CN116604898A - 碳钢表面陶瓷金属互锁叠层材料的结构及其制备方法 - Google Patents

碳钢表面陶瓷金属互锁叠层材料的结构及其制备方法 Download PDF

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Publication number
CN116604898A
CN116604898A CN202310586923.9A CN202310586923A CN116604898A CN 116604898 A CN116604898 A CN 116604898A CN 202310586923 A CN202310586923 A CN 202310586923A CN 116604898 A CN116604898 A CN 116604898A
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China
Prior art keywords
carbon steel
layer
metal
ceramic
carburization
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CN202310586923.9A
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English (en)
Inventor
赵梓源
潘瑛
薛翌倩
赵明轩
李均明
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Xian University of Technology
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Xian University of Technology
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Priority to CN202310586923.9A priority Critical patent/CN116604898A/zh
Publication of CN116604898A publication Critical patent/CN116604898A/zh
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/011—Layered products comprising a layer of metal all layers being exclusively metallic all layers being formed of iron alloys or steels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
    • B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
    • B32B3/30—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by a layer formed with recesses or projections, e.g. hollows, grooves, protuberances, ribs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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    • C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
    • C23C12/02—Diffusion in one step
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    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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Abstract

本发明公开了碳钢表面陶瓷金属互锁叠层材料的制备方法，包括以下步骤：(1)将碳钢表面进行打磨，然后进行渗碳；(2)将表面进行打磨和抛光，然后通过表面构型工艺在碳钢基体表面做出锯齿形结构；(3)采用膜层制备技术在锯齿形表面上交替沉积具有碳化物形成能力的金属层和铁层，最外层沉积铁层，然后将沉积表面打磨平整；(4)将表面具有锯齿形金属多层膜碳钢进行渗碳，经过上述处理，在碳钢表面制备了陶瓷金属互锁叠层材料，陶瓷层陶瓷相体积分数高且致密无孔，层间界面具有微观锯齿状具有冶金结合，材料强度、韧性、抗冲击能力、耐磨性得到显著提升。

Description

碳钢表面陶瓷金属互锁叠层材料的结构及其制备方法
技术领域
本发明属于金属材料表面改性方法技术领域，涉及碳钢表面陶瓷金属互锁叠层材料，还涉及碳钢表面陶瓷金属互锁叠层材料的制备方法。
背景技术
制备由高强度陶瓷层和韧性金属层交替排列的叠层结构材料是碳钢表面强韧化的有效途径。目前，陶瓷/金属叠层结构材料的制备技术主要包括物理气相沉积(PVD)和化学气相沉积(CVD)，气相沉积技术具有无污染、成膜速度快、可以精确地控制各层厚度、具有良好的工艺稳定性等优点而成为当前制备叠层材料的主要方法，然而，这种叠层材料的层间界面和膜基界面存在过于平直、缺乏冶金结合等共性特点，因此界面的结合力差，制约了多层膜的力学性能。
发明内容
本发明的目的是提供碳钢表面陶瓷金属互锁叠层材料，解决了现有技术中层间界面过于平直的问题，本发明的另一目的是碳钢表面陶瓷金属互锁叠层材料的制备方法，解决了现有技术中存在的层间界面和膜基界面过于平直、缺乏冶金结合的问题。
本发明碳钢表面陶瓷金属互锁叠层材料所采用的技术方案是，包括两个碳钢层，两个碳钢层之间设置有若干个锯齿形金属多层膜，锯齿形金属多层膜包括碳化物陶瓷层和铁层，碳化物陶瓷层与相邻铁层之间的界面为不规则锯齿状。
本发明碳钢表面陶瓷金属互锁叠层材料的制备方法所采用的技术方案具体按照以下步骤实施：
步骤1：将碳钢表面进行打磨至除去表面污染物，然后放入渗碳炉中进行第一次渗碳处理，获得带有渗碳层的碳钢，渗碳层厚度为L；
步骤2：将带有渗碳层的碳钢表面进行预处理，然后采用表面构型工艺将渗碳层做出锯齿形结构，获得具有锯齿形表面的碳钢；
步骤3：采用膜层制备工艺在锯齿形表面的碳钢表面上沉积形成具有碳化物形成能力的金属层，通过膜层制备工艺在具有碳化物形成能力的金属层表面沉积铁元素形成韧性金属层，多次交替沉积韧性金属层与具有碳化物形成能力的金属层，得到表面具有锯齿形金属多层膜的碳钢，表面具有锯齿形金属多层膜的碳钢的最外层为韧性金属层；
步骤4：将表面具有锯齿形金属多层膜的碳钢的最外层韧性金属层打磨和抛光至表面平整，得到碳钢表面陶瓷金属互锁叠层材料粗坯；
步骤5：将陶瓷金属互锁叠层材料粗坯放入渗碳炉中进行第二次渗碳处理，当具有碳化物形成能力的金属层转变为碳化物陶瓷层时，渗碳结束，随炉冷却至室温，得到碳钢表面陶瓷金属互锁叠层材料。
本发明的特点还在于：步骤1中的第一次渗碳处理方式为固体渗碳、气体渗碳、真空渗碳、等离子渗碳中的一种，第一次渗碳处理的温度范围为800℃-1000℃。
步骤1中渗碳层厚度L的范围为10-200μm；
步骤2中，预处理为打磨和抛光，抛光后表面粗糙度达到0.01μm-0.02μm，表面构型工艺为机械加工和刻蚀工艺中的一种，机加械工为车铣；刻蚀工艺为反应离子刻蚀、深度反应离子刻蚀、离子束溅射刻蚀、湿法刻蚀、激光刻蚀中的任意一种；
步骤2中，锯齿高度H不超过步骤1中的渗碳层厚度L，锯齿高度H与渗碳层厚度L的比值范围为0.5-0.9；
步骤3中具有碳化物形成能力的金属为W、Mo、Cr、Ta、Nb、Ti、Zr、V中的任意一种元素组成的金属；
步骤3中的膜层制备工艺为物理气相沉积、化学气相沉积、化学镀、电镀、喷涂中的一种；
