機繊維(A)と、熱可塑性樹脂(B)とを含有し、必要に応じて、その他の添加剤(C)をさらに含有することができる。
本発明で使用する無機繊維は、繊維状粒子から構成される粉末であり、平均繊維長1μm〜300μm、且つ平均アスペクト比3〜200である。平均繊維長は、好ましくは1μm〜200μmであり、より好ましくは3μm〜100μmであり、さらに好ましくは5μm〜50μmである。平均アスペクト比は、好ましくは3〜100であり、より好ましくは5〜50であり、さらに好ましくは8〜40である。上記平均繊維長及び平均アスペクト比を有する無機繊維を用いることにより、製造が容易で、かつ3次元プリンタを用いた造形において、造形物の層間剥離、造形物の反り等を改善することができる。造形物の剥離強度が向上することで、造形物の機械特性を更に向上することができる。
樹脂組成物に用いる熱可塑性樹脂としては、熱溶解積層方式3次元プリンタで使用できるものであり、後述するヘッド送り速度を落とすことなく安定的に吐出できる溶融時の流動特性を有していれば特に限定されないが、例えば、ポリプロピレン(PP)樹脂、ポリエチレン(PE)樹脂、環状ポリオレフィン(COP)樹脂、環状オレフィン・コポリマー(COC)樹脂等のポリオレフィン樹脂;ポリスチレン(PS)樹脂、シンジオタクチックポリスチレン(SPS)樹脂、耐衝撃性ポリスチレン(HIPS)樹脂、アクリロニトリル−ブチレン−スチレン共重合体(ABS)樹脂等のポリスチレン系樹脂;ポリ乳酸(PLA)樹脂、ポリエチレンテレフタレート(PET)樹脂、ポリブチレンテレフタレート(PBT)樹脂等のポリエステル系樹脂;ポリアセタール(POM)樹脂;ポリカーボネート(PC)樹脂;ポリアミド6樹脂、ポリアミド66樹脂、ポリアミド11樹脂、ポリアミド12樹脂、ポリアミド46樹脂、ポリアミド6樹脂とポリアミド66樹脂の共重合体(ポリアミド6/66樹脂)、ポリアミド6樹脂とポリアミド12樹脂の共重合体(ポリアミド6/12樹脂)等の脂肪族ポリアミド(PA)樹脂;ポリアミドMXD6樹脂、ポリアミド6T樹脂、ポリアミド9T樹脂、ポリアミド10T樹脂等の芳香環を有する構造単位と芳香環を有さない構造単位からなる半芳香族ポリアミド(PA)樹脂;ポリフェニレンサルファイド(PPS)樹脂;ポリエーテルサルフォン(PES)樹脂;液晶ポリエステル(LCP)樹脂;ポリエーテルケトン(PEK)樹脂、ポリエーテルエーテルケトン(PEEK)樹脂、ポリエーテルケトンケトン(PEKK)樹脂、ポリエーテルエーテルケトンケトン(PEEKK)樹脂等のポリエーテル芳香族ケトン樹脂;ポリエーテルイミド(PEI)樹脂;ポリアミドイミド(PAI)樹脂;熱可塑性ポリイミド(TPI)樹脂;等を例示することができる。
本発明の造形物を構成する樹脂組成物は、その好ましい物性を損なわない範囲において、その他の添加剤を含有することができる。その他の添加剤としては、耐衝撃改良剤;アラミド繊維、ポリフェニレンベンズオキサゾール(PBO)繊維、ガラス繊維、炭素繊維、アルミナ繊維、ボロン繊維、炭化ケイ素繊維、炭酸カルシム、雲母、マイカ、セリサイト、イライト、タルク、カオリナイト、モンモリナイト、ベーマイト、スメクタイト、バーミキュライト、二酸化チタン、シリカ、チタン酸カリウム、チタン酸リチウムカリウム、ベーマイト、ガラスビーズ、アルミナ等の上述の無機繊維(A)以外の無機充填材;ポリテトラフルオロエチレン(PTFE)、低密度ポリエチレン、直鎖状低密度ポリエチレン、中密度ポリエチレン、高密度ポリエチレン、超高分子量ポリエチレン等のポリオレフィン樹脂、グラファイト、二硫化モリブテン、二硫化タングステン、窒化ホウ素等の固体潤滑剤;銅化合物等の熱安定剤;ヒンダードフェノール系光安定剤等の光安定剤;核形成剤;アニオン性帯電防止剤、カチオン性帯電防止剤、非イオン系帯電防止