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    公司主營:沖擊試驗臺高低溫沖擊試驗箱氙燈老化試驗箱步入式環境試驗箱

    金屬材料的氧化試驗



    概述

    金屬材料的高溫抗氧化性能是材料的一項重要性能指標。對于某些在高溫條件下使用的材料,如爐料、爐輥、電爐加熱元件、內燃機汽缸活塞、燃氣輪機葉片和葉輪等,除了要求具有合適的高溫力學性能外,還要求具有一定的高溫抗氧化性能。廣‘義地講,金屬在高溫下和環境介質中的氧、硫、鹵素、水蒸氣、二氧化碳等發生反應并被氧化的過程都可以叫作高溫氧化。測定氧化過程的恒溫動力學曲線(Aml曲線)是研究氧化過程動力學的最基本的方法。它不僅可以提供許多關于氧化機理的資料,如氧化過程的速度限制性環節、膜的保護性、反應的速度常數及過程的激活能等,而且還可作為工程設計的依據。氧化動力學曲線大體可分為直線、拋物線、立方、對數及反對數五種類型。

    為研究高溫氧化動力學和氧化機理、評定合金抗氧化性能或發展新型抗氧化合金,通常采用質量法、容量法、壓力計法和電阻法等氧化試驗方法。

    It

    fit法是最簡單、最直接的測定氧化速度的方法。為進行氧化試驗所需要的設備包括:一臺準確的天平,一臺可控制溫度的加熱爐以及氣體控制裝置。氣體控制裝置的作用在于控制氣相成分、氣相流速和氣相分壓。根據試驗體系的不同,可分別采用質量損失法或質量增加法。如果試驗過程中產生大量氧化物并且很容易剝落,應采用質量損失法;如果氧化過程相當緩慢,氧化產物不多,且難以從金屬表面除去,應采用質最增加法。

    為了獲得試樣質量隨時間變化的曲線,可使用間斷稱量法或連續稱量法。所謂間斷稱最法,是將稱量以后的試樣放人高溫區(通常是在馬弗爐中進行)氧化,保持一定時間后取出冷卻、稱量;然后再放入爐內氧化,冷卻,再稱量。如此循環可測得不同時刻的試樣質址變化。也可將若干試樣同時置于同一高溫條件下氧化,分別在不同的時間間隔取出、冷卻、稱量。這樣,通過適當數量的試驗數據就可以得到一條試樣質量隨時間變化的氧化曲線。

    間斷稱傲法只能用一個試樣得到一個數據,或者經過一次加熱一冷卻循環得到一個數據,而且操作繁復、耗用試樣多;冷卻過程中氧化膜開裂對下一次循環過程有很大影響。而連續稱量的氧化試驗法可以克服.I二述缺點。所謂連續稱量是用專門設計的可連續稱量或連續指示質址變化的裝置,在整個試驗過程中連續不斷地記錄試樣質址隨時間的變化的方法。常用裝置有電子熱天平、石英彈簧天平、鑰絲彈簧天平和真空鎢絲扭力微天平等。圖418所示為一臺高溫氧化試驗熱天平,它可在一臺可控制氣氛的爐子中不必取出試樣進行連續稱址。此裝置精度較高,可同時試驗6個試樣。為了研究氧化過程,使用了石英或鑰絲彈簧天平,掛在彈簧.上的試樣氧化后使彈簧伸長,根據彈簧的伸長量就可得出相應的質量變化。例如用直徑0.2mm的鑰絲制成直徑10mm、總共200圈的翎絲彈簧天平,稱量載荷可達4g,測量精度為士0.0001g。為了研究氧化薄膜生長動力學,還發展出靈敏度更高的真空微天平。為一種真空鎢絲扭力微天平的示意圖。由熔融的透明石英棒加工成的天平骨架上,焊著一根直徑為0.025nun的退火鎢絲,作為天平橫梁的石英棒就架在鎢絲上,這樣構成的全石英天平安置在全玻璃真空系統中。天平一端懸掛試樣,另一端配以與試樣同樣質量的祛碼。試驗時先抽真空到133 x 1.06Pa,用純氫還原金屬表面的初始氧化膜,然后在恒定溫度下進行氧化試驗。也可以充以其他氣體進行氣體腐蝕試驗,試驗壓力可從很低的低壓直到101325 Pao用微米尺和顯微鏡觀察天平梁的位置變化。為避免干擾,天平不應暴露在電場、磁或熱場之中:,因此,加熱線圈應是無感應的。

