JP4126366B2 - Method for producing foamed inorganic powder - Google Patents

Method for producing foamed inorganic powder Download PDF

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Publication number
JP4126366B2
JP4126366B2 JP2001214948A JP2001214948A JP4126366B2 JP 4126366 B2 JP4126366 B2 JP 4126366B2 JP 2001214948 A JP2001214948 A JP 2001214948A JP 2001214948 A JP2001214948 A JP 2001214948A JP 4126366 B2 JP4126366 B2 JP 4126366B2
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Japan
Prior art keywords
inorganic powder
producing
foamed
fat
foamed inorganic
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JP2001214948A
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Japanese (ja)
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JP2003027157A (en
Inventor
透 清水
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
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National Institute of Advanced Industrial Science and Technology AIST
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Priority to JP2001214948A priority Critical patent/JP4126366B2/en
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Description

【0001】
【発明の属する技術分野】
本発明は、発泡金属(合金を含む)および発泡セラミックス等の無機粉末体の製造方法に関するものである。
【0002】
【従来の技術】
従来からの発泡金属の製造方法としては、
(1)溶融した金属中にガスを吹き込む、
(2)中空のバルーンを混入する、
(3)TiHなどの発泡材を投入する、
などして発泡させ、凝固させて製造するなどの手法がある。
【0003】
【発明が解決しようとする課題】
しかしながら、上記した製造方法では、実際に製造できる材料は、融点が比較的低く溶湯の取り扱いが容易である材料、発泡剤がガスを放出する温度と溶湯の温度域が一致する材料、という条件からアルミニウム材料等が中心であった。
さらに、溶湯内の気泡が抜けていかないように粘度の調整を行う必要があった。
また、これらの手法を改良する手段として粉末金属に発泡剤を混合し、その材料を粉末鍛造、押し出し等の処理により固体化し、その後、発泡剤のガス発生温度付近で焼結する事により発泡させる手法がある。いずれにせよ、これらの手法では製造可能な発泡材料の種類は発泡剤の発泡温度と材料の焼結温度の関係から発泡できる材料は限られ、結局、アルミニウム系合金が中心であった。
【0004】
本発明は、粉末材料を水系バインダーで凝固させる過程で凝結体を発泡させる手法を用いることにより、製造可能な発泡材料の種類を大幅に増やすとともに、より均質な高品質の発泡体を製造可能とすることを目的とする。
【0005】
【課題を解決するための手段】
本発明の発泡無機粉末体の製造方法は、凍結によりゲル化するポリマーの水溶液に無機粉末、油脂材及び界面活性剤を混合・混練した後、凍結ゲル化させ、次いで前記油脂成分を除去し、得られる凝固体を焼結することを特徴とする。
また、本発明の発泡無機粉末体の製造方法は、無機粉末が、金属粉又はセラミックス粉末であることを特徴とする。
また、本発明の発泡無機粉末体の製造方法は、無機粉末を混合・混練した後に油脂材及び界面活性剤を加えることを特徴する。
また、本発明の発泡無機粉末体の製造方法は、油脂材が室温付近の凝固点を有するものであることを特徴とする。
また、本発明の発泡無機粉末体の製造方法は、型に鋳込んで凍結ゲル化させることを特徴とする。
また、本発明の発泡無機粉末体の製造方法は、油脂成分を超臨界二酸化炭素による抽出により除去あるいは加熱により除去することを特徴とする。
【0006】
【発明の実施の形態】
以下、本発明による実施の形態を説明する。
発泡体を製造しようとする無機粉末、例えば、金属粉またはセラミックス粉と凍結ゲル化するポリビニールアルコールなどの水溶性ポリマーの0.5〜40mass%水溶液を準備し、粉体と水溶液の体積比が1:4から4:1の間の割合で混合・混練する。
さらに、パラフィンワックス等の室温から氷点付近で凝固する油脂を準備し、中性洗剤等の界面活性剤と一緒に混合すれば、油脂成分は泡状にスラリーに分散する。その材料を適当な型に鋳込みそのまま氷点下に冷やして凍結すれば形状が固定される。そのまま、約1日保冷して、室温で溶解することによって水溶液成分はゲル化して形状は固定される。なお、混合する油脂の分量は望む空孔率により変化させる。また、中性洗剤の分量も油脂の分量にあわせて適宜、変化させる。
【0007】
その後、この素材を60℃から100℃程度の恒温槽においてパラフィンワックスを溶解するか、あるいは、超臨界二酸化炭素中でパラフィンワックスを抽出すれば均質に発泡した粉体の凝結体が得られる。
さらに、この成形体を材質に応じた雰囲気・温度で焼結することにより、発泡無機粉末体を製造できる。このように、発泡剤の発泡温度と材料の焼結温度とを同じにする必要がないことから、従来、融点が高く発泡体を製造できなかった材料でも均質な発泡製品の製造が可能となる。
【0008】
【実施例】
金属粉として、平均粒径6.3μmのSUS304Lステンレス粉を用いた。ステンレス粉には重量100gに対して平均分子量100000、鹸化度99%のポリビニルアルコールの5%水溶液を体積比6:4で混合し、スラリーとする。このスラリーに融点43℃のパラフィンワックス100gと中性洗剤を加えて混合し、スラリー中にパラフィンワックスを泡状に分散させる。さらに、鋳型に流し込み凍結させて24時間保持する。成形体はそのまま乾燥させ、80℃での加熱、あるいは超臨界二酸化炭素による脱脂等によりパラフィンワックスを除去する。この発泡体を水素雰囲気1350℃の温度で2時間焼結することにより成形を終了する。この成形体の体積空隙率は約80%であった。
【0009】
【発明の効果】
以上説明したように本発明によれば、超硬材料のような難加工性材料から貴金属、セラミックスを含む幅広い無機材料から発泡金属、発泡セラミックス等の発泡無機粉末体を製造することができるとともに均一に発泡した高品質の発泡無機粉末体の製造が可能となる。
[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing an inorganic powder body such as foam metal (including an alloy) and foam ceramics.
[0002]
[Prior art]
As a conventional method for producing foam metal,
(1) Blowing gas into the molten metal
(2) Mixing a hollow balloon,
(3) A foam material such as TiH 2 is introduced.
For example, there are techniques such as foaming and coagulating to produce.
[0003]
[Problems to be solved by the invention]
However, in the manufacturing method described above, the material that can be actually manufactured is a material that has a relatively low melting point and is easy to handle the molten metal, and a material in which the temperature at which the blowing agent emits gas coincides with the temperature range of the molten metal. Mainly aluminum materials.
Furthermore, it is necessary to adjust the viscosity so that bubbles in the molten metal do not escape.
As a means to improve these methods, a foaming agent is mixed with powder metal, the material is solidified by a process such as powder forging and extrusion, and then foamed by sintering near the gas generation temperature of the foaming agent. There is a technique. In any case, the types of foam materials that can be produced by these methods are limited to the materials that can be foamed due to the relationship between the foaming temperature of the foaming agent and the sintering temperature of the material.
[0004]