步骤3中，具有碳化物形成能力的金属层的层数范围为1-50层，单层厚度范围为0.5μm-10μm，具有碳化物形成能力的金属层选用相同或不同的材料，最外层的韧性金属层其厚度不小于锯齿高度H，其余韧性金属层的厚度范围为0.5μm-10μm；
步骤4中第二次渗碳处理采用固体渗碳、气体渗碳、真空渗碳、等离子渗碳、间隙原子渗碳中的一种方法，第二次渗碳处理温度范围为900℃-1200℃。
本发明的有益效果是：
(1)仿生贝壳结构制备出波纹状有序微观结构的薄板，陶瓷层、韧性金属层形成一级有序薄层结构，而后各个薄层呈现出45°的锯齿形交叉互锁结构，形成二级有序结构，多级有序结构之间相互协同，使材料呈现出超强、超韧的特性；
(2)高温过程中层间界面元素互扩散，形成具有冶金结合的高强度层间界面，陶瓷层与金属层之间的界面呈现不规则锯齿状，相较于平直界面具有更好增韧效果；
(3)碳化物原位析出，晶界强度高，碳化物陶瓷相中固溶铁元素，生长速率更快，韧性更好；
(4)在步骤4中，碳钢中的碳原子向表面方向扩散，同时碳钢外部的碳原子向基体方向扩散，即碳原子双向扩散，有助于缩小碳原子的扩散距离，起到细化碳化物晶粒的作用；
(5)碳在铁中的固溶度高，因此铁层能够促进碳持续向内扩散；
(6)最外层的铁层能够显著提高过渡金属元素对活性碳原子的吸收效率，也可以防止金属层表面碳势过高造成陶瓷层疏松多孔的问题；
(7)各陶瓷层可采用不同的陶瓷相，有利于进一步优化复合材料的强韧性。
附图说明
图1是本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中渗碳层厚度示意图；
图2是本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中碳钢基体表面锯齿形剖面结构示意图；
图3是本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中沉积金属层剖面结构示意图；
图4是本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中沉积金属层打磨后剖面结构示意图；
图5是本发明碳钢表面陶瓷金属互锁叠层材料的剖面结构示意图；
图6是本发明碳钢表面陶瓷金属互锁叠层材料的碳化物陶瓷层结构示意图。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明涉及碳钢表面陶瓷金属互锁叠层材料，包括两个碳钢层，两个碳钢层之间设置有若干个锯齿形金属多层膜，锯齿形金属多层膜包括碳化物陶瓷层和铁层，碳化物陶瓷层与相邻铁层之间的界面为不规则锯齿状；
本发明涉及碳钢表面陶瓷金属互锁叠层材料的制备方法，如图1-图6所示，具体按照以下步骤实施：
步骤1：将碳钢表面进行打磨，然后进行第一次渗碳处理，获得带有渗碳层的碳钢，渗碳层的厚度为L的碳钢，渗碳层厚度L范围为10-200μm，第一次渗碳处理方式为固体渗碳、气体渗碳、真空渗碳、等离子渗碳中的一种方法。温度范围为800℃-1000℃；
步骤2：将带有渗碳层的碳钢表面进行打磨和抛光，然后采用表面构型工艺在碳钢基体表面做出锯齿形结构，锯齿形状为直角边与带有渗碳层的碳钢表面呈45°的等腰直角三角形，等腰直角三角形斜边的高为锯齿高度H，锯齿高度H不超过渗碳层厚度L，锯齿高度H与渗碳层厚度L的比值范围为0.5-0.9，获得具有锯齿形表面的碳钢，表面构型工艺为机械加工和刻蚀工艺中的一种，机械加工为车铣，车铣采用微米级高精度车铣中心；刻蚀工艺包括反应离子刻蚀、深度反应离子刻蚀、离子束溅射刻蚀、湿法刻蚀、激光刻蚀中的一种；
步骤3：采用膜层制备工艺在步骤2所得的锯齿形表面上沉积W、Mo、Cr、Ta、Nb、Ti、Zr、V中的任意一种元素形成具有碳化物形成能力的金属层，通过膜层制备工艺在具有碳化物形成能力的金属层表面沉积铁元素形成韧性金属层，交替沉积具有碳化物形成能力的金属层和韧性金属层形成多层膜，其中，最外层为沉积的韧性金属层，获得表面具有锯齿形金属多层膜碳钢，膜层制备技术包括物理气相沉积、化学气相沉积、化学镀、电镀、喷涂中的一种；具有碳化物形成能力的金属层的层数范围为1-50层，单层厚度范围为0.5μm-10μm，具有碳化物形成能力的金属层选用相同或不同的材料，各层厚度变量独立调控，互不干扰；除最外层韧性金属层外，其余韧性金属层的厚度范围为0.5μm-10μm；
