CN116519730B - Analysis method for purifying effectiveness of rare earth element on rare earth steel and application thereof - Google Patents
Analysis method for purifying effectiveness of rare earth element on rare earth steel and application thereof Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 192
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 126
- 239000010959 steel Substances 0.000 title claims abstract description 126
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 114
- 238000004458 analytical method Methods 0.000 title claims abstract description 20
- 230000005540 biological transmission Effects 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000009826 distribution Methods 0.000 claims description 29
- 238000010586 diagram Methods 0.000 claims description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 5
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 4
- 150000002602 lanthanoids Chemical class 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052706 scandium Inorganic materials 0.000 claims description 3
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 15
- 239000011159 matrix material Substances 0.000 abstract description 8
- 238000001556 precipitation Methods 0.000 description 10
- 239000002244 precipitate Substances 0.000 description 8
- 229910052684 Cerium Inorganic materials 0.000 description 7
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000010884 ion-beam technique Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N23/22—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 by measuring secondary emission from the material
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- G01N23/2251—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 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N23/02—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 by transmitting the radiation through the material
- G01N23/04—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 by transmitting the radiation through the material and forming images of the material
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N23/20—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 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention relates to the field of material analysis, and discloses an analysis method for purifying effectiveness of rare earth elements on rare earth steel and application thereof. According to the analysis method, the microscopic morphology of the rare earth steel is observed by adopting an electron scanning microscope, and the atomic arrangement mode in the rare earth steel matrix is observed by adopting a transmission electron microscope, so that whether the rare earth element effectively purifies the impurity element in the rare earth steel is accurately judged, the practicability is high, and the analysis method can be widely applied.
Description
Technical Field
The invention relates to the field of material analysis, in particular to an analysis method for purifying effectiveness of rare earth elements on rare earth steel and application thereof.
Background
Rare earth elements have very important influence on the structure and mechanical properties of steel and alloy. The rare earth has the functions of deep deoxidization and deep desulfurization, can modify and refine inclusions, and can inhibit growth of crystal grains, so that the toughness, the fatigue performance, the wear resistance, the corrosion resistance, the heat resistance and the like of the metal material are improved.
Rare earth elements are often added to high-end bearing steels to improve the mechanical properties of the high-end bearing steels. However, the manufacturing method of the high-end bearing steel is not known in China, and the reverse design and research and development of the bearing steel are important steps for manufacturing the bearing steel.
Therefore, an analysis method capable of determining whether the rare earth element in the rare earth steel is effective for purifying the impurity element in the rare earth steel is explored, and the analysis method has important significance for developing and reversely designing the high-end bearing steel.
Disclosure of Invention
The invention aims to solve the problem that whether the rare earth elements in the rare earth steel are effective in purifying the rare earth steel cannot be judged in the prior art.
In order to achieve the above object, a first aspect of the present invention provides a method for analyzing purification effectiveness of rare earth elements on rare earth steel, comprising the steps of:
s1: observing the rare earth steel by adopting an electron scanning microscope, wherein the rare earth steel contains iron element, carbon element and rare earth element, and the content of the carbon element in the rare earth element is 0.10-0.25 wt%;
if a second phase precipitated phase formed by the rare earth element is not observed, a result 1 is obtained, wherein the result 1 is that the rare earth element does not effectively purify the rare earth steel;
if the second phase precipitated phase formed by the rare earth element can be observed, carrying out transmission electron microscope sample preparation on the rare earth steel at the position of the second phase precipitated phase to obtain a sample to be detected;
s2: observing the sample to be detected by adopting a transmission electron microscope, and obtaining an atomic arrangement diagram of the sample to be detected;
if atoms in the atomic arrangement diagram are arranged side by side in a cross manner, a result 2 is obtained, wherein the result 2 is that the rare earth element effectively purifies the rare earth steel;
if the atoms in the atomic arrangement pattern are arranged in a clustered manner, the result 1 is obtained.
Preferably, step S2 further comprises the steps of: analyzing the distribution condition of each element in the sample to be detected through energy spectrum;
if the atomic distribution of each element is uniform, obtaining a result 1;
if the atomic distribution of each element is not uniform, the result 2 is obtained.
Preferably, the content of the carbon element in the rare earth steel is 0.15-0.20 wt%.
Preferably, the content of the rare earth element in the rare earth steel is 0.03wt% to 0.1wt%.
