JP6994638B2 - 3d印刷用供給原料およびその使用 - Google Patents
3d印刷用供給原料およびその使用 Download PDFInfo
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- JP6994638B2 JP6994638B2 JP2018518446A JP2018518446A JP6994638B2 JP 6994638 B2 JP6994638 B2 JP 6994638B2 JP 2018518446 A JP2018518446 A JP 2018518446A JP 2018518446 A JP2018518446 A JP 2018518446A JP 6994638 B2 JP6994638 B2 JP 6994638B2
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- acid
- printing
- suspension
- tcp
- fatty acids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/0003—Making bridge-work, inlays, implants or the like
- A61C13/0006—Production methods
- A61C13/0013—Production methods using stereolithographic techniques
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/58—Materials at least partially resorbable by the body
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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- B29C64/165—Processes of additive manufacturing using a combination of solid and fluid materials, e.g. a powder selectively bound by a liquid binder, catalyst, inhibitor or energy absorber
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B29C64/188—Processes of additive manufacturing involving additional operations performed on the added layers, e.g. smoothing, grinding or thickness control
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- 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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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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Description
-3D印刷機における押出圧力および/またはノズル断面を小さくすることができる。
-粒子間の潤滑性を高めることができ、それにより、粒子間摩擦が低減され、懸濁液の粘度が低下し、低い押出圧力および小さいノズルでも固体の含有量が高い供給原料を使用することができる。
-粒子との結合が優れていることから、加圧時に粒子懸濁液から液体のみが押し出されて粉末が乾燥し、印刷不可能となることを防ぐことができる。
-水を含まなくてよい。水は、金属粒子の酸化や、セラミック粒子の水和や硬化といった様々な化学反応における良好な媒体であることから、水は問題となることがある。
-揮発性有機化合物(VOC)を含まなくてよい。
-焼結時にインクが保護ガスおよび/または還元性ガスを発生しうるので、高価な焼結装置を使用する必要がない。
ならびに/または
-液相は、水素、炭素および酸素のみを含有していてもよい。
-液相は、室温では固体、高温域では液体であってもよい。このような性質により、懸濁液は加熱されると印刷が可能となり、堆積後、例えば室温での固化が可能である。
