JP2007180373A - METHOD OF MANUFACTURING NdFeB-BASED SINTERED MAGNET, AND MOLD FOR MANUFACTURING NdFeB-BASED SINTERED MAGNET - Google Patents
METHOD OF MANUFACTURING NdFeB-BASED SINTERED MAGNET, AND MOLD FOR MANUFACTURING NdFeB-BASED SINTERED MAGNET Download PDFInfo
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Abstract
Description
この発明は、NdFeB系焼結磁石の製造方法に関し、特に、NdFeB系焼結磁石用合金粉末（以下これを合金粉末という）を、製品の形状と寸法に対応して設計された容器（以下これをモールドという）に充填し、この合金粉末に磁界を印加して粉末の結晶方向をそろえ、合金粉末を入れたまま容器ごと加熱、焼結して所望の形状のNdFeB系焼結磁石を得る方法に関るものである。 The present invention relates to a method for producing a NdFeB-based sintered magnet, and in particular, an NdFeB-based sintered magnet alloy powder (hereinafter referred to as an alloy powder) is a container designed according to the shape and dimensions of a product (hereinafter referred to as this). To obtain a NdFeB sintered magnet of the desired shape by applying a magnetic field to the alloy powder, aligning the crystal orientation of the powder, and heating and sintering the entire container with the alloy powder in place. It is concerned.
従来の技術は、平均粒度2〜5μmの合金粉末を、充填密度が2.7g/cm3〜3.5g/cm3になるようにモールドに充填し、モールド上面にふたを載置して、粉末に磁界を印加して配向し、その後焼結して焼結体をモールドから取出して、時効処理するものであった。その内容は特許文献１に示されている。ここで前記平均粒度は、特許文献１には明記されていないが、この文献の出願時に広く用いられていたFisher法により測定されたものと考えられる。 The prior art, the alloy powder having an average particle size of 2 to 5 [mu] m, the filling density is charged into the mold so as to 2.7g / cm 3 ~3.5g / cm 3 , and placing the lid on the mold upper surface, a powder A magnetic field was applied for orientation, followed by sintering, and the sintered body was removed from the mold and subjected to an aging treatment. The contents are shown in Patent Document 1. Here, although the said average particle size is not specified in patent document 1, it is thought that it was measured by the Fisher method widely used at the time of the application of this literature.
本発明は特許文献１の技術を実施する過程で、この技術の重大な問題に気づいた。それは、合金粉末をモールドに充填して焼結するとき、合金粉末とモールドとの反応を抑えることができないことである。特許文献１には、未反応性金属容器を使用することが述べられており、「原料粉末との反応性が低く、耐熱性のすぐれた金属であればよく、Mo、W、Ta、Pt、Crなどが好ましく」とある。本発明者はこのいずれの材料の金属を使用しても焼結後に焼結体のモールド内面への溶着が起こり、焼結体をモールドから取出すことができなくなること、およびモールドが1回あるいは数回の使用で再使用不能になってしまうことを見出した。モールドを再利用し、多数回使用することができなければ、この方法によって生産されるNdFeB焼結磁石の価格が増大してしまう。工業技術として、価格の低減はきわめて重要であり、モールドの多数回使用は本技術を工業的に使用するためにどうしても必要である。 In the process of implementing the technique of Patent Document 1, the present invention noticed a serious problem of this technique. That is, when the alloy powder is filled in the mold and sintered, the reaction between the alloy powder and the mold cannot be suppressed. Patent Document 1 states that an unreactive metal container is used, and “a metal having low reactivity with raw material powder and excellent heat resistance may be used. Mo, W, Ta, Pt, Cr and the like are preferable. " The present inventor uses any of these metal materials to cause the sintered body to be welded to the inner surface of the mold after sintering, and the sintered body cannot be removed from the mold. It was found that it could not be reused after each use. If the mold cannot be reused and used many times, the price of the NdFeB sintered magnet produced by this method will increase. As an industrial technology, cost reduction is extremely important, and multiple use of molds is absolutely necessary for industrial use of this technology.
本発明が解決しようとする課題は、焼結後に焼結体がモールドに溶着することのないNdFeB系焼結磁石の製造方法を提供することにある。 The problem to be solved by the present invention is to provide a method for producing an NdFeB-based sintered magnet in which a sintered body is not welded to a mold after sintering.
