CN107290362B - Detection method for forming nanocrystals on surface of 690 high-strength steel - Google Patents
Detection method for forming nanocrystals on surface of 690 high-strength steel Download PDFInfo
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- CN107290362B CN107290362B CN201710455792.5A CN201710455792A CN107290362B CN 107290362 B CN107290362 B CN 107290362B CN 201710455792 A CN201710455792 A CN 201710455792A CN 107290362 B CN107290362 B CN 107290362B
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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Abstract
The invention discloses a method for detecting the formation of nanocrystals on the surface of 690 high-strength steel, which comprises the following steps: carrying out extreme plastic strain on a plurality of 690 high-strength steel samples under the same process and different process parameters; carrying out X-ray diffraction on the sample subjected to the extreme plastic strain to obtain a group of X-ray diffraction patterns; calculating the half-height width of the diffraction peak of the same crystal face under each process parameter; and drawing a curve graph of which the half-height width changes along with the process parameters, finding out a growing inflection point, and verifying that the process parameter of the extreme plastic strain corresponding to the growing inflection point is the minimum process parameter of forming the nano-crystals on the surface of the 690 high-strength steel through a transmission electron microscope and an electron diffraction experiment. According to the method for detecting the nanocrystalline formed on the surface of the 690 high-strength steel, the nanocrystalline formed on the surface of the 690 high-strength steel can be generated by adopting the extreme plastic strain performed by the process parameter exceeding the minimum process parameter for forming the nanocrystalline on the surface of the 690 high-strength steel, the 690 high-strength steel material surface does not need to be damaged for detection, and the method is suitable for the actual production process.
Description
Technical Field
The invention relates to a material detection method, in particular to a detection method for forming nanocrystals on the surface of 690 high-strength steel.
Background
With the growing population and the constant consumption of onshore oil and gas resources, the ocean has become the main field of oil and gas development in the world. The ocean platform is comprehensive ocean engineering equipment integrating oil field exploration, oil gas treatment, power generation, heat supply, crude oil product storage and transportation and personnel living, and is a working base for implementing seabed oil gas exploration and exploitation. The current trend of the world ocean oil and gas development towards deep sea and polar region is that higher requirements are put on the comprehensive performance of the steel for the ocean platform, and the steel for the ocean platform is important in the corrosion resistance of the ocean atmosphere and the seawater besides high strength, high toughness, fatigue resistance, lamellar tearing resistance, good weldability and cold processing performance. Some countries in the united states, japan and europe have since long begun to study steels for offshore oil platforms and developed a number of steel grades suitable for use in deep and polar regions, such as a514 in the ASTM specification, the wetten 80 in the JFE standard and 690 in the DNV specification. China has no specific steel standard for ocean platforms, and certain technical gap exists between the steel for the ultrahigh-strength ocean platforms with yield strength of more than 690 MPa and the steel for the ultrahigh-strength ocean platforms abroad. 690 high-strength steel is important marine steel, is very easy to generate corrosion damage and even corrosion fatigue fracture under the action of ocean tidal range, and can seriously threaten the safety of a marine platform.
690 high strength steel is widely used in the industries of ocean engineering, ships, port machinery and the like because of having excellent performances of high strength, high toughness, fatigue resistance, lamellar tearing resistance and the like, and good welding performance and cold processing performance. In recent years, with the increasing of world energy demand and the reduction of exploitable oil and gas resources, mankind has to explore and develop the highly acidic oil and gas resources which are rich in strong corrosive environments such as CO2, H2S, Cl and the like in the super-huge type marine natural gas field, and the super-huge type marine natural gas field is characterized by complex geological structure, high temperature, high pressure and high corrosivity. Therefore, the demand for 690 high strength steel is increasing at home and abroad.
