TWI636869B - Method of fabricating plastic-magnetic composite material - Google Patents
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Abstract
一種塑磁複合材料的製造方法，其包含步驟：提供5至15重量份的聚醯胺、85至95重量份的磁性粉體、0.1至5重量份的分散助劑及0.1至5重量份的抗氧化劑；進行一混煉步驟，將該聚醯胺、該磁性粉體、該分散助劑及該抗氧化劑混煉形成一混合物；進行一第一擠壓步驟，透過一單螺桿裝置擠壓該混合物以形成多個半成品複合塑膠顆粒，其中該第一擠壓步驟的一第一擠壓溫度係介於180至260℃之間；及進行一第二擠壓步驟，透過一雙螺桿裝置擠壓該些半成品複合塑膠顆粒以形成該塑磁複合材料，其中該第二擠壓步驟的一第二擠壓溫度係介於170至260℃之間。 A method for producing a plastic magnetic composite material, comprising the steps of: providing 5 to 15 parts by weight of polyamine, 85 to 95 parts by weight of magnetic powder, 0.1 to 5 parts by weight of a dispersing aid, and 0.1 to 5 parts by weight An anti-oxidant; performing a mixing step of kneading the polyamine, the magnetic powder, the dispersing aid and the antioxidant to form a mixture; performing a first pressing step, extruding the product through a single screw device Mixing to form a plurality of semi-finished composite plastic pellets, wherein a first extrusion temperature of the first extrusion step is between 180 and 260 ° C; and performing a second extrusion step, extruding through a twin screw device The semi-finished composite plastic particles form the plastic magnetic composite material, wherein a second extrusion temperature of the second extrusion step is between 170 and 260 °C.
Description
本發明係關於一種複合材料的製造方法，特別是關於一種塑磁複合材料的製造方法。 The present invention relates to a method of manufacturing a composite material, and more particularly to a method of manufacturing a plastic magnetic composite material.
傳統磁性材料是透過壓力機壓製成型，再進行燒結加工而完成。而塑磁複合材料的製作方法通常是在磁粉中添加高分子材料，並通過注塑機混煉加熱後把混合料射入到模具裡，得到各種形狀的產品。 Conventional magnetic materials are formed by press molding and then sintering. The plastic magnetic composite material is usually produced by adding a polymer material to the magnetic powder, and mixing and heating the mixture by an injection molding machine to inject the mixture into the mold to obtain products of various shapes.
然而，這種塑磁複合材料通常僅透過單道的擠壓步驟即完成，容易產生高分子材料與磁粉兩者之間的分散相不夠均勻，進而導致磁特性不佳的缺點。 However, such a plastic magnetic composite material is usually completed only by a single-pass extrusion step, and it is easy to cause a disadvantage that the dispersed phase between the polymer material and the magnetic powder is not uniform enough, resulting in poor magnetic properties.
故，有必要提供一種塑磁複合材料的製造方法，以解決習用技術所存在的問題。 Therefore, it is necessary to provide a method for manufacturing a plastic magnetic composite material to solve the problems of the conventional technology.
本發明之一目的在於提供一種塑磁複合材料的製造方法，其係先後透過單螺桿裝置與雙螺桿裝置的兩道擠壓步驟來製得塑磁複合材料，以獲得磁特性較佳的塑磁複合材料。 An object of the present invention is to provide a method for manufacturing a plastic magnetic composite material, which is obtained by successively passing two extrusion steps of a single screw device and a twin screw device to obtain a plastic magnetic composite material to obtain a magnetic magnetic property with better magnetic properties. Composite material.
