双辉等离子表面冶金Ni-Cr耐蚀钢板若干应用基础问题的研究
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摘要
普通碳钢材料以其良好的塑性和韧性、易加工、成本低等特点被广泛地应用于建筑、交通，机械和能源等领域。然而，碳钢材料却具有一个普遍的问题：易腐蚀。国内外的学者们通过开发各种耐蚀钢和耐候钢来改善钢铁的耐蚀性，但该类钢铁材料大量使用耐蚀合金元素使得材料成本上升，且不能有效地利用合金元素。碳钢钢板在钢铁材料中占有非常重要的地位。因此，在碳钢钢板表面形成不锈钢成为世界冶金界的一个梦想。本论文提出采用双辉等离子表面冶金技术在普通碳钢钢板表面制备镍基耐蚀合金层，以形成一种新型的等离子表面冶金耐蚀碳钢钢板。该新型钢板可以在保持基体碳钢良好的塑韧性的同时具有优秀的表面耐蚀性能，从而达到节约贵重合金元素，大幅度降低材料成本的作用。论文针对等离子表面冶金耐蚀钢板规模应用中涉及的一系列基础科学问题进行系统地研究。
为解决等离子表面冶金规模生产中合金元素供给量不足的问题，论文提出一种格栅状空心阴极源极结构，以Ni80Cr20合金靶为源极材料，在Q235低碳钢表面获得与基体结合良好，且成分呈梯度分布的Ni-Cr合金层，合金层的主要物相均为奥氏体相Ni2.9Cr0.7Fe0.36和少量镍铁矿相Ni3Fe。与平面状源极结构相比，格栅状空心阴极源极结构由于能够提供更充足的合金元素供给量，其Ni-Cr合金层具有更厚的厚度和更高的Ni、Cr合金元素含量，耐蚀性能也明显优于平面状源极结构下的合金层。
论文对等离子表面冶金工艺参数对Ni-Cr合金层的组织性能的影响进行了系统研究。结果表明，提高处理温度可以增加Ni-Cr合金层的厚度，增大合金层中Ni、Cr合金元素含量，从而改善Ni-Cr合金层的耐蚀性能，在1000℃左右的处理温度下能够获得耐蚀性能较好的Ni-Cr合金层。增大工作气压使得Ni-Cr合金层的厚度和Ni、Cr元素含量均呈现先增后减的趋势，Ni-Cr合金层的耐蚀性能也同样呈现先升后降的趋势，51Pa左右的工作气压下的Ni-Cr合金层耐蚀性能最好。增加极间距使得Ni-Cr合金层厚度和合金元素含量呈现先增后减的趋势，而其耐蚀性能同样呈现先升后降的趋势，其中在15mm左右的极间距下的Ni-Cr合金层耐蚀性能最好。延长保温时间可以获得更厚的Ni-Cr合金层，提高Ni-Cr合金层的耐蚀性能，但是保温3h后Ni-Cr合金层的耐蚀性的改善就不再十分明显。
研究了基体碳含量对合金层组织性能的影响规律。在Q235低碳钢、45钢和T8钢三种不同碳含量的碳钢表面制备了Ni-Cr合金层。合金层的扩散层厚度随着基体碳含量增多而增大。Q235低碳钢基体的合金层为致密的纤维状结构，45钢和T8钢基体的合金层为对腐蚀不利的多空的锥形柱状晶结构，且柱状晶随着基体碳含量增加而呈现粗化现象。电化学腐蚀试验结果显示：Q235低碳钢基体的Ni-Cr合金层的耐蚀性能最好，T8钢基体的合金层次之，而45钢基体的合金层的耐蚀性能表现最差。
Ni-Cr合金靶材成分对Ni-Cr合金层的元素成分和物相具有直接影响。当合金靶中合金元素Cr含量为20%时，Ni-Cr合金层的主要物相为Ni2.9Cr0.7Fe0.36相和少量Ni3Fe相；随着合金靶中Cr元素含量增加到40%时，Ni-Cr合金层的主要物相转变为Cr0.19Fe0.7Ni0.11相和少量Fe-Cr相；当合金靶中Cr元素的含量进一步增加，Ni-Cr合金层的物相中Fe-Cr相含量增加，Cr0.19Fe0.7Ni0.11相含量减少；当合金靶中Cr元素含量增加到80%时，Ni-Cr合金层的主要物相转变为Fe-Cr相和少量Cr0.19Fe0.7Ni0.11相。各成分的合金靶下，Ni-Cr合金层表面Ni、Cr元素都主要以单质Ni、Cr和NiO形式存在。通过对Ni-Cr合金层中Ni、Cr合金元素的成分偏析效应进行了研究，建立了合金靶成分与合金层成分的关系公式。纳米压痕试验表明，随着合金靶中Cr元素含量增加，合金层的塑韧性降低。增加合金靶中Cr元素含量，可以提高Ni-Cr合金层中的Cr元素含量，使得合金层表面更容易形成连续致密的钝化膜，合金层的耐蚀性能得到进一步提高。然而，由于Ni60Cr40合金靶下的Ni-Cr合金层厚度较薄，其耐蚀性能较Ni80Cr20合金靶下的合金层要差。
建立了Ni-Cr合金层中的主要物相Ni2.9Cr0.7Fe0.36的原子模型Ni9Cr2Fe1，并根据能量最低原理，得到了Ni2.9Cr0.7Fe0.36相的平衡态几何结构。Ni9Cr2Fe1晶体的成键电子主要由Cr3s和3p价电子贡献，而其Fermi能级处的态密度主要由Ni3d和Cr3d电子贡献。Ni-Cr合金层中Ni、Cr、Fe原子间的电荷交互作用使Fe原子呈现正电性，促使Fe原子电位上升，导致Fe原子较难发生电化学腐蚀反应。因此，Ni-Cr合金层能够为基体提供有效的腐蚀防护作用。