The present invention can greatly increase the number of types of foam materials that can be produced and can produce a more homogeneous high-quality foam by using a method of foaming the aggregate in the process of solidifying the powder material with an aqueous binder. The purpose is to do.
[0005]
[Means for Solving the Problems]
The method for producing a foamed inorganic powder body of the present invention comprises mixing and kneading an inorganic powder, an oil and fat material, and a surfactant in an aqueous solution of a polymer that gels upon freezing , then freezing and gelling, and then removing the oil and fat component, The obtained solidified body is sintered.
In the method for producing a foamed inorganic powder body of the present invention, the inorganic powder is a metal powder or a ceramic powder.
Moreover, the manufacturing method of the foamed inorganic powder body of this invention is characterized by adding an oil and fat material and a surfactant after mixing and kneading the inorganic powder.
Moreover, the manufacturing method of the foamed inorganic powder of the present invention is characterized in that the fat and oil material has a freezing point near room temperature.
Moreover, the manufacturing method of the foamed inorganic powder body of the present invention is characterized in that it is cast into a mold and freeze-gelated .
The method for producing a foamed inorganic powder of the present invention is characterized in that the fat and oil component is removed by extraction with supercritical carbon dioxide or by heating .
[0006]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments according to the present invention will be described below.
An inorganic powder to be used for producing a foam, for example, a metal powder or a ceramic powder and a 0.5 to 40 mass% aqueous solution of a water-soluble polymer such as polyvinyl alcohol to be freeze-gelated is prepared, and the volume ratio of the powder to the aqueous solution is 1: Mix and knead at a ratio between 4 and 4: 1.
Furthermore, when fats and oils that solidify near room temperature from the room temperature such as paraffin wax are prepared and mixed together with a surfactant such as a neutral detergent, the fat and oil components are dispersed in a slurry in the form of foam. The shape is fixed by casting the material into a suitable mold and cooling it to below freezing and freezing. The solution is kept for about one day as it is and dissolved at room temperature, whereby the aqueous solution component is gelled and the shape is fixed. In addition, the quantity of the fats and oils to mix is changed with the desired porosity. In addition, the amount of the neutral detergent is appropriately changed according to the amount of the fat.
[0007]
Thereafter, the paraffin wax is dissolved in a constant temperature bath of about 60 ° C. to 100 ° C., or the paraffin wax is extracted in supercritical carbon dioxide, whereby a homogeneously foamed powder aggregate is obtained.
Furthermore, a foamed inorganic powder body can be manufactured by sintering this molded body in an atmosphere and temperature according to the material. As described above, since it is not necessary to make the foaming temperature of the foaming agent and the sintering temperature of the material the same, it is possible to produce a homogeneous foamed product even with a material that has conventionally had a high melting point and could not produce a foam. .
[0008]
【Example】
As the metal powder, SUS304L stainless steel powder having an average particle diameter of 6.3 μm was used. The stainless steel powder is mixed with a 5% aqueous solution of polyvinyl alcohol having a mean molecular weight of 100,000 and a saponification degree of 99% with respect to a weight of 100 g at a volume ratio of 6: 4. To this slurry, 100 g of paraffin wax having a melting point of 43 ° C. and a neutral detergent are added and mixed, and the paraffin wax is dispersed in a foam form in the slurry. Further, it is poured into a mold and frozen for 24 hours. The molded body is dried as it is, and the paraffin wax is removed by heating at 80 ° C. or degreasing with supercritical carbon dioxide. The foam is sintered at a temperature of 1350 ° C. in a hydrogen atmosphere for 2 hours to complete the molding. The volume porosity of this molded body was about 80%.
[0009]
【The invention's effect】
As described above, according to the present invention, it is possible to produce foamed inorganic powder bodies such as foam metal and foam ceramic from a wide range of inorganic materials including precious metals and ceramics from difficult-to-work materials such as cemented carbide materials and uniform. It is possible to produce a high-quality foamed inorganic powder body that has been foamed.