Preferably, the rare earth element is at least one of lanthanoid element, yttrium element, and scandium element.
Preferably, the rare earth steel further contains at least one of manganese element, silicon element, aluminum element, molybdenum element, copper element, nickel element, titanium element and nitrogen element.
Further preferably, in the rare earth steel, the content of manganese is 1.75-1.80 wt%, the content of silicon is 0.25-0.30 wt%, the content of aluminum is 1.50-1.55 wt%, the content of molybdenum is 0.00-0.05 wt%, the content of copper is 0.005-0.015 wt%, the content of nickel is 0.005-0.010 wt%, the content of titanium is 0.00-0.005 wt%, the content of nitrogen is 0.000-0.005 wt%, and the balance is iron.
Preferably, in step S1, when observing the rare earth steel, the magnification of the electron scanning microscope is such that the observation scale is 1 μm to 10 μm.
Preferably, the thickness of the sample to be detected is 40 nm-80 nm.
Preferably, in step S2, when the sample to be detected is observed, the magnification of the transmission electron microscope makes the observation scale be 100 pm-1000 pm.
A second aspect of the present invention provides the use of the above analysis method for evaluating the purification effectiveness of rare earth elements on rare earth steel.
Through the technical scheme, the atomic arrangement mode of the rare earth elements in the rare earth steel can be intuitively observed, whether the rare earth elements effectively purify impurity elements in the rare earth steel or not can be accurately judged, and the rare earth element purifying device is clear in mechanism, high in practicability and capable of being widely applied.
Drawings
FIG. 1 is an electron scanning microscope image of a rare earth steel material I according to example 1 of the present invention when the observation scale is 5. Mu.m;
FIG. 2 is a preparation diagram of an electron scanning microscope (SEM) of the sample I to be measured according to example 1 of the present invention when the observation scale is 5 μm;
FIG. 3 is an electron scanning microscope image of a sample I to be measured according to example 1 of the present invention when the observation scale is 10. Mu.m;
FIG. 4 is a transmission electron microscope image of a sample I to be measured according to example 1 of the present invention at a measurement scale of 500 pm;
fig. 5 is an energy spectrum analysis chart of the sample I to be measured according to the embodiment 1 of the present invention when the observation scale is 500pm, wherein fig. 5 (a) is an S element distribution chart of the sample I to be measured, fig. 5 (b) is an O element distribution chart of the sample I to be measured, fig. 5 (c) is a rare earth element Ce element distribution chart of the sample I to be measured, and fig. 5 (d) is a Ca element distribution chart of the sample I to be measured;
FIG. 6 is a transmission electron microscope image of a sample II to be measured according to example 2 of the present invention at a measurement scale of 500 pm;
fig. 7 is an energy spectrum analysis chart of a sample II to be measured according to embodiment 2 of the present invention when the observation scale is 500pm, wherein fig. 7 (a) is an S element distribution chart of the sample II to be measured, fig. 7 (b) is an O element distribution chart of the sample II to be measured, fig. 7 (c) is a rare earth element Ce element distribution chart of the sample II to be measured, and fig. 7 (d) is a Ca element distribution chart of the sample II to be measured;
FIG. 8 is an electron scanning microscope (SEM) image of a rare earth steel III according to example 3 of the present invention with a scale of 5 μm;
FIG. 9 is a stress-strain curve of a rare earth steel material according to an embodiment of the present invention;
FIG. 10 is a flow chart of the steps of an analysis method according to an embodiment of the present invention.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
As described above, the first aspect of the present invention provides a method for analyzing the purification effectiveness of rare earth elements on rare earth steel, as shown in fig. 10, comprising the steps of:
s1: observing the rare earth steel by adopting an electron scanning microscope, wherein the rare earth steel contains iron element, carbon element and rare earth element, and the content of the carbon element in the rare earth element is 0.10-0.25 wt%;
if a second phase precipitated phase formed by the rare earth element is not observed, a result 1 is obtained, wherein the result 1 is that the rare earth element does not effectively purify the rare earth steel;
if the second phase precipitated phase formed by the rare earth element can be observed, carrying out transmission electron microscope sample preparation on the rare earth steel at the position of the second phase precipitated phase to obtain a sample to be detected;
s2: observing the sample to be detected by adopting a transmission electron microscope, and obtaining an atomic arrangement diagram of the sample to be detected;
if atoms in the atomic arrangement diagram are arranged side by side in a cross manner, a result 2 is obtained, wherein the result 2 is that the rare earth element effectively purifies the rare earth steel;
if the atoms in the atomic arrangement pattern are arranged in a clustered manner, the result 1 is obtained.
