發(fā)布時間：2018-04-26 15:38

  本文選題：自分層 + 脆弱��； 參考：《中國科學(xué)技術(shù)大學(xué)》2017年博士論文

【摘要】：絲織品文物是中華文明史中濃墨重彩的一筆,其種類繁多、工藝精美,是古代中國勞動人民智慧的集中展現(xiàn),具有極高的歷史、科研、藝術(shù)價值。但出土絲織品文物經(jīng)過長時間的埋藏,大多數(shù)腐蝕殆盡、不見蹤跡,極少數(shù)保留下來的也多半糟朽不堪、觸之即粉。絲織品文物的出土狀況通常呈現(xiàn)出兩個共性:嚴(yán)重糟朽、層間黏結(jié)。由于出土紡織品文物在埋藏過程中多數(shù)是折疊放置的,歷經(jīng)千百的埋藏之后,層與層之間發(fā)生黏結(jié),折痕處斷裂或極易斷裂。為使埋藏地下的瑰寶重?zé)ü獠?揭展無疑是紡織品文物保護、修復(fù)工作的首要工作。因此,利用現(xiàn)有的科學(xué)技術(shù)改善出土紡織品黏結(jié)、糟朽的現(xiàn)狀就是揭展工作要解決的最主要問題。目前,針對絲織品文物揭展劑和揭展技術(shù)的研究主要是利用物理、化學(xué)、生物的手段,通過降低絲織品層間黏結(jié)的作用力,完成出土絲織品的揭展工作。揭展劑的化學(xué)成分多數(shù)為表面活性劑、柔軟劑、滲透劑等生化助劑,可有效的降低絲織品層間黏結(jié)強度。然而脆弱出土絲織品文物即使成功降低層間黏結(jié)力,因絲織品自身強度太差,揭展工作仍會對絲織品文物有一定的損毀。絲織品文物滿足揭展的關(guān)鍵在于:絲織品本體強度足夠克服絲織品層間黏結(jié)的強度。也就是說,解決揭展難題的途徑可以概括為兩種:增加絲織品本體強度、降低層間黏結(jié)強度。一般而言,降低絲織品層間黏結(jié)力和提升絲織品力學(xué)強度是難以調(diào)和的悖論,也是制約揭展技術(shù)發(fā)展的主要矛盾。若使用加固劑以提升絲織品強度,則會使其滲透至絲織品層間,從而增加黏結(jié)強度。若僅降低層間黏結(jié),而忽略加強絲織品的強度,則無法滿足揭展的需要。針對這一難題,本研究利用自分層技術(shù)對絲織品文物進行揭展,在降低絲織品層間黏結(jié)強度的同時,增強蠶絲纖維的力學(xué)強度。本研究選取多種文物保護常用材料,利用表面能理論對自分層材料混合液成膜后的分層情況進行理論預(yù)判。選擇使用聚醋酸乙烯酯、硬脂酸鈉作為自分層材料,再通過掃描電子顯微鏡對樣品進行觀察,驗證分層效果,確認(rèn)硬脂酸鈉、聚醋酸乙烯酯混合乳液符合自分層揭展前提條件。在此基礎(chǔ)之上,將自分層揭展技術(shù)運用于模擬脆弱黏結(jié)絲織品的揭展中。通過剝離強度、抗拉強度表征揭展效果,對揭展劑濃度配比、作用時間設(shè)計正交試驗。最終確認(rèn)最優(yōu)方案為硬脂酸鈉濃度0.5%,聚醋酸乙烯酯濃度0.5%,作用時間為4h,揭展效果較好。使用聚焦離子束(FIB)加工技術(shù)對揭展劑膜進行刻蝕,獲取了揭展劑膜不同深度的梯度空間樣品,實現(xiàn)對樣品做不同深度的立體分析。加工后樣品分別用于原子力顯微鏡(AFM)分析、X射線光電子能譜(XPS)分析。掃描電子顯微鏡對揭展劑膜進行觀察,發(fā)現(xiàn)薄膜縱向出現(xiàn)明顯分層現(xiàn)象。通過比較上下表面、不同深度的揭展劑膜原子力相圖發(fā)現(xiàn):揭展劑膜上表面主要成分為硬脂酸鈉,隨著膜深度加深硬脂酸鈉含量逐漸減少、聚醋酸乙烯酯含量逐漸增多,呈明顯的梯度變化。利用對不同深度位置的X射線光電子能譜分析結(jié)果顯示,揭展劑膜上表面、中間不同深度位置、下表面Na相對含量依次為5.05%、3. 03%、0.37%、0.42%,變化趨勢明顯。根據(jù)激光共聚焦拉曼定量分析聚醋酸乙烯酯在揭展劑膜的不同位置相對含量結(jié)果依次是:18. 7%、22%、、61.7%、69. 2%,濃度存在梯度變化。因此,原子力顯微鏡、X射線光電子能譜、激光共聚焦拉曼的分析結(jié)果共同驗證了自分層揭展劑組分的分層情況。將自分層揭展技術(shù)應(yīng)用于模擬樣品、荊州謝家橋一號漢墓、荊州夏家臺楚墓、南陵鐵拐宋墓出土絲織品殘片的揭展工作。利用超景深光學(xué)顯微鏡對各樣品揭展效果進行觀察,對比發(fā)現(xiàn),樣品在揭展前后無明顯變化。使用掃描電子顯微鏡觀察絲織品揭展前后微觀形貌,則發(fā)現(xiàn)蠶絲表面形成了薄的包裹層。色差分析結(jié)果表明,模擬樣品、謝家橋樣品、南陵樣品、夏家臺樣品的色差平均值依次是0. 82、0.56、0.96、0.70,符合文物保護的色差變化范圍。對各個樣品進行硬挺度測試發(fā)現(xiàn),模擬樣品、古代樣品揭展后的懸垂硬挺度、抗彎剛度均較揭展前有大幅下降,說明黏附在蠶絲表面的黏結(jié)物、污染物在揭展過程中被部分清洗。揭展劑的使用在一定程度上也增加了蠶絲的柔軟度。模擬樣品、古代樣品熱重分析結(jié)果表明,使用揭展劑后,絲織品的熱穩(wěn)定性和熱分解速率受揭展劑成分影響發(fā)生了部分改變。對比模擬樣品、古代樣品動態(tài)熱機械分析結(jié)果后發(fā)現(xiàn),揭展后絲織品抗拉強度有明顯升高,斷裂伸長率變化不明顯。揭展屬于整個絲織品文物保護工作中前序階段,揭展劑必需具備良好的可再處理性才能符合現(xiàn)階段文物保護的需要。因此,本研究采用等溫滴定量熱技術(shù)、熱重分析、示差掃描量熱分析對自分層揭展技術(shù)的可再處理性進行了評估,實驗結(jié)果表明,其清除效果良好,進一步驗證了自分層揭展技術(shù)的實際可操作性。通過對模擬樣品、古代絲織品文物殘片的揭展,綜合考量揭展劑分層效果、揭展效果、揭展劑去除效果等因素。本研究將自分層揭展技術(shù)應(yīng)用于湖北荊州謝家橋一號漢墓、安徽南陵鐵拐宋墓、江西南昌�；韬顫h墓出土的不同時期、不同糟朽狀況的珍貴絲織品文物(計20件)進行了揭展、揭取,均取得了較好的成果。絲織品文物的自分層揭展技術(shù),改變了以往揭展技術(shù)以降低層間黏結(jié)強度為研究目的的單一途徑。形成了以增加絲織品力學(xué)強度、降低絲織品黏結(jié)強度兩者共同作用為目的的新研究視角,為絲織品文物揭展提供了新的思路和方法。自分層揭展技術(shù)的研究,也為其他類型文物的保護研究提供了一定的借鑒。
[Abstract]:Silk cultural relics are rich and heavy in the history of Chinese civilization, with a wide variety and exquisite craftsmanship. It is a concentrated display of the wisdom of the ancient Chinese working people. It has a high history, scientific research and artistic value. The unearthed condition of a silk cultural relic usually presents two commonalities: serious decay and interlayer bonding. Because most of the unearthed textile relics are folded in the course of burial, after hundreds of burial, the layers and layers are bonded, the creases are broken or very easily broken. No doubt, uncovering is the most important work for the protection of textile relics and repair work. Therefore, using the existing science and technology to improve the bonding of unearthed textiles is the most important problem to be solved. At present, the research of