KR100961220B1 - Fe-Sn-B AMORPHOUS ALLOY - Google Patents
Fe-Sn-B AMORPHOUS ALLOY Download PDFInfo
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Abstract
본 발명에 의한 비정질합금은 FexSnyBz으로 표시되고 상기 일반식에서 x, y, z는 각각 원자%이며, x, y, z의 합은 100인 것을 특징으로 한다.The amorphous alloy according to the present invention is represented by Fe x Sn y B z and in the general formula, x, y, z are each atomic%, characterized in that the sum of x, y, z is 100.
본 발명에 의한 비정질 합금은 3원자계 비정질 합금으로서, 철-보론 2원자계 비정질 합금에 비하여 보론의 함량을 줄이면서도 주석을 포함함에 따라 우수한 비정질 성능을 가진다.The amorphous alloy according to the present invention is a triatomic amorphous alloy, and has an excellent amorphous performance as it contains tin while reducing the boron content as compared to the iron-boron biatomic amorphous alloy.
비정질, 철-주석-보론, 큐리온도 Amorphous, Iron-Tin-Boron, Curie
Description
본 발명은 우수한 비정질 특성을 가지는 철-주석-보론 비정질 합금에 대한 것이다.The present invention relates to an iron-tin-boron amorphous alloy having good amorphous properties.
비정질 합금은 단범위 규칙도(Short-range order)를 갖는 합금으로서, 액상금속에서의 원자구조와 유사한 원자배열을 가진 채 유리전이온도(glass transition temperature) 이하로 냉각되어 굳은 고체이다.Amorphous alloys are alloys with short-range order, and are solidified by cooling below the glass transition temperature with an atomic arrangement similar to the atomic structure in liquid metals.
비정질 합금은 연자기 특성, 고내식성, 고강도 등 공업적으로 유용한 특성을 많이 가지고 있어, 전기배전(elctric distribution), 전력변압기(power transformers)제조용 자성코어 등 각종 자기장치에 사용되고 있다.Amorphous alloys have many industrially useful properties such as soft magnetic properties, high corrosion resistance, and high strength, and are used in various magnetic devices, such as magnetic cores for electric distribution and power transformers manufacturing.
특히 연자기 특성을 가지는 비정질 합금은 자화곡선의 직선성이 높고, 다양한 크기의 외부 바이어스 자장이 인가되어도 자기적 포화가 일어나지 않으며, 고주파 영역에서도 우수한 특성을 지니고 있다.In particular, amorphous alloys having soft magnetic properties have a high linearity in the magnetization curve, do not generate magnetic saturation even when an external bias magnetic field of various sizes is applied, and has excellent characteristics even in a high frequency region.
종래에는 비정질 합금으로 이원합금인 철-보론 합금이 알려져 왔는데, 이는 높은 포화자기값을 나타낸다. 그러나, 철-보론 합금은 비정질형태로 주조하기 어렵고, 코어손실 및 여자전력 요구치는 최소한으로만 수용하는 것으로 알려져 있어 주 조성 안정성 및 향상된 자기적 성능을 갖는 합금의 개발이 요구되고 있다.Conventionally, iron-boron alloys, which are binary alloys, have been known as amorphous alloys, which exhibit high saturation magnetic values. However, iron-boron alloys are difficult to cast in amorphous form, and the core loss and excitation power requirements are known to accept only minimally, and therefore, development of alloys having main compositional stability and improved magnetic performance is required.
또한, 보론의 경우 약 15~26원자%정도가 포함되는 경우 비정질 특성이 우수하고 보론의 함량이 증가할수록 비정질 특징이 우수한데, 보론은 값비싼 원료이기 때문에 그 함량을 줄이면서도 우수한 비정질 특성을 나타낼 수 있는 합금의 개발이 요구되고 있다.In addition, in the case of boron containing about 15 to 26 atomic%, the amorphous property is excellent and the amorphous property is excellent as the content of boron increases.Boron is an expensive raw material, so it shows excellent amorphous properties while reducing its content. There is a demand for development of an alloy that can be used.
