JP2019155915A - レーザ焼結用粉末 - Google Patents
レーザ焼結用粉末 Download PDFInfo
- Publication number
- JP2019155915A JP2019155915A JP2019031048A JP2019031048A JP2019155915A JP 2019155915 A JP2019155915 A JP 2019155915A JP 2019031048 A JP2019031048 A JP 2019031048A JP 2019031048 A JP2019031048 A JP 2019031048A JP 2019155915 A JP2019155915 A JP 2019155915A
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- JP
- Japan
- Prior art keywords
- crystalline polyester
- silica
- particles
- solution
- polyester resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 238000000149 argon plasma sintering Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 title claims description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 314
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 151
- 229920000728 polyester Polymers 0.000 claims abstract description 99
- 239000002245 particle Substances 0.000 claims abstract description 77
- 229920001225 polyester resin Polymers 0.000 claims abstract description 62
- 239000004645 polyester resin Substances 0.000 claims abstract description 62
- 239000000243 solution Substances 0.000 claims abstract description 59
- 239000002105 nanoparticle Substances 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 42
- 229920000642 polymer Polymers 0.000 claims abstract description 36
- 239000007864 aqueous solution Substances 0.000 claims abstract description 21
- 239000003381 stabilizer Substances 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 15
- 230000001376 precipitating effect Effects 0.000 claims abstract description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 43
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 42
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 26
- 239000003999 initiator Substances 0.000 claims description 22
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 20
- 229920005862 polyol Polymers 0.000 claims description 14
- 150000003077 polyols Chemical class 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 239000001530 fumaric acid Substances 0.000 claims description 10
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 239000012763 reinforcing filler Substances 0.000 abstract description 2
- 239000011859 microparticle Substances 0.000 description 48
- 238000000110 selective laser sintering Methods 0.000 description 25
- -1 polypropylene Polymers 0.000 description 21
- 239000000463 material Substances 0.000 description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 13
- 230000008569 process Effects 0.000 description 13
- 238000010146 3D printing Methods 0.000 description 12
- 239000010419 fine particle Substances 0.000 description 12
- 239000010410 layer Substances 0.000 description 11
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 9
- 239000004952 Polyamide Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 229920002647 polyamide Polymers 0.000 description 8
- 238000007639 printing Methods 0.000 description 8