In order to explore whether the rare earth element in the rare earth steel effectively purifies the impurity element in the rare earth steel, the inventor finds that the purification effectiveness of the rare earth element on the impurity element in the rare earth steel directly influences the mechanical property of the rare earth steel, so the inventor develops the analysis method, can intuitively observe the microscopic morphology and the atomic arrangement mode of the rare earth steel, and can intuitively and accurately judge whether the rare earth element effectively purifies the impurity element in the rare earth steel by observing the microscopic morphology and the atomic arrangement mode of the rare earth steel.
The inventors found that, when the addition amount of the rare earth element is insufficient, the rare earth element cannot effectively purify the impurity element dissolved in the matrix of the rare earth steel, and a stable second phase precipitate phase cannot be formed, and as shown in fig. 8, for example, the addition amount of the rare earth element is insufficient, and the second phase precipitate phase of the rare earth element cannot be observed at the micrometer scale.
When the addition amount of the rare earth element makes the impurity element in the matrix of the rare earth steel play an effective adsorption role, the second phase precipitated phase of the rare earth steel as shown in fig. 1 can be clearly observed at the micrometer scale.
Further, when the addition amount of the rare earth element is proper, the rare earth element can just effectively adsorb the impurity element in the matrix of the rare earth steel, and when the sample to be detected with proper addition amount of the rare earth element is observed under the nano scale, the cross side-by-side atomic arrangement diagram shown in fig. 4 can be observed.
When the addition amount of the rare earth element is excessive, the excessive rare earth element can be in the form of a simple substance to become an impurity element in a rare earth steel matrix, so that not only can the effective purification effect on the rare earth steel be not realized, but also the mechanical property of the rare earth steel can be reduced, and when the sample to be detected with the excessive addition amount of the rare earth element is observed under the nano scale, the aggregated atomic arrangement diagram shown in fig. 6 is observed.
In the step S1, observing the rare earth steel by adopting an electron scanning microscope, observing the microscopic morphology of the rare earth steel under a micrometer scale, and clearly observing the second phase precipitation phase formed by the adsorption effect of the rare earth element added in the rare earth steel on the impurity element in the rare earth steel when the addition amount of the rare earth element is enough; when the addition amount of the rare earth element is insufficient, the second phase precipitate phase cannot be observed at the micrometer scale. According to some preferred embodiments of the present invention, when observing the rare earth steel material, the magnification of the electron scanning microscope is such that the observation scale is 1 μm to 10 μm. In this preferred case, the second phase precipitate can be observed more clearly and intuitively.
According to a particularly preferred embodiment of the present invention, when observing the rare earth steel, the magnification of the electron scanning microscope is such that the observation scale is 5 μm, and illustratively, when the addition amount of the rare earth element is appropriate, as shown in fig. 1, the rare earth element in the rare earth steel is cerium element, the content of cerium element is 0.06wt%, and a spindle-shaped second phase precipitated phase can be clearly observed.
According to some preferred embodiments of the present invention, the rare earth steel contains iron (Fe), carbon (C) and rare earth (rare earth), wherein the content of the carbon is 0.10wt% to 0.25wt%. Preferably, the content of the carbon element is 0.15-0.20 wt%.
According to some preferred embodiments of the invention, the rare earth element is at least one of lanthanoid element (La), yttrium element (Y) and scandium element (Sc), and illustratively the lanthanoid element includes at least one of lanthanum element (La), cerium element (Ce) and samarium element (Sm).
According to some preferred embodiments of the present invention, the rare earth element content in the rare earth steel is 0.03wt% to 0.1wt%.
According to some preferred embodiments of the present invention, the rare earth steel further contains at least one of manganese (Mn), silicon (Si), aluminum (Al), molybdenum (Mo), copper (Cu), nickel (Ni), titanium (Ti), and nitrogen (N).