设计了一种新型的双辉等离子表面冶金装置以满足工业化的需求，这种新型的等离子表面处理装置能够对大面积碳钢钢板进行处理，从而获得等离子表面冶金Ni-Cr耐蚀钢板。静态浸泡腐蚀试验和中性盐雾腐蚀试验的结果均表明，等离子表面冶金Ni-Cr耐蚀钢板的耐蚀性能要明显优于基材Q235低碳钢，其耐蚀性能接近于316L不锈钢。
Carbon steel was widely used in many fields such as building, traffic, mechanism and energy,because of its well plasticity and toughness, easy processing and low cost. However, the carbon steelhas a common problem, low corrosion resistance. Scholars developed corrosion-resistant steel andweathering steel to improve the corrosion resistance of steel, but the corrosion-resistant alloyingelements increased the cost and can not be used effectively. The steel plat is very important for thesteel materials. Therefore, the formation of stainless steel on carbon steel plate has been the dream ofworld metallurgical industry. In this paper, to form a new type of plasma surface metallurgycorrosion-resistant carbon steel plate, double glow plasma surface metallurgy technique was used toprepare the nickel-base alloyed layer on carbon steel. This new surface metallurgy material, whichexhibits good plasticity, toughness and excellent corrosion resistance, can economize costly alloyingelements and reduce the cost of materials. Meanwhile, a series of basic scientific issues related to thescale application of surface metallurgy steel plate were studied systematically.
In order to solve the problem of insufficient allowance of alloying elements in scale production,grid-like hollow cathode source structure was introduced. Using Ni80Cr20alloyed target as sourcematerial, Ni-Cr alloyed layer was formed on Q235steel. The alloyed layer combined excellently withsubstrate and had gradient distribution of composition. The main phase of alloyed layer was austeniticsteel Ni2.9Cr0.7Fe0.36and a little of awaruite Ni3Fe. Compared with planar source structure, thegrid-like hollow cathode source structure could provide more adequate allowance of alloyingelements, so its Ni-Cr alloyed layer had thicker thickness and higher content of Ni, Cr alloyingelements which result in more excellent corrosion resistance.
