JP7163193B2 - 積層造形のための光硬化性配合物の生成 - Google Patents
積層造形のための光硬化性配合物の生成 Download PDFInfo
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- JP7163193B2 JP7163193B2 JP2018563527A JP2018563527A JP7163193B2 JP 7163193 B2 JP7163193 B2 JP 7163193B2 JP 2018563527 A JP2018563527 A JP 2018563527A JP 2018563527 A JP2018563527 A JP 2018563527A JP 7163193 B2 JP7163193 B2 JP 7163193B2
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Description
a)
成分(A)少なくとも2μmのD50値を有する少なくとも1種のセラミック材料と、
成分(B1)少なくとも1種の第1のアクリレートと、
成分(C)少なくとも1種の分散剤と
を含むセラミック分散体(CD)を用意する工程と、
b)
成分(B2)少なくとも1種の第2のアクリレートと、
成分(D)少なくとも1種の光開始剤と
を含む溶液(S)を用意する工程と、
c)
工程a)において用意されたセラミック分散体(CD)および工程b)において用意された溶液(S)を混合して、光硬化性配合物(F)を得る工程と
を含む方法により達成される。
工程a)において、セラミック分散体(CD)が用意される。このセラミック分散体(CD)は、成分(A)として少なくとも2μmのD50値を有する少なくとも1種のセラミック材料と、成分(B1)として少なくとも1種の第1のアクリレートと、成分(C)として少なくとも1種の分散剤とを含む。
工程b)において、成分(B2)として少なくとも1種の第2のアクリレートと、成分(D)として少なくとも1種の光開始剤とを含む溶液(S)が用意される。
成分(A)は、少なくとも2μmのD50値を有する少なくとも1種のセラミック材料である。
0.01~5μmの範囲内のD10値、
2~10μmの範囲内のD50値、および
20~35μmの範囲内のD90値を有する。
0.1~2μmの範囲内のD10値、
4~10μmの範囲内のD50値、および
25~35μmの範囲内のD90値を有する。
成分(B1)は、少なくとも1種の第1のアクリレートである。
成分(C)は、少なくとも1種の分散剤である。
成分(D)は、少なくとも1種の光開始剤である。
工程c)では、工程a)において用意されたセラミック分散体(CD)および工程b)において用意された溶液(S)を混合して、光硬化性配合物(F)を得る。
工程c)において、光硬化性配合物(F)が得られる。
本発明の別の目的は、積層造形プロセスにおける成形物の生成のための方法であって、
i)請求項11による光硬化性配合物(F)を用意する工程と、
ii)工程i)において用意された光硬化性配合物(F)の第1の部分の層を形成し、形成された層の少なくとも一部を、UV光源を使用して硬化させ、成形物を得る工程と
を含む方法である。
ii-1)工程i)において用意された光硬化性配合物(F)の第1の部分の層を形成する工程と、
ii-2)工程ii-1)において形成された光硬化性配合物(F)の第1の部分の層の少なくとも一部を、UV光源を使用して硬化させ、硬化層を得る工程と、
ii-3)工程i)において用意された光硬化性配合物(F)の第2の部分の第2の層を、工程ii-2)において得られた硬化層上に形成する工程と、
ii-4)工程ii-3)において形成された光硬化性配合物(F)の第2の部分の第2の層の少なくとも一部を、UV光源を使用して硬化させ、成形物を得る工程と
を含む。
ii-1)工程i)において用意された光硬化性配合物(F)の第1の部分の層を形成する工程と、
ii-2)工程ii-1)において形成された光硬化性配合物(F)の第1の部分の層の少なくとも一部を、UV光源を使用して硬化させ、硬化層を得る工程と、
ii-3)工程i)において用意された光硬化性配合物(F)の第2の部分の第2の層を、工程ii-2)において得られた硬化層上に形成する工程と、
ii-4)工程ii-3)において形成された光硬化性配合物(F)の第2の部分の第2の層の少なくとも一部を、UV光源を使用して硬化させ、成形物を得る工程と
を含む方法である。
高せん断分散機器として二重螺旋ミキサー(螺旋ピッチ1:1、撹拌器直径12.5インチ)を100rpmまでの撹拌器速度で使用して、成分(A)としての9μmのD50値を有する86.7質量%のシリカ(SiO2)粉末を、成分(B1)としてのヘキサンジオールジアクリレート(商品名:Laromer HDDA、BASF SE製)中で、成分(C)としての1.73質量%のポリプロポキシ第四級アンモニウムクロリド(商品名:Variquat CC NS 42、Evonik製)と混合することにより、セラミック分散体を製造した。