According to a further preferred embodiment of the present invention, in the rare earth steel, the content of manganese element is 1.75wt% to 1.80wt%, the content of silicon element is 0.25wt% to 0.30wt%, the content of aluminum element is 1.50wt% to 1.55wt%, the content of molybdenum element is 0.00 to 0.05wt%, the content of copper element is 0.005wt% to 0.015wt%, the content of nickel element is 0.005wt% to 0.010wt%, the content of titanium element is 0.00 to 0.005wt%, the content of nitrogen element is 0.000 to 0.005wt%, and the balance is iron element.
According to a more preferred embodiment of the present invention, the rare earth element is cerium element, and the second phase precipitate phase is spindle-shaped. In step S1, if no spindle-shaped second phase precipitate is observed, a result 1 is obtained, indicating that the cerium element in the rare earth steel material is not effective in purifying the rare earth steel material.
The specific method for preparing the sample of the transmission electron microscope is not particularly limited, as long as the rare earth steel material can be prepared into a sample to be measured suitable for observation in the transmission electron microscope.
According to some preferred embodiments of the invention, in step S1, the transmission electron microscope sample preparation is FIB preparation.
According to some particularly preferred embodiments of the present invention, the step of preparing a sample for a transmission electron microscope may be performed in the following manner, but is not limited to:
as shown in fig. 2, the steel structure around the second precipitate phase was cut by an ion beam to form a pit-like structure around the second precipitate phase, and the remaining steel material was cut to a thickness of 100nm or less to obtain a sample to be measured as shown in fig. 3.
According to some preferred embodiments of the present invention, the thickness of the sample to be measured is 40nm to 80nm. Under this preferable condition, a clearer and more intuitive atomic arrangement pattern can be obtained.
According to some preferred embodiments of the invention, step S2 further comprises the steps of: analyzing the distribution condition of each element in the sample to be detected through energy spectrum, if the atomic distribution of each element is uniform, obtaining a result 1, and indicating that the rare earth element effectively purifies the rare earth steel; if the atomic distribution of each of the elements is not uniform, the result 2 is obtained, which indicates that the rare earth element is not effective to purify the rare earth steel. With this preferred embodiment, it is possible to more accurately determine whether the rare earth element is effective in purifying the rare earth steel material.
According to some preferred embodiments of the present invention, in step S2, if the atoms in the atomic arrangement pattern are arranged in a cluster, it is indicated that the rare earth element content is too high, and the rare earth element is not effective to purify the rare earth steel.
According to some preferred embodiments of the present invention, in step S2, when the sample to be measured is observed, the magnification of the transmission electron microscope makes the observation scale 100pm to 1000pm.
A second aspect of the present invention provides the use of the above analysis method for evaluating the purification effectiveness of rare earth elements on rare earth steel.
Rare earth elements are often added to high-end bearing steels to improve the mechanical properties of the high-end bearing steels. The analysis method is applied to analysis of the element components, the atomic arrangement mode and the purification effectiveness of the high-end bearing steel, has the advantages of intuitionism, accuracy and strong operability, and has great significance for reverse design and research and development of the high-end bearing steel.
The present invention will be described in detail by examples.
The rare earth steel materials in the following examples are self-made rare earth steel materials, and the composition contents are shown in table 1 below:
TABLE 1
Example 1
S1: observing the rare earth steel I by adopting an electron scanning microscope, and determining a second phase precipitation phase of the rare earth steel I, wherein the second phase precipitation phase is observed to be spindle-shaped as shown in fig. 1; wherein the magnification of the electron scanning microscope is such that the observation scale is 5 μm;
as shown in fig. 2, cutting the steel structure around the second phase precipitation phase by an ion beam to form a pit-like structure around the second phase precipitation phase, and cutting the left rare earth steel to a thickness of 60nm to obtain a sample I to be measured as shown in fig. 3;
s2: observing the sample to be detected by adopting a transmission electron microscope, and obtaining an atomic arrangement diagram of the sample I to be detected as shown in fig. 4, wherein as is obvious from fig. 4, each atom is arranged side by side in a cross manner, so as to obtain a result 2, which shows that the rare earth element cerium effectively purifies the rare earth steel I;
and analyzing the distribution condition of each element of the sample I to be detected by adopting an energy spectrum to obtain an element distribution diagram shown in figure 5. Wherein, fig. 5 (a) is an S element distribution diagram in the sample I to be measured, fig. 5 (b) is an O element distribution diagram in the sample I to be measured, fig. 5 (c) is a rare earth element Ce element distribution diagram in the sample I to be measured, and fig. 5 (d) is a Ca element distribution diagram in the sample I to be measured, and it can be seen from fig. 5 that the S element, the O element, the Ce element, and the Ca element are uniformly distributed, which indicates that the addition amount of the Ce element is proper, and has good adsorption effect on the S element, the O element, and the Ca element, thereby improving the purity of the rare earth steel I and effectively purifying the rare earth steel I.