為達上述之目的，本發明提供一種塑磁複合材料的製造方法，其包含步驟：提供5至15重量份的聚醯胺、85至95重量份的磁性粉體、0.1至5重量份的分散助劑及0.1至5重量份的抗氧化劑；進行一混煉步驟，將該聚醯胺、該磁性粉體、該分散助劑及該抗氧化劑混煉形成一混合物；進行一第一擠壓步驟，透過一單螺桿裝置擠壓該混合物以形成多個半成品複合塑膠顆 粒，其中該第一擠壓步驟的一第一擠壓溫度係介於180至260℃之間；及進行一第二擠壓步驟，透過一雙螺桿裝置擠壓該些半成品複合塑膠顆粒以形成該塑磁複合材料，其中該第二擠壓步驟的一第二擠壓溫度係介於170至260℃之間。 In order to achieve the above object, the present invention provides a method for producing a plastic magnetic composite material comprising the steps of providing 5 to 15 parts by weight of polyamide, 85 to 95 parts by weight of magnetic powder, and 0.1 to 5 parts by weight of dispersion. An auxiliary agent and 0.1 to 5 parts by weight of an antioxidant; performing a mixing step, kneading the polyamine, the magnetic powder, the dispersing aid and the antioxidant to form a mixture; performing a first pressing step Extrusion of the mixture through a single screw device to form a plurality of semi-finished composite plastic pieces a pellet, wherein a first extrusion temperature of the first extrusion step is between 180 and 260 ° C; and a second extrusion step is performed to extrude the semi-finished composite plastic particles through a twin-screw device to form The plastic magnetic composite material, wherein a second extrusion temperature of the second extrusion step is between 170 and 260 °C.
在本發明之一實施例中，該混煉步驟的一混煉溫度係介於180至260℃之間、一轉子轉速係介於50至100RPM之間及一混煉時間介於5至30分之間。 In an embodiment of the present invention, a mixing temperature of the mixing step is between 180 and 260 ° C, a rotor speed is between 50 and 100 RPM, and a mixing time is between 5 and 30 minutes. between.
在本發明之一實施例中，該第二擠壓步驟的一螺桿轉速係介於200至600RPM之間。 In an embodiment of the invention, a screw speed of the second pressing step is between 200 and 600 RPM.
在本發明之一實施例中，該磁性粉體包含鍶氧化鐵粉體。 In an embodiment of the invention, the magnetic powder comprises bismuth iron oxide powder.
在本發明之一實施例中，該磁性粉體包含經表面改質的磁性粉體。 In an embodiment of the invention, the magnetic powder comprises a surface modified magnetic powder.
在本發明之一實施例中，提供該磁性粉體的步驟中更包含：透過一改質劑對該磁性粉體進行一改質步驟，其中該改質劑包含矽烷偶合劑或鈦鹽偶合劑中的至少一種。 In an embodiment of the present invention, the step of providing the magnetic powder further comprises: performing a upgrading step on the magnetic powder through a modifying agent, wherein the modifying agent comprises a decane coupling agent or a titanium salt coupling agent At least one of them.
在本發明之一實施例中，該分散助劑包含硬脂酸醯胺類與硬脂酸鋅類中的至少一種。 In an embodiment of the invention, the dispersing aid comprises at least one of decylamine stearate and zinc stearate.
在本發明之一實施例中，該分散助劑包含0.9至1重量份的硬脂酸醯胺及0.04至0.06重量份的硬脂酸鋅。 In one embodiment of the invention, the dispersing aid comprises 0.9 to 1 part by weight of decylamine stearate and 0.04 to 0.06 part by weight of zinc stearate.
在本發明之一實施例中，該抗氧化劑包含阻酚類抗氧化劑及亞磷酸酯中的至少一種。 In an embodiment of the invention, the antioxidant comprises at least one of a phenolic antioxidant and a phosphite.
在本發明之一實施例中，該聚醯胺係9重量份、該磁性粉體係90重量份、該分散助劑係1重量份及該抗氧化劑係0.5重量份。 In one embodiment of the present invention, the polyamine is 9 parts by weight, the magnetic powder system is 90 parts by weight, the dispersion aid is 1 part by weight, and the antioxidant is 0.5 parts by weight.
10‧‧‧方法 10‧‧‧ method
11~14‧‧‧步驟 11~14‧‧‧Steps
第1圖：本發明一實施例之塑磁複合材料的製造方法的流程示意圖。 Fig. 1 is a flow chart showing a method of manufacturing a plastic magnetic composite material according to an embodiment of the present invention.
