CN114147212A - 非晶纳米晶雾化粉末及其制备方法 - Google Patents
非晶纳米晶雾化粉末及其制备方法 Download PDFInfo
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Abstract
本发明提供的一种非晶纳米晶雾化粉末，其粉末颗粒均呈类球型状，其成分包括有Fe100‑a‑b‑c‑x‑y‑zSiaBbCcMnxCryXZ，式中X为P、Cu、Mo、Ni中的任意一种，其中8≤a≤15，6≤b≤12，0.2≤c≤3.0，0.1≤x≤3.5，0.5≤y≤2.5，0≤Z≤4.0；本发明的非晶纳米晶雾化粉末通过合金成分的设计优化，以使其制备的非晶纳米晶产品具有低损耗、高饱和磁感应强度及高直流偏置的特点。
Description
技术领域
本发明涉及软磁合金冶金技术领域，具体涉及一种非晶纳米晶雾化粉末及其制备方法。
背景技术
非晶材料具有高的饱和磁感、高磁导率、低矫顽力和低的高频损耗、良好的强硬度、耐磨性及耐腐蚀性、良好的温度及环境稳定性等，其优异的综合性能，代替坡莫合金、硅钢和铁氧体，在电力电子技术中应用，显示出体积小、效率高、节能等特点，在所有的金属软磁材料中具有最佳的性能价格比。
现有技术中，主要以羰基铁粉及铁硅铬粉以作一体成型电感的制备原料，但以上两种粉末具有更大的磁滞损耗，并且粉末体电阻率较低造成产品应用过程更大的涡流损耗，该类产品应用中具有较高的损耗，引起产品发热、能效降低等问题。
“非晶纳米晶”，于本领域而言可视为是对非晶、纳米晶两者的并列概念约定俗成称谓，而本领域中，基于合金的处理阶段不同，于非晶至纳米晶的转化过程中，或存在有非晶态、非晶态与纳米晶共存的形态及纳米晶态的三者形态，故该“非晶纳米晶”的限定描述，可视为是对非晶态、非晶且纳米晶态、纳米晶态三种的合金形态的上位概括概念。
发明内容
本发明的目的在于为克服现有技术的不足而提供一种非晶纳米晶雾化粉末及其制备方法。
非晶纳米晶雾化粉末，其粉末颗粒均呈类球型状，其成分包括有Fe100-a-b-c-x-y- zSiaBbCcMnxCryXZ,，式中X为P、Cu、Mo、Ni中的任意一种，其中8≤a≤15，6≤b≤12，0.2≤c≤3.0，0.1≤x≤3.5，0.5≤y≤2.5，0≤Z≤4.0。
进一步地，其中6≤b≤9，0.3≤y≤2.5。
进一步地，其成分包括有Fe75Si11B9C2.5Cr2.3Mn0.2。
进一步地，其成分包括有Fe74.8Si11B9C1.5Cr2.5Mn0.2P1或Fe74.8Si11B9C0.5Cr1.5Mn0.2P2或Fe73.8Si11B9C1.5Cr1.5Mn0.2P2或Fe79Si11B7C0.5Cr0.3Mn0.2P2或Fe79Si9B6.2C0.5Cr0.3Mn1P4。
进一步地，其成分包括有Fe74.8Si11B9C1.5Cr2.5Mn0.2Mo1或Fe76.8Si11B9C0.5Cr1.5Mn0.2Mo1或Fe73.8Si11B9C1.5Cr1.5Mn1.2Mo1或Fe78Si11B7C0.5Cr0.5Mn1Mo2。
进一步地，其成分包括有Fe74.8Si11B9C1.5Cr2.5Mn0.2Ni1或Fe74.8Si11B9C0.5Cr1.5Mn0.2Ni2或Fe74.8Si11B7C1.5Cr1.5Mn0.2Ni3或Fe76.8Si11B7C0.5Cr0.5Mn0.2Ni4。
该非晶纳米晶雾化粉末的制备方法，其包括以下步骤：
S1、将原料按上述成分分子式进行调配及冶炼，以制备有母合金；
S2、以雾化制粉方法将所得母合金进行非晶纳米晶粉末的制备，以得到有粉末颗粒呈类球型状的非晶纳米晶雾化粉末。
进一步地，于步骤S1中，所述母合金的制备方法具体如下：
S1-1、基于预设的成分式，以选取有对应元素成分中的金属原料置入冶炼炉进行冶炼；
S1-2、待冶炼上述金属原料至完全融化后，选取有对应元素成分中的合金原料或非金属原料进行二次冶炼；
