CN1115551C - 一种氧化膜临界开裂应力的测量方法及装置 - Google Patents
一种氧化膜临界开裂应力的测量方法及装置 Download PDFInfo
- Publication number
- CN1115551C CN1115551C CN 97100974 CN97100974A CN1115551C CN 1115551 C CN1115551 C CN 1115551C CN 97100974 CN97100974 CN 97100974 CN 97100974 A CN97100974 A CN 97100974A CN 1115551 C CN1115551 C CN 1115551C
- Authority
- CN
- China
- Prior art keywords
- oxide film
- stress
- acoustic emission
- critical cracking
- oxidation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000005336 cracking Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000003647 oxidation Effects 0.000 claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 17
- 238000005452 bending Methods 0.000 claims abstract description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 238000005259 measurement Methods 0.000 claims description 10
- 230000015556 catabolic process Effects 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003708 ampul Substances 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 238000000691 measurement method Methods 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract 1
- 230000035882 stress Effects 0.000 description 32
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Landscapes
- Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
一种氧化膜临界开裂应力的测量技术,其特征在于:在采用单面氧化弯曲方法测量氧化膜应力的同时,用声发射技术对氧化膜玻裂进行监测,监测到的第一个声发射信号即表征氧化膜的初始破裂,所对应的同一时刻的氧化膜应力即为氧化膜临界开裂应力。本发明可以准确直接地给出氧化膜的临界开裂应力。
Description
本发明涉及测量技术,特别提供了一种金属材料在高温腐蚀环境下氧化膜临界开裂应力的测量方法。
在高温腐蚀环境中,合金的抗腐蚀性能依赖于表面致密粘附的氧化膜,由于氧化膜内存在应力,常常导致膜发生开裂和剥落,一旦氧化膜发生开裂和剥落,膜的保护作用就会丧失,为研究氧化膜的破裂机理并进一步预测氧化膜的保护寿命,氧化膜的临界开裂应力成为一个重要的参量,在理论分析上,已给出了该参量的多种表达公式,但到目前为止尚无直接的测量方法。
本发明的目的在于提供一种氧化膜临界开裂应力的测量方法及其装置,其可以准确直接地给出氧化膜的临界开裂应力。
本发明提供了一种氧化膜临界开裂应力的测量方法,其特征在于:在采用单面氧化弯曲方法测量氧化膜内应力的同时,用声发射技术对氧化膜破裂进行监测,监测到的第一个声发射信号即表征氧化膜的初始破裂,所对应的同一时刻的氧化膜内应力即为氧化膜临界开裂应力。
本发明所提供的方法首次实现了氧化膜的临界开裂应力的动态测量,测量方法是基于氧化膜应力的单面氧化弯曲测量方法和声发射技术的结合,单面氧化弯曲法是金属高温腐蚀领域进行氧化膜应力测量最常用的方法,它可以动态的连续测量氧化膜生长应力和热应力,而声发射技术是一种应用于原位监测氧化膜破裂的最有效手段,将两种技术结合起来即可进行氧化膜临界开裂应力的原位测量。这项技术在航空、航天、电力、石化、煤化等领域的高温合金的研制或应用上有积极意义。
基于将氧化膜应力测量的单面氧化弯曲方法和声发射技术结合起来的技术,本发明实现了氧化膜临界开裂应力的高温原位动态测量,技术的关键是既用作声发射波导又用作固定氧化膜应力测量试样的高温合金或陶瓷材料夹具的设计。据此,本发明提供了一种专用于上述的氧化膜临界开裂应力测量方法的测量装置,由石英管3,电阻炉4,热电偶5,读数显微镜6,石英标丝8组成,其特征在于:试样7与一波导杆2固定,波导杆2另一端伸出电阻炉4外并在其端面上固定有声发射换能器1,波导杆材料为在高温下不发生相变及氧化的高温合金、陶瓷或石英,其直径在0.1~20mm之间,长度以伸出炉4体外端面温度降至室温为宜。
本发明具体实现方式如下:
(1)单面氧化弯曲方法测量氧化膜应力时,试样制备成薄条状,一个侧面镀SiO2或Pt作保护膜使该侧面完全不发生氧化,试样氧化时,仅一个侧面发生氧化,由于膜内应力导致试样弯曲,利用读数显微镜测量试样的弯曲度,即可计算氧化膜应力,计算公式为:σ=EH2D/[3(1-μ)ξL2],式中,σ为氧化膜内应力,ξ为氧化膜厚度,E、μ、L、H分别为试样的杨氏模量、泊桑比、长度、厚度,D为试样弯曲挠度。