步骤4：将表面具有锯齿形金属多层膜的碳钢的最外层韧性金属层打磨和抛光至表面平整，得到碳钢表面陶瓷金属互锁叠层材料粗坯；
步骤5：将步骤4得到的碳钢表面陶瓷金属互锁叠层材料粗坯放入渗碳炉中进行第二渗碳处理，当具有碳化物形成能力的金属层转变为碳化物陶瓷层时，渗碳结束，随炉冷却至室温，得到碳钢表面陶瓷金属互锁叠层材料，第二次渗碳采用为固体渗碳、气体渗碳、真空渗碳、等离子渗碳、间隙原子渗碳中的一种方法，第二次渗碳温度范围为900℃-1200℃。
在本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中：步骤1中渗碳的作用之一是使碳钢表层含碳量增加，因此，在步骤4对表面具有锯齿形金属多层膜碳钢的渗碳过程中，不仅有外部碳原子向叠层材料中扩散，即向内渗碳，碳钢基体表层的碳原子也向叠层材料内扩散，即向外扩散，从而达到了双向渗碳的效果，双向渗碳不仅能够有效的增加渗碳层厚度，而且能细化碳化物晶粒。
具有碳化物形成能力的金属层厚度为d1，韧性金属层厚度为d2，具有碳化物形成能力的金属层数N，最外层韧性金属层厚度为d3。
在本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中：步骤2中锯齿状构型的作用是使叠层材料形成互锁的几何构型，提高表面强韧性，其原理是：随着底层材料装配角度增加，强度呈线性增加趋势，韧性呈线性减小的趋势；随着外层材料装配角度增大，韧性呈线性减小趋势，而强度在装配角小于45°时呈增强趋势，超过45°时趋于稳定，因此，交叠材料装配角度为45°时，材料的强韧性达到最大值。故设计直角边与碳钢表面呈45°等腰直角三角形的锯齿状结构为最优解。
在本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中：步骤3中沉积最外层的铁层的作用为提高渗碳效率，降低陶瓷层孔隙率。其原理是：最外层的铁层在步骤4中对表面具有锯齿形金属多层膜碳钢渗碳时，能够高效的吸收环境中的活性碳原子，且碳原子能够穿过铁层向叠层材料中扩散，使具有碳化物形成能力的金属层转变为碳化物陶瓷层。最外层的铁层作为中间媒介，能够显著提高过渡金属元素对活性碳原子的吸收效率。另一方面，由于铁层对碳的固溶度有上限，因此当环境碳势过高时，可以防止金属层表面碳势过高造成陶瓷层疏松多孔的问题。
在本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中：步骤4的作用包括两方面，一是将具有碳化物形成能力的金属层转化为陶瓷层，二是促进层间界面的元素互扩散，形成具有冶金结合的层间界面。同时，碳化物在互扩散区析出时形成了微观不规则锯齿状层间界面，相较于平直界面具有更好增韧效果。
在本发明碳钢表面陶瓷金属互锁叠层材料的制备方法中：步骤4中各铁层在渗碳过程中的作用是能够存储和释放碳原子，促进碳持续向内扩散，将具有碳化物形成能力的金属层转化为高质量陶瓷层。
实施例
实施例1
步骤1：将Q215钢表面进行打磨，然后进行固体渗碳，渗碳温度为800℃，渗碳层厚度(L)范围为10μm。
步骤2：将步骤1中渗碳后的碳钢表面进行打磨和抛光，采用离子束溅射刻蚀在其表面做出锯齿形结构，锯齿形状为直角边与碳钢表面呈45°的等腰直角三角形，锯齿高度H为9μm，获得具有锯齿形表面的碳钢；
步骤3：采用阴极弧离子镀(物理气相沉积中的一种)在步骤2所得的锯齿形表面上交替沉积钨层和铁层。钨层共50层，各钨层厚度为0.5μm，除最外层铁层外，其余铁层的厚度为0.5μm，最外层沉积铁层，其厚度为12μm；
步骤4：将最外层沉积铁层表面打磨抛光至表面平整，得到互锁叠层材料粗坯；
步骤5：将步骤4得到的互锁叠层材料粗坯进行气体渗碳。渗碳温度为1200℃，当步骤3中制备的所有钨层转变为WC陶瓷层时，渗碳结束，渗碳之后随炉冷却至室温，得到碳钢表面陶瓷金属互锁叠层材料；