본 발명이 해결하고자 하는 과제는 열적특성 및 자기적 특성이 우수한 철-주석-보론 비정질 합금을 제공하는 것이다.The problem to be solved by the present invention is to provide an iron-tin-boron amorphous alloy excellent in thermal and magnetic properties.
본 발명에 의한 철-주석-보론 비정질합금은 일반식 FexSnyBz로 표시되고, x, y, z는 원자%를 나타내고, x, y, z의 합은 100인 것을 특징으로 한다.The iron-tin-boron amorphous alloy according to the present invention is represented by the general formula Fe x Sn y B z , x, y, z represents the atomic%, the sum of x, y, z is characterized in that 100.
또한, 보론의 원자%인 z는 14 내지 16이고, 철의 원자%인 x와 주석의 원자%인 y의 합은 85 내지 86일 수 있다.In addition, the atomic percentage z of boron is 14 to 16, and the sum of x which is the atomic% of iron and y which is the atomic% of tin may be 85 to 86.
또한, 주석의 원자%인 y는 1 내지 3일 수 있다.In addition, y, which is the atomic% of tin, may be 1 to 3.
또한, 철의 원자%인 x는 82 내지 85인 것을 특징으로 할 수 있다.In addition, x which is an atomic% of iron may be characterized in that 82 to 85.
또한, 보론의 원자%인 z는 14 내지 16이고, 철의 원자%인 x와 주석의 원자%인 y의 합은 85 내지 86이고, 주석의 원자%인 y는 1 내지 3인 것을 특징으로 할 수 있다.In addition, the atomic percentage z of boron is 14 to 16, the sum of x of atomic% of iron and y of atomic% of tin is 85 to 86, and y of atomic% of tin is 1 to 3. Can be.
본 발명에 의한 초크코일은 본 발명에 의한 비정질 합금을 자기코어로 포함한다.The choke coil according to the present invention includes the amorphous alloy according to the present invention as a magnetic core.
본 발명에 따르면 우수한 비정질 특성을 나타내는 철-주석-보론 비정질 합금을 제공할 수 있다.According to the present invention, it is possible to provide an iron-tin-boron amorphous alloy exhibiting excellent amorphous properties.
본 발명에 의한 비정질 합금은 철-주석-보론 비정질 합금으로서, 일반식 FexSnyBz으로 표시되고 상기 일반식에서, x, y, z는 각각 원자%(atomic%)로서, x, y, z의 합은 100이다.The amorphous alloy according to the present invention is an iron-tin-boron amorphous alloy, represented by the general formula Fe x Sn y B z , in which x, y, z are atomic% (atomic%), respectively, x, y, The sum of z is 100.
또한, 본 발명에 의한 비정질 합금의 보론의 원자%인 z는 14 내지 16이고, 철의 원자%인 x와 주석의 원자%인 y의 합은 84 내지 86일 수 있다.In addition, the atomic percentage z of boron of the amorphous alloy according to the present invention may be 14 to 16, and the sum of x which is the atomic% of iron and y which is the atomic% of tin may be 84 to 86.
기존의 철-보론 비정질 합금에서는 보론의 함량이 15~26%의 범위로 한정되어 왔는데, 이는 보론의 함량이 그보다 적은 경우에는 비정질 형성능이 우수하지 않기 때문이다. 즉, 비정질 합금을 형성하지 못하고 결정 구조를 가지는 합금이 제조되므로 원하고자 하는 연자기적 특성을 나타내지 못하게 된다.In the conventional iron-boron amorphous alloy, the content of boron has been limited to the range of 15 to 26%, because the amorphous formability is not excellent when the boron content is less than that. That is, since the alloy having a crystal structure is not formed without forming an amorphous alloy, it does not exhibit the desired soft magnetic properties.
