CN102749316A - Method for measuring microscopic residual stress of SiCf/Ti-based composite material interface - Google Patents
Method for measuring microscopic residual stress of SiCf/Ti-based composite material interface Download PDFInfo
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- CN102749316A CN102749316A CN2011101012680A CN201110101268A CN102749316A CN 102749316 A CN102749316 A CN 102749316A CN 2011101012680 A CN2011101012680 A CN 2011101012680A CN 201110101268 A CN201110101268 A CN 201110101268A CN 102749316 A CN102749316 A CN 102749316A
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Abstract
The invention relates to a residual stress measurement technology, and is a method for measuring the microscopic residual stress of a SiCf/Ti-based composite material interface. The method is characterized in that a linear relation of a C atomic Raman absorption peak wave number (v) varied by the stress sigma in an original SiC fiber C coating can be determined at first, the gradient k is calibrated, the residual stress effect and Raman absorption peak wave number change Delta v under the residual stress release state in the SiCf/Ti-based composite material can be respectively measured, and the residual stress of the fiber surface microscopic zone can be calculated according to the wave number change and the calibrated gradient. The method has the advantages that the microscopic zone of the fiber surface can be directly measured, the resolution is high, the test result is more accurate and the processes are easy to carry out.
Description
Technical field
The present invention relates to the residual stress measurement technology, a kind of specifically measurement SiC
fThe method of/Ti based composite material interface microcosmic residual stress.
Background technology
SiC
f/ Ti based composites is compared the conventional Ti alloy and is had advantages such as higher specific strength, specific modulus and better thermal stability; Become an important development direction of novel high-performance space structure material, can be widely used in following Aeronautics and Astronautics field with the high temperature of its preparation, high-strength, lightweight component.Yet, at SiC
f/ Ti based composites prepares in the process; Because can causing cooling off the back composite inner, the difference of SiC fiber and titanium alloy substrate thermal expansivity produces unrelieved stress; And along fiber axis to unrelieved stress can produce very big influence to the tensile property and the fatigue behaviour of compound substance; Therefore, accurately measuring the composite inner unrelieved stress reliably is on active service significant to the comprehensive mechanical property and the structural member thereof that improve compound substance at high temperature for a long time.
Multiple measurement SiC is arranged at present
fThe method of/Ti based composites unrelieved stress, as: X-ray diffraction method, neutron diffraction method, chemical corrosion method etc.Wherein X-ray diffraction method and neutron diffraction method are residual stress measuring method commonly used; These two kinds of methods all are that certain the crystal face interplanar distance d ' through measuring matrix or fiber contrasts the deflection that obtains this crystal face with interplanar distance d under the unstress state, calculate the residual-stress value of this face with known crystal face elastic modulus.X ray penetration capacity limited (≤7 μ m) can only be measured the stress (strain) in the material surface matrix, and the neutron ray penetration capacity is compared by force with the X ray penetration capacity, can measure the stress of matrix and fiber simultaneously, but cost is higher.Chemical corrosion method is to erode the part matrix material with corrosive liquid to make fiber expose out; The unrelieved stress of fiber obtains discharging like this; Measure the length that uncovered fibres exceeds original compound substance end, can obtain the overstrain of fiber, further calculate the size of the suffered unrelieved stress of fiber; Because this method utilizes microscopical focusing distance to measure length, so experimental error is bigger.In addition, the fiber unrelieved stress that this method records is the average residual-stress value of a section fibre.In theory; Also there are some models that the unrelieved stress of compound substance is predicted; Wherein the concentric cylinder model is acknowledged as the most approaching actual model; But this model is not considered the elastic modulus of matrix material and the factor that expansion coefficient changes with variation of temperature, therefore with true stress big gap is arranged also, as just experiment test result's auxiliary reference.
How accurately to measure the stress distribution at fiber and basal body interface place, for optimizing and the interface of design compound substance has crucial meaning with the influence of alleviating interface residual stress.
Summary of the invention
Above-mentionedly can only measure the whole unrelieved stress statistical value of fiber or matrix in order to overcome, weak point such as test result randomness and error are bigger the purpose of this invention is to provide a kind of SiC of meeting
f/ Ti based composite material structure characteristics can deep enoughly be measured near the interface microcosmos area of SiC fiber, a kind of measurement SiC with degree of precision and resolution
fThe method of/Ti based composite material interface microcosmic residual stress.