In the paper, the effect of process parameters on microstructure and properties of Ni-Cr alloyedlayer were studied systematically. The results showed that the thickness of Ni-Cr alloyed layer and thecontent of Ni and Cr alloying elements increased as the treatment temperature increased. As a result,the corrosion-resistant of Ni-Cr alloyed layer was improved, and the best corrosion resistance wasobtained when the treatment temperature reached about1000℃. With the increasing of workingpressure, the thickness of Ni-Cr alloyed layer and the content of Ni and Cr alloying elements inalloyed layer showed trend of first increased and then decreased. Meanwhile, the corrosion resistanceof alloyed layer also increased firstly and reduced afterwards, and the best corrosion resistance wasobtained when the working pressure was about51Pa. Increasing the electrode spacing, the thicknessof Ni-Cr alloyed layer, the content of Ni and Cr alloying elements and the corrosion resistance of alloyed layer exhibited the same results. The optimal electrode spacing was about15mm. Prolongingthe holding time could obtain thicker Ni-Cr alloyed layer, and improve the corrosion resistance ofalloyed layer. But the improvement was not significant anymore after heat for3h.
The influence of the carbon content of the substrate on the microstructure and properties of thealloyed layer was investigated. Ni-Cr alloyed layers were obtained on surface of Q235steel,45steeland T8steel. The thickness of diffusion layer of Ni-Cr alloyed layer increased as the carbon contentincreased. The Ni-Cr alloyed layer on Q235exhibited compact fibrous structure, while the alloyedlayer on45steel and T8steel showed porous tapered column structure which showed coarseningphenomenon as the carbon content increased. The fibrous structure is dense, while the tapered columnstructure contains voids. Therefore, the Ni-Cr alloyed layer on Q235steel had the bestcorrosion-resistant. For the tapered column structure Ni-Cr alloyed layer, the corrosion-resistant ofalloyed layer on T8steel was better than the alloyed layer on45steel due to its thicker thickness ofdiffusion layer.
The composition of Ni-Cr alloyed target has direct effect on the composition and phase of Ni-Cralloyed layer. When the content of Cr alloying element in alloyed target was20%, the main phase wasNi2.9Cr0.7Fe0.36and a little of Ni3Fe. Then the content increased to40%, the phase of alloyed layerchanged into Cr0.19Fe0.7Ni0.11and a little of Fe-Cr. As the content of Cr alloying element in alloyedtarget increased, the content of Cr0.19Fe0.7Ni0.11decreased and the content of Fe-Cr in alloyed layerincreased. Finally the content reached80%, the main phase of alloyed layer was Fe-Cr and a little ofCr0.19Fe0.7Ni0.11. Under different alloyed targets, the Ni and Cr elements on surface of Ni-Cralloyed layer exist in the form of simple substance Ni, Cr and NiO. The composition segregationeffect of Ni and Cr alloying elements in alloyed layer was investigated, and then the relation formulaof the composition of alloyed target and the composition of Ni-Cr alloyed layer was founded. Thenano-indentation test of Ni-Cr alloyed layer indicated that the plasticity and toughness of alloyedlayer reduced as the content of Cr alloying element in alloyed target increased. As the content of Cralloying element in alloyed target increased, the content of Cr alloying element in Ni-Cr alloyed layerincreased, the continuous dense passive film can be easily formed on surface of alloyed layer whichcould improve the corrosion-resistant of alloyed layer. However, thickness of Ni-Cr alloyed layerunder Ni60Cr40alloyed target was thin, thus its corrosion-resistant was worse than that underNi80Cr20alloyed target.
The atom model Ni9Cr2Fe1of Ni2.9Cr0.7Fe0.36, which was the main phase in Ni-Cr alloyed layer,was built. According to the energy minimum principle, equilibrium geometric structure ofNi2.9Cr0.7Fe0.36was obtained. The bonding electron of Ni9Cr2Fe1was contributed by the3s and3pvalence electron of Cr, while the density of states at the Fermi level was contributed by the3d electron of Ni and Cr. The charge interaction of Ni, Cr and Fe atoms in Ni-Cr alloyed layer made theFe atom exhibit positively charged and increased the potential of Fe atom which inreased thedifficulty of the electrochemical corrosion reaction of Fe atom. Therefore, the Ni-Cr alloyed layercould provide effective corrosion resistance for the substrate.