그런데, 보론은 매우 값비싼 원료이므로 이의 함량을 줄이면서도 비정질 특성이 우수한 합금의 제조가 요구되어지고 있다.However, since boron is a very expensive raw material, it is required to produce an alloy having excellent amorphous properties while reducing its content.
또한 주석의 함량이 3원자%를 초과하게 되면 비정질 합금이 부스러지는 경향이 있으므로 이 또한 제한되어지는 것이 바람직하다.In addition, when the content of tin exceeds 3 atomic%, the amorphous alloy tends to crumble, so this is also preferably limited.
따라서, 본 발명에서는 보론의 함량을 줄이고, 주석을 첨가함에 따라 철-보론 2원자계 비정질합금에 비하여 제조원가가 저렴하면서도 더 우수한 비정질 성능 을 가지는 합금을 제조하였다.Therefore, in the present invention, by reducing the content of boron and adding tin, an alloy having lower cost and higher amorphous performance than the iron-boron biatomic amorphous alloy was prepared.
본 발명에 의한 비정질 합금은 아크용해장치를 이용하여 모합금을 제조한 후, 이를 분쇄하고, 단롤 멜트 스피닝 장치를 이용하여 제조한다.The amorphous alloy according to the present invention is prepared by using the arc dissolving apparatus to prepare a mother alloy, and then pulverizing it, using a single roll melt spinning apparatus.
모합금은 철(99.9중량%), 보론(99.8중량%), 주석(99.9중량%)를 20g으로 계량하여 고순도 아르곤(99.99%)가스 분위기 하에서 아크 용해에 의하여 FexSnyBz (z= 14, 15,16, x+y=86, 85, 84, y=0, 1, 2, 3)의 조성을 가지도록 하여 제조하였다. 이때 합금성분의 편석을 없애기 위하여 시료를 5회 이상 반전시켜 용해하였다.The master alloy weighed 20g of iron (99.9% by weight), boron (99.8% by weight) and tin (99.9% by weight), and Fe x Sn y B z by arc melting under high purity argon (99.99%) gas atmosphere. It was prepared to have a composition of (z = 14, 15,16, x + y = 86, 85, 84, y = 0, 1, 2, 3). At this time, the sample was inverted five times or more to dissolve the segregation of the alloy component.
준비된 모합금은 적당한 크기로 분쇄한 후 단롤 멜트 스피닝(single roll melt spinning)방법으로 리본을 제조하였으며, 제조된 리본은 폭 약 2mm, 두께 약 10㎛의 치수를 가진다. The prepared master alloy was pulverized to an appropriate size, and then a ribbon was prepared by a single roll melt spinning method. The ribbons had dimensions of about 2 mm in width and about 10 μm in thickness.
도 1 및 도 2는 철-주석-보론 리본의 제조상태(as-spun)에서의 XRD(X-ray Diffraction; X선회절)분석결과를 나타낸 것이다. 이를 통해 비정질 형성여부를 검사하였다.1 and 2 show the results of X-ray diffraction (XRD) analysis in the as-spun state of the iron-tin-boron ribbon. This was examined for amorphous formation.
도 1 및 도 2에서 알 수 있듯이 본 발명의 비정질합금의 경우, 비정질상을 가지고 있는 것으로 나타났다.1 and 2, the amorphous alloy of the present invention was found to have an amorphous phase.
도 3 및 도 4는 본 발명에 의한 비정질 합금의 급속응고를 통해 제조된 리본에 대한 열적 안정성 및 유리 천이온도 그리고 결정화 열처리 온도를 결정하는 중요한 요소로 작용하는 결정화 온도를 분석하기 위해 승온 속도 40K/min으로 측정한 시차열 분석결과를 알려준다.3 and 4 is a temperature increase rate of 40K / to analyze the crystallization temperature which serves as an important factor in determining the thermal stability and glass transition temperature and the crystallization heat treatment temperature for the ribbon prepared through the rapid solidification of the amorphous alloy according to the present invention Indicate the result of differential thermal analysis measured in min.