To achieve these goals, the present invention adopts following technical scheme:
A kind of measurement SiC
fThe method of/Ti based composites fiber surface unrelieved stress, carry out as follows:
1) at the original SiC fiber axis to applying tensile stress sigma, the laser beam vertical irradiation of laser Raman spectrometer on the fiber surface C coating, is obtained corresponding Raman absorption peak wave number v; Change tension, measure same fiber C atom Raman absorption peak wave number under different tensile stress states; Draw the relation curve of v and σ, calibrate slope k behind the linear fit;
2) with SiC
fThe fiber surface C coating polishing at/Ti based composites sample middle part is exposed to being about to, and carries out electropolishing again until there being a small amount of C coating to expose; Then with the laser beam vertical irradiation of laser Raman spectrometer on the C coating microcell that has exposed, obtain corresponding Raman absorption peak wave number, be designated as v
1
3) utilize corrosive liquid with SiC
fThe matrix of the tabular sample of/Ti based composites end is removed, and makes the fiber surface C coating of end exposed fully, then with the laser beam vertical irradiation of laser Raman spectrometer on exposed C coating, obtain corresponding Raman absorption peak wave number, be designated as v
2
4) calculate the unrelieved stress of fiber surface interface microcosmos area according to following formula:
Δv＝v
1-v
2，σ
r＝Δv/k
Wherein Δ v is a step 2), 3) the Raman absorption peak wave number that obtains changes σ
rBe unrelieved stress.
The original SiC fiber axis is 0-4000Mpa to the scope that applies tension in the step 1);
Step 2) and 3) in adopt clear water, alcohol wash successively, oven dry at last before the laser beam irradiation of Raman spectrometer.
Corrosive liquid in the step 3) is a Ti alloy corrosion liquid.
Be used to produce SiC
fThe SiC fiber surface of/Ti based composites has the thick C coating of 1-5 μ m, adopts said method can obtain measurement result preferably;
C atom Raman absorption peak selects to characterize the G peak of graphite-structure vibration mode;
SiC
fThe matrix material of/Ti based composites is: TC4, Ti55, TC17, Ti
2Different types of titanium alloy such as AlNb, TiAl;
SiC
fThe shape of/Ti based composites can be for tabular or bar-shaped.
Preferred laser Raman spectrometer is micro-confocal laser Raman spectrometer among the present invention, spatial resolution≤1 μ m, copolymerization depth of focus degree analysis resolution≤2 μ m.
Step 2) SiC in
fThe a small amount of C layer of/Ti based composites sample middle part through exposing behind mechanical grinding and the electropolishing; Because bare area is small; Still receive the matrix constraint of near zone; Very about-face can't take place in suffered unrelieved stress, thus can think this C layer with imbed the unrelieved stress basically identical that the C layer in the matrix receives; And SiC
f/ Ti based composites sample end utilizes corrosive liquid to remove the C layer that exposes fully behind the matrix, no longer receives the constraint of matrix, sees step 3), can think that it is in the unrelieved stress release conditions.
The principle of the invention is: because material with carbon element generally has Raman active, graphite-like structure is 1000～1800cm in wave number
-1Two Raman absorption peak: 1330cm are arranged in the scope
-1Neighbouring D peak and 1580cm
-1Near G peak.Wherein the form at D peak and position be mainly by carbon atom aryl cyclisation degree decision, this key be present in more surface and graphite unilateral between, to fiber axis to suffered stress and insensitive.And G peak position (wave number) and the suffered stress of graphite-like structure have linear relationship, i.e. σ=v/k, and Raman peaks moves to the lower wave number direction when receiving tension, and Raman peaks then moves to high wave number direction during compression chord.Owing to be used to produce SiC
fThe SiC fiber surface of/Ti based composites all has the thick C coating of 1-5 μ m, and the graphite-like structure lamella in the C coating can reflect SiC fiber axial stress along the machine direction orientation so characterize the wave number at the G peak of graphite-structure vibration mode.Therefore, the G spike number that the present invention chooses C atom in the C coating that receives under unrelieved stress effect and the unrelieved stress release conditions changes, as the foundation of measuring fiber surface microcosmos area unrelieved stress.
