JP5675767B2 - 熱交換器のための熱磁気成形体を製造するための印刷方法 - Google Patents
熱交換器のための熱磁気成形体を製造するための印刷方法 Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/10—Formation of a green body
- B22F10/14—Formation of a green body by jetting of binder onto a bed of metal powder
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- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
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- C—CHEMISTRY; METALLURGY
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- C22C—ALLOYS
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- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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Description
(1)一般式(I)の化合物
(AyBy-1)2+δCwDxEz (I)
[式中、
Aは、MnまたはCoであり、
Bは、Fe、Cr、またはNiであり、
C、D、およびEは、C、D、およびEのうちの少なくとも2つが異なっており、僅かでない濃度を有し、P、B、Se、Ge、Ga、Si、Sn、N、As、およびSbから選択され、
δは、−0.2〜0.2の範囲の数字であり、
w、x、y、zは0〜1の範囲の数字であって、この場合、w+x+z=1である]、
(2)一般式(II)および/または(III)および/または(IV)のLaおよびFe系の化合物
La(FexAl1-x)13HyまたはLa(FexSi1-x)13Hy (II)
[式中、
xは0.7〜0.95の数字であり、
yは0〜3の数字である]
La(FexAlyCoz)13またはLa(FexSiyCoz)13 (III)
[式中、
xは0.7〜0.95の数字であり、
yは0.05〜1−xの数字であり、
zは0.005〜0.5の数字である]
LaMnxFe2-xGe (IV)
[式中、
xは1.7〜1.95の数字である]、ならびに
(3)MnTP型のホイスラー合金[式中、Tは遷移金属であり、Pは、原子中の電子数e/aが7〜8.5の範囲にあるp型ドーピング金属である)、
(4)一般式(V)のGdおよびSi系の化合物
Gd5(SixGe1-x)4 (V)
[式中、xは0.2〜1の数字である]
(5)Fe2P系の化合物
(6)ペロブスカイト型の水マンガン鉱
(7)一般式(VI)および(VII)の、希土類元素を含む化合物
Tb5(Si4-xGex) (VI)
[式中、x=0、1、2、3、4である]
XTiGe (VII)
[式中、X=Dy、Ho、Tmである]
(8)一般式(VIII)および(IX)のMnおよびSb系のあるいはAs系の化合物
Mn2-xZxSb (VIII)
Mn2ZxSb1-x (IX)
[式中、
Zは、Cr、Cu、Zn、Co、V、As、Geであり、
xは、0.01〜0.5である]
(ここで、ZがAsでない場合は、SbをAsで置き換えてもよい)
から選択される熱磁気材料を含む、熱交換器のための成形体を製造する方法であって、当該成形体が、流体熱交換媒体の通り道のための経路を有し、熱磁気材料の粉末をバインダー中に導入する工程、結果として得られる成形材料を印刷法により担持体に適用し、続いてバインダーおよび適切であるなら担持体を除去する工程、ならびに結果として得られる未焼結成形体を焼結する工程、を含む方法により達成される。
Gd5(SixGe1-x)4
[式中、xは0.2〜1の数である]
のGdおよびSi系の化合物は、例えば、Gd5(Si0.5Ge0.5)4、Gd5(Si0.425Ge0.575)4、Gd5(Si0.45Ge0.55)4、Gd5(Si0.365Ge0.635)4、Gd5(Si0.3Ge0.7)4、Gd5(Si0.25Ge0.75)4である。
a)化学量論的に当該金属系材料に対応する量の化学元素および/または合金を固相および/または液相で反応させる工程と、
b)適切であれば、工程a)からの反応生成物を固体に変換する工程と、
c)工程a)またはb)からの固体を焼結および/または熱処理する工程と、
d)工程c)からの焼結および/または熱処理された固体を少なくとも100K/sの冷却速度で急冷する工程と
を含む、熱磁気材料の製造方法が好ましい。
