JP2009531260A - 3次元形状セラミック体を製造するためのプロセスおよび装置 - Google Patents
3次元形状セラミック体を製造するためのプロセスおよび装置 Download PDFInfo
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- JP2009531260A JP2009531260A JP2009501930A JP2009501930A JP2009531260A JP 2009531260 A JP2009531260 A JP 2009531260A JP 2009501930 A JP2009501930 A JP 2009501930A JP 2009501930 A JP2009501930 A JP 2009501930A JP 2009531260 A JP2009531260 A JP 2009531260A
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/606—Drying
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
Abstract
【解決手段】支持材上で所望の2次元形状においてインクジェットプリンターを用いて、成形したセラミック体を形成するために必要とされる成分を含む懸濁液を層毎に印刷し、形成された複合層を乾燥および硬化することによって、3次元形状セラミック体を製造するためのプロセスであって、このプロセスは、水性ベーマイトゾル、少なくとも1つの低分子量アルコール、少なくとも1つの乾燥抑制剤、および少なくとも1つの有機流動化剤を含む分散媒中に50重量%〜80重量%のセラミック粒子を含む懸濁液を用いて印刷が達成されることを特徴とし、またこのプロセスを実施するための装置も記載する。
【選択図】なし
Description
本発明に従う分散媒に使用されるベーマイトゾルを作製するために、700mlの水を、65%濃度の硝酸に加えてpH2に調製した。その混合物を80℃に加熱し、2.1gのベーマイト(Sasol、Hamburgから得られるDispersal P2)を加え、この混合物を10分間、攪拌する。その混合物を室温まで冷やし、25%濃度のアンモニアをpH8.5になるまで加え、得た水性ベーマイトゾルをポリエチレンボトル中に保存する。
Claims (38)
- 支持材上で所望の2次元形状においてインクジェットプリンターを用いて、成形したセラミック体を形成するために必要とされる成分を含む懸濁液を層毎に印刷し、形成された複合層を乾燥および硬化することによって、3次元形状セラミック体を製造するためのプロセスであって、該プロセスは、水性ベーマイトゾル、少なくとも1つの低分子量アルコール、少なくとも1つの乾燥抑制剤および少なくとも1つの有機流動化剤を含む分散媒に50重量%〜80重量%のセラミック粒子を含む懸濁液を使用することによって、印刷が達成されることを特徴とする、プロセス。
- 前記ベーマイトゾルが、0.0001重量%〜2重量%、好ましくは0.001重量%〜1重量%、より好ましくは0.01重量%〜0.5重量%の固形成分含有量を有することを特徴とする、請求項1に記載のプロセス。
- 前記ベーマイトゾルが、微小結晶性ベーマイト粒子および溶解アルミニウム水和物を含むことを特徴とする、請求項1または2に記載のプロセス。
- 前記微小結晶性ベーマイト粒子が、3nm〜20nm、好ましくは4nm〜5nmの粒子サイズを有することを特徴とする、請求項1〜3のいずれか1項に記載のプロセス。
- 前記微小結晶性ベーマイト粒子が、1.4:1〜2.2:1の長さ対幅の比を有することを特徴とする、請求項1〜4のいずれか1項に記載のプロセス。
- 前記ベーマイトゾルが、溶解アルミニウム水和物として[Al(H2O)6]3+、[Al(H2O)5OH]2+、[Al(H2O)4(OH)2]+、Al(OH)3(aq)、[Al(OH)4]−および/またはAl13イオンを含むことを特徴とする、請求項1〜5のいずれか1項に記載のプロセス。
- 前記ベーマイトゾルが、1.7〜11のpHを有することを特徴とする、請求項1〜6のいずれか1項に記載のプロセス。
- 前記分散媒が、48重量%〜88重量%のベーマイトゾル、5重量%〜20重量%の低分子量アルコール、5重量%〜20重量%の乾燥抑制剤および2重量%〜12重量%の有機流動化剤を含むことを特徴とする、請求項1〜7のうちの少なくとも1項に記載のプロセス。
- 前記分散媒が、低分子量アルコールとしてメタノール、エタノール、プロパノール、イソプロパノールまたはそれらの混合物、乾燥抑制剤として多価アルコール、長鎖炭化水素またはそれらの混合物、ならびに有機流動化剤として合成有機高分子電解質および/またはカルボン酸調製物を含むことを特徴とする、請求項8に記載のプロセス。
