本文選題：高功率脈沖磁控濺射 + 斜入射沉積�。� 參考：《西南交通大學(xué)》2016年博士論文

【摘要】：采用磁控濺射技術(shù)在復(fù)雜形狀工件表面沉積薄膜過(guò)程中,工件各表面與濺射靶之間存在不同角度,這造成了薄膜的斜入射沉積。在斜入射沉積過(guò)程中,陰影效應(yīng)的產(chǎn)生將導(dǎo)致工件各表面薄膜厚度、結(jié)構(gòu)及性能存在差異。在工件服役過(guò)程中,薄膜性能最薄弱的地方首先發(fā)生失效,最終縮短了工件表面薄膜整體的服役壽命。為了減小復(fù)雜工件各表面薄膜結(jié)構(gòu)和性能的差異,增加工件各表面薄膜性能(包括應(yīng)力、結(jié)構(gòu)、硬度以及耐腐蝕性等)均勻性,通過(guò)控制薄膜沉積工藝來(lái)消除陰影效應(yīng)顯得十分必要。工作氣壓和基體偏壓是薄膜沉積工藝中兩個(gè)關(guān)鍵參數(shù),在調(diào)控薄膜成分、結(jié)構(gòu)及性能方面發(fā)揮著非常重要的作用。工作氣壓能用于改變?yōu)R射粒子的平均自由程和散射幾率；基體偏壓可用于改變基片附近電場(chǎng)的強(qiáng)弱并影響金屬或氣體離子的能量大小,進(jìn)而改變?yōu)R射粒子飛行路徑及到達(dá)基片時(shí)的入射方向。本論文針對(duì)復(fù)雜工件表面鍍膜改性問(wèn)題,在研究基片曲率法測(cè)試薄膜殘余應(yīng)力基礎(chǔ)上,分別采用直流磁控濺射技術(shù)(DCMS)和高功率脈沖磁控濺射技術(shù)(HPPMS)在與濺射靶成不同傾斜角度的硅和不銹鋼基體樣品表面上沉積(斜入射沉積)氮化鈦(TiN)薄膜,研究了工作氣壓和基體偏壓等參數(shù)對(duì)傾斜于濺射靶的表面上沉積薄膜的結(jié)構(gòu)和性能影響。在此基礎(chǔ)上,采用交替變換濺射角度的方法制備一種垂直生長(zhǎng)柱狀晶和傾斜生長(zhǎng)柱狀晶的多層薄膜結(jié)構(gòu)(“類(lèi)之字形”薄膜結(jié)構(gòu))來(lái)調(diào)控TiN薄膜應(yīng)力,研究了多層薄膜中傾斜生長(zhǎng)柱狀晶薄膜層的厚度對(duì)TiN薄膜應(yīng)力、硬度及抗磨損性能影響。最后,為改善復(fù)雜工件表面沉積薄膜的均勻性,在高功率脈沖磁控濺射技術(shù)(HPPMS)制備TiN薄膜過(guò)程中,采用增加HPPMS脈沖寬度的方法來(lái)提高金屬離化率,研究了脈沖寬度對(duì)(與濺射靶成不同角度的)傾斜表面上沉積TiN薄膜的結(jié)構(gòu)、性能及均勻性的影響。本論文獲得以下主要結(jié)論：(1)利用基片曲率法研究了Si(100)基片固定端和基片尺寸對(duì)薄膜應(yīng)力測(cè)量的影響。研究結(jié)果表明,基片固定端在一定程度上約束了基片在應(yīng)力作用下的變形,基片各位置處發(fā)生變形的難易程度不同,從而導(dǎo)致了基片變形不規(guī)則。當(dāng)基片長(zhǎng)寬比等于或大于3：1時(shí),沿基片長(zhǎng)度方向不同位置所測(cè)量的應(yīng)力值基本一致。因此,采用基片曲率法測(cè)量薄膜應(yīng)力時(shí)選用的Si片長(zhǎng)寬比應(yīng)大于等于3：1,且測(cè)量輪廓曲線(xiàn)時(shí)應(yīng)沿基片長(zhǎng)度方向進(jìn)行。(2)采用DCMS在硅基體上斜入射沉積制備TiN薄膜,研究了基體偏壓和工作氣壓對(duì)TiN薄膜結(jié)構(gòu)和性能的影響規(guī)律。研究結(jié)果表明,當(dāng)Si樣品表面傾斜于濺射靶時(shí),陰影效應(yīng)便會(huì)產(chǎn)生,即TiN薄膜結(jié)構(gòu)疏松且柱狀晶傾斜于樣品表面生長(zhǎng)。提高基體偏壓使得傾斜于靶的Si樣品表面上沉積薄膜的致密性和硬度明顯提高,但是,斜入射沉積過(guò)程中的陰影效應(yīng)仍然存在,且無(wú)法從根本上得以消除。提高工作氣壓使薄膜結(jié)構(gòu)變得疏松,陰影效應(yīng)同樣無(wú)法得到消除。(3)采用交替變換濺射角度的方法在硅和不銹鋼基體上制備一種“類(lèi)之字形”薄膜結(jié)構(gòu)來(lái)調(diào)控TiN多層薄膜應(yīng)力,研究了多層薄膜中傾斜生長(zhǎng)柱狀晶薄膜層厚度對(duì)不銹鋼基體上沉積的TiN多層薄膜的應(yīng)力、硬度及抗磨損性能影響。研究結(jié)果表明,“類(lèi)之字形”結(jié)構(gòu)能夠有效地調(diào)控TiN多層薄膜應(yīng)力,通過(guò)控制傾斜生長(zhǎng)柱狀晶薄膜層的厚度能夠提高不銹鋼基體上沉積的TiN薄膜硬度以及抗磨損性能。(4)研究了高功率脈沖磁控濺射技術(shù)(HPPMS)制備TiN薄膜過(guò)程中,工作氣壓和基體偏壓等關(guān)鍵參數(shù)對(duì)陰影效應(yīng)以及Ti、TiN薄膜結(jié)構(gòu)和性能的影響。研究結(jié)果表明,提高工作氣壓,可以使濺射粒子在散射作用下更容易垂直到達(dá)與濺射靶傾斜的Si樣品表面,從而使得Si基體上沉積的Ti薄膜的柱狀晶垂直于樣品表面生長(zhǎng),但其薄膜致密性及硬度明顯下降,這說(shuō)明高工作氣壓的采用也只是減輕了陰影效應(yīng)。提高基體偏壓,金屬離子在強(qiáng)的電場(chǎng)作用下能夠發(fā)生偏轉(zhuǎn)以及在高的能量驅(qū)使下容易產(chǎn)生遷移,使得傾斜Si樣品上沉積的TiN薄膜柱狀晶垂直于樣品表面生長(zhǎng)且薄膜結(jié)構(gòu)變得致密,從根本上消除了斜入射沉積過(guò)程中陰影效應(yīng),同時(shí)增加了離子的轟擊作用,薄膜具有更大的壓應(yīng)力。(5)為了提高復(fù)雜工件表面沉積薄膜的均勻性,高功率脈沖磁控濺射技術(shù)(HPPMS)制備TiN薄膜過(guò)程中,通過(guò)提高HPPMS脈沖寬度的方法來(lái)增加金屬離化率,研究了脈沖寬度對(duì)(與濺射靶成不同角度的)傾斜表面上(Si和不銹鋼基體)沉積的TiN薄膜結(jié)構(gòu)、性能及均勻性影響。研究結(jié)果表明,脈沖寬度的增加有利于提高金屬離化率,同時(shí)提高基體偏壓,更多濺射金屬離子在電場(chǎng)作用(基體偏壓)下能夠垂直到達(dá)與濺射靶傾斜的表面,從而導(dǎo)致與濺射靶傾斜的樣品表面上沉積TiN薄膜的致密性提高,最終,不同表面上沉積TiN薄膜的結(jié)構(gòu)、硬度和耐腐蝕性能均勻性得以改善。
[Abstract]:By using magnetron sputtering technology in the process of complex shape workpiece surface deposition of thin films, there are different angles between the workpiece surface and the sputtering target, which caused the oblique incidence of the deposited film. In oblique incidence deposition process, shadow effect will lead to the workpiece surface film thickness, structure and performance difference. In the course of service the properties of the films, place the weakest first failure, and ultimately