最终在Q215钢表面获得WC/Fe互锁叠层材料，其中WC层为固溶了Fe原子的陶瓷层，Fe层为以Fe为主要元素的铁碳合金层，层间界面在微观上呈不规则锯齿状且具有冶金结合。
通过上述方法，得到的碳钢表面陶瓷金属互锁叠层材料具有以下特征：(1)形成波纹状有序微观结构的薄板，陶瓷层、韧性金属层形成一级有序薄层结构，而后各个薄层呈现出45°的锯齿形互锁结构，形成二级有序结构。多级有序结构之间相互协同，使材料呈现出超强，超韧的特性；
(2)陶瓷层致密无孔，陶瓷层中碳化物体积分数高达95％；
(3)陶瓷层与铁层之间的界面在微观上呈不规则锯齿状，且具有冶金结合。层间界面结合力可达80N。
实施例2
步骤1：将45钢表面进行打磨，然后进行气体渗碳，渗碳温度为1000℃，渗碳层厚度(L)范围为200μm。
步骤2：将步骤1中渗碳后的碳钢表面进行打磨和抛光，采用微米级高精度车铣中心在其表面做出锯齿形结构，锯齿形状为直角边与碳钢表面呈45°的等腰直角三角形，锯齿高度H为100μm，获得具有锯齿形表面的碳钢；
步骤3：采用热喷涂在步骤2所得的锯齿形表面上交替沉积钽(Ta)层和铁层。钽层共10层，各钽层厚度为10μm。除最外层铁层外，其余铁层的厚度为2μm，最外层沉积铁层，其厚度为110μm；
步骤4：将最外层沉积铁层表面打磨抛光至表面平整，得到互锁叠层材料粗坯；
步骤5：将步骤3得到的互锁叠层材料粗坯进行等离子渗碳。渗碳温度为1200℃，当步骤3中制备的所有钽层转变为TaC陶瓷层时，渗碳结束，渗碳之后随炉冷却至室温，最终在45钢表面获得TaC/Fe互锁叠层材料，其中TaC层为固溶了Fe原子的陶瓷层，Fe层为以Fe为主要元素的铁碳合金层，层间界面在微观上呈不规则锯齿状且具有冶金结合。
通过上述方法，得到的碳钢表面陶瓷金属互锁叠层材料具有以下特征：(1)形成波纹状有序微观结构的薄板，陶瓷层、韧性金属层形成一级有序薄层结构，而后各个薄层呈现出45°的锯齿形互锁结构，形成二级有序结构。多级有序结构之间相互协同，使材料呈现出超强，超韧的特性；
(2)陶瓷层致密无孔，陶瓷层中TaC体积分数高达98％；
(3)陶瓷层与铁层之间的界面在微观上呈不规则锯齿状，且具有冶金结合。层间界面结合力可达100N。
实施例3
步骤1：将T12钢表面进行打磨，然后进行真空渗碳，渗碳温度为900℃，渗碳层厚度(L)范围为50μm；
步骤2：将步骤1中渗碳后的碳钢表面进行打磨和抛光，采用反应离子刻蚀在其表面做出锯齿形结构，锯齿形状为直角边与碳钢表面呈45°的等腰直角三角形，锯齿高度H为30μm，获得具有锯齿形表面的碳钢；
步骤3：采用电镀在步骤2所得的锯齿形表面上交替沉积钛层和铁层。钛层共1层，钛层厚度为10μm。除最外层铁层外，其余铁层的厚度为10μm。最外层沉积铁层，其厚度为30μm；
步骤4：将最外层沉积铁层表面打磨抛光至表面平整，得到互锁叠层材料粗坯；
步骤5：将步骤3得到的互锁叠层材料粗坯进行真空渗碳。渗碳温度为1100℃，当步骤3中制备的所有钛层转变为TiC陶瓷层时，渗碳结束，渗碳之后随炉冷却至室温，最终在T12钢表面获得TiC/Fe互锁叠层材料，其中TiC层为固溶了Fe原子的陶瓷层，Fe层为以Fe为主要元素的铁碳合金层，层间界面在微观上呈不规则锯齿状且具有冶金结合。
通过上述方法，得到的碳钢表面陶瓷金属互锁叠层材料具有以下特征：(1)形成波纹状有序微观结构的薄板，陶瓷层、韧性金属层形成一级有序薄层结构，而后各个薄层呈现出45°的锯齿形互锁结构，形成二级有序结构。多级有序结构之间相互协同，使材料呈现出超强，超韧的特性；
(2)陶瓷层致密无孔，陶瓷层中TiC体积分数高达92％；
(3)陶瓷层与铁层之间的界面在微观上呈不规则锯齿状，且具有冶金结合。层间界面结合力可达110N。
实施例4：
步骤1：将45钢表面进行打磨，然后进行等离子渗碳，渗碳温度为950℃，渗碳层厚度(L)范围为100μm；
步骤2：将步骤1中渗碳后的碳钢表面进行打磨和抛光，采用湿法刻蚀在其表面做出锯齿形结构，锯齿形状为直角边与碳钢表面呈45°的等腰直角三角形，锯齿高度H为60μm，获得具有锯齿形表面的碳钢；