S1-3、待二次冶炼上述材料均完全融化后，将所得合金熔液浇注入模具，而后冷却成型；以得到有非晶纳米晶母合金。
本发明的有益效果在于：
本发明的非晶纳米晶雾化粉末通过合金成分的设计优化，以使其制备的非晶纳米晶产品具有低损耗、高饱和磁感应强度及高直流偏置能力的特点。
具体实施方式
为了使本发明的技术方案、目的及其优点更清楚明白，以下实施例，对本发明进行进一步的解释说明。
本发明中的电感器制备方法，其具体涉及有以下步骤：
S1、将原料按预设的成分配方进行调配及冶炼，以制备得到有母合金；
S2、以现有技术中常规的制带破碎制粉方法或雾化制粉方法将所得母合金进行粉末的制备，以制备得到有非晶纳米晶粉末，其中，该以制带破碎制粉方法所得的粉末将呈不规则的片状；该雾化制粉方法所制得粉末将呈类球型状；
S3、将所得非晶纳米晶粉末进行绝缘包覆处理，以得到有包覆粉末；
S4、对所得包覆粉末进行成型处理，令相应粉末成粒状，以得到有非晶纳米晶绝缘成品粉末；
S5、将所得绝缘成品粉末进行进行压制成型并烘烤固化，后续处理以得到有所述电感器。
实施例1：
而基于步骤S1的应用中，本发明所预设的成分配方，其用于制备的合金成分包括有Fe100-a-b-c-x-y-zSiaBbCcMnxCryXZ,，式中X为P、Cu、Mo、Ni中的任意一种，其中8≤a≤15，6≤b≤12，0.2≤c≤3.0，0.1≤x≤3.5，0.5≤y≤2.5，0≤Z≤4.0。优选地，6≤b≤9，0.3≤y≤2.5。
该母合金的合金成分设置，将可使其后续制备的粉末具有较高非晶形成能力，强的耐腐蚀能力，高的饱和磁感应强度，低的矫顽力，其应用将具有着良好的应用前景。
上述合金成分方案优选应用为Fe74.8Si11B9C1.5Cr2.5Mn0.2P1或Fe74.8Si11B9C0.5Cr1.5Mn0.2P2或Fe73.8Si11B9C1.5Cr1.5Mn0.2P2或Fe79Si11B7C0.5Cr0.3Mn0.2P2或Fe79Si9B6.2C0.5Cr0.3Mn1P4。
而基于步骤S2的应用中，以该具有特定合金成分的母合金，可制备有相应的非晶纳米晶带材产品、呈片状的非晶纳米晶破碎粉末产品及呈类球状的非晶纳米晶雾化粉末产品。
则如附表1所示，以该母合金所制带材，其将具有以下性能特点。
附表1(不同成分非晶纳米晶带材试验性能)
而如附表2所示，以该母合金所制带材破碎成粉，通过现有技术的磁粉芯制备方式，其所制得的磁粉芯，将具有以下性能特点。
附表2(不同成分非晶纳米晶破碎粉末所制备磁粉芯试验性能)
而如附表3所示，基于现有技术的气雾化或水雾化或水气雾化联合方法，以该母合金所制雾化粉末，其性能将通过压环方式作评估，其性能评估结果将具有以下性能特点。
附表3(非晶纳米晶雾化粉末与常规粉末压环试验性能对比)
而如附表4所示，基于该合金成分的应用，则其中不同成分所制得的雾化粉末，其性能评估结果将具有以下性能特点。
附表4(不同成分非晶纳米晶雾化粉末压环试验性能对比)
实施例2：
本实施例与上述实施例1的区别在于，其合金成分方案优选应用为Fe74.8Si11B9C1.5Cr2.5Mn0.2Mo1或Fe76.8Si11B9C0.5Cr1.5Mn0.2Mo1或Fe73.8Si11B9C1.5Cr1.5Mn1.2Mo1或Fe78Si11B7C0.5Cr0.5Mn1Mo2。
而基于步骤S2的应用中，以该具有特定合金成分的母合金，可制备有相应的非晶纳米晶带材产品、呈片状的非晶纳米晶破碎粉末产品及呈类球状的非晶纳米晶雾化粉末产品。
则如附表5所示，以该母合金所制带材，其将具有以下性能特点。
附表5(不同成分非晶纳米晶带材试验性能)
而如附表6所示，以该母合金所制带材破碎成粉，通过现有技术的磁粉芯制备方式，其所制得的磁粉芯，将具有以下性能特点。
附表6(不同成分非晶纳米晶破碎粉末所制备磁粉芯试验性能)
而如附表7所示，基于现有技术的气雾化或水雾化或水气雾化联合方法，以该母合金所制雾化粉末，其性能将通过压环方式作评估，其性能评估结果将具有以下性能特点。
附表7(非晶纳米晶雾化粉末与常规粉末压环试验性能对比)