The present invention has following advantage:
1. the inventive method adopts micro-confocal laser Raman spectrometer; It has laser beam spot diameter little (≤1 μ m); The characteristics that measuring resolution is high adopt the microcosmos area that method of the present invention can deep enough measurement SiC fiber surface, and test result is more accurate; Solve existing method and can only measure fiber or the whole unrelieved stress statistical value of matrix, the problem that test result randomness and error are bigger;
2. adopt method of the present invention to SiC
f/ Ti based composites has universality, for example, is applicable to the compound substance of dissimilar Ti alloy substrates: TC4, Ti55, TC17, Ti
2AlNb, TiAl etc. are applicable to different shape compound substances: tabular, bar-shaped etc.;
Description of drawings
Fig. 1 for demarcate among the present invention original SiC fiber Raman absorption peak wave number (v)-the experimental provision synoptic diagram of stress (σ) linear relationship;
Fig. 2 for original SiC fiber Raman absorption peak wave number among the present invention (v)-stress (σ) linear relationship calibration result;
Fig. 3 is SiC among the present invention
fSiC in the/Ti based composite material interface microcosmic residual stress measuring process
fThe view of/Ti based composites;
Fig. 4 is SiC among the present invention
f/ Ti based composites sample middle part and end C layer Raman spectrum (the G spike is counted comparison diagram);
Wherein, symbolic representation among the figure: 1 is counterweight; 2 is removable anchor clamps; 3 is dynamometer; 4 are-Raman spectrometer; 5 is laser beam; 6 is testing sample; 7 is laser beam; 8 for receiving the C layer (middle part) of unrelieved stress effect; 9 is the Ti alloy substrate; 10 is the C layer (end) of unrelieved stress release conditions;
Embodiment
Below in conjunction with accompanying drawing to further explain of the present invention.
Fig. 1 for demarcate among the present invention original SiC fiber Raman absorption peak wave number (v)-the experimental provision synoptic diagram of stress (σ) linear relationship, as shown in Figure 1, be positioned at two coaxial removable anchor clamps on the guide rail; Wherein anchor clamps link to each other with weight tray, are used to produce tension, and another anchor clamps are connected with dynamometer; Measure stress value; During use, tested fiber two ends are respectively charged into coaxial mobile anchor clamps, and the laser beam of Raman spectrometer is aimed at tested fiber; Through changing the suffered stress of Different Weight counterweight adjustment SiC fiber, original SiC fiber surface C atom Raman absorption peak wave number v under the test different stress.
The Raman spectrometer that is adopted is micro-confocal laser Raman spectrometer, spatial resolution≤1 μ m, copolymerization depth of focus degree analysis resolution≤2 μ m.
Fig. 3 is SiC among the present invention
fSiC in the/Ti based composite material interface microcosmic residual stress measuring process
fThe view of/Ti based composites, as shown in Figure 3, with the laser beam of Raman spectrometer successively vertical irradiation at SiC
fOn the C coating microcosmos area that/Ti based composites tabular sample middle part and end have exposed, test corresponding C atom Raman absorption peak wave number respectively, v
1And v
2
The present invention measures SiC
fThe method of/Ti based composite material interface microcosmic residual stress, carry out as follows:
1) original SiC fiber (being utilized the W core SiC fiber of CVD method production by Metal Inst., Chinese Academy of Sciences) two ends is respectively charged between the coaxial removable anchor clamps, on weight tray, increases and decreases counterweight, pulling force is provided according to different stress numerical.Treat add pulling force stable after with the laser beam irradiation of Raman spectrometer on the SiC fiber, left standstill 3-5 minute, measure C atom Raman absorption peak G spike number.Be respectively 0,324,847,1229,1441 through changing the suffered stress of Different Weight counterweight adjustment SiC fiber, 1680MPa, measure C atom Raman absorption peak G spike number, each stress value is measured and is averaged for three times.The corresponding relation of the Raman absorption peak wave number v of each stress value σ and its measurement is as shown in Figure 2, utilizes DAS Origin8.0 that the raman data point that records is carried out linear fit, can obtain slope value k.