剤等の帯電防止剤;老化防止剤(酸化防止剤);耐候剤;金属不活性剤;ベンゾフェノン系紫外線吸収剤、ベンゾトリアゾール系紫外線吸収剤、トリアジン系紫外線吸収剤、サイリシレート系紫外線吸収剤等の紫外線吸収剤;防菌・防黴剤;防臭剤;炭素系導電剤、金属系導電剤、金属酸化物系導電剤、界面活性剤等の導電性付与剤;分散剤;ポリエステル系可塑剤、グリセリン系可塑剤、多価カルボン酸エステル系可塑剤、リン酸エステル系可塑剤、ポリアルキレングリコール系可塑剤、エポキシ系可塑剤等の軟化剤(可塑剤);カーボンブラック、酸化チタン等の顔料、染料等の着色剤;ホスファゼン系化合物、リン酸エステル、縮合リン酸エステル、無機リン系難燃剤、ハロゲン系難燃剤、シリコーン系難燃剤、金属酸化物系難燃剤、金属水酸化物系難燃剤、有機金属塩系難燃剤、窒素系難燃剤、ホウ素化合物系難燃剤等の難燃剤;ドリッピング防止剤;制振剤;中和剤;ブロッキング防止剤;流動性改良剤;脂肪酸、脂肪酸金属塩等の離型剤;滑剤;等が挙げられ、これらを1種又は2種以上を含有することができる。
樹脂組成物は、無機繊維(A)及び熱可塑性樹脂(B)、必要に応じて、更にその他の添加剤(C)の成分を、混合及び加熱(特に、溶融混練)することによって製造することができる。
本発明の造形物は、樹脂組成物を、特定の条件において、熱溶解積層方式の3次元プリンタ(付加製造装置ともいう)で造形することで、造形物中の無機繊維の配向をより一層高めることができる。
チタン酸カリウム(商品名:TISMO D102、大塚化学社製、平均繊維長:15μm、平均繊維径:0.5μm、平均アスペクト比:30)
ポリアミド12樹脂(商品名:ダイアミドL1800、ダイセル社製)
ポリアミドMXD6樹脂(商品名:MXPA6000、三菱瓦斯化学社製)
PPS樹脂(商品名:ジュラファイドW214A、ポリプラスチックス社製)
PEEK樹脂(商品名:PEEK181G、VICTREX社製)
オレフィン系重合体(無水マレイン酸変性エチレン・1−ブテン共重合体、商品名:タフマーMH5020、三井化学社製)
カーボンブラック(商品名:#3050、三菱化学社製、平均粒子径50nm、不定形状粒子)
タルク(平均粒子径8μm、板状粒子)
(フィラメントNo.1〜8)
表1に示す配合割合で、二軸押出機を用いて溶融混練し、それぞれペレットを製造した。なお、二軸押出機のシリンダ温度は、フィラメントNo.1、2及び6〜8においては190℃〜230℃とし、フィラメントNo.3においては230℃〜270℃とし、フィラメントNo.4においては280℃〜300℃とし、フィラメントNo.5においては350℃〜380℃とした。
(実施例1〜13、比較例1〜22)
上記で得られたフィラメントを、熱溶解積層方式3次元プリンタによって、表2に示したプリント条件にて縦100mm×横2mm×厚さ50mmの平板状の造形物を作製した。実施例1〜3及び比較例1〜6はMUTOH社製の熱溶解積層方式3次元プリンタ(商品名:MF1100)を、実施例4〜5及び比較例7〜8はMagnaRecta社製の熱溶解積層方式3次元プリンタ(商品名:Lepton2)を用いた。なお、造形は平板状の造形物の縦方向に進行し、厚さ方向に積層した。
(1)そり量
表2の条件で作製した平板状の造形物について、そり量をノギスで測定した。そり量Wは、図6に示すように、造形進行方向における中央部と端部での、造形積層方向における高さの差である。結果を表2に示した。
表2の条件で作製した平板状の造形物の収縮率を測定した。収縮率は、積層方向と進行方向において測定した。積層方向の収縮率は、図6に示す造形積層方向の厚さbにおける収縮率である。進行方向の収縮率は、図6に示す造形進行方向の長さaにおける収縮率である。結果を表2に示した。