為了讓本發明之上述及其他目的、特徵、優點能更明顯易懂，下文將特舉本發明較佳實施例，並配合所附圖式，作詳細說明如下。再者，本發明所提到的方向用語，例如上、下、頂、底、前、後、左、右、內、外、側面、周圍、中央、水平、橫向、垂直、縱向、軸向、徑向、最上層或最下層等，僅是參考附加圖式的方向。因此，使用的方向用語是用以說明及理解本發明，而非用以限制本發明。 The above and other objects, features and advantages of the present invention will become more <RTIgt; Furthermore, the directional terms mentioned in the present invention, such as upper, lower, top, bottom, front, rear, left, right, inner, outer, side, surrounding, central, horizontal, horizontal, vertical, longitudinal, axial, Radial, uppermost or lowermost, etc., only refer to the direction of the additional schema. Therefore, the directional terminology used is for the purpose of illustration and understanding of the invention.
請參照第1圖，第1圖係本發明一實施例之塑磁複合材料的製造方法10的流程示意圖。該塑磁複合材料的製造方法10主要包含下列步驟11至14：提供5至15重量份的聚醯胺、85至95重量份的磁性粉體、0.1至5重量份的分散助劑及0.1至5重量份的抗氧化劑(步驟11)；進行一混煉步驟，將該聚醯胺、該磁性粉體、該分散助劑及該抗氧化劑混煉形成一混合物(步驟12)；進行一第一擠壓步驟，透過一單螺桿裝置擠壓該混合物以形成多個半成品複合塑膠顆粒，其中該第一擠壓步驟的一第一擠壓溫度係介於180至260℃之間(步驟13)；及進行一第二擠壓步驟，透過一雙螺桿裝置擠壓該些半成品複合塑膠顆粒以形成該塑磁複合材料，其中該第二擠壓步驟的一第二擠壓溫度係介於170至260℃之間(步驟14)。本發明將於下文逐一詳細說明一實施例之上述各步驟的實施細節及其原理。 Please refer to FIG. 1. FIG. 1 is a schematic flow chart showing a method 10 for manufacturing a plastic magnetic composite material according to an embodiment of the present invention. The method 10 for manufacturing a plastic magnetic composite material mainly comprises the following steps 11 to 14: providing 5 to 15 parts by weight of polyamide, 85 to 95 parts by weight of magnetic powder, 0.1 to 5 parts by weight of dispersing aid, and 0.1 to 5 parts by weight of an antioxidant (step 11); performing a mixing step, kneading the polyamine, the magnetic powder, the dispersing aid and the antioxidant to form a mixture (step 12); performing a first The extrusion step, the mixture is extruded through a single screw device to form a plurality of semi-finished composite plastic particles, wherein a first extrusion temperature of the first pressing step is between 180 and 260 ° C (step 13); And performing a second pressing step of extruding the semi-finished composite plastic particles through a twin-screw device to form the plastic-magnetic composite material, wherein a second extrusion temperature of the second pressing step is between 170 and 260 Between °C (step 14). The details of the implementation of the above-described steps of an embodiment and the principles thereof will be described in detail below.
本發明一實施例之塑磁複合材料的製造方法10首先係步驟11：提供5至15重量份的聚醯胺、85至95重量份的磁性粉體、0.1至5重量份的分散助劑及0.1至5重量份的抗氧化劑。在本步驟11中，主要是提供該塑磁複合材料所需要的原料。在一範例中，該聚醯胺係9重量份、該磁性粉體係90重量份、該分散助劑係1重量份及該抗氧化劑係0.5重量份。在一實施例中，該聚醯胺例如是聚十二內醯胺，粒徑例如小於等於100微米。在另一實施例中，該磁性粉體包含鍶氧化鐵粉體(SrFe12O19)，粒徑例如介 於0.2至3.5微米之間。在又一實施例中，該磁性粉體包含經表面改質的磁性粉體，例如透過一改質劑對該磁性粉體進行一改質步驟，其中該改質劑包含矽烷偶合劑或鈦鹽偶合劑中的至少一種。在再一實施例中，該分散助劑包含硬脂酸醯胺類與硬脂酸鋅類中的至少一種。例如，該分散助劑包含0.9至1重量份的硬脂酸醯胺及0.04至0.06重量份的硬脂酸鋅。在另一實施例中，該抗氧化劑可用於使該磁性粉體具高分散性，例如該抗氧化劑包含阻酚類抗氧化劑及亞磷酸酯中的至少一種。 The method 10 for manufacturing a plastic magnetic composite material according to an embodiment of the present invention is first performed in step 11: providing 5 to 15 parts by weight of polyamido, 85 to 95 parts by weight of magnetic powder, 0.1 to 5 parts by weight of a dispersing aid, and 0.1 to 5 parts by weight of an antioxidant. In this step 11, the raw materials required for the plastic magnetic composite material are mainly provided. In one example, the polyamine is 9 parts by weight, the magnetic