uncovering agents and uncovering techniques for silk fabrics is mainly the use of physical, chemical and biological hands. Section, by reducing the bonding force between the silk fabric, the soil silk fabric is uncovered. Most of the chemical components of the uncovering agent are surface active agents, softeners, and osmosis agents, which can effectively reduce the bond strength between the silk fabrics. As the body strength is too poor, the uncovering work will still have a certain damage to the silk cultural relics. The key of the silk cultural relics to meet the uncovering is that the strength of the silk is strong enough to overcome the bond strength between the silk fabrics. That is to say, the way to solve the problem can be summarized as two kinds: increasing the strength of the silk fabric and reducing the bond strength between the layers. It is an incompatible paradox to reduce the bonding force between the silk fabrics and enhance the mechanical strength of silk fabrics. It is also a major contradiction that restricts the development of uncovered technology. If the strength of silk is enhanced by the use of reinforcing agents, it will penetrate into the silk fabric and increase the bonding strength. If only the interlayer bonding is reduced, the strength of the silk fabric will be neglected. In order to solve this problem, this study uses self stratification technology to uncover the silk fabric and enhance the mechanical strength of silk fiber while reducing the bond strength between the silk fabrics. This study selects a variety of cultural relics to protect the common materials, and uses the theory of surface energy to form the self layered material after the film is formed. Polyvinyl acetate and sodium stearate are selected as self stratified materials, and then the samples are observed by scanning electron microscope to verify the stratification effect, and the sodium stearate is confirmed and the polyvinyl acetate emulsion conforms to the self delamination precondition. Based on this, the self delamination technology will be transported. It is used to simulate the uncovering of fragile bonded silk fabrics. Through the stripping strength, tensile strength characterizing the uncovering effect, the orthogonal test is designed for the concentration ratio of the uncovering agent and the action time. Finally, the optimum scheme is that the optimal solution is 0.5% of sodium stearate, 0.5% of the concentration of polyvinyl acetate, the effect time is 4h, and the effect of uncovering is better. Focusing ion beam (FIB) is used. The technology was used to etch the film of the uncovering agent, obtain the gradient space sample with different depth of the film and realize the stereoscopic analysis of the different depth of the sample. The samples were used for atomic force microscope (AFM) analysis, X ray photoelectron spectroscopy (XPS) analysis. By comparing the upper and lower surfaces, the atomic force phase diagram of the uncovering agent membrane in different depths shows that the main component of the surface of the film is sodium stearate, and the content of sodium stearate gradually decreases with the depth of the membrane, and the content of polyvinyl acetate increases gradually. The X ray light of different depth positions is used. The results of electronic energy spectrum analysis show that the relative content of Na in the upper surface of the film is 5.05%, 3.03%, 0.37%, 0.42%, and the change trend is obvious. According to the laser confocal Raman Raman quantitative analysis, the relative content of polyvinyl acetate in