(2)声发射技术是用于监测氧化膜破裂的,声发射技术在高温下应用时,试样和换能器之间采用波导连接,以便将试样上发生的声发射信号传输至室温工作的换能器,波导特殊设计,即要固定试样,又要传输信号,还要在高温下不发生相变及氧化,即试样氧化期间波导杆不发生声发射信号。
(3)采用长的高温合金或陶瓷棒,一端可用螺钉和垫片固定试样,另一端伸出高温炉管外,并将声发射换能器固定在端面上,这样在测量氧化膜应力时,同时可监测氧化膜的破裂,由于声发射有极高的监测灵敏度,认为监测到的第一个声发射信号表征氧化膜的初始破裂,对应同一时刻的氧化膜应力即为氧化膜临界开裂应力。计算中所需氧化膜厚度的参量,可通过合金在相同氧化条件下的动力学获得,即由ζ=ΔWMOX/yAOρOX来计算,式中,ΔW为那一时刻单位面积氧化增重,MOX为氧化物的分子量,y为一个氧化物分子中所含氧原子个数,AO为氧原子量,ρOX为氧化物密度。
附图1为氧化膜临界开裂应力测量装置结构示意图;
附图2为一种波导管示意图。
实施例1
测量装置如图1所示,1-声发射换能器,2-波导杆,3-石英管,4-电阻炉,5-热电偶,6-读数显微镜,7-试样,8-石英标丝。
试样制备:(40-60)×(5-10)×(0.2-0.45)mm,单面利用四极离子溅射0.1-0.5μm厚的Pt膜或利用射频溅射0.06-0.5μm厚的SiO2膜。
试验操作:试样固定在声发射波导杆上,用铂丝将一细石英丝绑在试样一侧面上或直接悬挂到试样低部的小孔上,然后置入高温炉中,固定法兰,系统抽真空,真空度为10-5乇时,开始升温,到达设定温度时,充入氧化气体,同时利用读数显微镜观察石英丝,记录试样偏转;利用声发射监测氧化膜的破裂,到发现氧化膜破裂时,即可计算得到氧化膜破裂的临界应力,计算公式为:Δσ=EH2D/[3(1-μ)ξL2],式中,σ为氧化膜内应力,ξ为氧化膜厚度,E、μ、L、H分别为试样的杨氏模量、泊桑比、长度、厚度,D为试样弯曲挠度。
波导杆制备:高温合金(316L不锈钢)Φ15×600mm,底端部分热扩散渗铝以使其不发生严重氧化,螺钉用IN738合金制成,使用温度在850℃以下。
在500℃、550℃、600℃1atmO2中,测量Ta氧化膜临界开裂应力分别为23.3、38.5、18.4×106 kgf/m2,在450℃、475℃、500℃,1atmO2中,测量Nb氧化膜临界开裂应力分别为10.1、5.2、6.0×106kgf/m2。
实施例2
波导杆制备:耐热合金杆(316L不锈钢)Φ15×400mm,陶瓷杆Φ15×200mm;合金和陶瓷间采用热扩散方法焊接如图2示,使用温度1100℃以内。其他条件同实施例1,对Nb,Ta氧化膜临界开裂应力进行测量得到与实例1相同的结果。
Claims (2)
1.一种氧化膜临界开裂应力的测量方法,其特征在于:在采用单面氧化弯曲方法测量氧化膜内应力的同时,用声发射技术对氧化膜破裂进行监测,监测到的第一个声发射信号即表征氧化膜的初始破裂,所对应的同一时刻的氧化膜内应力即为氧化膜临界开裂应力。
2.一种权利要求1所述氧化膜临界开裂应力测量方法的测量装置,由石英管(3),电阻炉(4),热电偶(5),读数显微镜(6),石英标丝(8)组成,其特征在于:试样(7)与一波导杆(2)固定,波导杆(2)另一端伸出电阻炉(4)外并在其端面上固定有声发射换能器(1),波导杆材料为在高温下不发生相变及氧化的高温合金、陶瓷或石英。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 97100974 CN1115551C (zh) | 1997-03-17 | 1997-03-17 | 一种氧化膜临界开裂应力的测量方法及装置 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 97100974 CN1115551C (zh) | 1997-03-17 | 1997-03-17 | 一种氧化膜临界开裂应力的测量方法及装置 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1193735A CN1193735A (zh) | 1998-09-23 |
CN1115551C true CN1115551C (zh) | 2003-07-23 |
Family
ID=5165445
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN 97100974 Expired - Fee Related CN1115551C (zh) | 1997-03-17 | 1997-03-17 | 一种氧化膜临界开裂应力的测量方法及装置 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN1115551C (zh) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101122561B (zh) * | 2007-08-02 | 2010-06-30 | 上海交通大学 | 膜基结合性能的背面穿透式的测量方法 |
-
1997
- 1997-03-17 CN CN 97100974 patent/CN1115551C/zh not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