得られたセラミック分散体(CD)を、成分(B2)としてのヘキサンジオールジアクリレート(商品名:Laromer(登録商標)HDDA、Evonik製)およびエトキシル化トリメチロールプロパントリアクリレート(商品名:Laromer(登録商標)LR 8863、Evonik製)、成分(D)としてのヒドロキシシクロヘキシルフェニルケトン(商品名:Irgacure(登録商標)184、BASF SE製)、分散剤としてのポリプロポキシ第四級アンモニウムクロリド(商品名:Variquat(登録商標)CC NS 42、Evonik製)、ならびにUV吸収剤としての2-(2H-ベンゾトリアゾール-2-イル)-4-メチル-フェノール(商品名:Tinuvin(登録商標)171、BASF SE製)を含む溶液(S)と混合し、光硬化性配合物(F)を得た。得られた光硬化性配合物(F)は、以下の組成を有していた:80質量%のセラミック粉末、1.6質量%のポリプロポキシ第四級アンモニウムクロリド、15.5質量%のヘキサンジオールジアクリレート、1.94質量%のエトキシル化トリメチロールプロパントリアクリレート、1.05質量%のヒドロキシシクロヘキシルフェニルケトン、および0.04質量%の2-(2H-ベンゾトリアゾール-2-イル)-4-メチル-フェノール。セラミック分散体(CD)および溶液(S)の混合は、分散ディスク(直径:4cm)を使用して、800rpmで30分間行った。
Claims (10)
- 積層造形プロセスにおいて使用するための光硬化性配合物(F)の生成のための方法であって、
a)
成分(A)少なくとも2μmのD50値を有する少なくとも1種のセラミック材料と、
成分(B1)少なくとも1種の第1のアクリレートと、
成分(C)少なくとも1種の分散剤と
を含むセラミック分散体(CD)を用意する工程と、
b)
成分(B2)少なくとも1種の第2のアクリレートと、
成分(D)少なくとも1種の光開始剤と
を含む溶液(S)を用意する工程と、
c)工程a)において用意された前記セラミック分散体(CD)および工程b)において用意された前記溶液(S)を混合して、前記光硬化性配合物(F)を得る工程と
を含み、
工程a)で、セラミック分散体(CD)は、まず成分(B1)および(C)を混合し、次いでこの混合物に、凝集体の形成を防止するように、段階的に成分(A)が混合しつつ添加されることによって用意され、及び
工程c)において、前記セラミック分散体(CD)および前記溶液(S)の質量パーセントの合計に対して、75~99質量%の範囲内の前記セラミック分散体(CD)および1~25質量%の範囲内の前記溶液(S)を混合して、前記光硬化性配合物(F)を得る、方法。 - 成分(A)が、SiO2、ZrO2、Al2O3、ZnO、Fe2O3、Fe3O4、Y2O3、TiO2、SiC、Si3N4、TiBおよびAlNからなる群から選択される、請求項1に記載の方法。
- 成分(B1)および成分(B2)が、互いに独立して、アクリレートおよびメタクリレートからなる群から選択される、請求項1または2に記載の方法。
- 成分(C)が、エトキシル化脂肪アルコール、ポリオキシプロピレン/エチレンブロックコポリマー、エトキシル化ノニルフェノール、(ポリエチレングリコール)p-オクチルフェニルエーテル、アルコキシル化ジアミン、ラウリル硫酸ナトリウムおよびカチオン性分散剤からなる群から選択される、請求項1から3のいずれか一項に記載の方法。
- 成分(D)が、ベンゾフェノン、アルキルベンゾフェノン、ハロメチル化ベンゾフェノン、ミヒラーケトン、ベンゾイン、ベンゾインエーテル、ベンジルケタール、アセトフェノン誘導体、フェニルグリオキシル酸、アントラキノン、メチルアントラキノン、アシルホスフィンオキシドおよびビスアシルホスフィンオキシドからなる群から選択される、請求項1から4のいずれか一項に記載の方法。
- 工程a)において用意される前記セラミック分散体(CD)が、成分(A)、(B1)および(C)の体積パーセントの合計に対して、57~90体積%の範囲内の成分(A)、10~42体積%の範囲内の成分(B1)、および0.1~15体積%の範囲内の成分(C)を含む、請求項1から5のいずれか一項に記載の方法。
- 工程b)において用意される前記溶液(S)が、成分(B2)および(D)の質量パーセントの合計に対して、75~99.9質量%の範囲内の成分(B2)、および0.1~25質量%の範囲内の成分(D)を含む、請求項1から6のいずれか一項に記載の方法。
- 成分(B1)および成分(B2)が、互いに独立して、1以上~6の範囲内のC-C二重結合官能性を有する、請求項1から7のいずれか一項に記載の方法。
- 工程b)において用意される前記溶液(S)が、成分(C2)である少なくとも1種の分散剤をさらに含む、請求項1から8のいずれか一項に記載の方法。
- セラミック分散体(CD)の粘度は、Brookfield Viscometer(スピンドル64、6rpm)により25℃の温度で測定して15~50Pasの範囲内である、請求項1に記載の方法。
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