本発明者はいろいろな耐熱材料と合金粉末の反応性を調査した結果、TiN（窒化チタン）、BN（窒化硼素）やAl2O3（アルミナ）などのセラミック材料は比較的合金粉末との反応性が低いことを見い出した。しかし、これらのセラミック材料を主材料としてモールドを作ることは困難である。その理由は、第1に、所望形状のモールド作製に時間と労力がかかり高価なものになってしまうこと、第2に、本技術ではモールドに合金粉末を高密度に充填する必要があり、そのためにモールドに機械的タッピングを加える必要があるが、そのとき、セラミック材料でできたモールドは破損しやすいことである。
本技術では製品の所望形状に合わせてモールドを比較的高精度に作製する必要がある。そのため、切削加工あるいは深絞りなどの塑性加工といった高精度の加工ができるステンレスなどの金属材料でモールドを作製することが望ましい。本発明者は、このような高精度の加工が安価にできるモールドを使用し、その内面にセラミックなどのコーティングを施すことにより、繰返し使用できる安価で高精度で機械的に強いモールドが作製できることを見い出した。
As a result of investigating the reactivity of various heat-resistant materials and alloy powders, the present inventors have found that ceramic materials such as TiN (titanium nitride), BN (boron nitride), and Al 2 O 3 (alumina) react relatively with alloy powders. I found that the nature is low. However, it is difficult to make a mold using these ceramic materials as a main material. The reason for this is that, firstly, it takes time and effort to produce a mold having a desired shape, and it becomes expensive, and secondly, in this technology, it is necessary to fill the mold with alloy powder at a high density. It is necessary to add mechanical tapping to the mold, and at that time, the mold made of ceramic material is easily damaged.
In this technique, it is necessary to produce a mold with relatively high accuracy in accordance with a desired shape of a product. Therefore, it is desirable to produce a mold with a metal material such as stainless steel that can be processed with high precision such as plastic working such as cutting or deep drawing. The present inventor uses such a mold that can be processed with high accuracy at a low cost, and by applying a coating such as ceramic on the inner surface thereof, it is possible to produce a low-cost, high-accuracy and mechanically strong mold that can be used repeatedly. I found it.
ステンレス製モールドを切削加工で作り、モールド内面にいろいろな耐熱材料をコーティングして、合金粉末との焼結温度付近での反応性を調べた。その結果TiN、BNやアルミナなど各種セラミック材料のコーティングがモールドと合金粉末との溶着を抑制する効果があることを見い出した。これらのコーティングはCVD法やイオンプレーティング法、あるいは溶射法によって行われる。モールド内面にコーティングするために、モールドを組立て式にしておいて、モールド内面に当たる面にコーティングを施した後モールドに組立てるようにしてもよい。 Stainless steel molds were made by cutting, and various heat resistant materials were coated on the inner surface of the mold, and the reactivity with the alloy powder near the sintering temperature was investigated. As a result, it was found that coatings of various ceramic materials such as TiN, BN, and alumina have the effect of suppressing welding between the mold and the alloy powder. These coatings are performed by CVD, ion plating, or thermal spraying. In order to coat the inner surface of the mold, the mold may be assembled so that the surface that contacts the inner surface of the mold is coated and then assembled into the mold.
モールド内面にコーティングを施した後、そのモールドに合金粉末を充填して磁界配向した後に焼結することにより、焼結体はモールドに溶着することなく、容易に取出すことができる。その後、適当な熱処理を施すことにより、高性能のNdFeB焼結磁石を得ることができる。 After coating the inner surface of the mold, filling the mold with alloy powder and orienting the magnetic field, and then sintering, the sintered body can be easily taken out without welding to the mold. Thereafter, by performing an appropriate heat treatment, a high-performance NdFeB sintered magnet can be obtained.