- 前記分散媒が、多価アルコールとしてグリセロールおよび/またはエチレングリコールを含むことを特徴とする、請求項9に記載のプロセス。
- 前記分散媒が、合成有機高分子電解質として、好ましくはアルカリ金属またはアンモニウム塩の形態で、4000〜6000の重量平均分子量を有するポリアクリル酸および/またはポリメタクリル酸を含むことを特徴とする、請求項9に記載のプロセス。
- 前記分散媒が、62重量%〜91重量%のベーマイトゾル、5重量%〜15重量%のエタノール、2重量%〜15重量%のグリセロールおよび/またはエチレングリコールならびに2重量%〜8重量%の有機流動化剤を含むことを特徴とする、請求項1〜11のいずれか1項に記載のプロセス。
- 前記セラミック粒子が、純粋なAl2O3、純粋なZrO2、純粋なAl2O3−ZrO2、純粋なSi3N4、ベーマイトで安定化したAl2O3、Y2O3、HfO2、CeO2、MgOおよび/またはCaOで安定化したZrO2、Y2O3、HfO2、CeO2、MgOおよび/またはCaOで安定化したAl2O3−ZrO2、Al2O3、Y2O3、Fe2O3および/またはさらなる希土酸化物で安定化したSi3N4、あるいはそれらの混合物を含むことを特徴とする、請求項1〜12のうちの少なくとも1項に記載のプロセス。
- Y2O3、HfO2、CeO2、MgOおよび/またはCaOで安定化することができるAl2O3−ZrO2混合セラミックが、30重量%〜70重量%のAl2O3およびそれに対応して70重量%〜30重量%のZrO2を含むことを特徴とする、請求項13に記載のプロセス。
- 前記セラミック粒子が、前記懸濁液中に60重量%〜70重量%の量で存在することを特徴とする、請求項1〜14のいずれか1項に記載のプロセス。
- 前記セラミック粒子の粒子サイズが、印刷ヘッドノズルの開口部およびフィードラインより小さく、そして0.01μm〜3μmのd90の範囲内であることを特徴とする、請求項1〜15のいずれか1項に記載のプロセス。
- 前記懸濁液が、4〜11、好ましくは7〜9のpH、ならびに25℃でγ>400の剪断速度にて5mPas〜25mPasおよびγ<50の低剪断速度にて100mPas〜500mPasの粘度を有することを特徴とする、請求項1〜16のうちの少なくとも1項に記載のプロセス。
- 前記層が、平面支持材上に印刷されることを特徴とする、請求項1〜17のうちの少なくとも1項に記載のプロセス。
- 前記層が、支持材として0%〜10%の開放気孔率を有する黒鉛板、プラチナ板、セラミックまたはガラスセラミック上に印刷されることを特徴とする、請求項18に記載のプロセス。
- 前記層が、支持材上に印刷され、該支持材上に、1つ以上の層が規定された寸法を有し、該1つ以上の層は、前記複合層を硬化する間に蒸発する前記分散媒中の材料を含む懸濁液を用いて既に印刷されており、該複合層を硬化する間に取り除くことができることを特徴とする、請求項1〜19のうちの少なくとも1項に記載のプロセス。
- 前記1つ以上の層が、規定された寸法を有し、前記複合層を硬化する間に取り除くことができ、該1つ以上の層は、該複合層を硬化する間に蒸発する前記分散媒中の材料を含む懸濁液を用いて、第1の印刷ヘッドにより印刷された層の上または間に、第2の印刷ヘッドによって印刷されることを特徴とする、請求項1〜20のうちの少なくとも1項に記載のプロセス。
- 200℃より高い温度で蒸発するか、または400℃より高い温度で酸素の存在下で熱分解する物質が、前記複合層を硬化する間に蒸発する材料として使用されることを特徴とする、請求項20または21に記載のプロセス。
- 前記印刷ヘッドのノズルが、前記1つ以上の層を印刷した後、水、低分子量アルコールおよび多価アルコールを含む洗浄液により洗浄されることを特徴とする、請求項1〜22のうちの少なくとも1項に記載のプロセス。
- (6〜10):(1〜4):(1〜3)、好ましくは8:1:1の水:エタノール:多価アルコールの重量比で、水、エタノールおよび少なくとも1つの多価アルコールの混合物が、洗浄液として使用されることを特徴とする、請求項23に記載のプロセス。
- 前記印刷ヘッドのノズルの洗浄は、前記洗浄液が前記ノズルおよびノズルのアンティチェンバーに浸透するように実施されることを特徴とする、請求項1〜24のうちの少なくとも1項に記載のプロセス。
- 前記ノズルおよびノズルのアンティチェンバーへの前記洗浄液の浸透が、前記懸濁液を含む圧力カートリッジ内の増大した外圧または減圧下で達成されることを特徴とする、請求項25に記載のプロセス。
- 前記印刷ヘッドのノズルの洗浄が、前記洗浄液で浸透される物体によって達成され、該物体は0.01N/mm2〜1N/mm2、好ましくは0.02N/mm2〜0.05N/mm2の接触圧でノズル領域において周期的に前記印刷ヘッド上に移動されることを特徴とする、請求項26に記載のプロセス。