CN1193735A (zh) | 1998-09-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Merker et al. | High temperature mechanical properties of the platinum group metals | |
Sung Oh et al. | Subcritical Crack Growth along Ceramic‐Metal Interfaces | |
Saunders et al. | Oxidation growth stresses in an alumina-forming ferritic steel measured by creep deflection | |
JPS58184103A (ja) | 光フアイバ用被膜 | |
Yun et al. | Time/temperature dependent tensile strength of SiC and Al2O3-based fibers | |
CA1098337A (en) | Pyrometric sheath and process | |
Jönsson et al. | High temperature properties of a new powder metallurgical FeCrAl alloy | |
Renusch et al. | Measuring and modeling the TBC damage kinetics by using acoustic emission analysis | |
CN1115551C (zh) | 一种氧化膜临界开裂应力的测量方法及装置 | |
Kim et al. | Oxidation behavior and flexural strength of aluminum nitride exposed to air at elevated temperatures | |
da Cunha et al. | High temperature sensing technology for applications up to 1000 C | |
Da Cunha | High-temperature harsh-environment saw sensor technology | |
JPH1194787A (ja) | 測定装置 | |
Smith et al. | Development of electrically insulating coatings on vanadium alloys for lithium-cooled blankets | |
Zhao et al. | Fabrication and microstructure evolution of Al2O3/ZrBN-SiCN/Al2O3 high-temperature oxidation-resistant composite coating | |
EP3351924A1 (en) | Sensor for monitoring corrosion by means of measurements of electrochemical impedance and noise and of resistance to polarisation and use of same | |
Godefroy et al. | Thin‐film temperature sensors deposited by radio frequency cathodic sputtering | |
Pint et al. | Long-term stability of ceramics in liquid lithium | |
Warren et al. | Fiber damage during the consolidation of PVD Ti 6Al 4V coated nextel 610TM alumina fibers | |
CN114965553A (zh) | 一种基于平板弯曲曲率的高温涂层热膨胀系数的计算方法 | |
Rugg et al. | Interfacial behavior of microcomposites during creep at elevated temperatures | |
Mullendore et al. | Mechanical properties of chemical vapor deposited coatings for fusion reactor application | |
Gregory et al. | A low TCR nanocomposite strain gage for high temperature aerospace applications | |
Prakash et al. | Development of thin film temperature sensors for high performance turbo-jet engines | |
Natesan et al. | Electrically insulating coatings for V-Li self-cooled blanket in a fusion system |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C19 | Lapse of patent right due to non-payment of the annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |