鋁合金表面復(fù)合硅烷膜的制備及性能研究
發(fā)布時(shí)間:2018-02-07 13:44
本文關(guān)鍵詞: 硅烷偶聯(lián)劑 復(fù)合硅烷膜 耐蝕性能 鈰鹽改性 雜化硅烷膜 出處:《山東大學(xué)》2017年碩士論文 論文類型:學(xué)位論文
【摘要】:隨著社會(huì)對(duì)環(huán)境保護(hù)的重視,具有高度污染性的鉻酸鹽鈍化處理技術(shù)正逐步退出鋁合金表面處理的舞臺(tái),環(huán)境友好型的硅烷化處理技術(shù)應(yīng)運(yùn)而生,憑借其工藝簡單、能耗低、處理液無毒性、膜層耐蝕性能高等一系列優(yōu)點(diǎn)受到越來越多的關(guān)注。然而由于傳統(tǒng)的硅烷膜功能單一、機(jī)械性能差、膜層不具備"自愈"能力,限制了硅烷化處理的應(yīng)用發(fā)展。本實(shí)驗(yàn)針對(duì)傳統(tǒng)硅烷化處理技術(shù)中存在的缺陷,在鋁合金表面制備了復(fù)合硅烷膜并對(duì)其進(jìn)行了一系列的表征測試;結(jié)合稀土轉(zhuǎn)化膜的特點(diǎn),實(shí)驗(yàn)選用硝酸鈰銨改性復(fù)合硅烷膜,制備了具有一定自修復(fù)能力的雜化硅烷膜。本實(shí)驗(yàn)將兩種性質(zhì)不同的硅烷偶聯(lián)劑KH560和PTMS進(jìn)行復(fù)配,制備復(fù)合硅烷處理液。通過監(jiān)測溶液水解過程中的電導(dǎo)率,采用控制變量法研究了不同因素對(duì)復(fù)合硅烷液水解過程的影響,并確定了處理液的最佳水解體系為甲醇用量15wt%、硅烷偶聯(lián)劑濃度8wt%、水解液pH為6、水解溫度30!。將達(dá)到水解平衡的硅烷液用于鋁合金表面處理工藝中,通過對(duì)硅烷濃度、固化溫度、成膜時(shí)間等條件進(jìn)行優(yōu)化,在鋁合金表面制備一層復(fù)合硅烷膜層。對(duì)膜層進(jìn)行耐蝕性和機(jī)械性能測試,結(jié)果表明:用KH560:PTMS為1:2的處理液在150℃高溫下干燥1.5h后制備的復(fù)合硅烷膜性能最好。紅外光譜測試揭示了復(fù)合膜層的形成機(jī)理,通過與不同膜層試樣進(jìn)行對(duì)比測試,直觀評(píng)價(jià)了復(fù)合硅烷膜的綜合性能,其中,在電化學(xué)測試中復(fù)合硅烷膜的腐蝕電流為1.641×10^-8A/cm2較單一膜層下降了 1個(gè)數(shù)量級(jí)、較氧化膜試樣下降了 2個(gè)數(shù)量級(jí),表明復(fù)合膜層試樣的腐蝕速率最慢;接觸角測試中復(fù)合膜層與水的接觸角為92.5°,較其他試樣具有更高的疏水性;而膜層表面SEM掃描圖則表明復(fù)合硅烷膜層更加平整均勻。實(shí)驗(yàn)選用硝酸鈰銨對(duì)復(fù)合硅烷膜進(jìn)行改性,研究了硝酸鈰銨的摻雜對(duì)成膜工藝帶來的變化。結(jié)果表明:添加了 0.5g硝酸鈰銨的復(fù)合硅烷處理液在180℃下固化1.0h后形成的雜化膜層綜合性能最好。紅外譜圖中沒有出現(xiàn)與鈰相關(guān)的吸收峰,表明在成膜過程中硝酸鈰銨不與硅烷偶聯(lián)劑反應(yīng);雜化膜層的SEM掃描圖中出現(xiàn)顆粒狀物質(zhì),經(jīng)EDS分析知顆粒物中含有Ce;XRD測試結(jié)果中出現(xiàn)鈰的氧化物的吸收峰,表明在雜化膜成膜過程中硝酸鈰銨鈰以其氧化物的形式對(duì)硅烷膜進(jìn)行了填充。將雜化膜層與硅烷膜層進(jìn)行一系列的對(duì)比測試,直觀的體現(xiàn)了硝酸鈰銨的加入對(duì)膜層的各方面性能的提高,而鹽霧試驗(yàn)則證明了雜化膜層所具有的自修復(fù)能力。
[Abstract]:With the attention of society to environmental protection, chromate passivation technology with high pollution is gradually withdrawing from the stage of aluminum alloy surface treatment. The environmentally friendly silane treatment technology emerges as the times require, with its simple process and low energy consumption. A series of advantages, such as non-toxicity of the treatment solution and high corrosion resistance of the film, have attracted more and more attention. However, due to the single function and poor mechanical properties of the traditional silane film, the film does not have the ability of "self-healing". In view of the defects of traditional silane treatment technology, the composite silane film was prepared on the aluminum alloy surface and a series of characterization tests were carried out, which combined with the characteristics of rare earth conversion film. Hybrid silane membranes were prepared by cerium ammonium nitrate modified composite silane membranes. In this experiment, two silane coupling agents, KH560 and PTMS with different properties, were prepared. By monitoring the conductivity of the solution during hydrolysis, the influence of different factors on the hydrolysis process of the composite silane solution was studied by the method of controlling variables. The optimum hydrolysis system was determined as follows: methanol dosage 15 wtt, silane coupling agent concentration 8 wt, hydrolytic solution pH 6, hydrolysis temperature 30.1 鈩,
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