JP4641209B2 - Method for producing porous metal body - Google Patents
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- JP4641209B2 JP4641209B2 JP2005104019A JP2005104019A JP4641209B2 JP 4641209 B2 JP4641209 B2 JP 4641209B2 JP 2005104019 A JP2005104019 A JP 2005104019A JP 2005104019 A JP2005104019 A JP 2005104019A JP 4641209 B2 JP4641209 B2 JP 4641209B2
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- 229910052751 metal Inorganic materials 0.000 title claims description 26
- 239000002184 metal Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000002245 particle Substances 0.000 claims description 34
- 239000011148 porous material Substances 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 26
- 239000008187 granular material Substances 0.000 claims description 24
- 239000011230 binding agent Substances 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 229910052719 titanium Inorganic materials 0.000 description 11
- 239000010936 titanium Substances 0.000 description 11
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 10
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 10
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 10
- 239000001099 ammonium carbonate Substances 0.000 description 10
- 229910001069 Ti alloy Inorganic materials 0.000 description 9
- 238000000465 moulding Methods 0.000 description 9
- 238000003825 pressing Methods 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000011164 primary particle Substances 0.000 description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- 229930182556 Polyacetal Natural products 0.000 description 5
- 238000009689 gas atomisation Methods 0.000 description 5
- 229920006324 polyoxymethylene Polymers 0.000 description 5
- 229920005177 Duracon® POM Polymers 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PFPYHYZFFJJQFD-UHFFFAOYSA-N oxalic anhydride Chemical compound O=C1OC1=O PFPYHYZFFJJQFD-UHFFFAOYSA-N 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical compound O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
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Description
この発明は、金属多孔体の製造方法に関する。この方法で製造される金属多孔体は、気孔同士が互いに連通していて且つ高い機械的強度を有し、フィルタ、触媒、吸音材、断熱材、熱交換器などに好適に利用されうる。 The present invention relates to a method for producing a metal porous body. The porous metal body produced by this method has pores communicating with each other and high mechanical strength, and can be suitably used for filters, catalysts, sound absorbing materials, heat insulating materials, heat exchangers, and the like.
従来、金属多孔体を製造する方法として、大小種々の粒径の金属粉末と有機バインダーとからなる混練物を成形後に焼成する周知技術の他、金属粉末、有機バインダー及び必要により気孔形成材を含む混練物を２０〜４００μｍに造粒し、成形後に焼成する技術（特許文献１＆４）、金属粉末等を有機物多孔体に付着もしくは含浸させ、焼成して当該有機物多孔体を焼失させる技術（特許文献２＆３）等が提案されている。
Conventionally, as a method for producing a metal porous body, a metal powder, an organic binder, and, if necessary, a pore forming material are included in addition to a well-known technique in which a kneaded material composed of metal powders of various sizes and sizes and an organic binder is fired after molding. A technique of granulating the kneaded material to 20 to 400 μm and baking it after molding (Patent Documents 1 and 4), a technique of attaching or impregnating a metal powder or the like to an organic porous material, and baking to burn the organic porous material (
しかし、上記従来の技術で製造された金属多孔体は、気孔同士が連通してはいるが金属粒子同士の結合強度が弱くて脆いか、機械的強度は高いが気孔が閉塞しているかのいずれかであり、フィルタ、触媒、熱交換器などの用途に適していなかった。
それ故、この発明の課題は、気孔同士が互いに連通していて且つ高い機械的強度を有する金属多孔体を提供することにある。
However, in the metal porous body manufactured by the above-described conventional technique, the pores communicate with each other, but the bonding strength between the metal particles is weak and brittle, or the mechanical strength is high but the pores are blocked. However, it was not suitable for applications such as filters, catalysts, and heat exchangers.
Therefore, an object of the present invention is to provide a porous metal body having pores communicating with each other and having high mechanical strength.
