JP2005194615A - Method (one-step) for manufacturing component from metallic powder - Google Patents
Method (one-step) for manufacturing component from metallic powder Download PDFInfo
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- JP2005194615A JP2005194615A JP2004028647A JP2004028647A JP2005194615A JP 2005194615 A JP2005194615 A JP 2005194615A JP 2004028647 A JP2004028647 A JP 2004028647A JP 2004028647 A JP2004028647 A JP 2004028647A JP 2005194615 A JP2005194615 A JP 2005194615A
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- degreasing
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- sintering
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- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- 239000011230 binding agent Substances 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 238000004898 kneading Methods 0.000 claims description 8
- 238000003672 processing method Methods 0.000 claims 1
- 238000005238 degreasing Methods 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000007796 conventional method Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000012255 powdered metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
Description
この発明は、金属紛末数紛と数種バインダーとの加圧混錬された材料を製作する為の金型製作、製品を成形する為のバインダー、成形後の脱脂・燒結工程を同一炉内で行う、脱指・燒結方法(ONE−STEP)と、そのバインダーである。 This invention is the same furnace for mold production for producing pressure-kneaded material of powdered metal powder and several binders, binder for molding products, and degreasing and sintering processes after molding. The finger removal / sintering method (ONE-STEP) and its binder.
従来、金属粉末成形法では、材料金属紛の混合、バインダーとの混錬、成形、脱バインダー、燒結の5工程から構成されて、脱脂、燒結が別々の装置で行われてた。 Conventionally, the metal powder molding method is composed of five steps: mixing of metal powder, kneading with a binder, molding, debinding, and sintering, and degreasing and sintering are performed in separate apparatuses.
脱脂工程「バインダー摘出」には、脱脂と仮燒結を行う脱脂炉又はバインダーを溶剤抽出の2通りである。 In the degreasing process “binder extraction”, a degreasing furnace or binder for degreasing and temporary sintering is used in two ways: solvent extraction.
加熱脱脂を行って後、燒結する方法として、▲1▼脱脂炉と燒結炉とを用いる方法と、▲2▼脱脂と燒結を一つの炉を用いて連続的に行う、二つの方法であった。 After heating and degreasing, there are two methods of sintering, namely, (1) a method using a degreasing furnace and a sintering furnace, and (2) a method of continuously performing degreasing and sintering using one furnace. .
ここで、▲1▼の方法では完全にバインダーを摘出すると、脱脂炉から燒結炉に移動するときに崩壊、酸化する、の欠点がある。 Here, in the method (1), when the binder is completely extracted, there is a drawback that it collapses and oxidizes when moving from the degreasing furnace to the sintering furnace.
▲2▼の方法では所要時間が短くて済むという長所はあるが、連続的という時点でのバインダーの分解のよる酸化によるために、完全な燒結体が出来にくく、イニシャルコストが高く、材料に限定されるという欠点がある。 The method (2) has the advantage that the required time can be shortened, but due to the oxidation due to the decomposition of the binder at the time of continuous, it is difficult to form a complete sintered body, the initial cost is high, and it is limited to the material There is a drawback of being.
特許公開昭64−28303 Patent Publication No. 64-28303
特許公開昭62−250103 Patent Publication 62-250103
特許公開平4−83802 Patent Publication 4-83802
特許公開平5−51605 Patent Publication 5-51605
そこでこの発明は、金属粉末成形に複雑形状であっても、脱脂燒結を同一炉内で脱脂燒結を行う(ONE−STEP)する事による、容易に,且つ、精度良く製品が出来る事を主たる課題としたバインダーと,同一真空炉での操作方法(ONE−STEP)、その手順である。 Therefore, the main problem of the present invention is that a product can be easily and accurately manufactured by performing degreasing and sintering in the same furnace (ONE-STEP) even if the metal powder has a complicated shape. And the operating method (ONE-STEP) in the same vacuum furnace and the procedure.
その為の手段は、成形後の脱脂・燒結を同一炉内で行うに原料紛体を成形保持し、完全な燒結体を得るバインダーとその加圧混錬する手順を特徴とする。 Means for this purpose are characterized by a procedure for forming and holding the raw material powder in order to perform degreasing and sintering after molding in the same furnace, and a procedure for kneading and pressurizing the binder.
