本文關(guān)鍵詞： 電沉積 X射線衍射 Ni-Zr C 織構(gòu) 內(nèi)應(yīng)力 組織結(jié)構(gòu)　出處：《上海交通大學(xué)》2015年博士論文　論文類型：學(xué)位論文

【摘要】：電沉積鎳基復(fù)合鍍層的織構(gòu)、內(nèi)應(yīng)力及組織結(jié)構(gòu),決定了鍍層的性能表現(xiàn)。復(fù)合鍍層中第二相顆粒的存在,使得復(fù)合鍍層的織構(gòu)、內(nèi)應(yīng)力及組織結(jié)構(gòu)不同于純金屬鍍層。本文通過(guò)復(fù)合電沉積技術(shù),制備了微米Zr C(mZr C)和納米Zr C(nZr C)顆粒復(fù)合鎳基鍍層,研究了電沉積參數(shù)、鍍液中Zr C顆粒濃度及顆粒尺寸對(duì)Ni-Zr C復(fù)合鍍層的織構(gòu)、內(nèi)應(yīng)力及組織結(jié)構(gòu)的影響。利用X射線衍射(XRD)分析技術(shù),對(duì)Ni-Zr C復(fù)合鍍層的織構(gòu)、內(nèi)應(yīng)力及組織結(jié)構(gòu)的影響因素、調(diào)整方法、形成及變化機(jī)制等進(jìn)行了研究分析。利用相對(duì)織構(gòu)系數(shù)、Rietveld全譜擬合極圖以及XRD實(shí)測(cè)極圖,研究了鎳基復(fù)合鍍層中的織構(gòu)隨電沉積參數(shù)、鍍液中顆粒濃度及顆粒尺寸的變化,三種分析方法所得結(jié)果一致。隨著電流密度的升高,Ni-Zr C復(fù)合鍍層逐漸呈現(xiàn)出[200]絲織構(gòu),而隨著顆粒濃度的升高,鍍層的[200]絲織構(gòu)逐漸消失。在相同的電流密度及顆粒濃度時(shí),Ni-nZr C鍍層的[200]絲織構(gòu)強(qiáng)度低于Ni-mZrC鍍層。研究了鎳基鍍層的織構(gòu)在電沉積過(guò)程中的變化,發(fā)現(xiàn)在電沉積Ni以及Ni-Zr C鍍層的初期,鍍層均呈現(xiàn)出[111]初始織構(gòu),隨著電沉積過(guò)程的進(jìn)行,Ni鍍層逐漸呈現(xiàn)出[200]強(qiáng)織構(gòu),而Ni-Zr C復(fù)合鍍層的晶體擇優(yōu)取向則逐漸消失。Ni-Zr C鍍層織構(gòu)隨著ZrC顆粒濃度的變化可以分為兩個(gè)階段,在第一階段中,鍍層的絲織構(gòu)隨著顆粒濃度的升高而被不斷抑制;而在第二階段,鍍層幾乎不存在擇優(yōu)取向,并不再隨ZrC顆粒濃度而變化。本文結(jié)合Voigt均應(yīng)力和Reuss均應(yīng)變模型,通過(guò)修正Hill加權(quán)平均模型的方法,對(duì)具有絲織構(gòu)鍍層的X射線應(yīng)力測(cè)試方程進(jìn)行修正。利用優(yōu)化的X射線應(yīng)力分析方法,研究了Ni-Zr C復(fù)合鍍層中的內(nèi)應(yīng)力隨電流密度、顆粒濃度及尺寸的變化,發(fā)現(xiàn)Ni-ZrC鍍層內(nèi)應(yīng)力隨電流密度變化不大,而隨著鍍液中顆粒濃度的升高而降低。在相同的電流密度及顆粒濃度時(shí),Ni-mZr C鍍層的表面拉應(yīng)力高于Ni-nZr C鍍層。發(fā)現(xiàn)Ni及Ni-Zr C鍍層內(nèi)應(yīng)力在電沉積過(guò)程中,隨著鍍層厚度的增加而先降低后升高。研究了電沉積過(guò)程中的超聲波處理、對(duì)基底施加預(yù)加拉應(yīng)力以及后續(xù)熱處理手段調(diào)整鎳基鍍層的內(nèi)應(yīng)力狀態(tài),發(fā)現(xiàn)該三種方法都可以降低鎳基鍍層表面拉應(yīng)力,而利用熱處理的方法可以將鍍層的內(nèi)應(yīng)力狀態(tài)由拉應(yīng)力調(diào)整為壓應(yīng)力,并且壓應(yīng)力的值隨熱處理溫度的升高而升高。利用XRD單峰線形分析以及Rietveld全譜擬合,研究了Ni-Zr C鍍層組織結(jié)構(gòu)隨電沉積參數(shù)及Zr C顆粒濃度及尺寸的變化規(guī)律。鍍層組織結(jié)構(gòu)的變化也可以分為兩個(gè)階段,在第一階段,隨著顆粒濃度的增加,[200]相關(guān)的晶粒尺寸不斷降低,而[111]及[220]相關(guān)的晶粒尺寸則變化不明顯;在第二階段,隨著顆粒濃度的增加,晶體擇優(yōu)取向沒(méi)有較大改變,各方向相關(guān)的晶粒尺寸不斷降低,各(hkl)晶面相關(guān)的顯微畸變不斷升高。結(jié)合織構(gòu)變化規(guī)律,將這兩個(gè)階段分別稱為織構(gòu)調(diào)整階段和晶粒細(xì)化階段。利用退火處理及XRD分析技術(shù),計(jì)算得到了Ni-Zr C鍍層的晶粒長(zhǎng)大激活能,在低溫時(shí)為51.88 KJ/mol,在高溫時(shí)為112.9 KJ/mol。探討了鍍層的力學(xué)性能與電沉積條件的關(guān)系,發(fā)現(xiàn)隨著鍍液中Zr C顆粒濃度的升高或電流密度的降低,Ni-mZr C鍍層硬度不斷增大,最大值達(dá)到475 HV左右,而Ni-nZrC復(fù)合鍍層的顯微硬度則先增大后減小,鍍層硬度最大值約為435 HV。利用原位X射線分析技術(shù),對(duì)Ni-mZrC鍍層的力學(xué)性能進(jìn)行研究,計(jì)算得到了其楊氏模量、泊松比及屈服強(qiáng)度分別為:236 GPa、0.297以及290 MPa。
[Abstract]:The texture of electrodeposited nickel based composite coating, internal stress and organizational structure, determines the performance of the coating. The second phase particles in composite coatings, the texture of the composite coating, internal stress and organizational structure is different from the pure metal coating. The composite electrodeposition technology, micro Zr to prepare C (mZr C Zr C (nZr) and nano C particles) composite nickel coating, on the electrodeposition parameters, plating particle concentration and particle size of Zr C liquid Ni-Zr C composite coating on the texture of the effect of internal stress and organizational structure. By using X ray diffraction (XRD) analysis technology, texture of Ni-Zr C composite coating the influence of stress factors, organizational structure and the adjustment method, the formation and change mechanism were studied. The relative coefficient of texture, Rietveld whole pattern fitting pole figure and XRD measured polar diagram, texture of Ni based composite coating with the electrodeposition parameters of plating The variation of particle concentration and particle size in the solution, the three methods of analysis. The result is consistent with the increase of current density of Ni-Zr C composite coatings gradually showing [200] fiber texture, and with the increase of particle concentration, coating the [200] texture