その課題を解決するために、この発明の金属多孔体の製造方法は、
最大粒径１８０μｍ以下の金属粉末と、有機バインダーとからなり、それらの体積比が６５：３５〜７０：３０である混練物を粉砕して得られた粒径０．３〜１．８ｍｍの範囲の顆粒を、加圧成形した後、焼成することを特徴とする。
この方法によれば、金属粉末と有機バインダーとからなる顆粒が加圧成形されているので、成形体は最大粒径１８０μｍ以下の一次粒子の群と有機バインダーからなる多数の顆粒が圧縮されたものである。即ち、図１に示すように、隣り合う顆粒１同士は多数の一次粒子２同士の接点を有するとともに、顆粒間には顆粒の直径と成形条件に対応する大きな気孔３が形成されている。従って、これを焼成すると、従来周知の金属多孔体製造技術において図２に示すように大小種々の一次粒子２同士が少ない接点で結合するのと異なり、顆粒１内の一次粒子２同士だけでなく顆粒１間の多数の一次粒子２同士が互いに結合する。その結果、焼結体の機械的強度が高く且つ気孔同士も連通する。
In order to solve the problem, the method for producing a porous metal body of the present invention includes:
It is composed of a metal powder having a maximum particle size of 180 μm or less and an organic binder, and a kneaded product having a volume ratio of 65:35 to 70:30 and having a particle size of 0.3 to 1.8 mm. A range of granules is characterized in that it is pressed and then fired.
According to this method, since the granule composed of the metal powder and the organic binder is pressure-molded, the compact is a compact of a large number of granules composed of a group of primary particles and an organic binder having a maximum particle size of 180 μm or less. It is. That is, as shown in FIG. 1, adjacent granules 1 have a large number of
この発明では、上記のように高い強度の多孔質体が得られるので、金属粉末として１８０μｍ程度のサイズのものも含まれていてよい。従って、金属粉末の収率が向上し、低コスト化を実現できる。但し、１８０μｍを超える一次粒子が含まれていると多孔質体の強度が低下するので、最大粒径を１８０μｍとした。また、顆粒の直径が０．１ｍｍ未満であったり、２．０ｍｍを超えていたりすると、加圧成形条件を調整するだけでは所定の気孔率の多孔質焼結体を得ることが困難であるから、確実性を期すため顆粒の直径を０．３〜１．８ｍｍとした。特に好ましいのは０．６〜１．５ｍｍである。また、焼成後の気孔率が４０％に満たないと連通気孔が少なくなって多孔体の各種用途に適さなくなる。他方、７０％を超えると機械的強度が著しく低下する。 In the present invention, since a porous body having a high strength is obtained as described above, a metal powder having a size of about 180 μm may be included. Therefore, the yield of metal powder can be improved and cost reduction can be realized. However, when the primary particles exceeding 180 μm are contained, the strength of the porous body is lowered, so the maximum particle size was set to 180 μm. Further, if the diameter of the granule is less than 0.1 mm or exceeds 2.0 mm, it is difficult to obtain a porous sintered body having a predetermined porosity only by adjusting the pressure molding conditions. In order to ensure certainty, the diameter of the granules was set to 0.3 to 1.8 mm. Particularly preferred is 0.6 to 1.5 mm. Further, if the porosity after firing is less than 40%, the continuous air holes are reduced and the porous body becomes unsuitable for various uses. On the other hand, if it exceeds 70%, the mechanical strength is remarkably lowered.
前記金属粉末としては、その酸素含有量が０．３０重量％以下であるものが好ましい。このような金属粉末は、粒子表面の酸素が少ないので活性であり、焼成工程で一次粒子間の結合が進みやすい。従って、一層高い機械的強度が得られる。
前記顆粒は当該金属粉末と有機バインダーとの混練物を粉砕して得られるものであるから、バインダーが水溶性に限定されない。このため、対象とする金属粉末が限定されない点で優れる。
前記顆粒は、単独ではなく気孔形成材と混合することができる。気孔形成材と混合すると、焼成後に気孔となる部分が気孔形成材により確保されるので、高い圧力で成形することが可能となる。従って、気孔形成材の抜けた跡が連通気孔となるとともに、顆粒間がより密に接触し、焼成工程で顆粒間の結合が進みやすくなり、一層高い機械的強度が得られる。
The metal powder preferably has an oxygen content of 0.30% by weight or less. Such a metal powder is active because there is little oxygen on the particle surface, and the bonding between the primary particles tends to proceed in the firing step. Therefore, higher mechanical strength can be obtained.