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- 239000011347 resin Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 7
- 229940116351 sebacate Drugs 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 239000008119 colloidal silica Substances 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 6
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- 238000009826 distribution Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 229920002554 vinyl polymer Polymers 0.000 description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 5
- 239000002202 Polyethylene glycol Substances 0.000 description 5
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- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
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- 238000000113 differential scanning calorimetry Methods 0.000 description 4
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- 239000000047 product Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
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- 238000012545 processing Methods 0.000 description 3
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- 229960002317 succinimide Drugs 0.000 description 3
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- 229920002614 Polyether block amide Polymers 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
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- 239000013078 crystal Substances 0.000 description 2
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- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- GHLKSLMMWAKNBM-UHFFFAOYSA-N dodecane-1,12-diol Chemical compound OCCCCCCCCCCCCO GHLKSLMMWAKNBM-UHFFFAOYSA-N 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
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- 230000006872 improvement Effects 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
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- 235000006408 oxalic acid Nutrition 0.000 description 2
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- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
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- FVQMJJQUGGVLEP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOOC(C)(C)C FVQMJJQUGGVLEP-UHFFFAOYSA-N 0.000 description 1
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
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- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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Abstract
Description
特定の実施形態によれば、本明細書において、結晶性樹脂から調製されるシリカ注入結晶性微粒子を開示する。結晶性樹脂の例としては、ポリエステル、ポリアミド、ポリイミド、ポリオレフィン、ポリエチレン、ポリブチレン、ポリイソブチレート、エチレン−プロピレンコポリマー、エチレン−酢酸ビニルコポリマー、ポリプロピレン、およびそれらの混合物などが挙げられ得る。特定の実施形態では、結晶性樹脂は結晶性ポリアミド樹脂または結晶性ポリエステル樹脂である。
本明細書に開示されている結晶性ポリエステル樹脂および微粒子は、架橋剤としても知られている開始剤を使用することによってさらに強化され得る。特定の実施形態によれば、開始剤は、本明細書に開示される不飽和結晶性ポリエステルの不飽和炭素ポリマー主鎖に作用して、ポリエステル同士のさらなる架橋を開始してもよい。硬化とも称されるこの追加の架橋は、結晶性ポリエステル樹脂および微粒子に強度を追加するように機能する。