上記バインダーは、STF20%、PW20%,CB122%、P.P32%、D.O.P6%を基準にして、金属粉末紛の流形・粒度から収縮率を求めて、バインダーの容量をコントロールする。 The binder includes STF 20%, PW 20%, CB 122%, P.I. P32%, D.I. O. Based on P6%, the shrinkage is determined from the flow shape and particle size of the metal powder powder, and the binder capacity is controlled.
その手順として、金属紛を主たる求める金属を作るには、元素周期表の左が1AグループからOグループにある。左右が離れてる元素を金属にするには、非常に困難である為に、ここに極端に離れてる場合は、元素をも金属間同士のバインダーに使用することもある。 As the procedure, in order to make a metal that mainly seeks metal powder, the left of the periodic table is in the 1A group to the O group. Since it is very difficult to make an element whose left and right sides are separated from each other, it is very difficult to use the element as a binder between metals when it is extremely far away.
金属粉末で100%の元素を使用することは非常に困難であるために、上記の元素をバインダーとして、周期表の周期と族との関係にある。 Since it is very difficult to use 100% of the element in the metal powder, there is a relationship between the period of the periodic table and the group using the above element as a binder.
例えば、比重18以上の密度を求めるとき、Wの比重の19.4は求められるが、部品としての構造,組織的には適さない、そこで、W95%,Ni2%,Cu2%,Nb1%のように周期、族を如何に混合するかにある。 For example, when obtaining a density of 18 or more, the specific gravity of W is 19.4, but it is not suitable in terms of the structure and organization of the part. Therefore, W95%, Ni2%, Cu2%, Nb1%, etc. How to mix the period and family.
混合された金属紛を形状、粒度による、バインダーとの比率を計算して、金属紛の1/2を60度に熱された混錬機に投入し、その時にSTFを1/2を投入する、30分後に残りの金属紛を投入して、30分後に残りのSTFを投入する。 Calculate the ratio of the mixed metal powder to the binder according to the shape and particle size, and put 1/2 of the metal powder into the kneader heated to 60 degrees, and then put STF at 1/2 30 minutes later, the remaining metal powder is charged, and after 30 minutes, the remaining STF is charged.
1時間経過したら、80度時にPW20%、180度になるとCB122%,1時間後にP.Pの32%を投入して,加圧すること約1時間混錬する。その後,D.O.P6%を30分加圧混練する。 After 1 hour, PW 20% at 80 degrees, CB 122% at 180 degrees, P. Add 32% of P and press for about 1 hour. Then D. O. P6% is pressure-kneaded for 30 minutes.
上記の混練物を(フィードストック)3センチ又は5センチ角にして、完全な室温になるまで冷却する、その後ペレットにするか、成形方法によっては、粉砕することも出来る。 The above-mentioned kneaded product is made into (feedstock) 3 cm or 5 cm square, cooled to complete room temperature, then pelletized, or pulverized depending on the molding method.
上記フィードストック(金属紛材料)から部品を成形されたシルバー体(燒結前)を真空燒結炉に入れて、真空炉の常温から、製品の形状によるが、昇温と時間、保持時間を設定して、バインダーとの温度が重要になる。 Put the silver body (before sintering) molded parts from the above feedstock (metal powder material) into the vacuum sintering furnace and set the temperature rise, time and holding time from room temperature of the vacuum furnace depending on the shape of the product. Thus, the temperature with the binder becomes important.
STFは金属紛に酸化防止の役目、PWは他のバインダーとの繋ぎ、CB1は粘性、PPは形状保持、DOPは400℃から金属紛の分子結合までのフィラ−(骨材)としての働きがあり、その後は、炉を開ける事無く、プログラムで700℃、900℃、1280℃、1320℃、1420℃等々に昇温、保持時間を設定して、金属によってはアルゴン、窒素、水素等を各工程で設定して、求める部品が完了する。これをMIMのONE−STEPという。 STF serves to prevent oxidation of metal powder, PW connects to other binders, CB1 serves as a viscosity, PP maintains shape, DOP functions as a filler (aggregate) from 400 ° C to molecular bond of metal powder. Yes, after that, without opening the furnace, set the temperature and hold time to 700 ° C, 900 ° C, 1280 ° C, 1320 ° C, 1420 ° C, etc., depending on the metal, argon, nitrogen, hydrogen etc. Set in the process and complete the desired part. This is called MIM's ONE-STEP.