shorten the service life of the whole film surface. In order to reduce the fluctuation of the structure and properties of the complex workpiece surface film, increase the performance of the workpiece surface thin film (including stress, structure, hardness and corrosion resistance) uniformity, by controlling the deposition process to eliminate the shadow effect is very necessary. Working pressure and bias are two key parameters of thin film deposition process, the control of the film composition, structure and performance. Play a very important role. Working pressure can be used to change the mean free path of the sputtered particles and scattering probability; substrate bias can be used to change the substrate near the electric field strength and impact energy size of metal or gas ions, and then change the flight path and the sputtered particles. When the incident direction of Scientology for the modification of the complex the workpiece surface coating film on the substrate in the test of residual stress based on curvature method, respectively with DC magnetron sputtering (DCMS) technology and high power pulsed magnetron sputtering (HPPMS) at different angles of silicon and stainless steel sample surface deposition and sputtering target (oblique incidence deposition) of titanium nitride (TiN) the film, study the working pressure and bias parameters on structure and properties of thin films deposited on the surface of inclined sputtering target effect. On this basis, using alternating sputtering angle The invention relates to a method for preparing vertical columnar crystal and Inclined Multilayer Thin Films Growth of columnar crystal ("glyph" film structure) to stress regulation of TiN thin films, multilayer films in inclined columnar crystal film thickness on the stress of TiN thin film, hardness and abrasion resistance to impact finally, for improving the uniformity of complex workpiece surface thin film deposition, in high power pulsed magnetron sputtering (HPPMS) TiN thin film preparation process, by adding HPPMS pulse width to increase the ionization rate, the pulse width of (different angles and sputtering target) inclined structure deposition of TiN thin films on the surface, affecting the performance and uniformity. The main conclusions are as follows: (1) Si was studied by substrate curvature method (100) substrate fixed end and the size of the substrate stress measurement of thin films. The results show that the substrate in a fixed end The degree of constraint on the substrate during deformation under the action of stress, deformation at each position of the substrate in varying degrees of difficulty, resulting in irregular substrate deformation. When the base length width ratio is equal to or greater than 3:1, measured along the length direction of the substrate position of the stress value of a therefore, the substrate curvature method for stress measurement of thin films with Si length width ratio should be greater than or equal to 3:1, and the measurement curve should be carried out along the length direction of the substrate. (2) by DCMS on silicon substrate with oblique incidence deposition of TiN thin films, studied the influence of substrate bias voltage and working pressure on the structure and properties of TiN films. The results show that when the Si sample surface inclined to the sputtering target, shadow effect will