a)約0.5μm〜450μmの範囲の平均粒径を有する粉末状の出発材料または出発材料混合物を、薄層において基材に適用する工程と、次いで、この層上の選択された部位において、当該粉末をバインダーおよび必要な任意の助剤と混合することにより、または、照射または別の方法により処理することにより、当該粉末をこれらの部位において接着させ、その結果として、当該粉末を層内および隣接する層の両方に対して接着させる工程と、工作物の所望の形状が、形成された粉末床において再現されるまでこの操作を繰り返す工程と、バインダーによって接着されていない粉末を除去することにより、接着した粉末を所望の成形体の形状において残す工程と、を、所望の成形体が個々の層から完全に形成されるまで繰り返すことによる、粉末ベースのラピッドプロトタイピング法によって成形体を製造する工程、
b)場合により、熱処理、好ましくは成形体の焼結および/または焼成を実施する工程であって、最初にバインダーの除去を実施することが可能な工程、
c)場合により、少なくとも1種の触媒活性な成分を当該成形体に適用する工程
d)場合により、さらなる熱処理実施する工程
を含む方法によって得ることができ、この場合、工程b)、c)、および/またはd)を2回以上実施してもよい。
実施例1
粉末を焼結するために、加圧成形されたMnFePGeの試料の入った真空の石英アンプルを、1100℃で10時間維持した。この焼結の後に、均質化するために650℃で60時間熱処理した。オーブン中において室温までゆっくりと冷却するのではなく、直ちに、当該試料を水で室温まで急冷した。水中での急冷により、試料表面においてある程度の酸化が生じた。外側の酸化されたシェルを、希酸でエッチングすることにより除去した。XRDパターンは、すべての試料が、Fe2P型の構造で結晶化していることを示した。
Mn1.1Fe0.9P0.81Ge0.19、Mn1.1Fe0.9P0.78Ge0.22、Mn1.1Fe0.9P0.75Ge0.25、およびMn1.2Fe0.8P0.81Ge0.19。熱ヒステリシスに対して観察された値は、これらの試料に対してこの順に7K、5K、2K、および3Kである。熱ヒステリシスが10Kを超えるようなゆっくり冷却された試料と比較して、熱ヒステリシスは大幅に減少している。
MnFeP(GeSb)の溶融紡糸
最初に、国際公開第2004/068512号およびJ.Appl.Phys.99,08 Q107(2006)に記載されているように、ボールミル中において、高エネルギーを用いて、固相反応法により多結晶MnFeP(Ge、Sb)合金を製造した。次いで、当該材料片を、ノズルを備えた石英管に導入した。チャンバーを10-2mbarまで脱気し、次いで高純度アルゴンガスで満たした。試料を高周波によって溶融させ、回転する銅ドラムを収容するチャンバーへ圧力差によりノズルから噴霧した。銅ホイールの表面速度は調整可能であり、約105K/sの冷却速度が達成された。続いて、当該溶融紡糸リボンを900℃で1時間熱処理した。
基礎原料は、Turbulaミキサー(Willy A.Bachofen Ag社,4058 Basle,Switzerland)を用いて200メッシュキサンタン固体バインダー(Koenig&Wiegand社,40472 Dusseldorf)と混合された熱磁気材料粉末である。固体バインダーの割合は、熱磁気粉末に対して10質量%である。三次元印刷法は、水系のZB54バインダー溶液(Z−Corporation社,Burlington,MA 01803,USA)を使用して、Z−プリンター310(Z−Corporation社,Burlington,MA 01803,USA)により実施する。2%の液体バインダーを用いる。印刷後、最初に、当該部品を60℃で8時間乾燥し、次いで、圧搾空気を吹き付けて乾燥させる。焼結は、2時間の保持時間により1600℃で行われる。
ラピッドプロトタイピングによる成形は、ProMetal RCT S15(ProMetal RCT GmbH社,86167 Augsburg)において、粉末およびバインダーの層を繰り返し堆積させることによって実施する。使用する粉末は熱磁気材料であり、バインダーはフラン型樹脂−酸混合物である。Askuran 120(Ashland−Suedchemie社,40721 Hilden)およびRPT 100(Ashland−Suedchemie社,40721 Hilden)によるこのバインダー混合物を100:40の混合比において用い、当該樹脂を当該粉末に加え、印字ヘッドノズルにより硬化剤を計量供給する。約1.5%の量の樹脂を対応する量の粉末に加える。多数の層を積み上げることによって成形物を製造し、室温で一夜乾燥させる。
Claims (11)
- (1)一般式(I)の化合物
(AyB 1-y )2+δCwDxEz (I)
[式中、
Aは、MnまたはCoであり、
Bは、Fe、Cr、またはNiであり、
C、D、およびEは、C、D、およびEのうちの少なくとも2つが異なっており、零ではない濃度を有し、P、B、Se、Ge、Ga、Si、Sn、N、As、およびSbから選択され、
δは、−0.2〜0.2の範囲の数字であり、
w、x、y、zは、0〜1の範囲の数字であって、この場合、w+x+z=1である]、
(2)一般式(II)および/または(III)および/または(IV)のLaおよびFe系の化合物
La(FexAl1-x)13HyまたはLa(FexSi1-x)13Hy (II)