In order to meet the needs of industrialization, a new type of double glow plasma surfacemetallurgy device was designed. The large area of carbon steel plate could be processed in theequipment to obtain plasma surface metallurgy Ni-Cr corrosion-resistant steel plate. The results ofstatic immersion corrosion test and salt spray corrosion test demonstrated that the corrosion-resistantof plasma surface metallurgy Ni-Cr corrosion-resistant steel plate was better than that of Q235lowcarbon steel, and its corrosion-resistant was close to that of316L stainless steel.
为解决等离子表面冶金规模生产中合金元素供给量不足的问题，论文提出一种格栅状空心阴极源极结构，以Ni80Cr20合金靶为源极材料，在Q235低碳钢表面获得与基体结合良好，且成分呈梯度分布的Ni-Cr合金层，合金层的主要物相均为奥氏体相Ni2.9Cr0.7Fe0.36和少量镍铁矿相Ni3Fe。与平面状源极结构相比，格栅状空心阴极源极结构由于能够提供更充足的合金元素供给量，其Ni-Cr合金层具有更厚的厚度和更高的Ni、Cr合金元素含量，耐蚀性能也明显优于平面状源极结构下的合金层。
论文对等离子表面冶金工艺参数对Ni-Cr合金层的组织性能的影响进行了系统研究。结果表明，提高处理温度可以增加Ni-Cr合金层的厚度，增大合金层中Ni、Cr合金元素含量，从而改善Ni-Cr合金层的耐蚀性能，在1000℃左右的处理温度下能够获得耐蚀性能较好的Ni-Cr合金层。增大工作气压使得Ni-Cr合金层的厚度和Ni、Cr元素含量均呈现先增后减的趋势，Ni-Cr合金层的耐蚀性能也同样呈现先升后降的趋势，51Pa左右的工作气压下的Ni-Cr合金层耐蚀性能最好。增加极间距使得Ni-Cr合金层厚度和合金元素含量呈现先增后减的趋势，而其耐蚀性能同样呈现先升后降的趋势，其中在15mm左右的极间距下的Ni-Cr合金层耐蚀性能最好。延长保温时间可以获得更厚的Ni-Cr合金层，提高Ni-Cr合金层的耐蚀性能，但是保温3h后Ni-Cr合金层的耐蚀性的改善就不再十分明显。
研究了基体碳含量对合金层组织性能的影响规律。在Q235低碳钢、45钢和T8钢三种不同碳含量的碳钢表面制备了Ni-Cr合金层。合金层的扩散层厚度随着基体碳含量增多而增大。Q235低碳钢基体的合金层为致密的纤维状结构，45钢和T8钢基体的合金层为对腐蚀不利的多空的锥形柱状晶结构，且柱状晶随着基体碳含量增加而呈现粗化现象。电化学腐蚀试验结果显示：Q235低碳钢基体的Ni-Cr合金层的耐蚀性能最好，T8钢基体的合金层次之，而45钢基体的合金层的耐蚀性能表现最差。
Ni-Cr合金靶材成分对Ni-Cr合金层的元素成分和物相具有直接影响。当合金靶中合金元素Cr含量为20%时，Ni-Cr合金层的主要物相为Ni2.9Cr0.7Fe0.36相和少量Ni3Fe相；随着合金靶中Cr元素含量增加到40%时，Ni-Cr合金层的主要物相转变为Cr0.19Fe0.7Ni0.11相和少量Fe-Cr相；当合金靶中Cr元素的含量进一步增加，Ni-Cr合金层的物相中Fe-Cr相含量增加，Cr0.19Fe0.7Ni0.11相含量减少；当合金靶中Cr元素含量增加到80%时，Ni-Cr合金层的主要物相转变为Fe-Cr相和少量Cr0.19Fe0.7Ni0.11相。各成分的合金靶下，Ni-Cr合金层表面Ni、Cr元素都主要以单质Ni、Cr和NiO形式存在。通过对Ni-Cr合金层中Ni、Cr合金元素的成分偏析效应进行了研究，建立了合金靶成分与合金层成分的关系公式。纳米压痕试验表明，随着合金靶中Cr元素含量增加，合金层的塑韧性降低。增加合金靶中Cr元素含量，可以提高Ni-Cr合金层中的Cr元素含量，使得合金层表面更容易形成连续致密的钝化膜，合金层的耐蚀性能得到进一步提高。然而，由于Ni60Cr40合金靶下的Ni-Cr合金层厚度较薄，其耐蚀性能较Ni80Cr20合金靶下的合金层要差。
建立了Ni-Cr合金层中的主要物相Ni2.9Cr0.7Fe0.36的原子模型Ni9Cr2Fe1，并根据能量最低原理，得到了Ni2.9Cr0.7Fe0.36相的平衡态几何结构。Ni9Cr2Fe1晶体的成键电子主要由Cr3s和3p价电子贡献，而其Fermi能级处的态密度主要由Ni3d和Cr3d电子贡献。Ni-Cr合金层中Ni、Cr、Fe原子间的电荷交互作用使Fe原子呈现正电性，促使Fe原子电位上升，导致Fe原子较难发生电化学腐蚀反应。因此，Ni-Cr合金层能够为基体提供有效的腐蚀防护作用。
设计了一种新型的双辉等离子表面冶金装置以满足工业化的需求，这种新型的等离子表面处理装置能够对大面积碳钢钢板进行处理，从而获得等离子表面冶金Ni-Cr耐蚀钢板。静态浸泡腐蚀试验和中性盐雾腐蚀试验的结果均表明，等离子表面冶金Ni-Cr耐蚀钢板的耐蚀性能要明显优于基材Q235低碳钢，其耐蚀性能接近于316L不锈钢。