occur, i.e. TiN thin film structure loose and columnar crystal tilt to the sample surface growth. Increase of substrate bias makes tilt to the target Si sample surface deposition The density and hardness of the film increased obviously, but the shadow effect of oblique incidence deposition process still exist, and can not be fundamentally eliminated. Improve the working pressure of the film structure becomes loose, the shadow effect also cannot be eliminated. (3) on silicon and stainless steel substrate for the preparation of a "zigzag" the film structure to control the TiN multilayer thin film stress by alternating sputtering angle, the stress of multi-layer films of inclined columnar crystal film thickness deposited on stainless steel substrate and TiN multilayer films, the hardness and abrasion resistance can influence. Research results show that the "zigzag" structure can effectively the regulation of TiN multilayer thin film stress, by controlling the inclined columnar crystal film thickness can improve the hardness of TiN films deposited on stainless steel substrates and anti wear properties. (4) research on the high power pulse magnet The technology of magnetron sputtering (HPPMS) TiN thin film preparation process, the key parameters of working pressure and bias of the shadow effect and Ti effect, structure and properties of TiN thin films. The results show that the increase of working pressure, can make the sputtered particles in the scattering more easily under the action of vertical to the sample surface Si and sputtering target tilt thus, Ti films deposited on Si substrate by columnar crystal growth perpendicular to the sample surface, but the film density and hardness decreased significantly, indicating that the use of high pressure is just to reduce the shadow effect. To improve the substrate bias, the metal ions can deflect and in high energy driven generating shift in under the strong electric field, the tilt of Si samples of TiN films deposited on the columnar crystal growth perpendicular to the sample surface and the film structure becomes more compact, fundamentally eliminate the effects of oblique incidence deposition process of Bardo At the same time, increase the ion bombardment, the film has greater compressive stress. (5) in order to improve the uniformity of thin film deposition complex workpiece surface, high power pulsed magnetron sputtering (HPPMS) TiN thin film preparation process, to increase the ionization rate by increasing the pulse width of the HPPMS. Study on pulse width (different angles and sputtering target) on inclined surfaces (Si and stainless steel) TiN thin film deposition, influence of performance and uniformity. The results show that the increase of the pulse width is beneficial to improve the ionization rate, while increasing the substrate bias, more sputtering of metal ions in the electric field (under the vertical bias) can reach the surface tilt and sputtering target, which leads to the compactness of the tilt and the sputtering target samples deposited on the surface of TiN films increased, eventually, TiN films were deposited on different surface structure, hardness and corrosion resistance The energy uniformity can be improved.

【學(xué)位授予單位】：西南交通大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2016
【分類(lèi)號(hào)】：TQ134.11;TB383.2

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