[式中、
xは0.7〜0.95の数字であり、
yは0〜3の数字である];
La(FexAlyCoz)13またはLa(FexSiyCoz)13 (III)
[式中、
xは0.7〜0.95の数字であり、
yは0.05〜1−xの数字であり、
zは0.005〜0.5の数字である];
LaMnxFe2-xGe (IV)
[式中、
xは1.7〜1.95の数字である]、ならびに
(3)MnTP型のホイスラー合金[式中、Tは遷移金属であり、Pは、原子中の電子数e/aが7〜8.5の範囲にあるp型ドーピング金属である]、
(4)一般式(V)のGdおよびSi系の化合物、
Gd5(SixGe1-x)4 (V)
[式中、
xは0.2〜1の数である]、
(5)Fe2P系の化合物、
(6)ペロブスカイト型の水マンガン鉱、
(7)一般式(VI)および(VII)の、希土類元素を含む化合物
Tb5(Si4-xGex) (VI)
[式中、
x=0,1,2,3,4である]、
XTiGe (VII)
[式中、
X=Dy、Ho、Tmである]、
(8)一般式(VIII)および(IX)のMnおよびSb系のあるいはAs系の化合物、
Mn2-xZxSb (VIII)
Mn2ZxSb1-x (IX)
[式中、
Zは、Cr、Cu、Zn、Co、V、As、Geであり、
xは、0.01〜0.5である]
(ここで、ZがAsでない場合は、SbをAsで置き換えてもよい)、
から選択される熱磁気材料に基づく、流体熱交換媒体の通り道のための経路を有する熱交換器のための成形体を製造する方法であって、該熱磁気材料の粉末をバインダー中に導入し、結果として得られる該成形材料をスクリーン印刷、インクジェット印刷およびラピッドプロトタイピング/3D印刷から選択される印刷法により担持体に適用し、続いて該バインダーを除去し、そして結果として得られる該未焼結成形体を焼結し、かつ異なる温度において磁気熱量効果を示す異なる熱磁気材料が、同じ前記成形体中に存在するように、複数の異なる熱磁気材料が互いに並べておよび/または積み重ねて印刷される前記方法。 - 前記熱磁気材料の粉末をバインダー中に導入し、結果として得られる前記成形材料をスクリーン印刷、インクジェット印刷およびラピッドプロトタイピング/3D印刷から選択される印刷法により担持体に適用し、続いて該バインダーを除去する時に、前記担持体も除去されることを特徴とする請求項1に記載の方法。
- 前記成形材料として、熱磁気材料(1)〜(8)から選択される熱磁気材料を、成形材料の固形分に対して50〜99質量%含む成形材料が、印刷のために使用されることを特徴とする請求項1又は2に記載の方法。
- 少なくとも1つの空間軸に沿って前記磁気熱量効果が各場合において生じる温度の準連続的な上昇または降下がもたらされるように、該少なくとも1つの空間軸に沿って異なる前記熱磁気材料が三次元配置される、請求項1〜3の何れか1項に記載の方法。
- 前記熱磁気材料の前記粉末が、0.1〜100μmの範囲の平均粒径を有する、請求項1〜4の何れか1項に記載の方法。
- 前記熱磁気材料が、Mn、Fe、Pのほかに、さらに、Ge、あるいはSi、あるいはAs、あるいはGeおよびSi、あるいはGeおよびAs、あるいはSiおよびAs、あるいはGeおよびSiおよびAsを含む、前記一般式(I)の、少なくとも四成分を含む化合物から選択される、請求項1から5までのいずれか1項に記載の方法。
- 前記一般式(I)の、少なくとも四成分を含む化合物が、更にSbを含む、請求項6に記載の方法。
- 前記成形体中の前記経路が、0.1〜2000μmの範囲の平均径を有する、請求項1から7までのいずれか1項に記載の方法。
- 前記経路が、前記流体熱交換媒体のための1つ以上の導入口および放出口を提供するように構成され、ならびに該経路が、前記成形体の均一な温度制御を可能にするように配置されている、請求項1から8までのいずれか1項に記載の方法。
- 前記成形材料が、機械的特性、耐食性、および/または伝導性を向上させるためにさらなる添加剤を含む、請求項1から9までのいずれか1項に記載の方法。
- 前記印刷法がラピッドプロトタイピング/3D印刷であることを特徴とする、請求項1から10までのいずれか1項に記載の方法。
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TW201040248A (en) | 2010-11-16 |
KR20110139757A (ko) | 2011-12-29 |
CN102438777A (zh) | 2012-05-02 |
EP2411174B1 (de) | 2016-05-18 |
AU2010227586A1 (en) | 2011-11-10 |
WO2010108883A3 (de) | 2010-11-25 |
EP2411174A2 (de) | 2012-02-01 |
JP2012521647A (ja) | 2012-09-13 |
KR101673639B1 (ko) | 2016-11-22 |
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