Since the granule is obtained by pulverizing a kneaded product of the metal powder and an organic binder , the binder is not limited to being water-soluble . For this reason, it is excellent in that the target metal powder is not limited.
The granules can be mixed with the pore former rather than alone. When mixed with the pore-forming material, portions that become pores after firing are secured by the pore-forming material, so that molding can be performed at a high pressure. Therefore, the traces of the pore-forming material being removed become the continuous air holes, and the granules are in closer contact with each other, and the bonding between the granules is facilitated in the firing step, so that higher mechanical strength can be obtained.
尚、所定の気孔率を得るための成形条件及び焼成条件については、成形条件を一定にして焼成条件を種々変更し、気孔率と例えば焼成温度との関係を示す検量線を作成しておくか、又は焼成条件を一定にして成形条件を種々変更し、気孔率と例えば圧縮率もしくは圧力との関係を示す検量線を作成しておくことにより、設定することが可能である。 As for the molding conditions and firing conditions for obtaining a predetermined porosity, whether the calibration conditions are variously changed while keeping the molding conditions constant, and a calibration curve showing the relationship between the porosity and, for example, the firing temperature is prepared. Alternatively, it is possible to set the firing conditions by changing the molding conditions variously and preparing a calibration curve indicating the relationship between the porosity and, for example, the compression rate or pressure.
この発明の製造方法で得られる金属多孔体は、連通気孔を有していながら高い機械的強度を有するので、気孔内に流体を通過させる必要のある種々の用途に長期間安定して利用することができる。 Since the metal porous body obtained by the production method of the present invention has high mechanical strength while having continuous air holes, it should be used stably for a long period of time in various applications that require fluid to pass through the pores. Can do.
金属粉末としては、チタン、ニッケル、タンタル、コバルト、鉄、貴金属及びこれらの合金など種々のものが適用可能である。有機バインダーも特に限定されず、ポリアセタール、ポリプロピレン、ポリエチレンなどであってよい。酸素含有量０．３０重量％以下の金属粉末を得る手段としては、不活性ガス雰囲気中で金属を粉砕するか又は金属の溶湯を噴霧する、所謂ガスアトマイズ方が挙げられる。気孔形成材としては、常温で固体であって２００℃以下で昇華もしくは分解する化合物（例えば炭酸水素アンモニウム、シュウ酸無水物、シュウ酸二水和物）や、これらのいずれかとワックス類との混合物が挙げられる。 Various metal powders such as titanium, nickel, tantalum, cobalt, iron, noble metals, and alloys thereof can be applied. The organic binder is not particularly limited, and may be polyacetal, polypropylene, polyethylene or the like. As a means for obtaining a metal powder having an oxygen content of 0.30% by weight or less, a so-called gas atomization method in which a metal is pulverized or sprayed with a molten metal in an inert gas atmosphere can be mentioned. As the pore-forming material, a compound that is solid at room temperature and sublimes or decomposes at 200 ° C. or lower (for example, ammonium hydrogen carbonate, oxalic acid anhydride, oxalic acid dihydrate), or a mixture of any of these with waxes. Is mentioned.
−実施例１−
ガスアトマイズ法により製造した酸素含有量０．１２重量％、最大粒径４５μｍのチタン粉末とポリアセタール（株式会社ポリプラスチック製ジュラコンＭ２７０）を６５：３５の体積比で混練した。体積比は各々の真密度と重量から算出した。混練して得られた塊を粉砕し、篩いにかけて０．６〜１．５ｍｍの粒径の顆粒を得た。顆粒を金型に充填し、１３０℃に加熱すると共に加圧前に対して加圧後の体積が４３％となるようにプレス機のストローク量を調整して圧力を加えることにより、成形した。成形体を真空炉内に置き、脱脂後、１２００℃で２時間保持することにより、直径２２ｍｍ×高さ１８ｍｍの円柱状のチタン多孔体を製造した。
Example 1
Titanium powder having an oxygen content of 0.12% by weight and a maximum particle size of 45 μm produced by a gas atomizing method and polyacetal (Duracon M270 manufactured by Polyplastics Co., Ltd.) were kneaded at a volume ratio of 65:35. The volume ratio was calculated from each true density and weight. The lump obtained by kneading was pulverized and sieved to obtain granules having a particle size of 0.6 to 1.5 mm. The granules were filled in a mold, heated to 130 ° C., and molded by applying pressure by adjusting the stroke amount of the press so that the volume after pressing was 43% of that before pressing. The molded body was placed in a vacuum furnace, degreased and held at 1200 ° C. for 2 hours to produce a cylindrical titanium porous body having a diameter of 22 mm and a height of 18 mm.