the film of the uncovering agent is 18.7%, 22%, 61.7%, 69.2%, and strong. There is a gradient change. Therefore, atomic force microscopy, X ray photoelectron spectroscopy and laser confocal Raman analysis jointly verify the stratification of the self stratified uncovering agent components. The self stratified uncovering technology is applied to the simulated samples, the tomb of the No. 1 Han tomb in Shijia bridge in Jingzhou, the chusantai tomb in Jingzhou, and the remnants of the native silk fabrics in the tombs of the iron Guixiang of Nanling. It is found that the sample has no obvious change before and after uncovering. Using scanning electron microscope to observe the micromorphology before and after the uncovering of silk fabrics, it is found that the silk surface forms a thin layer of wrapping. The color difference analysis results show that the sample, Shijia bridge, is the sample. The average color difference of the Nanling sample is 0. 82,0.56,0.96,0.70, which is in line with the color difference range of cultural relic protection. The use of the dye was partially cleaned during the uncovering process. The use of the uncovering agent also increased the silkworm softness to a certain extent. The results of the analogue samples. The results of the thermogravimetric analysis of the ancient samples showed that the thermal stability and the thermal decomposition rate of the silk fabrics were partly influenced by the composition of the uncovering agent after using the uncovering agent. The results of the thermal mechanical analysis showed that the tensile strength of the silk fabric increased obviously and the elongation at break was not obvious. The uncovering was the preorder stage of the whole silk cultural relic protection work, and the uncovering agent must have good reprocessing ability to meet the needs of the present protection of cultural relics. Therefore, the isothermal titration was used in this study. The reprocessing property of the self delamination technology is evaluated by thermogravimetry, thermogravimetric analysis and differential scanning calorimetry. The results of the experiment show that the removal efficiency is good and the practical operability of the self delamination technology is verified. In this study, the self delamination technology was applied to the Han Tombs No. 1 in Jingzhou, Hubei, the tomb of the Nanling iron guikuo in Anhui, and the different periods of the unearthed Tomb of the Han tomb in the Nanchang sea of Nanchang, Jiangxi, and the precious silk cultural relics (20 pieces) with different rotten conditions were uncovered and taken out. The self delamination technology of silk fabric has changed the single way to reduce the interlayer bonding strength in the past. A new research perspective has been formed to increase the mechanical strength of silk fabrics and reduce the bonding strength of silk fabrics, which provides a new way of thinking and method for the uncovering of silk fabrics. The research of layer unfolding technology also provides some reference for the protection research of other types of cultural relics.

【學(xué)位授予單位】：中國科學(xué)技術(shù)大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：TS146;K876.9

【參考文獻】

相關(guān)期刊論文 前10條

1 程增會;林永超;劉美紅;劉玉鵬;王春鵬;;D3級耐水聚醋酸乙烯酯乳液膠粘劑的合成[J];中國膠粘劑;2015年03期

2 陳昌富;陳彪;;文物保護與修復(fù)[J];廣西民族大學(xué)學(xué)報(自然科學(xué)版);2014年03期

3 陳淑英;張然;柳敏;;青銅文物緩蝕劑效率及封護劑抗腐蝕能力的比較研究[J];文物保護與考古科學(xué);2013年04期

4 馬文哲;桑勝波;胡杰;張文棟;李朋偉;李剛;;聚二甲基硅氧烷薄膜的襯底硅烷化及測試分析[J];現(xiàn)代化工;2013年09期

5 高秀云;任小翠;鄒祥龍;蘭云軍;;含氟丙烯酸酯共聚物表面性能研究[J];皮革與化工;2013年02期

6 郝曉劍;張斌珍;楊潞霞;范新磊;姚_稱，

本文編號：1806628