gradually disappear. At the same current density and particle concentration, Ni-nZr C coating the [200] fiber texture strength is less than that of Ni-mZrC coating. The change texture of nickel coating in the electrodeposition process, found in the electrodeposition of Ni and Ni-Zr C were the early [111] coatings show the initial texture, with the deposition of Ni coating, showing a strong [200] texture and Ni-Zr C composite coating the crystal orientation gradually disappeared.Ni-Zr C coating texture change with ZrC particle concentration can be divided into two stages. In the first stage, coating fiber texture with the increase of particle concentration is constant Inhibition; and in the second stage, the coating has almost no preferred orientation, and no longer with the ZrC particle concentration change. The uniform stress and Reuss strain model of Voigt in this paper, the correction method of the Hill weighted average model, the stress test equation is modified with X ray texture coating. Using X ray optimization the method of stress analysis, the stress of Ni-Zr C composite coating with the current density of the variation of particle concentration and size, found little change with the internal stress of coating Ni-ZrC current density, and decreases with increasing particle concentration in the bath. The current density and particle concentration in the same time, the surface of Ni-mZr C coating the tensile stress is higher than that of Ni-nZr. Ni and Ni-Zr found that C coating C coating stress in the electrodeposition process, with the increase of coating thickness and increased after the first reduction. The effects of ultrasonic treatment during the electrodeposition process, the basal fertilizer Gallas and pre stress and subsequent heat treatment of nickel based coating method to adjust the internal stress status, found that the three methods can reduce the nickel coating surface tensile stress, and using the method of heat treatment can be plating internal stress from tensile stress to compressive stress and compressive stress value with the increase of heat treatment temperature increased. Using the XRD linear unimodal analysis and Rietveld whole pattern fitting, studied the change law of Ni-Zr C coating structure with the concentration and size of electrodeposition parameters and Zr C particles. Changes in coating structure can be divided into two stages, in the first stage, with the increase of particle concentration [200], the grain size decreases, while the [111] and [220] related to the grain size did not change significantly; in the second stage, with the increase of particle concentration, the crystal orientation is not changed, the direction of grain size Inch (hkl) decreases, the crystal surface micro distortion related rising. With variation of texture, the two phases are called texture adjustment stage and grain refinement stage. By annealing and XRD analysis, calculated the grain growth activation energy of Ni-Zr C coating, when the low temperature is 51.88 KJ/mol at high temperature is 112.9 KJ/mol., discusses the relationship between the mechanical properties and coating deposition conditions, it was found that with the decrease of Zr increased C in the plating solution of particle concentration and current density, Ni-mZr C hardness increases, the maximum value of 475 HV, and the microhardness of Ni-nZrC composite coating is increased first and then decreased. The maximum hardness of the coating is about 435 HV. by in situ X ray analysis technology to research the mechanical properties of Ni-mZrC coatings, the young's modulus, Poisson's ratio and yield strength were 236 GPa, 0.297 and 2 90 MPa.

【學(xué)位授予單位】：上海交通大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ153

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