결정화 반응에 대한 엔탈피 변화(△H) 등을 시차열분석기(differential scanning calorimeter)를 이용하여 25~800℃의 온도 범위에서 측정하였으며, 시차열 분석은 약 10mg의 시료를 약 2mm길이로 잘라서 장입한 뒤, 99.99% 순도의 Ar분위기에서 40K/mim(=0.67K/s)의 일정한 승온속도로 행하였다.The enthalpy change (△ H) for the crystallization reaction was measured in a temperature range of 25 ~ 800 ℃ by using a differential scanning calorimeter (differential scanning calorimeter), the differential thermal analysis was cut into a 10mm sample cut into about 2mm length Thereafter, it was performed at a constant heating rate of 40 K / mim (= 0.67 K / s) in an Ar atmosphere of 99.99% purity.
아래의 표 1은 상기 시차열 분석결과를 정리한 것이며, 각 조성에 대한 일차 및 이차 결정화 온도(crystallization temperatue, Tx1, Tx2)와, 큐리온도를 정리하였다.Table 1 below summarizes the results of the differential thermal analysis, and summarizes the primary and secondary crystallization temperature (T x1 , T x2 ) and Curie temperature for each composition.
[표 1]TABLE 1
결정화 큐리 온도는 주석의 첨가량이 증가할수록 증가하여 열적안정성이 우수한 것으로 나타났다.이는 주석(1.41Å)의 원자 반경이 다른 구성 원소와 비교해 매우 크기 때문에 소량의 주석의 첨가로 비정질상의 충진 밀도를 높이기 때문이다. 그러나, 주석이 3원자%를 초과하는 경우에는 비정질 합금의 형상이 연속적이지 않고, 불연속적이어서 리본의 부스러짐 등이 발생하므로 주석의 원자%는 1~3인 것이 바람직하다. The crystallization Curie temperature increased with increasing amount of tin, indicating excellent thermal stability because the atomic radius of tin (1.41Å) is very large compared to other constituents, and the addition of a small amount of tin increases the packing density of the amorphous phase. to be. However, when tin exceeds 3 atomic%, the shape of the amorphous alloy is not continuous, and because the chip is broken because of discontinuity, it is preferable that the atomic% of tin is 1-3.
또한, 결정화 온도(Tx)도 주석이 첨가된 경우 주석이 첨가되지 않은 경우보다 높게 나타나 비정질 형성능이 우수함을 알 수 있었다.In addition, the crystallization temperature (Tx) was also higher than when tin is added, it can be seen that the amorphous forming ability is excellent.
표 1에서 알 수 있듯이 Fe86B14보다 Fe85B15 보론의 함량이 증가할수록 큐리온도가 증가하여 비정질 특성이 우수함을 알 수 있었다.As can be seen from Table 1, the higher the content of Fe 85 B 15 boron than Fe 86 B 14 , the Curie temperature increases, it was found that the excellent amorphous properties.
그러나, 본 발명은 Fe85B15보다 보론의 함량이 적은 Fe85Sn1B14 가 큐리온도는 더 높고, 결정화온도도 높거나 비슷하여 주석이 포함됨에 따라 비정질 특성이 향상됨을 알 수 있었다.However, in the present invention, Fe 85 Sn 1 B 14 having a lower boron content than Fe 85 B 15 has a higher Curie temperature, higher or similar crystallization temperature, and it was found that the amorphous properties were improved as tin was included.
즉, 본 발명에 의한 철-주석-보론 3원자계 비정질 합금의 경우, 철-보론 비정질합금의 경우보다 보론의 함량이 적음에도 큐리온도가 더 높고 결정화온도가 높아 비정질 특성이 우수함을 알 수 있었다.That is, in the case of the iron-tin-boron triatomic amorphous alloy according to the present invention, even though the boron content is less than that of the iron-boron amorphous alloy, the Curie temperature is higher and the crystallization temperature is higher, indicating that the amorphous property is excellent. .