この多孔体の気孔率を、多孔体の重量とチタンの真密度とから算出したところ、４０％であった。また、多孔体の酸素含有量を非分散型赤外吸収法により分析したところ、０．２１重量％であった。多孔体から直径６ｍｍ×高さ１０ｍｍの試験片を切り出し、圧縮速度１ｍｍ／分で圧縮したところ、圧縮強度は１８５ＭＰａであり、粒子の脱落は無い状態で変形した。 The porosity of the porous body was calculated from the weight of the porous body and the true density of titanium, and was 40%. Moreover, it was 0.21 weight% when the oxygen content of the porous body was analyzed by the non-dispersion type infrared absorption method. When a test piece having a diameter of 6 mm and a height of 10 mm was cut out from the porous body and compressed at a compression speed of 1 mm / min, the compressive strength was 185 MPa, and the sample was deformed without any dropout.
−比較例１−
実施例１において加圧前に対して加圧後の体積が３２％となるように圧力を加えることにより成形したこと以外は、実施例１と同一条件でチタン多孔体を製造した。気孔率は３５％であった。このチタン多孔体及び実施例１のチタン多孔体をＣＴ検査したところ、本例のチタン多孔体は実施例１のものに比べて独立気孔が多かった。
-Comparative Example 1-
A porous titanium body was produced under the same conditions as in Example 1, except that in Example 1, the pressure was applied so that the volume after pressurization was 32% of that before pressurization. The porosity was 35%. When this titanium porous body and the titanium porous body of Example 1 were subjected to CT examination, the titanium porous body of this example had more independent pores than that of Example 1.
−実施例２及び３−
実施例１において加圧前に対して加圧後の体積が６４％（実施例２）又は７１％（実施例３）となるように圧力を加えることにより成形したこと以外は、実施例１と同一条件でチタン多孔体を製造した。気孔率はそれぞれ４９％及び５５％であった。実施例２及び実施例３の多孔体の圧縮強度はそれぞれ１４８ＭＰａ及び１２５MPaであり、粒子の脱落は無い状態で変形した。
-Examples 2 and 3-
In Example 1, except that it was molded by applying pressure so that the volume after pressurization was 64% (Example 2) or 71% (Example 3) with respect to before pressurization. A porous titanium body was produced under the same conditions. The porosity was 49% and 55%, respectively. The compressive strengths of the porous bodies of Example 2 and Example 3 were 148 MPa and 125 MPa, respectively, and were deformed without any dropout of particles.
−比較例２及び３−
実施例１において加圧前に対して加圧後の体積が７４％（比較例２）又は７６％（比較例３）となるように圧力を加えることにより成形したこと以外は、実施例１と同一条件でチタン多孔体を製造した。気孔率はそれぞれ６０％及び６５％であった。これらの多孔体の圧縮強度はそれぞれ９２ＭＰａ及び６０ＭＰａで粒子の脱落が認められた。
-Comparative Examples 2 and 3-
Example 1 is the same as Example 1 except that it was molded by applying pressure so that the volume after pressurization was 74% (Comparative Example 2) or 76% (Comparative Example 3). A porous titanium body was produced under the same conditions. The porosity was 60% and 65%, respectively. These porous bodies had a compressive strength of 92 MPa and 60 MPa, respectively.
−実施例４−
実施例１においてチタン粉末の最大粒径が１８０μｍであることと、加圧前に対して加圧後の体積が６４％となるように圧力を加えることにより成形したこと以外は、実施例１と同一条件で直径２２ｍｍ×高さ２１ｍｍの円柱状のチタン多孔体を製造した。気孔率は５１％であった。また、圧縮強度は１３０ＭＰａであり、粒子の脱落は無い状態で変形した。
Example 4
In Example 1, except that the maximum particle size of the titanium powder is 180 μm and that it is molded by applying pressure so that the volume after pressurization is 64% with respect to that before pressurization. A cylindrical titanium porous body having a diameter of 22 mm and a height of 21 mm was manufactured under the same conditions. The porosity was 51%. Further, the compressive strength was 130 MPa, and the particles were deformed without any particles falling off.