更に、本発明者は最も望ましいコーティングはつぎのようなものであることを発見した。それはモールドをステンレスなどの切削加工や塑性加工できる金属で作製した後、そのモールドの内面に、焼結処理のための加熱を行う度に破壊されて消耗するコーティング（消耗型コーティング）を施すことである。この場合、焼結処理の度に毎回コーティングを行う。コーティングのコストは以下に述べる方法により安価に抑えることができるため、焼結処理の度に毎回コーティングを行っても、最終製品であるNdFeB焼結磁石の価格はほとんど増加しない。 In addition, the inventor has discovered that the most desirable coating is: This is because the mold is made of a metal that can be cut or plastically processed, such as stainless steel, and then the inner surface of the mold is subjected to a coating (consumable coating) that is destroyed and consumed every time heating for the sintering process is performed. is there. In this case, coating is performed every time the sintering process is performed. Since the cost of coating can be kept low by the method described below, the price of the final NdFeB sintered magnet hardly increases even if coating is performed each time the sintering process is performed.
消耗型コーティングの典型的な構成はセラミック粉体と樹脂の混合物からなるものである。このようなコーティングはつぎのような方法によって形成される。
（1）モールド内面に粘着性の樹脂を薄く塗付し、その上にセラミック粉末を押しつけて塗布する。
（2）モールド内面に、粘着性の樹脂とセラミック粉末の混合物を塗付する。
A typical configuration for a consumable coating consists of a mixture of ceramic powder and resin. Such a coating is formed by the following method.
(1) Apply a thin layer of adhesive resin to the inner surface of the mold, and press the ceramic powder onto it.
(2) Apply a mixture of adhesive resin and ceramic powder to the inner surface of the mold.
上記（1）の方法において、粘着性樹脂の塗付方法として特開2004-359873号公報に記載のインパクトメディアを使う方法が有効である。この方法によってモールド内面に粘着層を形成した後、特開平05-302176号公報に記載されている方法によりセラミック粉体をインパクトメディアにより粘着層中に埋めこむことによりセラミック粉体層を形成することができる。 In the above method (1), a method using impact media described in JP-A-2004-359873 is effective as a method for applying the adhesive resin. After forming the adhesive layer on the inner surface of the mold by this method, the ceramic powder layer is formed by embedding the ceramic powder in the adhesive layer with impact media by the method described in JP-A No. 05-302176. Can do.
上記（2）の方法においても、特開2004-359873号公報に記載の方法を使用して、モールド内面にセラミック粉末を含む樹脂コーティングを施すことができる。すなわちセラミック粉末と液状樹脂およびインパクトメディアの混合体をモールド内に注入し、この混合体を振動撹拌させてモールド内面にセラミック粉末と樹脂の混合物の膜を形成する。これにより、能率的なコーティングができる。 Also in the method (2), a resin coating containing ceramic powder can be applied to the inner surface of the mold using the method described in JP-A-2004-359873. That is, a mixture of ceramic powder, liquid resin, and impact media is poured into a mold, and this mixture is vibrated and stirred to form a film of a mixture of ceramic powder and resin on the inner surface of the mold. Thereby, efficient coating can be performed.
これらのコーティングはセラミックと樹脂の混合体であるが、樹脂として未硬化の熱硬化性樹脂を使用することができる。この場合、熱硬化性樹脂とセラミック粉体の混合体の膜をモールド内面に形成した後、樹脂の硬化温度以上に加熱して、膜をモールド内面に固着させる。 These coatings are a mixture of ceramic and resin, but uncured thermosetting resin can be used as the resin. In this case, after a film of a mixture of thermosetting resin and ceramic powder is formed on the inner surface of the mold, the film is fixed to the inner surface of the mold by heating to a temperature higher than the curing temperature of the resin.
上記（1）の方法において、液状樹脂を塗付して粘着層を形成した後にセラミック粉体をインパクトメディアによって粘着層中に埋めこむとき、セラミック粉末に少量の粉体樹脂を混ぜておくこともできる。粉体層を形成した後、加熱して液状樹脂と粉体樹脂の両方を硬化させることにより、モールド内面に強固なセラミックと樹脂の混合物の膜が形成できる。 In the above method (1), after embedding the liquid resin and forming the adhesive layer, when embedding the ceramic powder in the adhesive layer with impact media, a small amount of powder resin may be mixed with the ceramic powder. it can. After the powder layer is formed, both the liquid resin and the powder resin are cured by heating, whereby a strong ceramic and resin mixture film can be formed on the inner surface of the mold.