powder system is 90 parts by weight, the dispersion aid is 1 part by weight, and the antioxidant is 0.5 parts by weight. In one embodiment, the polyamine is, for example, polydodecanamide having a particle size of, for example, 100 microns or less. In another embodiment, the magnetic powder comprises bismuth iron oxide powder (SrFe 12 O 19 ) having a particle size of, for example, between 0.2 and 3.5 microns. In still another embodiment, the magnetic powder comprises a surface-modified magnetic powder, for example, a modification step is performed on the magnetic powder through a modifier, wherein the modifier comprises a decane coupling agent or a titanium salt. At least one of the coupling agents. In still another embodiment, the dispersing aid comprises at least one of decylamine stearate and zinc stearate. For example, the dispersing aid comprises 0.9 to 1 part by weight of decylamine stearate and 0.04 to 0.06 part by weight of zinc stearate. In another embodiment, the antioxidant can be used to impart high dispersibility to the magnetic powder, for example, the antioxidant comprises at least one of a phenolic antioxidant and a phosphite.
本發明一實施例之塑磁複合材料的製造方法10接著係步驟12：進行一混煉步驟，將該聚醯胺、該磁性粉體、該分散助劑及該抗氧化劑混煉形成一混合物。在本步驟12中，可透過市售的一密閉式混煉機(例如筌盛實業股份有限公司、型號YKI-3、中華民國製造)來將該聚醯胺、該磁性粉體、該分散助劑及該抗氧化劑混煉形成該混合物。在一實施例中，該混煉步驟的一混煉溫度係介於180至260℃之間(例如為190℃)、一轉子轉速係介於50至100RPM(例如為75RPM)之間及一混煉時間介於5至30分之間(例如為15分)。 The method 10 for manufacturing a plastic magnetic composite material according to an embodiment of the present invention is followed by the step 12: performing a kneading step of kneading the polyamine, the magnetic powder, the dispersing aid and the antioxidant to form a mixture. In this step 12, the polyamide, the magnetic powder, the dispersion aid can be obtained through a commercially available closed mixer (for example, Yu Sheng Industrial Co., Ltd., model YKI-3, manufactured by the Republic of China). The agent and the antioxidant are kneaded to form the mixture. In one embodiment, a mixing temperature of the mixing step is between 180 and 260 ° C (eg, 190 ° C), a rotor speed is between 50 and 100 RPM (eg, 75 RPM), and a mixture The refining time is between 5 and 30 minutes (for example, 15 points).
本發明一實施例之塑磁複合材料的製造方法10接著係步驟13：進行一第一擠壓步驟，透過一單螺桿裝置擠壓該混合物以形成多個半成品複合塑膠顆粒，其中該第一擠壓步驟的一第一擠壓溫度係介於180至260℃之間。在本步驟13中，該單螺桿裝置例如可以是市售的單螺桿裝置(例如筌盛實業股份有限公司、型號YKF-40、中華民國製造)。在一具體範例中，該第一擠壓溫度可以是多段式的控制方式，例如該第一擠壓溫度可從180℃開始，依序升溫至210℃、215℃、220℃、230℃、240℃、250℃，而最後提升至260℃。 The method 10 for manufacturing a plastic magnetic composite material according to an embodiment of the present invention is followed by a step 13 of performing a first extrusion step of extruding the mixture through a single screw device to form a plurality of semi-finished composite plastic particles, wherein the first extrusion A first extrusion temperature of the pressing step is between 180 and 260 °C. In this step 13, the single screw device may be, for example, a commercially available single screw device (for example, Yusheng Industrial Co., Ltd., model YKF-40, manufactured by the Republic of China). In a specific example, the first extrusion temperature may be a multi-stage control mode, for example, the first extrusion temperature may start from 180 ° C, and sequentially increase the temperature to 210 ° C, 215 ° C, 220 ° C, 230 ° C, 240. °C, 250 ° C, and finally raised to 260 ° C.