而如附表8所示，基于该合金成分的应用，则其中不同成分所制得的雾化粉末，按照一体成型电感评估方式进行评估，其性能评估结果将具有以下性能特点。
附表8(不同成分非晶纳米晶雾化粉末按照一体电感评估方式的性能对比)
实施例3：
本实施例与上述实施例1的区别在于，其合金成分方案优选应用为：Fe74.8Si11B9C1.5Cr2.5Mn0.2Ni1或Fe75.8Si11B9C0.5Cr1.5Mn0.2Ni2或Fe75.8Si11B7C1.5Cr1.5Mn0.2Ni3或Fe76.8Si11B7C0.5Cr0.5Mn0.2Ni4。
而基于步骤S2的应用中，以该具有特定合金成分的母合金，可制备有相应的非晶纳米晶带材产品、呈片状的非晶纳米晶破碎粉末产品及呈类球状的非晶纳米晶雾化粉末产品。
则如附表9所示，以该母合金所制带材，其将具有以下性能特点。
附表9(不同成分非晶纳米晶带材试验性能)
而如附表10所示，以该母合金所制带材破碎成粉，通过现有技术的磁粉芯制备方式，其所制得的磁粉芯，将具有以下性能特点。
附表10(不同成分非晶纳米晶破碎粉末所制备磁粉芯试验性能)
而如附表11所示，基于现有技术的气雾化或水雾化或水气雾化联合方法，以该母合金所制雾化粉末，其性能将通过压环方式作评估，其性能评估结果将具有以下性能特点。
附表11(非晶纳米晶雾化粉末与常规粉末压环试验性能对比)
而如附表12所示，基于该合金成分的应用，则其中不同成分所制得的雾化粉末，按照一体成型电感评估方式进行评估，其性能评估结果将具有以下性能特点。
附表12(不同成分非晶纳米晶雾化粉末按照一体电感评估方式的性能对比)
实施例4：
基于上述实施例1至3的应用情况下，为了对粉末流动性及松装密度的优化，则于该步骤S2所制备的的雾化粉末，我们可对其进行干燥、分级处理，以将其分设为不同目数级别进行应用。而作为优选的实施方式，将使该雾化粉末分设有-800目、-500目及-325目这三个级别；所采用粉末配比优选-800：-500：-325＝1:3:6；粉末混合配制优选超声分散的混合方式；粉末松装密度范围为3.2～4.5g/cm3。
下述附表13中，按照一体成型电感评估方式进行评估，将列明有不同粉末配比的性能区别效果。
附表13(不同粉末配比压环试验性能对比)
而基于本发明中的雾化粉末制备应用下，因该雾化粉末其形状呈类球型状，则于其粉末于粉末之间，或将存在有较多的间隙情况；则以此直接进行电感器产品生产，则其产品性能仍将存在有局限。
则本实施例中，于步骤S3应用，将使所得非晶纳米晶的雾化粉末进行绝缘包覆处理前，添加有填充粉末以充分搅拌混合；该填充粉末选择应用为铁硅铬和/或羰基铁粉，而令该非晶纳米晶的雾化粉末之间间隙形成填充，以混合形成有一种非晶纳米晶混合粉末，从而有效增加其中粉粒之间的结合强度，以有效地提升其后续产品的密度，达到改善产品性能的效果。
在非晶纳米晶混合粉末的应用情况下，则其所采用的雾化粉末的粒度范围将为-325～+500目，而该填充粉末的粒度范围为-600～800目，该填充粉末相对于非晶纳米晶混合粉末整体的添加比例为2～15％。
则下述附表14及附表15中，将列明有不同非晶纳米晶粉末与铁硅铬粉、羰基铁粉等不同配比情况下的压环试验性能对比结果。
附表14(非晶纳米晶粉末与铁硅铬粉末配比压环试验性能对比)
附表15(非晶纳米晶粉末与羰基铁粉配比压环试验性能对比)
实施例5：
对于步骤S5的应用过程中，为了精简电感器的压制成型流程，本发明针对有一体成型电感器结构形式以作出了其中的压制成型处理改进。
具体而言，对所得非晶纳米晶绝缘成品粉末进行加热处理并作进一步的搅拌混合，以令所得非晶纳米晶绝缘成品粉末的分离均匀受热；使该非晶纳米晶绝缘成品粉末整体加热至100～250摄氏度后，而后保温备用。
准备好对应的成型模腔，则对电感器设计有预制的线圈，将该预制的线圈放入成型模腔内，并填入有加热处理的非晶纳米晶绝缘成品粉末，以常规的冷压设备对成型模腔进行电感器的压制成型，以得到有一体电感胚料。该压制成型过程中，压力范围为400～800Mpa。