上述の（1）、（2）の方法において、粘着性樹脂として、熱可塑性樹脂を使うことも可能である。そのためには、コーティングのときの温度を、熱可塑性樹脂の融点以上に上げておく必要がある。例えば50℃の融点をもつワックスを使用するときには、インパクトメディアと少量の、融点が50℃のワックスおよびセラミック粉末の混合体をモールドのキャビティー中に入れ、全体を50℃より少し高い温度に加熱してモールドを振動させる。こうして内面に液状樹脂とセラミック粉末の混合物の膜が形成される。その後モールドからインパクトメディアを出して、モールドを室温にすると、モールド内面にセラミック粉末と樹脂の混合物の膜が形成される。 In the above methods (1) and (2), it is also possible to use a thermoplastic resin as the adhesive resin. For that purpose, it is necessary to raise the temperature at the time of coating above the melting point of the thermoplastic resin. For example, when using a wax with a melting point of 50 ° C., place the impact media and a small amount of a mixture of wax and ceramic powder with a melting point of 50 ° C. into the mold cavity and heat the whole to a temperature slightly higher than 50 ° C. Then, the mold is vibrated. Thus, a film of a mixture of liquid resin and ceramic powder is formed on the inner surface. Thereafter, when the impact media is taken out from the mold and the mold is brought to room temperature, a film of a mixture of ceramic powder and resin is formed on the inner surface of the mold.
上述した方法でセラミック粉末と樹脂の混合物の膜をモールド内面に形成した後、このモールドに合金粉末を高密度に充填し、これを磁界配向、加熱して合金粉末を焼結する。この加熱により、まずモールド内面のコーティング中の樹脂が蒸発あるいは分解してセラミック粉末だけが残る。このセラミック粉末により、合金粉末の焼結時に形成される液状のNdリッチ相とモールド材料が直接接触することが阻止されるため、焼結体はモールドに溶着することなく生成される。焼結体をモールドから取出すとき、セラミック粉末の一部は焼結体表面に付着し、他はモールド内に粉体として残る。モールドを再使用するときには、この残留した粉体を圧縮空気などで吹きとばして、再度上述の（1）あるいは（2）の方法によってセラミック粉末と樹脂の混合物の膜を形成する。セラミック粉末としては、BN、アルミナ、ジルコニア等、融点がNdFeB焼結磁石の焼結温度以上のあらゆる種類のセラミック粉末を使用することができる。マイカ（雲母）やタルク（滑石）などの粉末も使用できる。
なお上述のセラミック粉体のかわりに、MoやWなどの、融点がNdFeB焼結磁石の焼結温度以上の金属の粉末を使うこともできる。また、上述の樹脂と無機物質の粉末との混合物のコーティングは、インパクトメディアを用いた方法の他に、無機物質の粉末と樹脂を溶剤と混合してスプレー法で膜形成を行うこと等によって形成することもできる。
After the film of the mixture of ceramic powder and resin is formed on the inner surface of the mold by the above-described method, the mold is filled with the alloy powder with high density, and this is magnetically oriented and heated to sinter the alloy powder. This heating first evaporates or decomposes the resin in the coating on the inner surface of the mold, leaving only the ceramic powder. This ceramic powder prevents the liquid Nd-rich phase formed during sintering of the alloy powder from coming into direct contact with the mold material, so that the sintered body is generated without welding to the mold. When the sintered body is taken out of the mold, a part of the ceramic powder adheres to the surface of the sintered body and the other remains as a powder in the mold. When the mold is reused, the remaining powder is blown off with compressed air or the like, and a film of a mixture of ceramic powder and resin is formed again by the above method (1) or (2). As the ceramic powder, any kind of ceramic powder such as BN, alumina, zirconia and the like whose melting point is higher than the sintering temperature of the NdFeB sintered magnet can be used. Powders such as mica (mica) and talc (talc) can also be used.
In place of the above ceramic powder, a metal powder such as Mo or W having a melting point equal to or higher than the sintering temperature of the NdFeB sintered magnet can be used. In addition to the above-mentioned method using impact media, the coating of the mixture of the resin and the inorganic substance powder is formed by mixing the inorganic substance powder and the resin with a solvent to form a film by a spray method or the like. You can also
（発明の効果）
本発明により、NdFeB焼結磁石の用途として最重要な形状の製品が焼結体とモールドとの溶着の問題なく量産できるようになり、モールドが繰返し再利用できるので、このような製品を低価格で生産できるようになった。
(The invention's effect)
The present invention makes it possible to mass-produce products with the most important shape for NdFeB sintered magnet applications without the problem of welding between the sintered body and the mold, and the mold can be reused repeatedly. Can now be produced.