Claims (6)

凍結によりゲル化するポリマーの水溶液に無機粉末、油脂材及び界面活性剤を混合・混練した後、凍結ゲル化させ、次いで前記油脂成分を除去し、得られる凝固体を焼結することを特徴とする発泡無機粉末体の製造方法。 It is characterized by mixing and kneading an inorganic powder, an oil and fat material, and a surfactant in an aqueous solution of a polymer that gels upon freezing , then freeze-gelling , then removing the oil and fat component, and sintering the resulting solidified body. A method for producing a foamed inorganic powder body. 無機粉末が、金属粉又はセラミックス粉末であることを特徴とする請求項1記載の発泡無機粉末体の製造方法。  The method for producing a foamed inorganic powder body according to claim 1, wherein the inorganic powder is a metal powder or a ceramic powder. 無機粉末を混合・混練した後に油脂材及び界面活性剤を加えることを特徴する請求項1又は請求項2記載の発泡無機粉末体の製造方法。  The method for producing a foamed inorganic powder body according to claim 1 or 2, wherein the fat and oil material and the surfactant are added after mixing and kneading the inorganic powder. 油脂材が室温付近の凝固点を有するものであることを特徴とする請求項1乃至請求項3のいずれかに記載の発泡無機粉末体の製造方法。  The method for producing a foamed inorganic powder body according to any one of claims 1 to 3, wherein the fat and oil material has a freezing point near room temperature. 型に鋳込んで凍結ゲル化させることを特徴とする請求項1乃至請求項4のいずれかに記載の発泡無機粉末体の製造方法。The method for producing a foamed inorganic powder body according to any one of claims 1 to 4, wherein the foamed inorganic powder body is cast into a mold and freeze-gelated . 油脂成分を超臨界二酸化炭素による抽出により除去あるいは加熱により除去することを特徴とする請求項1乃至請求項5のいずれかに記載の発泡無機粉末体の製造方法。The method for producing a foamed inorganic powder body according to any one of claims 1 to 5, wherein the fat and oil component is removed by extraction with supercritical carbon dioxide or by heating .
JP2001214948A 2001-07-16 2001-07-16 Method for producing foamed inorganic powder Expired - Lifetime JP4126366B2 (en)

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US7481968B2 (en) 2004-03-17 2009-01-27 National Institute Of Advanced Industrial Science And Technology Method for preparing a sintered porous body of metal or ceramic
FR3019176A1 (en) * 2014-03-27 2015-10-02 Commissariat Energie Atomique PROCESS FOR THE PREPARATION OF A MACROPOROUS AND MESOPOROUS GEOPOLYMER WITH CONTROLLED POROSITY

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