    容量法

    容量法是一種高溫氧化試驗方法,它是在恒定壓力下測量因氧化而被消耗掉的氧的體積,圖4-20是一種簡化的用容量法研究高溫氧化的裝置。石英管(2)的一端連接磨口石英蓋(3),安裝在石英蓋上的細石英管(4)用作試樣支架,且從一端裝人熱電偶(5)0量氣管(9)用于測量氧化過程中吸收的氣體體積的。調整漏斗(11)的高度可使量氣管中的液面重新達到它的初始水平。量氣管中的液體應該具有很低的蒸氣壓,并和試驗氣體不起作用。若試驗氣體溶于這種液體,則應在氣體人口(6)事先用試驗氣體使液體飽和。填有玻璃棉的管(7)置于管(9)和管(2)之間。安放試樣(8)的全部空間在試驗前必須充滿試驗氣體,升高漏斗盡址提高量氣管中的液面,兒乎充滿上端的球泡,以逐出量氣管中所有的空氣。然后連續通以試驗氣體,把量氣管中的液面降到零點位置。調節變壓器(12)使加熱爐(1)的溫度升到所需溫度。

    關掉活閥(14)(13),.由標尺(10)讀取hi氣管的讀數。這種方法試驗裝置比較簡單,但在組裝和操作時須特別小心,尤其是在研究薄膜生長時。大多數容覺法試驗是在!333293324Pa的純氧中進行。容量法的靈敏度比重量法大得多,這種方法在相當低的壓力下是特別靈敏的,甚至一點點氧化也會導致壓力顯著變化。采用這種方法,可由一個試樣獲得完整的氧化一時間曲線。主要的誤差來源是溫度變化,系統溫度變化'cc,26664Pa壓力下將引起約0.01 numl氧的誤差。對于生成揮發性產物的休系,不宜采用這種方法。總之,如果很仔細地使用容量法,結果還是相當可靠的。當溫度控制在10.25℃時,容量法和質魷損失法的結果只相差土2%0

    壓力計法

    壓力計法是在恒定體積下測量氧化過程中反應室內的壓力下降。試驗裝置基本上由一個加熱反應管、一個壓力計和一個供氣系統組成。此方法由于簡單而用得比較普遍。圖421為簡化的壓力計法試驗裝置。試樣置于反應管中,反應管通過三通活塞分別與壓力計和大氣相通。在壓力計上可讀出氧化試驗時所消耗的氧。旋轉三通活塞可以補充消耗掉的空氣。如果需要得到氣體消耗的絕對值,還需測定裝置的容積。

    果需要得到氣體消耗的絕對值,還需測定裝置的容彩壓力計法最適合用于單一組分氣體的氧化試驗,如果反應氣體為空氣或其他棍合氣體,就會出現一些問題。各種不同的氣體對金屬腐蝕破壞的速度是不一樣的,例如對于空氣來說,氧的消耗往往比氮快得多,空氣中所含的水分由于反應也改變它的濃度。即使時時補充新鮮空氣,試驗管中仍會出現氮的富集。為了減小這種作用,裝置的容積與反應消耗的氣體體積之比應當很大,可這又會降低這種方法的靈敏度。

    即使使用單組分試驗氣體,由于反應室和壓力計處于不同溫度之下,或者由于試驗壓力很低(如小于133Pa),為準確測量壓力仍需對這些因素進行校正。反應區的溫度必須嚴格保持恒定,任何溫度變化都會顯著改變反應管中的壓力。金屬試樣的表面必須完全潔凈,因為任何表面站污物的揮發都會影響試驗結果。凡試驗過程中會發生二次氣體反應的體系都不能應用此法。如鋼一氧體系,800℃以上鋼將會發生脫碳,有Co氣體產生。如果試樣中可能有溶解氣體存在,則應事先進行處理除氣。如果考慮了上:述這些限制和預防措施,莊力計法與質量法相比還是有許多優點的,例如可以連續讀數,裝置簡單和很靈敏等。圖421的裝置還可作各種改進,如在低于1333 Pa壓力下試驗II寸,應將壓力計置于恒溫浴中,以減少溫度波動的影響等。