-供給原料は、生体適合性化合物および/または人体に通常存在する化合物のみを含有していてもよい。多くの一般的なインクは、非生体適合性化合物を使用しているため、このような化合物を燃焼により除去した後、得られた造形物を使用することになるが、本発明のインクは、液体の状態であっても固体の状態であっても、液相を含んだまま医療目的で使用することができる。
-少なくとも1つの(懸濁された)セラミック材料および/または(懸濁された)金属材料および/または(懸濁された)ポリマー材料および/または(懸濁された)炭素含有材料を、懸濁液の全重量の50~95重量%(w/w)含み、かつ
-1以上の脂肪酸またはその誘導体、好ましくは飽和脂肪酸を、懸濁液の全重量の少なくとも3重量%、好ましくは少なくとも4重量%、さらに好ましくは少なくとも5重量%含む
懸濁液に関する。
a)本発明の懸濁液を提供する工程;
b)前記懸濁液を供給原料として使用して、3次元物体を3D印刷または押出成形する工程;ならびに
c)任意選択で、3D印刷または押出成形した物体を、例えば、焼結、水和、コーティング、溶融、浸漬、凍結、結晶化、析出および/または架橋からなる群より選択される方法により固化させる工程
を含む、3次元物体を3D印刷または押出成形する方法を提供することである。
上述した通り、本発明は、特に、3D印刷方法または押出成形方法において優れた特性を有する懸濁液に関する。したがって、一態様において、本発明は、
-少なくとも1つの金属材料および/またはセラミック材料および/またはポリマー材料および/または固形の炭素含有材料を、懸濁液の全重量の50~95重量%(w/w)含み、かつ
-1以上の脂肪酸またはその誘導体、好ましくは飽和脂肪酸を、懸濁液の全重量の少なくとも3重量%、好ましくは少なくとも4重量%、さらに好ましくは少なくとも5重量%含む
懸濁液に関する。
本明細書において、脂肪酸またはその誘導体は、1以上の疎水性炭化水素と結合している1以上の遊離カルボン酸、遊離スルホン酸または遊離ホスホン酸として理解されるものであり、該疎水性炭化水素は、脂肪族または芳香族であってもよく、また、それらの混合物であってもよい。天然脂肪酸は種々存在するが、一般的には、飽和または不飽和のアルキル基と結合しているカルボン酸であり、該アルキル基は非分岐鎖状、すなわち、直鎖状であってもよく、分岐鎖状であってもよい。その他の合成または天然の両親媒性物質を用いてもよく、このような両親媒性物質には、例えば芳香族基および/または環状の脂肪族基と結合している酸が含まれる。
で示される化合物である。
本発明の一実施形態において、「材料」という用語は、固形材料または該固形材料の粉末に関する。当然のことながら、本発明の懸濁液に含まれる材料は、その大部分が懸濁液中に懸濁された形態で存在している。本発明の懸濁液中の材料は、その大部分が懸濁液中で懸濁された状態を保てるような粒径を有しており、例えば、1nm~1mmの粒径を有している。懸濁液中の材料の粒径のより詳細な数値は、各材料によって異なる。
金属材料の印刷に関して言えば、様々な金属が本発明の懸濁液の一部となりうる。したがって、一実施形態において、前記金属材料は、銅、亜鉛、アルミニウム、鉄、銀、金、パラジウム、プラチナ、スズ、アンチモン、ビスマス、鉛、ニッケル、コバルト、バナジウム、マンガン、クロム、チタン、タンタル、タングステン、ネオジム、リチウム、ナトリウム、オスミウム、イリジウム、ウラン、トリウム、プルトニウム、イットリウム、ジルコニウム、ニオブ、モリブデン、ロジウム、カドミウム、ハフニウム、レニウム、水銀、ガリウム、インジウム、タリウム、ランタン、セリウム、プラセオジム、プロメチウム、サマリウム、ユーロピウム、ガドリニウム、テルビウム、ジスプロシウム、ホルミウム、エルビウム、ツリウム、イッテルビウム、ルテチウム、カリウム、カルシウム、マグネシウム、ストロンチウム、バリウム、ゲルマニウム、ヒ素、アスタチン、ならびにこれらの合金および水素化物からなる群より選択される。実施例3に、銅を印刷する例を示し、実施例6に、銀を印刷する例を示し、実施例7に、銅と鋼鉄を印刷する例を示す。