本明細書に開示される結晶性ポリエステル微粒子は、シリカナノ粒子などの無機材料を含む。理論に拘束されることを望まないが、結晶性ポリエステルポリマーマトリックスにシリカナノ粒子を添加すると、結晶性ポリエステルポリマーマトリックスの脆弱性を増大させることなく、引張強度、機械的強度、および耐衝撃性が増大したハイブリッド微粒子が得られ得る。さらに、結晶性ポリエステルへのシリカの添加は、最初の粒子/粉末、ならびにSLSなどの3D印刷の使用を通して製造される任意の結果として生じる部品の両方を向上させ得る。特定の実施形態では、本明細書に開示されるシリカ注入結晶性微粒子を使用して製造された3D印刷部品は、向上した断熱特性、溶媒および揮発性生成物に対して増大したバリア特性、ならびに高温での熱劣化の低減を有し得る。結晶性ポリエステル樹脂をシリカナノ粒子でコーティングすることによって、粒子凝集の低減、ならびに静電荷の低減が達成され得る。シリカ注入結晶性ポリエステル微粒子は、接着剤、保護コーティング、生体材料、複合材料、薄膜、マイクロエレクトロニクスなどとしての用途を見出し得る。
本明細書に開示されるシリカ注入結晶性ポリエステル微粒子は、様々な方法によって調製され得る。結晶性ポリエステル微粒子中および/または結晶性ポリエステル微粒子上のシリカの位置は、シリカ注入結晶性ポリエステル微粒子の調製方法に基づいて決定されてもよい。シリカは、ポリエステルに対して比較的良好な親和性を有するが、凝固における問題が生じる可能性があるので、ポリエステル中のシリカ粒子の分散性は劣る可能性があり、それは粒子の表面上に粗い突起の形成をもたらし得る。特定の実施形態では、本明細書に開示されるシリカ注入結晶性ポリエステル微粒子は、結晶性樹脂中および/または結晶性樹脂上にシリカナノ粒子の実質的に均一な分散性を有する。
フマル酸、および25モル%の1,4−ブタンジオールと75モル%の1,6−ヘキサンジオールとの混合物を用いて不飽和結晶性ポリエステルを調製した。機械式撹拌機、蒸留装置、および底部排出バルブを備えた2リットルのBuchi反応器に、フマル酸(479.5グラム)、1,4−ブタンジオール(94.6グラム)、および1,6−ヘキサンジオール(375.5グラム)を入れた。混合物を窒素下で1時間かけて165℃に加熱した。バッチ温度が120℃に達したときに撹拌を開始した。次にバッチ温度が191℃に達するまで反応温度を毎分0.5℃上昇させた。粘度測定は、ブルックフィールド粘度計を用いて120℃(100rpm)で行い、次いで粘度が170Paに達するまで定期的にサンプリングした。反応混合物を金属容器に排出し、一晩室温に冷却させた。
本明細書に開示される実施形態に従って、4つの異なるバッチのシリカ注入結晶性微粒子を調製した。
焼結能力についての粒子の試験を、選択的レーザ焼結(SLS)に基づくSharebot SnowWhiteプリンタを使用して行った。このプリンタは、CADのデジタルファイルから製造される3次元オブジェクトへと作製される熱可塑性粉末を使用する。ポリマー粉末は、同時に焼結されて薄い層に融合されてもよく、これは、優れた鮮明度を有する小さい物体の構築を可能にする。このプリンタは、CO2レーザを使用しており、ナイロンなどの様々な粉末を焼結することができる。
Claims (20)
- 粉末組成物であって、
少なくとも1つの結晶性ポリエステル樹脂と、前記粒子の総重量に対して約5重量%〜約60重量%の範囲の量で前記粒子中に存在するシリカナノ粒子と、を含む、レーザ焼結用シリカ注入結晶性ポリエステル粒子を含む、粉末組成物。 - 前記シリカナノ粒子は、前記粒子の総重量に対して約10重量%〜約30重量%の範囲の量で前記粒子中に存在する、請求項1に記載の粉末組成物。
- 前記結晶性ポリエステル樹脂は、少なくとも1つの有機二塩基酸および少なくとも1つのポリオールから誘導される不飽和結晶性ポリエステル樹脂である、請求項1に記載の粉末組成物。
- 前記少なくとも1つのポリオールは、1,4−ブタンジオールと1,6−ヘキサンジオールとの混合物である、請求項3に記載の粉末組成物。
- 前記少なくとも1つの有機二塩基酸は、フマル酸である、請求項3に記載の粉末組成物。
- 前記シリカ注入結晶性ポリエステル粒子は、約5ミクロン〜約500ミクロンの範囲の体積平均粒径を有する、請求項1に記載の粉末組成物。
- 前記シリカ注入結晶性ポリエステル粒子は、約30ミクロン〜約50ミクロンの範囲の体積平均粒径を有する、請求項1に記載の粉末組成物。
- 前記シリカ注入結晶性ポリエステル粒子の溶融温度(Tm)は、約50℃〜約100℃の範囲にある、請求項1に記載の粉末組成物。
- レーザ焼結用シリカ注入結晶性ポリエステル粒子の製造方法であって、
有機溶媒に溶解された結晶性ポリエステル樹脂およびポリマー安定剤を含む溶液を調製することと、
前記溶液に、水溶性ポリマーの水溶液、およびシリカナノ粒子を添加することと、
シリカ注入結晶性ポリエステル粒子を沈殿させることと、を含む、方法。 - 前記シリカナノ粒子を前記溶液に添加する前に、前記水溶性ポリマーの水溶液を前記溶液に添加する、請求項9に記載の方法。
- 前記水溶性ポリマーは、ポリビニルアルコールである、請求項9に記載の方法。
- 前記溶液に少なくとも1つの熱開始剤を添加することをさらに含む、請求項9に記載の方法。
- 前記ポリマー安定剤は、ポリビニルアルコールである、請求項9に記載の方法。
- 前記結晶性ポリエステル樹脂および前記ポリマー安定剤は、約80℃〜約100℃の範囲の温度で前記有機溶媒に溶解される、請求項9に記載の方法。
- 前記シリカナノ粒子は、前記シリカナノ粒子が、前記粒子の総重量に対して約10重量%〜約60重量%の範囲の量で前記シリカ注入結晶性ポリエステル粒子中に存在するような量で、前記溶液に添加される、請求項9に記載の方法。
- レーザ焼結用シリカ注入結晶性ポリエステル粒子の製造方法であって、
有機溶媒に溶解された結晶性ポリエステル樹脂、シリカナノ粒子、およびポリマー安定剤を含む溶液を調製することと、
前記溶液に水溶性ポリマーの水溶液を添加することと、
シリカ注入結晶性ポリエステル粒子を沈殿させることと、を含む、方法。 - 前記水溶性ポリマーは、ポリビニルアルコールである、請求項16に記載の方法。
- 前記溶液に少なくとも1つの熱開始剤を添加することをさらに含む、請求項16に記載の方法。
- 前記結晶性ポリエステル樹脂、前記シリカナノ粒子、および前記ポリマー安定剤は、約80℃〜約100℃の範囲の温度で有機溶媒に溶解される、請求項16に記載の方法。
- 前記シリカナノ粒子は、前記シリカナノ粒子が、前記粒子の総重量に対して約10重量%〜約60重量%の範囲の量で前記粒子中に存在するような量で、前記溶液に添加される、請求項16に記載の方法。
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