Failure behaviors (e.g., contact fatigue failure, frictional wear, etc.) occur on the surface of the test specimen due to most engineering materials, and these failure behaviors are highly sensitive to the surface texture and properties of the material. Therefore, the structure and the performance of the surface of the material are optimized, and the overall service life of the engineering material can be effectively prolonged. Nanocrystalline material refers to crystalline material having a grain size on the order of nanometers. Such solids are polycrystalline bodies composed of structural units (predominantly crystals) of at least a few nanometers in size (in one direction). Since the nano-crystalline grains are extremely fine, a large number of atoms are located at the interfaces between the crystalline grains, making the interfaces a non-negligible structural unit. The unique structural characteristic enables the nanocrystalline material to be a new material different from polycrystalline and amorphous materials, so that the material has a plurality of excellent performances in the aspects of mechanics, magnetism, dielectricity, superconductivity, photons and the like. Particularly, when the grains are refined to the nanometer level, many mechanical properties of the material can be obviously changed, such as the strength and the hardness are improved, and the superplasticity phenomenon also occurs in some materials. Therefore, whether the nanocrystals are formed or not becomes one of the important indexes for corrosion prevention of key parts of the marine platform using 690 high-strength steel as a material.
At present, no nano-crystal detection macroscopic detection method for metal materials exists in China, and only the observation of local grain size can be carried out by shooting a sample through a transmission electron microscope, and meanwhile, through electron diffraction, when the diffraction pattern of the nano-crystal detection macroscopic detection method is in a concentric ring form, the nano-crystal can be formed in the observed area of the sample, but the method has the defects of overlong detection period, damage to the surface of the material, high contingency, large error in the measured grain size and the like, so the detection method cannot be applied in actual production, and therefore a new detection method for detecting whether the nano-crystal is formed on the surface of 690 high-strength steel is urgently needed in the actual production process.
Disclosure of Invention
The invention aims to solve the technical problems of long inspection period, damage to the surface of a material, high contingency and large error in the size of a measured crystal grain in the conventional 690 high-strength steel surface nanocrystal detection technology.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the detection method for forming the nanocrystals on the surface of the 690 high-strength steel has the innovation point that the method comprises the following steps:
s1, preparing a plurality of 690 high-strength steel samples;
s2, enabling a plurality of 690 high-strength steel samples to generate extreme plastic strain under the same process and different process parameters;
s3, performing X-ray diffraction on each 690 high-strength steel sample subjected to extreme plastic strain by using an X-ray diffractometer to obtain a group of X-ray diffraction patterns;
s4, analyzing diffraction peaks of the same crystal face in a group of X-ray diffraction patterns, and calculating the full width at half maximum of the diffraction peak of the same crystal face under each process parameter;
s5, establishing a two-dimensional coordinate system of the process parameters and the half width, and drawing a curve graph of the half width of the same crystal face along with the change of the process parameters;
s6, finding out an increasing inflection point in a curve graph of which the full width at half maximum changes along with the process parameters, and verifying that the process parameters of extreme plastic strain corresponding to the increasing inflection point are the minimum process parameters of 690 nanocrystals formed on the surface of the high-strength steel through a transmission electron microscope and an electron diffraction experiment; when the process parameter corresponding to the extreme plastic strain exceeds the minimum process parameter, the surface of the high-strength steel 690 forms nanocrystals.
Wherein, the process for generating the extreme plastic strain is one of a laser shock peening process, an ultrasonic shot blasting process, a surface mechanical grinding process and a surface mechanical rolling process.
The process parameter of the laser shock peening process is power density.
The method for detecting the formation of the nanocrystals on the surface of the 690 high-strength steel further comprises a process of performing surface treatment on the 690 high-strength steel sample subjected to the extreme plastic strain between the step S2 and the step S3.
Preferably, the surface treatment process specifically includes the following steps: a. soaking and cleaning the sample by adopting a pure ethanol or acetone cleaning agent for 3-10 min; b. and carrying out ultrasonic cleaning on the sample after soaking and cleaning, wherein the ultrasonic cleaning time is 1-5min, and ensuring that no residual impurities exist on the surface of the sample.
The transmission electron microscope and electron diffraction experiment comprises the following steps: firstly, respectively shooting transmission electron microscope pictures of a plurality of samples subjected to X-ray diffraction, and detecting the size of local grains; and then, respectively carrying out electron diffraction on a plurality of samples after the electron microscope picture is shot, and when the patterns in the electron diffraction picture are in the shape of concentric rings, the crystal grain orientation is random, and the nano-crystals are uniformly distributed, namely the nano-crystals which are uniformly distributed exist in the observed area.