−実施例５−
ガスアトマイズ法により製造した酸素含有量０．１８重量％、最大粒径１８０μｍのチタン合金（Ｔｉ−６Ａｌ−４Ｖ）粉末とポリアセタール（株式会社ポリプラスチック製ジュラコンＭ２７０）を６５：３５の体積比で混練した。体積比は各々の真密度と重量から算出した。混練して得られた塊を粉砕し、篩いにかけて０．６〜１．５ｍｍの粒径の顆粒を得た。顆粒を金型に充填し、１３０℃に加熱すると共に加圧前に対して加圧後の体積が６４％となるようにプレス機のストローク量を調整して圧力を加えることにより、成形した。成形体を真空炉内に置き、脱脂後、１２５０℃で２時間保持することにより、直径２２ｍｍ×高さ２１ｍｍの円柱状のチタン多孔体を製造した。重量と真密度とから算出した気孔率は５２％であった。また、圧縮強度は２０６ＭＰａであり、粒子の脱落は無い状態で変形した。
-Example 5
A titanium alloy (Ti-6Al-4V) powder having an oxygen content of 0.18% by weight and a maximum particle size of 180 μm produced by a gas atomization method and polyacetal (Duracon M270 manufactured by Polyplastics Co., Ltd.) were kneaded at a volume ratio of 65:35. . The volume ratio was calculated from each true density and weight. The lump obtained by kneading was pulverized and sieved to obtain granules having a particle size of 0.6 to 1.5 mm. The granules were filled in a mold, heated to 130 ° C., and molded by applying pressure by adjusting the stroke amount of the press so that the volume after pressing was 64% of that before pressing. The molded body was placed in a vacuum furnace, degreased, and held at 1250 ° C. for 2 hours to produce a cylindrical titanium porous body having a diameter of 22 mm and a height of 21 mm. The porosity calculated from the weight and the true density was 52%. Moreover, the compressive strength was 206 MPa, and it was deformed in a state where no particles were dropped.
−実施例６−
ガスアトマイズ法により製造した酸素含有量０．１８重量％、最大粒径１８０μｍのチタン合金（Ｔｉ−６Ａｌ−４Ｖ）粉末とポリアセタール（株式会社ポリプラスチック製ジュラコンＭ２７０）を７０：３０の体積比で混練した。体積比は各々の真密度と重量から算出した。混練して得られた塊を粉砕し、篩いにかけて０．６〜１．５ｍｍの粒径の顆粒を得た。また別途、炭酸水素アンモニウム粉末を２５０〜５００μｍに粒度調整した。
-Example 6
A titanium alloy (Ti-6Al-4V) powder having an oxygen content of 0.18% by weight and a maximum particle size of 180 μm produced by a gas atomization method and polyacetal (Duracon M270 manufactured by Polyplastics Co., Ltd.) were kneaded at a volume ratio of 70:30. . The volume ratio was calculated from each true density and weight. The lump obtained by kneading was pulverized and sieved to obtain granules having a particle size of 0.6 to 1.5 mm. Separately, the particle size of ammonium hydrogen carbonate powder was adjusted to 250 to 500 μm.
そして、前記顆粒を粒度調整した炭酸水素アンモニウム粉末と５８：４２の体積比で混合し、この混合粉末を金型に充填し、７０℃に加熱すると共に８０ＭＰａの圧力を加えることにより、成形した。成形体を真空炉内に置き、脱脂後、１２５０℃で２時間保持することにより、直径２２ｍｍ×高さ１９ｍｍの円柱状のチタン合金多孔体を製造した。気孔率を水銀ポロシメータで測定すると７２％であり、気孔径範囲は３〜４００μｍ、平均気孔径は１１２μｍであった。また、圧縮強度は１００ＭＰａであり、粒子の脱落は無い状態で変形した。 Then, the granules were mixed with an ammonium hydrogen carbonate powder whose particle size was adjusted at a volume ratio of 58:42, this mixed powder was filled in a mold, heated to 70 ° C., and a pressure of 80 MPa was applied to form. The formed body was placed in a vacuum furnace, degreased and held at 1250 ° C. for 2 hours to produce a cylindrical titanium alloy porous body having a diameter of 22 mm and a height of 19 mm. When the porosity was measured with a mercury porosimeter, it was 72%, the pore diameter range was 3 to 400 μm, and the average pore diameter was 112 μm. Moreover, the compressive strength was 100 MPa, and it was deformed in a state in which no particles dropped out.