Carbon steel was widely used in many fields such as building, traffic, mechanism and energy,because of its well plasticity and toughness, easy processing and low cost. However, the carbon steelhas a common problem, low corrosion resistance. Scholars developed corrosion-resistant steel andweathering steel to improve the corrosion resistance of steel, but the corrosion-resistant alloyingelements increased the cost and can not be used effectively. The steel plat is very important for thesteel materials. Therefore, the formation of stainless steel on carbon steel plate has been the dream ofworld metallurgical industry. In this paper, to form a new type of plasma surface metallurgycorrosion-resistant carbon steel plate, double glow plasma surface metallurgy technique was used toprepare the nickel-base alloyed layer on carbon steel. This new surface metallurgy material, whichexhibits good plasticity, toughness and excellent corrosion resistance, can economize costly alloyingelements and reduce the cost of materials. Meanwhile, a series of basic scientific issues related to thescale application of surface metallurgy steel plate were studied systematically.
In order to solve the problem of insufficient allowance of alloying elements in scale production,grid-like hollow cathode source structure was introduced. Using Ni80Cr20alloyed target as sourcematerial, Ni-Cr alloyed layer was formed on Q235steel. The alloyed layer combined excellently withsubstrate and had gradient distribution of composition. The main phase of alloyed layer was austeniticsteel Ni2.9Cr0.7Fe0.36and a little of awaruite Ni3Fe. Compared with planar source structure, thegrid-like hollow cathode source structure could provide more adequate allowance of alloyingelements, so its Ni-Cr alloyed layer had thicker thickness and higher content of Ni, Cr alloyingelements which result in more excellent corrosion resistance.
In the paper, the effect of process parameters on microstructure and properties of Ni-Cr alloyedlayer were studied systematically. The results showed that the thickness of Ni-Cr alloyed layer and thecontent of Ni and Cr alloying elements increased as the treatment temperature increased. As a result,the corrosion-resistant of Ni-Cr alloyed layer was improved, and the best corrosion resistance wasobtained when the treatment temperature reached about1000℃. With the increasing of workingpressure, the thickness of Ni-Cr alloyed layer and the content of Ni and Cr alloying elements inalloyed layer showed trend of first increased and then decreased. Meanwhile, the corrosion resistanceof alloyed layer also increased firstly and reduced afterwards, and the best corrosion resistance wasobtained when the working pressure was about51Pa. Increasing the electrode spacing, the thicknessof Ni-Cr alloyed layer, the content of Ni and Cr alloying elements and the corrosion resistance of alloyed layer exhibited the same results. The optimal electrode spacing was about15mm. Prolongingthe holding time could obtain thicker Ni-Cr alloyed layer, and improve the corrosion resistance ofalloyed layer. But the improvement was not significant anymore after heat for3h.