Wherein, the Raman spectrometer model is French JY-RH800 type, and optical maser wavelength is 488nm, power 1.5mW, integral time 180s, spatial resolution 1 μ m, copolymerization depth of focus degree analysis resolution 2 μ m.
2) utilize the pre-grinding machine with SiC
f/ Ti based composites, present embodiment adopts SiC
f/ Ti-22Al-26Nb compound substance (adopting the preparation of magnetron sputtering precursor wire method) by Metal Inst., Chinese Academy of Sciences, SiC fiber surface C coating thickness is 2 μ m, shape adopts tabular sample; The fiber surface C coating polishing of center is exposed to being about to; Again it is carried out electropolishing until there being a small amount of C coating to expose, utilize clear water, alcohol wash, oven dry; With the laser beam vertical irradiation of Raman spectrometer on the C coating microcosmos area that has exposed, test corresponding C atom Raman absorption peak wave number v
1
3) with SiC
f40%HF solution is immersed in the tabular sample of/Ti-22Al-26Nb compound substance end; Immersion depth 5mm, treat that matrix Ti-22Al-26Nb removes fully after, the C coating of SiC fiber surface is exposed fully; Utilize clear water, alcohol wash; Oven dry, with the laser beam vertical irradiation of Raman spectrometer on exposed C coating, test corresponding C atom Raman absorption peak wave number v
2
4) according to above-mentioned steps 2), 3) the Raman absorption peak position that obtains is illustrated in figure 4 as SiC among the present invention
f/ Ti based composites sample middle part and end C layer Raman spectrum (the G spike is counted comparison diagram) calculate in the middle part of institute's test sample article and the C atom Raman absorption peak wave number changes delta v=v of end
1-v
2=1.02cm
-1, by formula σ
r=Δ
v/ k calculates the unrelieved stress σ that SiC fiber surface C coating receives
rFor-573MPa, on behalf of the fiber surface C layer, negative sign receive compressive stress.
Be with embodiment 1 difference:
Step 1) is changed the Different Weight counterweight, and the suffered stress of adjustment original SiC fiber is respectively 0,642,1248,1872,2496,2996MPa;
Step 2) and 3) in adopt SiC
fThe bar-shaped sample of/Ti-22A1-26Nb compound substance (adopting the preparation of magnetron sputtering precursor wire method) by Metal Inst., Chinese Academy of Sciences; Sample exposes in 200 hours vacuum heat of 900 ℃ of warps to be handled; Its residual stress state changes, sample interior SiC fiber surface C coating thickness 2.5 μ m.The preparation of LR laser raman specimen is identical with embodiment 1 with the unrelieved stress test process;
4) according to above-mentioned steps 2), 3) the Raman absorption peak position that obtains, calculate in the middle part of institute's test sample article and the C atom Raman absorption peak wave number changes delta v=v of end
1-v
2=0.55cm
-1, by formula σ
r=Δ v/k calculates the unrelieved stress σ that SiC fiber surface C coating receives
rFor-295MPa, vacuum heat significantly reduces when exposing the back unrelieved stress than the hot pressing attitude.
Adopt the result of the method measurement of embodiment 1 and 2 to verify to residual-stress value through concentric cylinder Model Calculation shaft, identical basically.
Claims (9)
1. measure SiC for one kind
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that, as follows:
1) at the original SiC fiber axis to applying tensile stress sigma, the laser beam vertical irradiation of laser Raman spectrometer on the fiber surface C coating, is obtained corresponding Raman absorption peak wave number v; Change tension, measure same fiber C atom Raman absorption peak wave number under different tensile stress states; Draw the relation curve of v and σ, calibrate slope k behind the linear fit;
2) with SiC
fThe fiber surface C coating polishing at/Ti based composites sample middle part is exposed to being about to, and carries out electropolishing again until there being a small amount of C coating to expose; Then with the laser beam vertical irradiation of laser Raman spectrometer on the C coating microcell that has exposed, obtain corresponding Raman absorption peak wave number, be designated as v
1
3) utilize corrosive liquid with SiC
fThe matrix of the tabular sample of/Ti based composites end is removed, and makes the fiber surface C coating of end exposed fully, then with the laser beam irradiation of laser Raman spectrometer on exposed C coating, obtain corresponding Raman absorption peak wave number, be designated as v
2
4) calculate the unrelieved stress of fiber surface interface microcosmos area according to following formula:
Δv＝v
1-v
2，σ
r＝Δv/k
Wherein Δ v is a step 2), 3) the Raman absorption peak wave number that obtains changes σ
rBe unrelieved stress.
2. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: the original SiC fiber axis is 0-4000Mpa to the scope that applies tension in the step 1).
3. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: be used to produce SiC
fThe SiC fiber surface of/Ti based composites has the thick C coating of 1-5 μ m.
4. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: the corrosive liquid in the step 3) is a Ti alloy corrosion liquid.
5. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: said C atom Raman absorption peak wave number is the G peak that characterizes the graphite-structure vibration mode in the Raman absorption peak.
6. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: step 2) and 3) in adopt clear water, alcohol wash successively, oven dry at last before the laser beam irradiation of Raman spectrometer.
7. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: SiC
fThe matrix material of/Ti based composites is: TC4, Ti55, TC17, Ti
2AlNb, TiAl.
8. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: SiC
fBeing shaped as of/Ti based composites is tabular or bar-shaped.
9. according to the said measurement of claim 1 SiC
fThe method of/Ti based composite material interface microcosmic residual stress is characterized in that: described laser Raman spectrometer is micro-confocal laser Raman spectrometer, spatial resolution≤1 μ m, copolymerization depth of focus degree analysis resolution≤2 μ m.
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Cited By (6)
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| CN105973703A (en) * | 2016-05-06 | 2016-09-28 | 金思宇 | Apparatus and method for detecting interfacial shear strength of composite material based on laser Raman spectrometer |
| WO2017120988A1 (en) * | 2016-01-15 | 2017-07-20 | 清华大学深圳研究生院 | Method of inspecting aging state of composite insulating material |
| CN107748026A (en) * | 2017-09-06 | 2018-03-02 | 北京航空航天大学 | A kind of synchronous across yardstick residual stress detection method |
| CN111164242A (en) * | 2017-09-22 | 2020-05-15 | 株式会社德山 | Group III nitride single crystal substrate |
| CN111678785A (en) * | 2020-05-26 | 2020-09-18 | 上海航天精密机械研究所 | Laser scanning test system suitable for plate preloading |
| CN113984463A (en) * | 2021-10-09 | 2022-01-28 | 中国航发北京航空材料研究院 | Method for calculating residual stress of continuous SiC fiber reinforced titanium-based composite material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017120988A1 (en) * | 2016-01-15 | 2017-07-20 | 清华大学深圳研究生院 | Method of inspecting aging state of composite insulating material |
| US10209197B2 (en) | 2016-01-15 | 2019-02-19 | Graduate School At Shenzhen, Tsinghua University | Method for inspecting aging state of silicone rubber composite insulating material |
| CN105973703A (en) * | 2016-05-06 | 2016-09-28 | 金思宇 | Apparatus and method for detecting interfacial shear strength of composite material based on laser Raman spectrometer |
| CN105973703B (en) * | 2016-05-06 | 2019-07-16 | 金思宇 | Composite material interface shear strength detection device and method based on laser Raman spectrometer |
| CN107748026A (en) * | 2017-09-06 | 2018-03-02 | 北京航空航天大学 | A kind of synchronous across yardstick residual stress detection method |
| CN111164242A (en) * | 2017-09-22 | 2020-05-15 | 株式会社德山 | Group III nitride single crystal substrate |
| CN111678785A (en) * | 2020-05-26 | 2020-09-18 | 上海航天精密机械研究所 | Laser scanning test system suitable for plate preloading |
| CN111678785B (en) * | 2020-05-26 | 2023-03-17 | 上海航天精密机械研究所 | Laser scanning test system suitable for plate preloading |
| CN113984463A (en) * | 2021-10-09 | 2022-01-28 | 中国航发北京航空材料研究院 | Method for calculating residual stress of continuous SiC fiber reinforced titanium-based composite material |
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Application publication date: 20121024 |