- 前記印刷ヘッドのノズルの洗浄が、超音波の作動下で実施されることを特徴とする、請求項1〜27のうちの少なくとも1項に記載のプロセス。
- 前記印刷ヘッドのノズルの洗浄が、前記印刷カートリッジまたは前記印刷ヘッドにおける圧力サイクルの間に超音波の作動下で周期的に実施されることを特徴とする、請求項28に記載のプロセス。
- 前記印刷された層が、65℃〜105℃の温度で乾燥されることを特徴とする、請求項1〜29のうちの少なくとも1項に記載のプロセス。
- 各々の層が、印刷後に乾燥されることを特徴とする、請求項30に記載のプロセス。
- 適切な場合、液体の蒸気を取り除くように、ファン、減圧の付与または対流を用いて、65℃〜105℃、好ましくは68℃〜85℃の範囲の温度まで熱することによって、各々の印刷された層が、前記インクジェットプリンターの印刷領域において乾燥されることを特徴とする、請求項31に記載のプロセス。
- 前記熱することが、ハロゲンランプの照射、赤外線ランプの照射、イオン線照射、レーザー照射、または前記印刷領域に配置される加熱要素を用いて達成されることを特徴とする、請求項32に記載のプロセス。
- 前記セラミック材料の各々の印刷された層が、乾燥後、1μm〜30μm、好ましくは0.05μm〜10μmの厚さを有し、前記複合層を硬化する間に蒸発する前記材料の各々の印刷された層が、0.05μm〜5μmの厚さを有することを特徴とする、請求項1〜33のうちの少なくとも1項に記載のプロセス。
- 適切な場合、前記乾燥した複合層の硬化が、乾燥機中で約80℃での保存後、前記セラミック材料を焼結することによって達成されることを特徴とする、請求項1〜34のうちの少なくとも1項に記載のプロセス。
- 前記焼結が、800℃〜1500℃の温度で実施されることを特徴とする、請求項35に記載のプロセス。
- 前記焼結が、理論密度の100%、好ましくは理論密度の98%の焼結密度まで実施されることを特徴とする、請求項35または請求項36に記載のプロセス。
- 医療用セラミックプロテーゼ、特に身体、肢および頭部、顔、口腔、歯のインプラント、歯のインレー、歯冠ならびに歯のブリッジの領域におけるプロテーゼが、3次元形状セラミック体として製造されることを特徴とする、請求項1〜37のうちの少なくとも1項に記載のプロセス。
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DE102006015014A DE102006015014B4 (de) | 2006-03-31 | 2006-03-31 | Verfahren zur Herstellung dreidimensionaler keramischer Formkörper |
PCT/EP2007/002693 WO2007112885A1 (de) | 2006-03-31 | 2007-03-27 | Verfahren und vorrichtung zur herstellung dreidimensionaler keramischer formkörper |
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ES2349023T3 (es) | 2010-12-21 |
CN101415655B (zh) | 2013-05-29 |
DE102006015014B4 (de) | 2008-07-24 |
BRPI0710116B8 (pt) | 2021-07-27 |
EP2007698B1 (de) | 2010-07-14 |
EP2007698A1 (de) | 2008-12-31 |
DK2007698T3 (da) | 2010-11-08 |
HK1130764A1 (en) | 2010-01-08 |
WO2007112885A1 (de) | 2007-10-11 |
CN101415655A (zh) | 2009-04-22 |
US20100040767A1 (en) | 2010-02-18 |
ATE473950T1 (de) | 2010-07-15 |
DE102006015014A1 (de) | 2007-10-31 |
BRPI0710116B1 (pt) | 2017-12-12 |
US8409655B2 (en) | 2013-04-02 |
DE502007004399D1 (de) | 2010-08-26 |
BRPI0710116A2 (pt) | 2011-08-02 |
JP4886026B2 (ja) | 2012-02-29 |
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