The influence of the carbon content of the substrate on the microstructure and properties of thealloyed layer was investigated. Ni-Cr alloyed layers were obtained on surface of Q235steel,45steeland T8steel. The thickness of diffusion layer of Ni-Cr alloyed layer increased as the carbon contentincreased. The Ni-Cr alloyed layer on Q235exhibited compact fibrous structure, while the alloyedlayer on45steel and T8steel showed porous tapered column structure which showed coarseningphenomenon as the carbon content increased. The fibrous structure is dense, while the tapered columnstructure contains voids. Therefore, the Ni-Cr alloyed layer on Q235steel had the bestcorrosion-resistant. For the tapered column structure Ni-Cr alloyed layer, the corrosion-resistant ofalloyed layer on T8steel was better than the alloyed layer on45steel due to its thicker thickness ofdiffusion layer.
The composition of Ni-Cr alloyed target has direct effect on the composition and phase of Ni-Cralloyed layer. When the content of Cr alloying element in alloyed target was20%, the main phase wasNi2.9Cr0.7Fe0.36and a little of Ni3Fe. Then the content increased to40%, the phase of alloyed layerchanged into Cr0.19Fe0.7Ni0.11and a little of Fe-Cr. As the content of Cr alloying element in alloyedtarget increased, the content of Cr0.19Fe0.7Ni0.11decreased and the content of Fe-Cr in alloyed layerincreased. Finally the content reached80%, the main phase of alloyed layer was Fe-Cr and a little ofCr0.19Fe0.7Ni0.11. Under different alloyed targets, the Ni and Cr elements on surface of Ni-Cralloyed layer exist in the form of simple substance Ni, Cr and NiO. The composition segregationeffect of Ni and Cr alloying elements in alloyed layer was investigated, and then the relation formulaof the composition of alloyed target and the composition of Ni-Cr alloyed layer was founded. Thenano-indentation test of Ni-Cr alloyed layer indicated that the plasticity and toughness of alloyedlayer reduced as the content of Cr alloying element in alloyed target increased. As the content of Cralloying element in alloyed target increased, the content of Cr alloying element in Ni-Cr alloyed layerincreased, the continuous dense passive film can be easily formed on surface of alloyed layer whichcould improve the corrosion-resistant of alloyed layer. However, thickness of Ni-Cr alloyed layerunder Ni60Cr40alloyed target was thin, thus its corrosion-resistant was worse than that underNi80Cr20alloyed target.
The atom model Ni9Cr2Fe1of Ni2.9Cr0.7Fe0.36, which was the main phase in Ni-Cr alloyed layer,was built. According to the energy minimum principle, equilibrium geometric structure ofNi2.9Cr0.7Fe0.36was obtained. The bonding electron of Ni9Cr2Fe1was contributed by the3s and3pvalence electron of Cr, while the density of states at the Fermi level was contributed by the3d electron of Ni and Cr. The charge interaction of Ni, Cr and Fe atoms in Ni-Cr alloyed layer made theFe atom exhibit positively charged and increased the potential of Fe atom which inreased thedifficulty of the electrochemical corrosion reaction of Fe atom. Therefore, the Ni-Cr alloyed layercould provide effective corrosion resistance for the substrate.
In order to meet the needs of industrialization, a new type of double glow plasma surfacemetallurgy device was designed. The large area of carbon steel plate could be processed in theequipment to obtain plasma surface metallurgy Ni-Cr corrosion-resistant steel plate. The results ofstatic immersion corrosion test and salt spray corrosion test demonstrated that the corrosion-resistantof plasma surface metallurgy Ni-Cr corrosion-resistant steel plate was better than that of Q235lowcarbon steel, and its corrosion-resistant was close to that of316L stainless steel.
引文
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