−実施例７−
実施例６において炭酸水素アンモニウム粉末に代えて粒度調整した炭酸水素アンモニウム粉末８８体積％にパラフィンワックス１２体積％をコーティングしたものを用いたこと以外は、実施例６と同一条件でチタン合金多孔体を製造した。気孔率を水銀ポロシメータで測定すると７２％であり、気孔径範囲は３〜４００μｍ、平均気孔径は９５μｍであった。また、圧縮強度は１００ＭＰａであり、粒子の脱落は無い状態で変形した。
-Example 7-
A porous titanium alloy was prepared under the same conditions as in Example 6 except that 88% by volume of ammonium bicarbonate powder whose particle size was adjusted instead of ammonium bicarbonate powder in Example 6 and 12% by volume of paraffin wax were coated. Manufactured. When the porosity was measured with a mercury porosimeter, it was 72%, the pore diameter range was 3 to 400 μm, and the average pore diameter was 95 μm. Moreover, the compressive strength was 100 MPa, and it was deformed in a state in which no particles dropped out.
−実施例８−
実施例６において炭酸水素アンモニウム粉末として粒度５００〜１５００μｍの範囲に調整したものを用いたこと以外は、実施例６と同一条件でチタン合金多孔体を製造した。気孔率を水銀ポロシメータで測定すると６７％であり、気孔径範囲は３〜４００μｍ、平均気孔径は１４５μｍであった。また、圧縮強度は１１４ＭＰａであり、粒子の脱落は無い状態で変形した。
-Example 8-
A titanium alloy porous body was produced under the same conditions as in Example 6 except that the ammonium hydrogen carbonate powder adjusted to a particle size in the range of 500 to 1500 μm was used in Example 6. The porosity was 67% as measured with a mercury porosimeter, the pore diameter range was 3 to 400 μm, and the average pore diameter was 145 μm. Moreover, the compressive strength was 114 MPa, and it was deformed in a state where no particles were dropped.
−実施例９−
ガスアトマイズ法により製造した酸素含有量０．２１重量％、最大粒径４５μｍのチタン合金（Ｔｉ−６Ａｌ−４Ｖ）粉末とポリアセタール（株式会社ポリプラスチック製ジュラコンＭ２７０）を７０：３０の体積比で混練した。体積比は各々の真密度と重量から算出した。混練して得られた塊を粉砕し、篩いにかけて０．３〜０．６５ｍｍの粒径の顆粒を得た。また別途、炭酸水素アンモニウム粉末を１００〜２００μｍに粒度調整した。
-Example 9-
A titanium alloy (Ti-6Al-4V) powder having an oxygen content of 0.21% by weight and a maximum particle size of 45 μm produced by a gas atomization method and polyacetal (Duracon M270 manufactured by Polyplastics Co., Ltd.) were kneaded at a volume ratio of 70:30. . The volume ratio was calculated from each true density and weight. The lump obtained by kneading was pulverized and sieved to obtain granules having a particle size of 0.3 to 0.65 mm. Separately, the particle size of ammonium hydrogen carbonate powder was adjusted to 100 to 200 μm.