步骤3：采用多弧离子镀(物理气相沉积中的一种)在步骤2所得的锯齿形表面上交替沉积钼层和铁层，钼层共20层，各钼层厚度为2μm，除最外层铁层外，其余铁层的厚度为0.5μm，最外层沉积铁层，其厚度为65μm，然后将沉积表面磨平；，
步骤4：将最外层沉积铁层表面打磨抛光至表面平整，互锁叠层材料粗坯；
步骤5：将步骤4得到的互锁叠层材料粗坯进行固体渗碳，渗碳温度为900℃，当步骤3中制备的所有钼层转变为Mo2C陶瓷层时，渗碳结束，渗碳之后随炉冷却至室温，最终在45钢表面获得Mo2C/Fe互锁叠层材料，其中Mo2C层为固溶了Fe原子的陶瓷层，Fe层为以Fe为主要元素的铁碳合金层，层间界面在微观上呈不规则锯齿状且具有冶金结合。
通过上述方法，得到的碳钢表面陶瓷金属互锁叠层材料有以下特征：
(1)形成波纹状有序微观结构的薄板，陶瓷层、韧性金属层形成一级有序薄层结构，而后各个薄层呈现出45°的锯齿形互锁结构，形成二级有序结构，多级有序结构之间相互协同，使材料呈现出超强，超韧的特性；
(2)陶瓷层致密无孔，陶瓷层中碳化物体积分数高达99％；
(3)陶瓷层与铁层之间的界面在微观上呈不规则锯齿状，且具有冶金结合，层间界面结合力可达90N。
实施例5：
步骤1：将Q235钢表面进行打磨，然后进行固体渗碳，渗碳温度为800℃，渗碳层厚度(L)范围为20μm。
步骤2：将步骤1中渗碳后的碳钢表面进行打磨和抛光，采用激光刻蚀在其表面做出锯齿形结构，锯齿形状为直角边与碳钢表面呈45°的等腰直角三角形，锯齿高度H为10μm，获得具有锯齿形表面的碳钢；
步骤3：采用化学气相沉积在步骤2所得的锯齿形表面上以锆层、铁层、钽层、铁层为周期沉积，锆层共3层，钽层共3层，沿着基体到表面方向各锆层和钽层的厚度分别为1μm、2μm、3μm，除最外层铁层外，其余铁层的厚度为0.5μm，最外层沉积铁层，其厚度为12μm；，
步骤4：将最外层沉积铁层表面打磨抛光至表面平整，得到互锁叠层材料粗坯；
步骤5：将步骤4得到的互锁叠层材料粗坯进行气体渗碳，渗碳温度为1100℃，当步骤3中制备的所有锆层和钽层分别转变为ZrC陶瓷层和TaC陶瓷层时，渗碳结束，随炉冷却至室温，最终在Q235钢表面获得ZrC(TaC)/Fe互锁叠层材料，其中ZrC层和TaC为固溶了Fe原子的陶瓷层，Fe层为以Fe为主要元素的铁碳合金层，层间界面在微观上呈不规则锯齿状且具有冶金结合。
通过上述方法，得到的碳钢表面陶瓷金属互锁叠层材料有以下特征：
(1)形成波纹状有序微观结构的薄板，陶瓷层、韧性金属层形成一级有序薄层结构，而后各个薄层呈现出45°的锯齿形互锁结构，形成二级有序结构，多级有序结构之间相互协同，使材料呈现出超强，超韧的特性；
(2)陶瓷层致密无孔，陶瓷层中碳化物体积分数高达98％；
(3)陶瓷层与铁层之间的界面在微观上呈不规则锯齿状，且具有冶金结合，层间界面结合力可达95N。
对本实施例1-5制备的碳钢表面陶瓷金属互锁叠层材料进行层间界面结合力测试，测试结果如下表：
编号 层间界面结合力
实施例1 80N
实施例2 100N
实施例3 110N
实施例4 90N
实施例5 95N
通过以上方式，本发明的陶瓷层与铁层之间的界面在微观上呈不规则锯齿状，且冶金结合层间界面结合力超过80N，相较于平直界面具有更好增韧效果；陶瓷层、韧性金属层形成一级有序薄层结构，而后各个薄层呈现出45°的锯齿形交叉互锁结构，形成二级有序结构，多级有序结构之间相互协同，使材料呈现出超强、超韧的特性。

Claims (10)

1.碳钢表面陶瓷金属互锁叠层材料，其特征在于，包括两个碳钢层，所述两个碳钢层之间设置有若干个锯齿形金属多层膜，所述锯齿形金属多层膜包括碳化物陶瓷层和铁层，所述碳化物陶瓷层上方设置有铁层，每个所述碳化物陶瓷层与相邻铁层之间的界面为不规则锯齿状。
2.碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，具体包括以下步骤：
步骤1：将碳钢表面进行打磨至除去表面污染物，然后放入渗碳炉中进行第一次渗碳处理，获得带有渗碳层的碳钢，所述渗碳层厚度为L；