本明細書において、「セラミック材料」は、金属元素および非金属元素からなる化合物から作られた無機質の非金属材料である。セラミック材料の印刷に関して言えば、様々なセラミックが本発明の懸濁液の一部となりうる。したがって、一実施形態において、前記セラミック材料は、TCP(リン酸三カルシウム)、MCP(リン酸一カルシウム)、DCP(リン酸二カルシウム)、リン酸四カルシウム、ハイドロキシアパタイト、α-TCP、β-TCP、酸化チタン(チタニア)、酸化アルミニウム(アルミナ)、酸化ジルコニウム(ジルコニア)、酸化イットリウム(イットリア)、イットリア安定化ジルコニア、酸化インジウム、酸化インジウムスズ、窒化ホウ素、炭化ケイ素、炭化ホウ素、炭化タングステン、酸化ベリリウム、ゼオライト、酸化セリウム(セリア)、二ケイ化タングステン、ケイ化ナトリウム、ケイ化白金、窒化ジルコニウム、窒化タングステン、窒化バナジウム、窒化タンタル、窒化ニオブ、ホウ化ケイ素、クレー、土(earth)、土壌、セメント、ポルトランドセメント、シリカ、チタン酸バリウム、チタン酸ジルコン酸鉛(lead zirconate titanium)、酸化亜鉛、ニオブ酸カリウム、ニオブ酸リチウム、タングステン酸ナトリウム、ガラス、ジオポリマー、塩化ナトリウム、硝酸ナトリウム、硝酸カリウム、塩化カリウム、塩化マグネシウム、塩化カルシウム、硝酸カルシウム、硝酸マグネシウム、酸化ストロンチウム、リン酸ストロンチウム、硫酸カルシウム、硫酸バリウム、炭酸カルシウム、炭酸ナトリウム、フッ化ナトリウムおよびこれらの混合物からなる群より選択される。実施例1および2に、本発明の懸濁液を用いて、種々のセラミックを印刷する例を示す。
ポリマー材料の印刷に関して言えば、様々なポリマーが本発明の懸濁液の一部となりうる。したがって、一実施形態において、前記ポリマー材料は、ポリ乳酸(PLA)、ポリカプロラクトン(PCL)、ポリグリコール酸(PGA)、ポリスチレン(PS)、ポリエチレン(PE)、ポリプロピレン(PP)、ポリカーボネート(PC)、ポリ(メチルメタクリレート)(PMMA)、ポリ(1,4-フェニレンスルフィド)(PPS)、ポリ(2,6-ジメチル-1,4-フェニレンオキシド)(PPO)、ポリアミド(PA)、ポリブチレンテレフタレート(PBT)、ポリエーテルエーテルケトン(PEEK)、ポリエーテルケトン(PEK)、ポリエチレンテレフタレート(PET)、ポリイミド(PI)、ポリオキシメチレン(POM)、ポリスルホン(PSU)、ポリウレタン(PU)、ポリブタジエン(PB)、ポリテトラフルオロエチレン(PTFE)、ポリフッ化ビニル(PVF)、ポリフッ化ビニリデン(PVDF)、ポリクロロトリフルオロエチレン(PCTFE)、ペルフルオロアルコキシポリマー(PFA)、フッ化エチレン-プロピレン(FEP)、ポリエチレンテトラフルオロエチレン(ETFE)、ポリエチレンクロロトリフルオロエチレン(ECTFE)、ポリエチレングリコール(PEG)、ポリヒドロキシアルカン酸(PHA)、ポリヒドロキシ吉草酸(PHV)、ポリヒドロキシ酪酸(PHB)、液晶ポリマー、ポリアクリレート、ポリアセタール、ポリアミドイミド(PAI)、ポリブチレン(PB)、ポリ塩化ビニル(PVC)、アクリロニトリルブタジエンスチレン(ABS)、ポリフェニルスルホン(PPSU)、ポリメチルペンタン(PMP)、アルギナート、キチン、キトサン、アクリル酸、ヒアルロン酸、デンプン、アミロース、アミロペクチン、ペクチン、デキストラン、プルラン、アラビアゴム、キサンタンガム、プルラン、セルロース、エラスチン、コラーゲン、ゼラチン、フィブロネクチン、絹、多糖、タンパク質、核酸、ゴム、シリコーンおよびこれらのコポリマーからなる群より選択される。
炭素含有材料の印刷に関して言えば、様々な分子が本発明の懸濁液の一部となりうる。したがって、一実施形態において、前記炭素含有材料は、黒鉛、グラフェン、カーボンナノチューブなどの炭素同素体;グルコース、スクロース、クエン酸、シュウ酸;ペニシリン、テトラサイクリンなどの抗生物質;鎮痛薬、鎮痛剤、ビタミン、ステロイド、ホルモン、化学療法剤などの薬物および製剤;ならびにこれらの混合物;ならびにヒト、動物、細胞培養物などの生物に由来する骨基質、脱水した骨基質および脱細胞化骨基質などの複雑な天然組成物からなる群より選択される。実施例6に、黒鉛を印刷する例を示す。
以上および後述の実施例に記載の通り、本発明の懸濁液は、特に3D印刷方法に適している。したがって、本発明の一態様は、3D印刷方法または押出成形方法における、好ましくは3D印刷方法における本発明の懸濁液の使用に関する。別の言い方をすれば、さらに別の一態様において、本発明は、3D印刷機用または押出成形機用の供給原料、インク、堆積される材料または押出成形される材料としての本発明の懸濁液の使用に関する。
-少なくとも1つのセラミック材料および/または金属材料および/またはポリマー材料および/または黒鉛などの炭素含有材料を、懸濁液の全重量の50~95重量%(w/w)含み、かつ
-1以上の脂肪酸またはその誘導体を、懸濁液の全重量の少なくとも5重量%(w/w)含む
懸濁液の、3D印刷方法または押出成形方法における使用に関する。
本発明は、本発明の懸濁液を用いて、3次元物体を製造する方法にも関する。したがって、一態様において、本発明は、3次元物体を3D印刷または押出成形する方法であって、
a)本発明の懸濁液を提供する工程;
b)前記懸濁液を供給原料として使用して、3次元物体を3D印刷または押出成形する工程;ならびに
c)任意選択で、3D印刷または押出成形した物体を、例えば、焼結、水和、コーティング、溶融、浸漬、凍結、結晶化、析出および/または架橋からなる群より選択される方法により固化させる工程
を含む方法に関する。
a)-少なくとも1つのセラミック材料および/または金属材料および/またはポリマー材料および/または黒鉛などの炭素含有材料を、懸濁液の全重量の50~95重量%(w/w)含み、かつ
-1以上の脂肪酸またはその誘導体を、懸濁液の全重量の少なくとも5重量%(w/w)含む
懸濁液を提供する工程;
b)前記懸濁液を供給原料として使用して、所望の3次元物体を3D印刷または押出成形する工程;ならびに
c)任意選択で、3D印刷または押出成形により得られた物体を、焼結、水和、コーティング、溶融、浸漬および/または架橋からなる群より選択される方法により固化させる工程
を含む方法に関する。好ましくは、焼結工程が含まれる。
さらに別の一態様において、本発明は、本発明の方法により得られた/得られる、3D印刷または押出成形された3次元物体に関する。
本発明は、種々の製品の組み合わせとして定義されるものであってもよい。
-3D印刷機;および
-本発明の懸濁液
を含むキットに関する。
-3D印刷機;および
-本発明の懸濁液を供給原料として用いて3次元物体を印刷するための取扱説明書
を含むキットに関する。
-本発明の懸濁液;および
-該懸濁液を供給原料として用いて3次元物体を印刷するための取扱説明書
を含むキットに関する。
-本発明に係る1以上の脂肪酸;および
-3D印刷機用または押出成形機用の供給原料として使用される本発明の懸濁液を調製するために、前記1以上の脂肪酸を使用するための取扱説明書
を含むキットに関する。
-本発明に係る1以上の材料;および
-3D印刷機用または押出成形機用の供給原料として使用される本発明の懸濁液を調製するために、前記1以上の材料を使用するための取扱説明書
を含むキットに関する。
固形材料としてリン酸三カルシウム(TCP)を用い、以下のインク/供給原料を調製した。
11. 15g(75%w/w)のTCPと5g(25%w/w)のグリセリン
12. 15g(75%w/w)のTCPと5g(25%w/w)のラノリン
13. 15g(75%w/w)のTCPと5g(25%w/w)のタラ油
14. 15g(75%w/w)のTCPと5g(25%w/w)のオレイン酸
15. 20g(80%w/w)のTCPと5g(20%w/w)のオレイン酸
16. 25g(83.3%w/w)のTCPと5g(16.7%w/w)のオレイン酸
以下のインク/供給原料を調製し、19:1ギア減速機と1mm径のノズルとを有するEMO-25ディスペンサーを備えたHyrel System 30M 3D印刷機を用いて、以下の印刷結果を得た。
1. 26g(83.9%w/w)のTCP+5g(16.1%w/w)のリノール酸:良好に印刷された。
2. 25g(83.3%w/w)のTCP+5g(16.7%w/w)のオレイン酸:良好に印刷された。
3. 21gのTCP+5gのオレイルアルコール:印刷は不可能で、液相が流出した。
4. 23gのTCP+5gのオレイルアルコール:印刷は不可能で、液相が流出した。
5. 25g(83.3%w/w)のTCP+5g(16.7%w/w)のオレイルアルコール:印刷は不可能で、液相が流出した。
6. 26gのTCP+5gのオレイルアルコール:印刷は不可能で、液相が流出した。
7. 20gのTCP+5gのオレイン酸メチル:印刷は不可能で、加圧下で硬化した。
8. 22gのTCP+5gのオレイン酸メチル:印刷は不可能で、加圧下で硬化した。
9. 23gのTCP+5gのオレイン酸メチル:印刷は不可能で、加圧下で硬化した。
10. 25g(83.3%w/w)のTCP+5g(16.7%w/w)のオレイン酸メチル:印刷は不可能で、加圧下で硬化した。
11. 35gのTCP+15gの水:ノズルから水滴が垂れて、均一に印刷されなかった。
12. 15gのTCP+15gの水+1.25gのHEC(実施例1のインク9と同じ):印刷可能であった。