そして、前記顆粒を粒度調整した炭酸水素アンモニウム粉末８８体積％にパラフィンワックス１２体積％をコーティングしたものと５８：４２の体積比で混合し、この混合粉末を金型に充填し、１３０℃に加熱すると共に８０ＭＰａの圧力を加えることにより、成形した。成形体を真空炉内に置き、脱脂後、１２５０℃で２時間保持することにより、直径２２ｍｍ×高さ２０ｍｍの円柱状のチタン合金多孔体を製造した。気孔率を水銀ポロシメータで測定すると６９％であり、気孔径範囲は３〜２１０μｍ、平均気孔径は９４μｍであった。また、圧縮強度は１０７ＭＰａであり、粒子の脱落は無い状態で変形した。 Then, 88% by volume of the ammonium hydrogen carbonate powder whose particle size is adjusted and 12% by volume of paraffin wax coated are mixed in a 58:42 volume ratio, and this mixed powder is filled in a mold and heated to 130 ° C. And molding was performed by applying a pressure of 80 MPa. The compact was placed in a vacuum furnace, degreased, and held at 1250 ° C. for 2 hours to produce a cylindrical titanium alloy porous body having a diameter of 22 mm and a height of 20 mm. When the porosity was measured with a mercury porosimeter, it was 69%, the pore diameter range was 3 to 210 μm, and the average pore diameter was 94 μm. Moreover, the compressive strength was 107 MPa, and it was deformed in a state where no particles were dropped.
−実施例１０−
実施例９において炭酸水素アンモニウム粉末として粒度３０〜１００μｍの範囲に調整したものを用いたこと以外は、実施例９と同一条件でチタン合金多孔体を製造した。気孔率を水銀ポロシメータで測定すると６８％であり、気孔径範囲は３〜９８μｍ、平均気孔径は５０μｍであった。また、圧縮強度は１０８ＭＰａであり、粒子の脱落は無い状態で変形した。
-Example 10-
A titanium alloy porous body was produced under the same conditions as in Example 9, except that the ammonium hydrogen carbonate powder adjusted to a particle size of 30 to 100 μm was used in Example 9. When the porosity was measured with a mercury porosimeter, it was 68%, the pore diameter range was 3 to 98 μm, and the average pore diameter was 50 μm. Moreover, the compressive strength was 108 MPa, and it was deformed in a state where no particles were dropped.
−実施例１１−
実施例９において炭酸水素アンモニウム粉末に代えて粒度２５０〜５００μｍの範囲に調整したシュウ酸無水物８８体積％を用いたことと、焼成温度を１３８０℃に変えて１２５０℃としたこと以外は、実施例９と同一条件でチタン合金多孔体を製造した。気孔率を水銀ポロシメータで測定すると７０％であり、気孔径範囲は３〜４００μｍ、平均気孔径は７５μｍであった。また、圧縮強度は１０５ＭＰａであり、粒子の脱落は無い状態で変形した。
-Example 11-
In Example 9, except that 88 volume% of oxalic anhydride adjusted to a particle size range of 250 to 500 μm was used instead of ammonium hydrogen carbonate powder, and that the firing temperature was changed to 1380 ° C. to 1250 ° C. A titanium alloy porous body was produced under the same conditions as in Example 9. When the porosity was measured with a mercury porosimeter, it was 70%, the pore diameter range was 3 to 400 μm, and the average pore diameter was 75 μm. Moreover, the compressive strength was 105 MPa, and it was deformed in a state where no particles were dropped.
上記実施例１〜１１及び比較例１〜３の気孔率と圧縮強度との関係を図３にグラフとして示す。 The relationship between the porosity of Examples 1 to 11 and Comparative Examples 1 to 3 and the compressive strength is shown as a graph in FIG.
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| JPS5270496A (en) * | 1975-12-08 | 1977-06-11 | Ekusuperimentarunui Nii Metaro | Porous materials for use in tool electrode and method of manufacturing thereof |
| JPH04308048A (en) * | 1991-04-04 | 1992-10-30 | Tokyo Tungsten Co Ltd | Production of porous tungsten material |
| JP2002047501A (en) * | 1996-07-30 | 2002-02-15 | Toho Titanium Co Ltd | Titanium base powder |
| JP2004349683A (en) * | 2003-04-28 | 2004-12-09 | Showa Denko Kk | Valve action metallic sintered body, manufacturing method therefor and solid electrolytic capacitor |
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| JPH04308048A (en) * | 1991-04-04 | 1992-10-30 | Tokyo Tungsten Co Ltd | Production of porous tungsten material |
| JP2002047501A (en) * | 1996-07-30 | 2002-02-15 | Toho Titanium Co Ltd | Titanium base powder |
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