The technical scheme of the invention has the following beneficial effects: the method for detecting the nanocrystals formed on the surface of the 690 high-strength steel verifies the reliability of the method for forming the nanocrystals on the surface of the 690 high-strength steel, can generate the nanocrystals formed on the surface of the 690 high-strength steel through extreme plastic strain by adopting the process parameters exceeding the minimum process parameters of the nanocrystals formed on the surface of the 690 high-strength steel, does not need to damage the surface of the 690 high-strength steel material for detection, and is suitable for the actual production process.
Drawings
FIG. 1 shows a set of X-ray diffraction curves for several 690 high-tensile steel samples after laser impact at different power densities in an embodiment of the present invention;
FIG. 2 is a graph of half-width as a function of power density for the same crystal plane in an example of the present invention;
FIG. 3 is a Transmission Electron Microscope (TEM) shot of each 690 high-strength steel sample after laser shock under multiple power density conditions in an embodiment of the present invention;
FIG. 4 shows that the power density of the sample in the embodiment of the present invention is 5.09GW/cm2Electron diffraction pattern after laser shock under the conditions.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
A detection method for forming nanocrystals on the surface of 690 high-strength steel comprises the following steps:
several pieces 690 of high tensile steel samples were prepared.
And carrying out extreme plastic strain on a plurality of 690 high-strength steel samples under the same process and different process parameters.
And (3) carrying out surface treatment on the 690 high-strength steel sample subjected to the extreme plastic strain.
And (3) carrying out X-ray diffraction on each 690 high-strength steel sample subjected to extreme plastic strain by using an X-ray diffractometer to obtain a group of X-ray diffraction patterns.
Analyzing the diffraction peak of the same crystal face in a group of X-ray diffraction patterns, and calculating the full width at half maximum of the diffraction peak of the same crystal face under each process parameter.
Establishing a two-dimensional coordinate system of the process parameters and the half-width, and drawing a curve graph of the half-width of the same crystal face along with the change of the process parameters.
Finding out an increasing inflection point in a curve graph of which the half-height width changes along with the process parameters, wherein the increasing inflection point is a descending inflection point in the ascending process, and verifying that the process parameter of extreme plastic strain corresponding to the increasing inflection point is the minimum process parameter of forming the nano-crystals on the surface of the 690 high-strength steel through a transmission electron microscope and an electron diffraction experiment; when the process parameter corresponding to the extreme plastic strain exceeds the minimum process parameter, the surface of the high-strength steel 690 forms nanocrystals.
The process for generating the extreme plastic strain comprises one of a laser shock peening process, an ultrasonic shot blasting process, a surface mechanical grinding process and a surface mechanical rolling process, wherein the process parameter of the laser shock peening process is power density.
Examples
A detection method for forming nanocrystals on the surface of 690 high-strength steel comprises the following steps:
several pieces 690 of high tensile steel samples were prepared.
The power density of a plurality of 690 high-strength steel samples is respectively 1.53GW/cm2、1.98 GW/cm2、2.77 GW/cm2、4.07 GW/cm2、5.09 GW/cm2And carrying out a laser shock peening process.
Carrying out surface treatment on the 690 high-strength steel sample subjected to laser shock peening; the surface treatment specifically comprises the following steps: a. soaking and cleaning the sample by adopting a pure ethanol or acetone cleaning agent for 3-10 min; b. and carrying out ultrasonic cleaning on the sample after soaking and cleaning, wherein the ultrasonic cleaning time is 1-5min, and ensuring that no residual impurities exist on the surface of the sample.
And (3) carrying out X-ray diffraction measurement on the plurality of 690 high-strength steel samples with the cleaned surfaces to obtain a group of X-ray diffraction curves after laser impact under different power densities, as shown in figure 1.