本発明に係るNdFeB焼結磁石の製造方法の第１実施例について説明する。まず、非磁性ステンレスSUS304、およびモリブデンでキャビティー内径23mm、深さ6mm、肉厚2mmの円柱形モールドを作製した。またステンレスモールドに、イオンプレーティング法でTiNのコーティングを、CVD法でアルミナのコーティングを、それぞれ施した。このように作製した、本実施例の(1)TiNコーティングを施したステンレスモールド、及び、(2)アルミナコーティングを施したステンレスモールド、並びに、比較例の(3)コーティングのないステンレスモールド、及び、(4)コーティングのないモリブデンモールドについて、焼結テストを行った。合金粉末として重量比で31.5％Nd、1％B、0.2％Al、0.1％Cu、残部Feの組成を持ち、レーザー式粒度分布計で測定した粉末の平均粒径の中央値D50＝2.9μmのNdFeB焼結磁石用粉末を使用した。この合金粉末にカプロン酸メチルを0.5％添加して、撹拌混合した。カプロン酸メチルを混ぜた上記合金粉末を、上述の4種類のモールドに、充填密度3.7g/cm3になるように充填し、ふたをして、パルス磁界を円柱状キャビティーの軸方向に印加した。その後合金粉末をモールドごと真空中で、975℃に加熱して焼結した。焼結後冷却してモールドのふたを開けると、比較例（コーティングを施さないもの）については、ステンレス製も、モリブデン製も両方モールドに焼結体が溶着していた。焼結体を強く引っぱってモールドから引離すと、焼結体を取出すことができたが、焼結体表面に大きい傷が生じてしまった。それに対して、本実施例のTiNおよびアルミナのコーティングを施したものについては、焼結体をモールドから容易に取出すことができた。 A first embodiment of the method for producing a sintered NdFeB magnet according to the present invention will be described. First, a cylindrical mold having a cavity inner diameter of 23 mm, a depth of 6 mm, and a wall thickness of 2 mm was made of nonmagnetic stainless steel SUS304 and molybdenum. Stainless steel molds were coated with TiN by ion plating and alumina by CVD. Stainless steel mold with (1) TiN coating of this example, and (2) stainless steel mold with alumina coating, and (3) uncoated stainless steel mold of comparative example, and (4) A sintering test was performed on the molybdenum mold without coating. The median value D 50 = 2.9 μm of the average particle diameter of the powder having a composition of 31.5% Nd, 1% B, 0.2% Al, 0.1% Cu and the balance Fe as the alloy powder and measured with a laser type particle size distribution meter NdFeB sintered magnet powder was used. 0.5% of methyl caproate was added to the alloy powder and mixed with stirring. The above alloy powder mixed with methyl caproate is filled in the above four types of molds to a packing density of 3.7 g / cm 3 , covered, and a pulsed magnetic field is applied in the axial direction of the cylindrical cavity did. Thereafter, the alloy powder was sintered together with the mold by heating to 975 ° C. in vacuum. When the mold lid was opened after cooling after sintering, the sintered bodies were welded to the molds of both the stainless steel and the molybdenum for the comparative example (those not coated). When the sintered body was pulled strongly and separated from the mold, the sintered body could be taken out, but a large scratch was generated on the surface of the sintered body. On the other hand, the sintered body could be easily taken out of the mold for the TiN and alumina coatings of this example.