本発明は、材料紛選択の自由度から、限定されず、金型製作の材料の選定を自由度があり、成形後の部品は同一真空燒結炉で処理する為に、脱脂工程での装置を必要としない。同一炉は雰囲気ガスにN2(窒素),アルゴンガスを使用できる、また、水素等を選択出来るようにプログラムでのコントロールすれば、脱脂・燒結を同一炉で完全な燒結体を得ることが出来る。 The present invention is not limited because of the freedom of material powder selection, and there is a degree of freedom in the selection of materials for mold production, and parts after molding are processed in the same vacuum sintering furnace. do not need. In the same furnace, N2 (nitrogen) and argon gas can be used as the atmospheric gas. If the program is controlled so that hydrogen or the like can be selected, a complete sintered body can be obtained in the same furnace for degreasing and sintering.
本発明は、実施形態を、金属紛の混合、バインダーとの加圧混練、ペレット又は、粉砕、金型使用して成形、脱脂・燒結、検査、出荷、以上が工程である。別紙に図示。 In the present invention, the steps are mixing, degreasing and sintering, inspecting, shipping, and the like of the embodiment by mixing metal powder, pressure kneading with a binder, pellets or pulverization, using a mold. Illustrated on a separate sheet.
金属粉末Ti95%、C0.5%、Cu1%、Fe2%、Nb1.5%の重量に対して、バインダー粉末STF20%、PW20%、CB122%、PP32%、DOP6%の容量を1リッター加圧混錬機に用意する。 Metal powder Ti 95%, C 0.5%,
混練内部を60℃に熱せられた容器内に、金属粉末1/2を投入し、30分混合、STFを1/2投入して、30分後に、残りの金属紛を投入する。30分温度を保ち、加圧混練。80℃になるとバインダーPWを投入、加圧混練し、180℃になると、CB1を投入して、1時間保持、その後にPPを投入して、加圧混練1時間保持、最後にDOPを投入して、1時間加圧混錬。 In a container heated to 60 ° C. inside the kneading, 1/2 metal powder is charged, mixed for 30 minutes, 1/2 STF is charged, and 30 minutes later, the remaining metal powder is charged. Keep the temperature for 30 minutes and press knead. When the temperature reaches 80 ° C., the binder PW is charged and pressure-kneaded. When the temperature reaches 180 ° C., CB1 is charged and held for 1 hour, then PP is charged and then pressure-kneaded for 1 hour, and finally DOP is charged. 1 hour press kneading.
上記加圧混練後、室内温度まで冷却、そのペレットを3〜5cm角にして、ペレット又は、粉砕する。成形機の状態にする為。 After the above-mentioned pressure kneading, the mixture is cooled to room temperature, and the pellets are made into 3 to 5 cm square and pulverized or pulverized. To make it a state of a molding machine.
成形機に幅10mm x 長さ12mm x 厚2mm形状の試験片を成形して、真空燒結炉に入れて、脱脂・燒結を12時間で行い、最高温度は1100℃、45分保持、その時の炉内は2x10−5Torrの真空である。 A test piece of width 10mm x length 12mm x thickness 2mm is molded into a molding machine, put into a vacuum sintering furnace, degreased and sintered in 12 hours, the maximum temperature is kept at 1100 ° C for 45 minutes, the furnace at that time The inside is a vacuum of 2 × 10 −5 Torr.
近年、金属粉末やセラミックの完成品は一般工業材料から電子部品、光ファイバー部品、耐熱性材料、耐食性材料等に至るまで広く利用されるようになってきた。これら製品の寸法精度、物性、形状等に厳しい要求がなされるようになった。このような要求に対処するためにバインダーの開発、このバインダーを摘出する(脱脂)工程、燒結工程を同時に行うことによる、イニシャルコスト削減により、従来加工できずに、溶接、他の機械加工分野にも簡単に、参入出来、業界の発展に大いに期待される。 In recent years, finished products of metal powder and ceramic have been widely used from general industrial materials to electronic parts, optical fiber parts, heat resistant materials, corrosion resistant materials and the like. Strict demands have been made on the dimensional accuracy, physical properties, shape, etc. of these products. Development of binders to cope with these requirements, simultaneous removal of this binder (degreasing), and sintering process, reducing initial costs, making it difficult to perform conventional processing, and welding and other machining fields It is easy to enter and is highly expected for the development of the industry.
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CN103231058A (en) * | 2013-05-13 | 2013-08-07 | 中原工学院 | Preparation method of high temperature silicon molybdenum rods |
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CN103231058A (en) * | 2013-05-13 | 2013-08-07 | 中原工学院 | Preparation method of high temperature silicon molybdenum rods |
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