表2の条件で作製した平板状の造形物を、積層方向に幅10mmの短冊状にカットし、得られた短冊をオートグラフAG−5000(島津製作所社製)にて支点間距離30mmの3点曲げ試験により曲げ応力を測定し、界面密着力とした。結果を表2に示した。
表3及び表4の条件にて作製した引張ダンベル試験片について、オートグラフAG−1(島津製作所社製)にて引張強度を測定し、結果を表3及び表4に示した。
表3及び表4の条件にて作製した引張ダンベル試験片において表層から深さ1mm、表5及び表6の条件にて作製した摺動リング試験片において表層から0.05mmにおける無機繊維の配向角度を測定した。なお、引張ダンベル試験片については、図3に破線で示す位置、すなわち引張ダンベル試験片の長さ方向の中央部分の位置の表層から深さ1mmにおける無機繊維の配向角度を測定した。また、3次元プリンタによる摺動リング試験片1については、摺動面2の任意の位置の表層から深さ0.05mmにおける無機繊維の配向角度を測定した。また、射出成形による摺動リング試験片11については、図5に示す摺動面2を平面視したときに、ゲート3とウェルドライン4との中間部5の位置の表層から深さ0.05mmにおける無機繊維の配向角度を測定した。上記部位について、X軸が造形進行方向になるように試験片のように配置したうえで、得られた試験片の表面を走査型電子顕微鏡(SEM、日立ハイテクノロジーズ社製、S−4800)を用いて、反射電子検出器(BSE検出器、GW社製、)を使用して組成コントラスト像を撮影した。写真倍率は5000倍とした。なお、一例として、実施例11の走査型電子顕微鏡写真を図7に、比較例21の走査型電子顕微鏡写真を図8に、比較例22の走査型顕微鏡写真を図9に示す。
表5及び表6の条件にて作製した摺動リング試験片について、鈴木式摩擦摩耗試験機(エー・アンド・ディ社製、EFM−III−F)を用いて各試験片について摩耗量を求めた。摩擦摩耗試験の条件は、面圧0.5MPa、周速度0.15m/秒、時間3時間、相手材S45Cとした。
表7の条件にて作製したIZOD試験片について、JIS K7110に準じ、ノッチ付きアイゾット(IZOD)衝撃値を測定した。
2…摺動面
3…ゲート
4…ウェルドライン
5…中間部
Claims (7)
- 平均繊維長1μm〜300μm、且つ平均アスペクト比3〜200である無機繊維と、熱可塑性樹脂とを含有する樹脂組成物から構成される造形物であり、前記無機繊維の配向角度の平均値が24°以下であり、3次元プリント造形物である、造形物。
- 前記無機繊維のモース硬度が5以下である、請求項1に記載の造形物。
- 前記無機繊維が、チタン酸カリウム、ワラストナイトから選ばれる少なくとも1種である、請求項1又は2に記載の造形物。
- 前記無機繊維の含有量が、樹脂組成物の合計量100質量%中に1質量%〜40質量%である、請求項1〜3のいずれか一項に記載の造形物。
- 前記熱可塑性樹脂が、ポリオレフィン樹脂、ポリスチレン系樹脂、ポリエステル系樹脂、ポリアセタール(POM)樹脂、ポリカーボネート(PC)樹脂、脂肪族ポリアミド(PA)樹脂、半芳香族ポリアミド(PA)樹脂、ポリフェニレンサルファイド(PPS)樹脂、ポリエーテルイミド(PEI)樹脂、ポリエーテルエーテルケトン(PEEK)樹脂から選ばれる少なくとも1種である、請求項1〜4のいずれか一項に記載の造形物。
- 熱溶解積層方式3次元プリンタによる造形物である、請求項1〜5のいずれか一項に記載の造形物。
- 請求項1〜6のいずれか一項に記載の造形物の製造方法であって、平均繊維長1μm〜300μm、且つ平均アスペクト比3〜200である無機繊維と、熱可塑性樹脂とを含有する樹脂組成物からなるフィラメントを、熱溶解積層方式3次元プリンタにより造形する、造形物の製造方法。
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