步骤2：将带有渗碳层的碳钢表面进行预处理，然后采用表面构型工艺将渗碳层做出锯齿形结构，获得具有锯齿形表面的碳钢；
步骤3：采用膜层制备工艺在锯齿形表面的碳钢表面上沉积形成具有碳化物形成能力的金属层，通过膜层制备工艺在具有碳化物形成能力的金属层表面沉积铁元素形成韧性金属层，多次交替沉积韧性金属层与具有碳化物形成能力的金属层，得到表面具有锯齿形金属多层膜的碳钢，所述表面具有锯齿形金属多层膜的碳钢的最外层为韧性金属层；
步骤4：将表面具有锯齿形金属多层膜的碳钢的最外层韧性金属层打磨和抛光至表面平整，得到碳钢表面陶瓷金属互锁叠层材料粗坯；
步骤5：将陶瓷金属互锁叠层材料粗坯放入渗碳炉中进行第二渗碳处理，当具有碳化物形成能力的金属层转变为碳化物陶瓷层时，渗碳结束，随炉冷却至室温，得到碳钢表面陶瓷金属互锁叠层材料。
3.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤1中所述的第一次渗碳处理方式为固体渗碳、气体渗碳、真空渗碳、等离子渗碳中的一种，所述第一次渗碳处理的温度范围为800℃-1000℃。
4.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤1中所述渗碳层厚度L的范围为10-200μm。
5.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤2中，所述预处理为打磨和抛光，抛光后表面粗糙度达到0.01μm-0.02μm，所述的表面构型工艺为机械加工和刻蚀工艺中的一种，所述机加械工为车铣；所述刻蚀工艺为反应离子刻蚀、深度反应离子刻蚀、离子束溅射刻蚀、湿法刻蚀、激光刻蚀中的任意一种。
6.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤2中，所述锯齿高度H不超过步骤1中的渗碳层厚度L所述锯齿高度H与渗碳层厚度L的比值范围为0.5-0.9。
7.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤3中所述具有碳化物形成能力的金属层W、Mo、Cr、Ta、Nb、Ti、Zr、V中的任意一种元素。
8.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤3中所述的膜层制备工艺为物理气相沉积、化学气相沉积、化学镀、电镀、喷涂中的一种。
9.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤3中所述具有碳化物形成能力的金属层的层数范围为1-50层，单层厚度范围为0.5μm-10μm，具有碳化物形成能力的金属层选用相同或不同的材料，最外层的韧性金属层其厚度不小于锯齿高度H，其余韧性金属层的厚度范围为0.5μm-10μm。
10.根据权利要求2所述的碳钢表面陶瓷金属互锁叠层材料的制备方法，其特征在于，步骤4中所述的第二次渗碳处理采用固体渗碳、气体渗碳、真空渗碳、等离子渗碳、间隙原子渗碳中的一种方法，所述第二次渗碳处理温度范围为900℃-1200℃。
CN202310586923.9A 2023-05-23 2023-05-23 碳钢表面陶瓷金属互锁叠层材料的结构及其制备方法 Pending CN116604898A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117966083A (zh) * 2024-04-02 2024-05-03 西安理工大学 镜面对称双梯度叠层复合材料表面渗硼方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117966083A (zh) * 2024-04-02 2024-05-03 西安理工大学 镜面对称双梯度叠层复合材料表面渗硼方法
CN117966083B (zh) * 2024-04-02 2024-06-04 西安理工大学 镜面对称双梯度叠层复合材料表面渗硼方法

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