13. 25g(83.3%w/w)のTCP+5g(16.7%w/w)のステアリン酸:加熱すると、印刷可能であり、室温で固体であった。
14. 25g(78.1%)のTCP+7g(21.9%)のナフテン酸:印刷可能であった。
15.27g(81.8%)のTCP+6g(18.2%)のオクタン酸:印刷可能であった。
-オレイルアルコールまたはオレイン酸メチルを用いた組み合わせはいずれも印刷不可能であり、アルコール基またはエステル基は酸性基の代わりにはならないことが明らかであることから、酸性基は本印刷方法において必須である。
-オレイン酸、リノール酸などの天然長鎖脂肪酸、オクタン酸などの天然短鎖脂肪酸のみならず、ナフテン酸などの合成分岐鎖状脂肪酸も使用することができることから、酸性基および疎水性炭化水素が必須の特徴であることが示唆される。
以下の銅/オレイン酸インクを調製し、19:1ギア減速機と1mm径のノズルとを有するEMO-25ディスペンサーを備えたHyrel System 30M 3D印刷機を用いて印刷した。
1. 27g(84.3%w/w)の銅+5g(15.6%w/w)のオレイン酸:良好に印刷された。図5を参照。
ステアリン酸(5g)およびTCP(25g)(平均粒度:1~5μm)から多孔性シートを3D印刷し、得られたシートを分割して多孔性インプラントを得た。得られたインプラントを焼結させて、これに、テロメラーゼにより不死化したヒト間葉系幹細胞(eGFP+)を100,000個、またはテロメラーゼにより不死化したヒト間葉系幹細胞(eGFP-)を200,000個播種した。2日間培養した後、一部は、骨芽細胞分化培地で培養した。焼結プロセスおよび得られたインプラントの特性を、走査電子顕微鏡法(図6)、機械的試験(図7)、ラマン分光法およびラマンイメージング(図8)、顕微鏡法(図9)、マイクロコンピューター断層撮影、生存率アッセイおよびアルカリホスファターゼ分泌アッセイ(図10)、ならびにコラーゲンおよびタンパク質の沈着(図11)により明らかにした。
乳鉢と乳棒を用いて、焼結スキャフォールド(実施例4のものと同一)および非焼結スキャフォールドを不均一な粒状に粉砕し、この粉末材料40mgを、先端をカットした1mLのシリンジに入れて、シリンジ開口部を綿で塞ぎ、シリンジを120℃でオートクレーブ滅菌した。このシリンジは、施術に使用する直前まで乾燥した状態で保存し、使用時に200μL生理食塩水を加えた。シリンジに充填された粉末を、NOD-SCIDマウスの背部の皮下ポケットに注入した。各マウスには、それぞれ4つのポケットが設けられ、それぞれのポケットに同一のインプラントが注入された。
ステアリン酸と銀粉末(5gのSA:40gの銀)、またはステアリン酸と黒鉛粉末(20gのSA:25gの黒鉛)を混合し、これらの混合物を堆積させて、単純回路、矩形電極(20mm×30mm×2mm)、または直線状線材(長さ20mm、幅2mm)を作製した(図14)。
ステアリン酸と銅(5gのSA:50gの銅)、またはステアリン酸と鋼鉄(15gのSA:100gの鋼鉄)を混合、加熱し、面上に堆積させて造形物を作製した(図16)。
ステアリン酸とTCP(平均粒度:1~5μm)(5g:25g)を混合し、棒材を鋳造した。この棒材を、標準的なグルーガンに装填し、面上に手動で堆積させた(図17)。
Claims (14)
- 3次元物体を3D印刷する方法であって、
a)-少なくとも1つのセラミック材料を、懸濁液の全重量の50~95重量%(w/w)含み、かつ
-1以上の脂肪酸を、懸濁液の全重量の少なくとも5重量%(w/w)含む
懸濁液を提供する工程;
b)前記懸濁液を供給原料として使用して、所望の3次元物体を3D印刷する工程;ならびに
c)任意選択で、3D印刷により得られた物体を、焼結、水和、コーティング、溶融、浸漬および/または架橋からなる群より選択される方法により固化させる工程
を含み、
前記1以上の脂肪酸が、1以上の疎水性炭化水素と結合している1以上の遊離カルボン酸であって、少なくとも1つのC5-C30炭化水素と結合している、カルボン酸基を含む方法。 - 前記セラミック材料が、TCP(リン酸三カルシウム)、MCP(リン酸一カルシウム)、DCP(リン酸二カルシウム)、リン酸四カルシウム、ハイドロキシアパタイト、α-TCP、β-TCP、酸化チタン(チタニア)、酸化アルミニウム(アルミナ)、酸化ジルコニウム(ジルコニア)、酸化イットリウム(イットリア)、イットリア安定化ジルコニア、酸化インジウム、酸化インジウムスズ、窒化ホウ素、炭化ケイ素、炭化ホウ素、炭化タングステン、酸化ベリリウム、ゼオライト、酸化セリウム(セリア)、二ケイ化タングステン、ケイ化ナトリウム、ケイ化白金、窒化ジルコニウム、窒化タングステン、窒化バナジウム、窒化タンタル、窒化ニオブ、ホウ化ケイ素、クレー、土(earth)、土壌、セメント、ポルトランドセメント、シリカ、チタン酸バリウム、チタン酸ジルコン酸鉛(lead zirconate titanium)、酸化亜鉛、ニオブ酸カリウム、ニオブ酸リチウム、タングステン酸ナトリウム、ガラス、ジオポリマー、塩化ナトリウム、硝酸ナトリウム、硝酸カリウム、塩化カリウム、塩化マグネシウム、塩化カルシウム、硝酸カルシウム、硝酸マグネシウム、酸化ストロンチウム、リン酸ストロンチウム、硫酸カルシウム、硫酸バリウム、炭酸カルシウム、炭酸ナトリウム、フッ化ナトリウムおよびこれらの混合物からなる群より選択される、請求項1に記載の方法。
- 前記セラミック材料の粒径が、1nm~1mmの範囲、例えば、500μm未満、354μm未満、250μm未満、149μm未満、105μm未満、74μm未満、44μm未満、10μm未満、1μm未満、500nm未満または100nm未満であり、好ましくは10μm未満である請求項1又は2に記載の方法。
- 前記少なくとも1つのセラミック材料を、懸濁液の全重量の60~95%(w/w)の範囲で含み、例えば60~95%、例えば70~95%、例えば80~95%、例えば85~95%、例えば90~95%、例えば80~85%、例えば80~84%、例えば80~83%、例えば80~82%、例えば81~85%、例えば82~85%または例えば83~85%含む、請求項1~3のいずれかに記載の方法。
- 前記1以上の脂肪酸が、カプリル酸、カプリン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキジン酸、ベヘン酸、リグノセリン酸、セロチン酸、ミリストレイン酸、パルミトレイン酸、サピエン酸、オレイン酸、エライジン酸、バクセン酸、リノール酸、リノレライド酸、α-リノレン酸、アラキドン酸、イコサペンタエン酸、エルカ酸およびドコサヘキサエン酸からなる群より選択され、好ましくはステアリン酸である、請求項1~4のいずれかに記載の方法。
- 前記懸濁液が、脂肪酸を、懸濁液の全重量の5~50%の範囲で含み、例えば10~50%の範囲で、例えば10~40%の範囲で、例えば10~30%、例えば12~30%、例えば15~30%、例えば15~20%、例えば15~18%または例えば15~17%含む、請求項1~5のいずれかに記載の方法。
- 80~85%(w/w)のセラミック材料と15~20%(w/w)の遊離脂肪酸との混合物を含み、例えば、80~85%(w/w)のTCPと15~20%(w/w)のオレイン酸との混合物、80~85%(w/w)のTCPと15~20%(w/w)のリノール酸との混合物、または80~85%(w/w)のTCPと15~20%(w/w)のステアリン酸との混合物を含む、請求項1~6のいずれかに記載の方法。
- 前記セラミック材料が、生体適合性を有する、請求項1~7のいずれかに記載の方法。
- 前記セラミック材料が、生分解性を有する、請求項1~8のいずれかに記載の方法。
- 前記物体が、骨インプラントまたは歯科インプラントなどの医療用インプラントである、請求項1~9のいずれかに記載の方法。
- -少なくとも1つのセラミック材料を、懸濁液の全重量の50~95重量%(w/w)含み、かつ
-1以上の脂肪酸を、懸濁液の全重量の少なくとも5重量%(w/w)含み、
前記1以上の脂肪酸が、1以上の疎水性炭化水素と結合している1以上の遊離カルボン酸であって、少なくとも1つのC5-C30炭化水素と結合している、カルボン酸基を含む懸濁液の、3D印刷方法における使用。 - 前記3D印刷方法が、ロボキャスティング、直接インク書き込み法、インクジェット印刷、バインダージェット法、選択的加熱焼結、選択的レーザー焼結、選択的レーザー溶融、光造形法、フィラメント印刷、ペレット印刷、粉体印刷、自由形状造形法、ラピッドプロトタイピングおよびロボットアーム式堆積法からなる群より選択される、請求項11に記載の使用。
- 前記3D印刷方法が、ロボキャスティング、直接インク書き込み法、インクジェット印刷、光造形法、フィラメント印刷、ペレット印刷、およびロボットアーム式堆積法からなる群より選択される請求項1に記載の方法又は請求項11に記載の使用。
- 前記3D印刷方法が、ロボキャスティングおよび直接インク書き込み法からなる群より選択される請求項1に記載の方法又は請求項11に記載の使用。
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