则下述附表16中，展示有不同加热温度情况下的非晶纳米晶绝缘成品粉末以冷压设备进行冷压的性能区别情况。
附表16(不同粉末温度压环试验性能对比)
之后，对所得一体电感胚料以150～220摄氏度的温度范围进行烘烤处理，烘烤处理时间1～2.5h；再因应具体产品的设计需要而对该电感器其中的线脚部分进行折弯处理，即可得到有所述电感器。
而进一步地为了提升产品磁导率，降低线圈变形情况，可选择采用分步成型组合的方式以进行电感器的制备。
例如，对一种采用T型预制磁体与U型预制磁体组合设置的电感器产品，则可因应结构特征，设置有相应的T形状成型模腔与U形状成型模腔；则使加热后的非晶纳米晶绝缘成品粉末粉料填入至相应成型模腔内，以先制取有该T型预制磁体与U型预制磁体。而后，将线圈放入该T型预制磁体与U型预制磁体间隙，进一步地通过填充粉料以进行二次压制，而获取有相应的电感器产品。
而另一方面，线圈放入该T型预制磁体与U型预制磁体间隙后，或可采用磁胶将两者接触边界粘结并以此填充产品内间隙，得到所需电感器产品。
基于“非晶纳米晶”的概念定义情况，上述相关非晶纳米晶合金产品，可认为是选择相应的非晶态合金产品、非晶态且纳米晶态合金产品或纳米晶态合金产品进行的应用。
以上所述仅为本发明的优选实施方式，对于本技术领域的技术人员，在不脱离本发明的实施原理前提下，依然可以对所述实施例进行修改，而相应修改方案也应视为本发明的保护范围。
Claims (8)
1.非晶纳米晶雾化粉末，其特征在于，其粉末颗粒均呈类球型状，其成分包括有Fe100-a-b-c-x-y-zSiaBbCcMnxCryXZ,，式中X为P、Cu、Mo、Ni中的任意一种，其中8≤a≤15，6≤b≤12，0.2≤c≤3.0，0.1≤x≤3.5，0.5≤y≤2.5，0≤Z≤4.0。
2.如权利要求1所述的非晶纳米晶雾化粉末，其特征在于，其中6≤b≤9，0.3≤y≤2.5。
3.如权利要求1所述的非晶纳米晶雾化粉末，其特征在于，其成分包括有Fe75Si11B9C2.5Cr2.3Mn0.2。
4.如权利要求2所述的非晶纳米晶雾化粉末，其特征在于，其成分包括有Fe74.8Si11B9C1.5Cr2.5Mn0.2P1或Fe74.8Si11B9C0.5Cr1.5Mn0.2P2或Fe73.8Si11B9C1.5Cr1.5Mn0.2P2或Fe79Si11B7C0.5Cr0.3Mn0.2P2或Fe79Si9B6.2C0.5Cr0.5Mn1P4。
5.如权利要求1所述的非晶纳米晶雾化粉末，其特征在于，其成分包括有Fe74.8Si11B9C1.5Cr2.5Mn0.2Mo1或Fe76.8Si11B9C0.5Cr1.5Mn0.2Mo1或Fe73.8Si11B9C1.5Cr1.5Mn1.2Mo1或Fe78Si11B7C0.5Cr0.5Mn1Mo2。
6.如权利要求1所述的非晶纳米晶雾化粉末，其特征在于，其成分包括有Fe74.8Si11B9C1.5Cr2.5Mn0.2Ni1或Fe74.8Si11B9C0.5Cr1.5Mn0.2Ni2或Fe74.8Si11B7C1.5Cr1.5Mn0.2Ni3或Fe76.8Si11B7C0.5Cr0.5Mn0.2Ni4。
7.如权利要求1至6任一所述的非晶纳米晶雾化粉末的制备方法，其特征在于，包括以下步骤：
S1、将原料按上述成分分子式进行调配及冶炼，以制备有母合金；
S2、以雾化制粉方法将所得母合金进行非晶纳米晶粉末的制备，以得到有粉末颗粒呈类球型状的非晶纳米晶雾化粉末。
8.如权利要求7所述的制备方法，其特征在于，于步骤S1中，所述母合金的制备方法具体如下：
S1-1、基于预设的成分式，以选取有对应元素成分中的金属原料置入冶炼炉进行冶炼；
S1-2、待冶炼上述金属原料至完全融化后，选取有对应元素成分中的合金原料或非金属原料进行二次冶炼；
S1-3、待二次冶炼上述材料均完全融化后，将所得合金熔液浇注入模具，而后冷却成型；以得到有非晶纳米晶母合金。
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