本発明に係るNeFeB焼結磁石の製造方法の第２実施例を、図１〜図３を用いて説明する。まず、融点が50℃のロウ１１と平均粒径5μmのBN粉末１２を重量比で60：40に混合し、この混合物2.5gを直径0.5mmのジルコニアボール１３（インパクトメディア）1kgに添加して混合した（図１(a)）。この混合体１４を、容量が500ccで金属製のビーカ１５に入れて80℃に加熱し、ビーカ１５を揺動させて、混合体を撹拌した(b)。その後混合体１４を各種形状のパーマロイ製モールド１６に入れ(c)、モールド１６を揺動させた(d)後、モールド１６から混合体１４を出して室温に冷却した。これにより、モールド１６の内面に粉体とロウの混合物から成るコーティング膜１７を形成した(e)。 The 2nd Example of the manufacturing method of the NeFeB sintered magnet which concerns on this invention is described using FIGS. 1-3. First, wax 11 having a melting point of 50 ° C. and BN powder 12 having an average particle diameter of 5 μm are mixed at a weight ratio of 60:40, and 2.5 g of this mixture is added to 1 kg of zirconia balls 13 (impact media) having a diameter of 0.5 mm. Mixed (FIG. 1 (a)). The mixture 14 was placed in a metal beaker 15 having a capacity of 500 cc and heated to 80 ° C., the beaker 15 was swung, and the mixture was stirred (b). Thereafter, the mixture 14 was put in a permalloy mold 16 having various shapes (c), and the mold 16 was swung (d), and then the mixture 14 was taken out from the mold 16 and cooled to room temperature. As a result, a coating film 17 made of a mixture of powder and wax was formed on the inner surface of the mold 16 (e).
このようにしてコーティングされたモールド１６に、実施例１と同様に作製した合金粉末１８を充填密度が3.7g/cm3になるように充填し(f)、磁界を印加して合金粉末１８を配向した(g)後、合金粉末１８が入ったモールド１６を975℃に加熱(h)して合金粉末の焼結体１９を作製した(i)。この焼結後の焼結体１９はモールドに全く溶着していなかった。このサイクルを30回繰返してもモールド１５の変形や溶着によるモールド１５の損傷は起こらなかった。繰り返し使用後のモールド１６及びこれらのモールドにより作製された焼結体１９を図２に示す。図の上側に示したものがモールドであり、左から順に、板状磁石を１個作製するためのモールド１６１、棒状磁石を１個作製するためのモールド１６２、弓形の板状磁石を多数個作製するための多数個取りモールド１６３、平板状の磁石用の多数個取りモールド１６４である。図の下側には、それぞれのモールドで作製した磁石１９１〜１９４を示す。 The mold 16 coated in this way is filled with the alloy powder 18 produced in the same manner as in Example 1 so that the packing density is 3.7 g / cm 3 (f), and a magnetic field is applied to form the alloy powder 18. After orientation (g), the mold 16 containing the alloy powder 18 was heated to 975 ° C. (h) to produce a sintered body 19 of the alloy powder (i). The sintered body 19 after the sintering was not welded to the mold at all. Even when this cycle was repeated 30 times, the mold 15 was not damaged or deformed by welding. FIG. 2 shows the mold 16 after repeated use and the sintered body 19 produced by these molds. The mold shown in the upper part of the figure is a mold, and in order from the left, a mold 161 for producing one plate-shaped magnet, a mold 162 for producing one bar-shaped magnet, and many arc-shaped plate-shaped magnets are produced. A multi-cavity mold 163 for performing the process, and a multi-cavity mold 164 for a plate-like magnet. On the lower side of the figure, magnets 191 to 194 manufactured with respective molds are shown.
図２に示したモールドのうち、多数個取りモールドについては、図３に示すように、各キャビティーのしきり板２１は、外側の枠に切った溝にはめこんで保持されている。これらのしきり板２１をはめこんだ後で、上述のインパクトメディアによる膜形成を行うと、しきり板２１と両側の外枠２２で形成されるコーナー部に膜形成ができない。そのため、しきり板２１を全部はずした状態で、外枠２２だけでキャビティーのコーティングを行うと共に、しきり板２１は別の容器中で全面に膜を形成し、その後外枠２２にしきり板２１をはめこんだ。これにより、内面全面にBNとロウでできた膜が形成された多数個取りモールド２４を得た。このように、コーティングを施したモールドを用いることにより、図２に示すように、多数個の焼結体を一度に、全く溶着の問題もなく作製することができた。 Among the molds shown in FIG. 2, as for the multi-cavity mold, as shown in FIG. 3, the cutting plate 21 of each cavity is held by being fitted in a groove cut in the outer frame. If the above-mentioned impact media is used to form a film after fitting these threshold plates 21, the film cannot be formed at the corners formed by the threshold plate 21 and the outer frames 22 on both sides. For this reason, the cavity plate is coated only with the outer frame 22 in a state in which all of the threshold plate 21 is removed, and the threshold plate 21 forms a film on the entire surface in another container, and then the outer plate 22 is covered with the threshold plate 21. I was in. As a result, a multi-piece mold 24 in which a film made of BN and solder was formed on the entire inner surface was obtained. In this way, by using the coated mold, as shown in FIG. 2, a large number of sintered bodies could be produced at one time without any problem of welding.