표 2에서는 본 발명에 의한 철-주석-보론 비정질 합금에 첨가된 주석의 첨가량에 따른 자기적 특성을 나타내었다. Table 2 shows the magnetic properties according to the amount of tin added to the iron-tin-boron amorphous alloy according to the present invention.
[표 2]TABLE 2
자기적 특성의 분석에서는 진동시료형 자력계(VSM)로 인가자장을 5kOe로 하여 포화자화(Ms)를 측정하였으며, BH analyzer로 보자력을, impedance analyzer로 실효투자율을 측정하였다.In the analysis of the magnetic properties, the saturation magnetization (Ms) was measured with the applied magnetic field of 5kOe using the vibration sample magnetometer (VSM), the coercive force was measured with the BH analyzer, and the effective permeability was measured with the impedance analyzer.
주석이 함유된 경우 함유되지 않은 경우와 비교할 때 자기적 특성이 우수함을 알 수 있는데, 주석이 3원자% 첨가된 Fe82Sn3B15에서 보자력 Hc는 7.8 A/m로 가장 낮게 측정되었고, 포화자화값(Ms) 및 실효투자율(μe)도 모두 주석이 첨가된 경우가 가장 높게 나와서 주석이 함유되지 않은 경우보다 주석이 함유된 경우 비정질 특성이 우수함을 알 수 있었다.It can be seen that the magnetic properties are excellent when tin is contained, compared with the case where tin is not contained. The coercive force Hc of Fe 82 Sn 3 B 15 with 3 atomic percent tin was lowest at 7.8 A / m and was saturated. The magnetization value (Ms) and the effective permeability (μe) were also the highest when tin was added, and it was found that the amorphous property was better when tin was contained than when tin was not contained.
또한, 본 발명에 의한 비정질합금은 초크코일등과 같은 전기소자에 사용될 수 있는데, 초크코일은 높은 주파수의 전류와 교류 전류의 통과를 막거나 제한하기 위하여 사용되는 코일로서, 본 발명은 고주파 영역에서 사용될 수 있는 우수한 비정질 특성을 가지므로 본 발명에 의한 비정질 합금을 초크코일 등과 같은 전기소자 에 사용시 고주파 노이즈를 제거하는데 효과적이다.In addition, the amorphous alloy according to the present invention can be used in an electric element such as a choke coil, the choke coil is a coil used to prevent or limit the passage of high frequency current and alternating current, the present invention in the high frequency region Since it has excellent amorphous properties that can be used, it is effective to remove high frequency noise when the amorphous alloy according to the present invention is used in an electric element such as a choke coil.
초크코일용 자기 코어로는 연자기 특성을 갖는 재료가 유효한데, 본 발명에 의한 비정질 합금을 사용시 보론의 함량을 줄여 저렴한 가격으로 제조가 가능하면서도 비정질 특성은 우수하다. 또한 자기코어의 형상은 특별히 제한되지 않으며 원형 코어(toroidal core), EE 코어, EI 코어 등 모든 형상의 자기 코어를 사용가능하다.As the magnetic core for the choke coil, a material having soft magnetic properties is effective. When the amorphous alloy according to the present invention is used, it is possible to manufacture at low cost by reducing the content of boron and excellent in amorphous properties. In addition, the shape of the magnetic core is not particularly limited, and any shape of magnetic core such as a toroidal core, an EE core, and an EI core may be used.
도 1 및 도 2는 본 발명에 의한 비정질 합금이 비정질상을 나타냄을 나타낸 도면이다.1 and 2 is a view showing that the amorphous alloy according to the present invention shows an amorphous phase.
도 3 및 도4는 본 발명에 의한 비정질 합금의 승온 속도 40K/min으로 측정한 시차열분석 결과를 도시한 것이다.3 and 4 illustrate the results of differential thermal analysis measured at a temperature raising rate of 40 K / min of the amorphous alloy according to the present invention.
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