    電阻法

    (l.:某些情況卜,也可川金屬絲的電阻變化來測量由于氧化引起的金屬橫截面積的減小。只有在電阻的增加完全是由于橫截面積的減少引起的情況下,這種方法才是有效的。因此,要求材料的電阻在高in氧化狀態下不會由于熱處理而變化,以區別氧化對橫截面積的影響。

    此外,要求合金的組分不會產生選擇性氧化,以免由于合金組分比例發生改變引起電阻變化的影響。

    電阻法研究高溫氧化的裝置。試樣是一個螺旋金屬絲,作為反應器的石英管放在加熱爐中。金屬絲的兩端通過磨I1石英蓋.L的兩個小孔引出,而用耐溫枯接劑密封之,、分別通過1幾下兩個活塞引人和排出氣體。試驗時可關掉活寨(恒定體積),或在緩慢氣流中進行。因為試樣的電阻不僅受氧化的影響,而且受電阻率溫度系數的影響,試驗應當按下列方式進行:在室溫下先測定未氧化試樣的電阻,然后把試樣加熱到規定的溫度氧化,保持一定時間后冷卻到室i品,再一次測址試樣的電阻。接著再升高溫度繼續下一個階段的堿化,冷卻到室溫再測量電阻,如此循環直至試驗結束。取單位時間內相對氧化前初始電阻的變化就可測定氧化速度,根據各個實驗點作出氧化一時間曲線。

    水蒸氣氛化試驗

    奧氏體不銹鋼因過熱水蒸氣引起的氧化,主要是針對火力發電川鍋爐過熱器和原子能發電用材料在使用時所出現的問題而提出的。隨著鍋爐的發展.火力發電鍋爐用的過熱器管或再熱器管上使用的不銹鋼所承受的蒸汽溫度,最高可達5711:,、金屬的溫度還要比之高305090。不銹鋼管被高溫水蒸氣氧化,內壁生成具有雙層結構的氧化皮。氧化皮生長到某個厚度,其外層發生剝離。剝離的氧化皮堆積在管道的U形部位,成為啟動時過熱噴泄事故的原因。

    通常水蒸氣氧化試驗用的不銹鋼為10mm x 30mm x 2mm的長條形試樣,經10000/15min退火,以調整其晶粒度,然后酸洗供試驗使用。實驗室水蒸氣氧化試驗裝置。試驗爐為"1 l Omm x 1000mm的鎳鉻絲爐。為了使溫度均勻性好,在爐內插人#90nim x 450mm的鋼管作為試驗室。管內吊以試樣.兩端密封使其保持在所定溫度。管中間250mm的范圍內,可調節溫度使其保持在以X)℃土5cC0水槽‘卜的水通以純氛氣脫氧,可使水中溶解氧降低到0.1 AUL以下。脫氣后的水保存在妙,:水梢中,從管道流人燒瓶進行加熱,加熱沸騰后的水蒸氣經過預熱室流入試驗室,最后在冷凝器中被冷卻凝結。

    通常試驗是在600650℃范圍內進行,試驗時間為5002000h。試驗后的試樣在NaOHKMr1O4溶液中去除氧化皮后,測定其質量損失。此外,也可用金相顯微鏡觀察試樣斷而。用電子探針分析氧化皮的成分。氧化皮的剝離試驗可用圖424所示的裝置來進行。豎插在電爐中的不銹鋼管試樣,因加熱,冷卻的溫度變化而剝落下來的氧化皮,可在下面的玻璃容器中觀察到。其他,如水蒸氣發生部分的裝w,為了使實驗室試驗所選定的鋼材實用化,可將其制成實物大小的鋼管試樣,將其插到實際鍋爐的部分區域中進行現場試驗,以評價材料的使用可能性。

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