上述のコーナー部の膜形成ができないという問題を避け、本発明のインパクトメディアを使うコーティングを行うのに都合が良いように、モールド内面にはインパクトメディアの半径より小さいコーナー部を持つ部分がないようにモールドを設計し、作製すると、モールド内面を一度に（しきり板をとりはずさなくても）膜形成ができる。 In order to avoid the above-mentioned problem that the film cannot be formed on the corner portion and to be convenient for coating using the impact media of the present invention, there is no portion having a corner portion smaller than the radius of the impact media on the inner surface of the mold. If a mold is designed and manufactured, a film can be formed on the inner surface of the mold at once (without removing the cutting plate).
１１…ロウ
１２…BN粉末
１３…ジルコニアボール（インパクトメディア）
１４…ロウ・BN粉末・インパクトメディア混合体
１５…ビーカ
１６…モールド
１７…コーティング膜
１８…合金粉末
１９…焼結体
２１…しきり板
２２…外枠
11 ... wax 12 ... BN powder 13 ... zirconia ball (impact media)
14 ... wax / BN powder / impact media mixture 15 ... beaker 16 ... mold 17 ... coating film 18 ... alloy powder 19 ... sintered body 21 ... slit plate 22 ... outer frame
Claims (6)
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| WO2013166103A1 (en) * | 2012-05-01 | 2013-11-07 | United Technologies Corporation | Metal powder casting |
| CN103551563A (en) * | 2013-10-11 | 2014-02-05 | 南通万宝磁石制造有限公司 | REPM (rear earth permanent magnet) material recycling method |
| JPWO2015012412A1 (en) * | 2013-07-24 | 2017-03-02 | Ｎｄｆｅｂ株式会社 | Rare earth sintered magnet manufacturing method and rare earth sintered magnet sintering mold |
| CN106653343A (en) * | 2015-10-29 | 2017-05-10 | 威乐欧洲股份公司 | Method and apparatus for producing permanent magnets |
| US9831034B2 (en) | 2007-08-20 | 2017-11-28 | Intermetallics Co., Ltd. | Method for making NdFeB sintered magnet and mold for making the same |
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| US9831034B2 (en) | 2007-08-20 | 2017-11-28 | Intermetallics Co., Ltd. | Method for making NdFeB sintered magnet and mold for making the same |
| WO2013166103A1 (en) * | 2012-05-01 | 2013-11-07 | United Technologies Corporation | Metal powder casting |
| US9475118B2 (en) | 2012-05-01 | 2016-10-25 | United Technologies Corporation | Metal powder casting |
| JPWO2015012412A1 (en) * | 2013-07-24 | 2017-03-02 | Ｎｄｆｅｂ株式会社 | Rare earth sintered magnet manufacturing method and rare earth sintered magnet sintering mold |
| CN103551563A (en) * | 2013-10-11 | 2014-02-05 | 南通万宝磁石制造有限公司 | REPM (rear earth permanent magnet) material recycling method |
| CN103551563B (en) * | 2013-10-11 | 2016-02-17 | 南通万宝磁石制造有限公司 | A kind of regeneration method of rare earth permanent-magnetic material |
| CN106653343A (en) * | 2015-10-29 | 2017-05-10 | 威乐欧洲股份公司 | Method and apparatus for producing permanent magnets |
| CN106653343B (en) * | 2015-10-29 | 2020-06-16 | 威乐欧洲股份公司 | Method and apparatus for manufacturing permanent magnet |
| CN111809100A (en) * | 2020-07-17 | 2020-10-23 | 西安交通大学 | NiCrAlY high-temperature sintered ZTA particle reinforced steel-based composite material and preparation method thereof |
| CN111809100B (en) * | 2020-07-17 | 2022-02-11 | 西安交通大学 | NiCrAlY high-temperature sintered ZTA particle reinforced steel-based composite material and preparation method thereof |
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