Measuring the half-height width of the same crystal face in a group of X-ray diffraction curves in the obtained figure 1 to obtain a group of diffraction peak half-height width values of the same crystal face in X-ray diffraction, preferably, analyzing the X-ray diffraction curves through jade software, and determining the half-height width of the diffraction curves through peak searching, preliminary phase searching, main phase position diffraction peak determination and diffraction crystal face labeling; meanwhile, the jade software analyzes 690 that the high-strength steel belongs to a Body Centered Cubic (BCC) structure and has three crystal faces, namely an inertial plane {110}, an inertial plane {200} and an inertial plane {211}, and as shown in FIG. 1, the three groups of wave crests respectively correspond to diffraction peaks of the inertial plane {110}, the inertial plane {200} and the inertial plane {211 }; the rule is obtained according to the relation between the X-ray diffraction full width at half maximum and the grain size, the relation between the integration width of lattice distortion broadening and the integration width of full width at half maximum is 0 when the sum of h, k and l is an even number, namely the integration width of lattice distortion broadening has no influence on the integration width of full width at half maximum, and as the sum of h, k and l of three crystal faces of 690 high-strength steel is an even number, the broadening degree of full width at half maximum is completely determined by the grain refining degree when extreme plastic deformation occurs on the surface of 690 high-strength steel, so that the forming degree of the nano-crystal represented by full width at half maximum is reasonable.
The method for calibrating the habit surface, namely the crystal face index comprises the following steps: 1) Setting a reference coordinate system in the dot matrix, wherein the setting method is the same as that for determining the crystal orientation index; 2) Finding out the intercept of the crystal face to be determined on three crystal axes, if the crystal face is parallel to a certain axis, the intercept on the axis is infinite; if the crystal plane intercepts a certain axis in the negative direction, the intercept on the axis is a negative value; 3) Taking the reciprocal of each intercept; 4) The index of the face is expressed by reciprocal of three as a ratio of integers of relative prime and adding parentheses and is noted as (h k l). The index of a crystal plane represents not only a certain crystal plane but also a group of crystal planes parallel to each other. In addition, the interplanar spacing and distribution of atoms on the interplanar planes within the crystal are identical except that planes with different spatial orientations can be grouped into the same family of planes, denoted by { hkl }, which represents the sum of several sets of equivalent planes linked by symmetry.
Aiming at the half-height width values of the corresponding X-ray diffraction curves at different power densities, a two-dimensional coordinate system is established, a curve graph of the half-height width of the same crystal face along with the change of the power density is drawn in the two-dimensional coordinate system, optionally, an origin drawing is used for drawing the curve graph of the half-height width of the same crystal face along with the change of the power density, as shown in fig. 2, fig. 2 is the curve graph of the half-height width of a {110} plane of an inertial plane along with the change of the power density.
Searching a first increasing inflection point a of a curve graph of which the half-height width changes along with the power density, wherein the power density of the laser shock peening process corresponding to the increasing inflection point a is 2.77GW/cm2。
By transmission electron microscopy and electron diffraction experiments, as shown in FIG. 3, wherein FIG. 3A shows a power density of 1.53GW/cm2The transmission electron microscope image after laser impact under the condition, FIG. 3B is the power density of 1.98 GW/cm2The transmission electron microscope image after laser impact under the condition, FIG. 3C is the power density 2.77GW/cm2The transmission electron microscope image after laser impact under the condition, and the power density of 4.07 GW/cm is shown in figure 3D2The transmission electron microscope was used to take pictures after laser impact under the conditions, and FIG. 3E shows the power density at 5.09GW/cm2The grain size is detected by a transmission electron microscope shooting picture after laser impact under the condition, and the grain size is detected by the transmission electron microscope shooting picture, and the grain size is observed to be less than 2.77GW/cm under the microscope2No nanocrystallization phenomenon is found in the 690 high-strength steel sample after the laser impact of the power density, and the crystal grain is 2.77GW/cm2The power density of the crystal particles is nano-sized after laser impact, and the crystal particles with the size of 50-200nm occupy and examineMore than 80% of the measurement area proves that when the 690 high-strength steel sample block is subjected to laser shock strengthening by the power density corresponding to the increased inflection point a, the 690 high-strength steel material realizes surface nanocrystallization, and the degree of the surface nanocrystallization of the 690 high-strength steel material is further deepened along with the rise of the power density of the laser shock strengthening process, and the power density is 5.09GW/cm2Meanwhile, as shown in fig. 4, the electron diffraction pattern is concentric circles, and it is proved that the orientation of the grains in the observed area is random, and the distribution of the nanocrystals is uniform, that is, the observed area has uniformly distributed nanocrystals.