本發明一實施例之塑磁複合材料的製造方法10最後係步驟14：進行一第二擠壓步驟，透過一雙螺桿裝置擠壓該些半成品複合塑膠顆粒以形成該塑磁複合材料，其中該第二擠壓步驟 的一第二擠壓溫度係介於170至260℃之間。在本步驟14中，該雙螺桿裝置例如可以是市售的雙螺桿裝置(例如澤機工業有限公司、型號ZPT-32HT、中華民國製造)。在一具體範例中，該第二擠壓溫度可以是多段式的控制方式，例如該第一擠壓溫度可從170℃開始，依序升溫至180、190、200、210、220及225℃，而最後略為降溫並維持至220℃。在另一實施例中，該第二擠壓步驟的一螺桿轉速係介於200至600RPM之間(例如為400RPM)。 The method for manufacturing a plastic magnetic composite material according to an embodiment of the present invention is finally a step 14: performing a second extrusion step of extruding the semi-finished composite plastic particles through a twin-screw device to form the plastic magnetic composite material, wherein Second extrusion step A second extrusion temperature is between 170 and 260 °C. In this step 14, the twin-screw device may be, for example, a commercially available twin-screw device (for example, Zeji Industrial Co., Ltd., model ZPT-32HT, manufactured by the Republic of China). In a specific example, the second extrusion temperature may be a multi-stage control mode, for example, the first extrusion temperature may start from 170 ° C, and sequentially increase the temperature to 180, 190, 200, 210, 220, and 225 ° C. At the end, it was slightly cooled and maintained at 220 °C. In another embodiment, a screw speed of the second extrusion step is between 200 and 600 RPM (eg, 400 RPM).
要提到的是，本發明一實施例之塑磁複合材料的製造方法的特點之一是透過兩道式的擠壓步驟來製得該塑磁複合材料，其磁力性質可優於僅使用一道式的擠壓步驟(例如僅使用一道雙螺桿裝置)所製得的塑磁複合材料。 It is to be noted that one of the features of the method for manufacturing a plastic magnetic composite material according to an embodiment of the present invention is that the plastic magnetic composite material is obtained through a two-step extrusion step, and the magnetic property is superior to that of using only one A plastic magnetic composite material produced by a pressing step (for example, using only one twin screw device).
以下將舉出實施例與比較例，以證明本發明一實施例之塑磁複合材料的製造方法優於僅使用一道式處理步驟所製得的塑磁複合材料。 The examples and comparative examples will be exemplified below to demonstrate that the method for producing a plastic magnetic composite material according to an embodiment of the present invention is superior to the plastic magnetic composite material obtained by using only one one-step processing step.
實施例 Example
首先，提供9重量份的聚醯胺、90重量份的磁性粉體、0.95重量份的硬脂酸醯胺、0.05重量份的硬脂酸鋅、及0.5重量份的抗氧化劑。接著，利用密閉式混煉機進行一混煉步驟，以使該聚醯胺、該磁性粉體、該分散助劑及該抗氧化劑混煉形成一混合物，其中該混煉步驟的一混煉溫度約為190℃、一轉子轉速係約為75RPM及一混煉時間約為15分。 First, 9 parts by weight of polyamine, 90 parts by weight of magnetic powder, 0.95 parts by weight of decylamine stearate, 0.05 parts by weight of zinc stearate, and 0.5 parts by weight of an antioxidant are provided. Next, a kneading step is performed by a closed kneader to knead the polyamine, the magnetic powder, the dispersing aid and the antioxidant to form a mixture, wherein a kneading temperature of the kneading step At about 190 ° C, a rotor speed is about 75 RPM and a mixing time is about 15 minutes.
之後，進行一第一擠壓步驟，透過一單螺桿裝置擠壓該混合物以形成多個半成品複合塑膠顆粒，其中該第一擠壓步驟的第一擠壓溫度係介於180至215℃之間。最後，進行一第二擠壓步驟，透過一雙螺桿裝置擠壓該些半成品複合塑膠顆粒以形成該塑磁複合材料，其中該第二擠壓步驟的一第二擠壓溫度係介於170至225℃之間及一螺桿轉速係約為400RPM。之後，透過磁性分析儀器對所製得的塑磁複合材料進行磁性分析，所得之磁特性如下表1。 Thereafter, performing a first pressing step of extruding the mixture through a single screw device to form a plurality of semi-finished composite plastic particles, wherein the first extrusion step of the first extrusion step is between 180 and 215 ° C . Finally, performing a second pressing step of extruding the semi-finished composite plastic particles through a twin-screw device to form the plastic-magnetic composite material, wherein a second extrusion temperature of the second pressing step is between 170 and Between 225 ° C and a screw speed is about 400 RPM. Thereafter, the obtained magnetic composite material was magnetically analyzed by a magnetic analysis instrument, and the magnetic properties obtained are shown in Table 1 below.