From the above, the power density of the laser shock peening process corresponding to the increasing inflection point a is verified to be 2.77GW/cm2Forming 690 a minimum power density of the nanocrystals on the surface of the high-strength steel; when the power density of the laser shock peening process exceeds its minimum power density, 690 nanocrystals are formed on the surface of the high strength steel.
The method for detecting the nanocrystals formed on the surface of the 690 high-strength steel verifies the reliability of the method for forming the nanocrystals on the surface of the 690 high-strength steel, can generate the nanocrystals formed on the surface of the 690 high-strength steel through extreme plastic strain by adopting the process parameters exceeding the minimum process parameters of the nanocrystals formed on the surface of the 690 high-strength steel, does not need to damage the surface of the 690 high-strength steel material for detection, and is suitable for the actual production process.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. A detection method for forming nanocrystals on the surface of 690 high-strength steel is characterized by comprising the following steps:
s1, preparing a plurality of 690 high-strength steel samples;
s2, respectively carrying out laser shock strengthening on the plurality of 690 high-strength steel samples prepared in the step S1, and respectively generating extreme plastic strain at different power densities;
s3, performing X-ray diffraction on each 690 high-strength steel sample subjected to extreme plastic strain by using an X-ray diffractometer to obtain a group of X-ray diffraction patterns;
s4, analyzing diffraction peaks of the same crystal face in a group of X-ray diffraction patterns, and calculating the full width at half maximum of the diffraction peak of the same crystal face under each power density;
s5, establishing a two-dimensional coordinate system of process parameters and half width, and drawing a curve graph of half width of the same crystal face along with the change of power density;
s6, finding out an increasing inflection point in a curve graph of which the full width at half maximum changes along with the power density, and verifying that the power density of extreme plastic strain corresponding to the increasing inflection point is 690 through a transmission electron microscope and an electron diffraction experiment, wherein the power density is the minimum power density of the nanocrystals formed on the surface of the high-strength steel through an impact strengthening process; and when the power density parameter corresponding to the extreme plastic strain exceeds the minimum power density, 690 forming the nano-crystals on the surface of the high-strength steel.
2. The method for detecting the formation of the nanocrystals on the surface of the 690 high strength steel as claimed in claim 1, further comprising a step of performing a surface treatment on the 690 high strength steel sample after the extreme plastic strain between the step S2 and the step S3.
3. The method for detecting the formation of the nanocrystals on the surface of the 690 high-strength steel as claimed in claim 2, wherein the surface treatment process specifically comprises the following steps: a. soaking and cleaning the sample by adopting a pure ethanol or acetone cleaning agent for 3-10 min; b. and carrying out ultrasonic cleaning on the sample after soaking and cleaning, wherein the ultrasonic cleaning time is 1-5min, and ensuring that no residual impurities exist on the surface of the sample.
4. The method for detecting the formation of the nanocrystals on the surface of the 690 high-strength steel as claimed in claim 1, wherein the transmission electron microscope and the electron diffraction experiment comprise the following steps: firstly, respectively shooting transmission electron microscope pictures of a plurality of samples subjected to X-ray diffraction, and detecting the size of local grains; and then, respectively carrying out electron diffraction on a plurality of samples after the electron microscope picture is shot, and when the patterns in the electron diffraction picture are in the shape of concentric rings, the crystal grain orientation is random, and the nano-crystals are uniformly distributed, namely the nano-crystals which are uniformly distributed exist in the observed area.
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| CN109613032A (en) * | 2018-12-28 | 2019-04-12 | 江苏江华阀业有限公司 | A kind of nanosizing detection method applied to Fluid valve inner surface |
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