比較例 Comparative example
比較例的製作方式相似於實施例，惟其不同之處在於比較例未進行第一擠壓步驟。換言之，比較例在進行混煉步驟之後即利用雙螺桿裝置進行第二擠壓步驟，而未進行第一擠壓步驟。透過比較例所得之塑磁複合材料的磁特性如上表1所述。 The comparative example was made in a manner similar to the examples except that the first extrusion step was not performed in the comparative example. In other words, the comparative example performs the second pressing step using the twin-screw apparatus after the kneading step, without performing the first pressing step. The magnetic properties of the plastic magnetic composite obtained by the comparative example were as described in Table 1 above.
從上表1可知，實施例的磁特性中，剩磁Br、矯頑磁力bHc、最大磁能積BHmax與飽和磁化強度4 π Is皆大於比較例，故可證明透過二道式的擠壓步驟可製得磁特性較佳的塑磁複合材料。值得一提的是，雖然實施例的本質矯頑磁力iHc低於比較例，但此數值在塑磁複合材料的使用領域仍是可接受的。另一方面，申請人亦將實施例與比較例的塑磁複合材料進行機械性質的測試，其中實施例的塑磁複合材料的熔融流動速率為127克/10分，及彎曲強度為97N/mm2，而比較例的塑磁複合材料的熔融流動速率僅有117克/10分，及彎曲強度為79N/mm2。顯見，實施例所製得的塑磁複合材料的機械性質亦較佳。 As can be seen from the above Table 1, in the magnetic characteristics of the embodiment, the remanence Br, the coercive force bHc, the maximum magnetic energy product BHmax and the saturation magnetization 4 π Is are larger than the comparative example, so that it can be confirmed that the two-step extrusion step can be performed. A plastic magnetic composite material having better magnetic properties is obtained. It is worth mentioning that although the intrinsic coercive force iHc of the examples is lower than that of the comparative examples, this value is still acceptable in the field of use of plastic magnetic composite materials. On the other hand, the applicant also tested the mechanical properties of the plastic magnetic composite materials of the examples and the comparative examples, wherein the plastic magnetic composite material of the example had a melt flow rate of 127 g/10 min and a bending strength of 97 N/mm. 2 , and the plastic magnetic composite material of the comparative example had a melt flow rate of only 117 g/10 min and a flexural strength of 79 N/mm 2 . It is apparent that the mechanical properties of the plastic magnetic composite material obtained in the examples are also preferred.
雖然本發明已以較佳實施例揭露，然其並非用以限制本發明，任何熟習此項技藝之人士，在不脫離本發明之精神和範圍內，當可作各種更動與修飾，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 The present invention has been disclosed in its preferred embodiments, and is not intended to limit the invention, and the present invention may be modified and modified without departing from the spirit and scope of the invention. The scope of protection is subject to the definition of the scope of the patent application.
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| CN104194325A (en) * | 2014-09-17 | 2014-12-10 | 中山大学 | Preparing method of heat-conductive and injection-molded magnetic composite |
| CN105949758A (en) * | 2016-05-30 | 2016-09-21 | 四川安费尔高分子材料科技有限公司 | High-fluidity polyamide magnetic composite material and preparation method thereof |
| CN107189457A (en) * | 2017-06-23 | 2017-09-22 | 华娜 | A kind of Magnetic nylon composite material and preparation method thereof |
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| CN104194325A (en) * | 2014-09-17 | 2014-12-10 | 中山大学 | Preparing method of heat-conductive and injection-molded magnetic composite |
| CN105949758A (en) * | 2016-05-30 | 2016-09-21 | 四川安费尔高分子材料科技有限公司 | High-fluidity polyamide magnetic composite material and preparation method thereof |
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