Example 2
S1: observing the rare earth steel II by adopting an electron scanning microscope, determining a second phase precipitation phase of the rare earth steel II, and observing that the second phase precipitation phase is spindle-shaped; wherein the magnification of the electron scanning microscope is such that the observation scale is 5 μm;
cutting the steel material tissue around the second phase precipitation phase by an ion beam, forming a pit-shaped structure around the second phase precipitation phase, and cutting the left rare earth steel material to a thickness of 60nm to obtain a sample II to be detected shown in figure 3;
s2: observing the sample to be detected by adopting a transmission electron microscope, and obtaining an atomic arrangement diagram of the sample II to be detected as shown in fig. 6, wherein as is obvious from fig. 6, each atom is arranged in an aggregation mode, which indicates that the atomic arrangement mode of each element does not reach a stable form, certain elements or simple substances exist and remain in the form of impurity elements, and a result 1 is obtained, wherein the rare earth elements do not effectively purify the rare earth steel II;
and analyzing the distribution condition of each element of the sample II to be detected by adopting an energy spectrum to obtain an element distribution diagram shown in figure 7. Wherein, fig. 7 (a) is a distribution diagram of S element in the sample II to be measured, fig. 7 (b) is a distribution diagram of O element in the sample II to be measured, fig. 7 (c) is a distribution diagram of rare earth element Ce element in the sample II to be measured, fig. 7 (d) is a distribution diagram of Ca element in the sample II to be measured, and as can be seen from fig. 7, the S element, O element, ce element, ca element are unevenly distributed, and the rare earth steel II is not purified effectively. Analysis shows that the excessive addition of the rare earth element Ce leads to the original rare earth element Ce for absorbing the impurity element, and the rare earth element Ce becomes the impurity element in the rare earth steel II matrix in a simple substance form due to the excessive addition, so that the effective purification effect on the rare earth steel II can not be realized, and the mechanical property of the rare earth steel II can be reduced.
Example 3
S1: and observing the rare earth steel III by adopting an electron scanning microscope, wherein the magnification of the electron scanning microscope enables an observation scale to be 5 mu m, as shown in fig. 8, the microstructure is uniform, a spindle-shaped second phase precipitation phase is not observed, and a result 1 is obtained, which shows that the addition amount of Ce element is too low, so that the impurity element dissolved in the rare earth steel III matrix cannot be effectively purified, and the Ce atom is dissolved into the rare earth steel III matrix due to the too small addition amount, so that the rare earth steel III cannot be effectively purified.
Test case
And (3) mechanical property verification test: the rare earth steel I described in example 1, the rare earth steel II described in example 2, and the rare earth steel III described in example 3 were subjected to mechanical property test at room temperature (25 ℃) to obtain stress-strain curves as shown in FIG. 9.
As can be seen from fig. 9, the mechanical properties of the rare earth steel I are significantly better than those of the rare earth steel II and the rare earth steel III, which means that the rare earth elements in the rare earth steel I effectively purify the rare earth steel I, while the rare earth elements in the rare earth steel II and the rare earth steel III do not effectively purify the rare earth steel II and the rare earth steel III, respectively, which is consistent with the results of examples 1 to 3.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (9)
1. A method for analyzing the purification effectiveness of rare earth elements on rare earth steel is characterized by comprising the following steps:
s1: observing the rare earth steel by adopting an electron scanning microscope, wherein the rare earth steel contains iron element, carbon element and rare earth element, and the content of the carbon element is 0.10-0.25 wt%;
if a second phase precipitated phase formed by the rare earth element is not observed, a result 1 is obtained, wherein the result 1 is that the rare earth element does not effectively purify the rare earth steel;
if the second phase precipitated phase formed by the rare earth element can be observed, carrying out transmission electron microscope sample preparation on the rare earth steel at the position of the second phase precipitated phase to obtain a sample to be detected;
s2: observing the sample to be detected by adopting a transmission electron microscope, and obtaining an atomic arrangement diagram of the sample to be detected;
if atoms in the atomic arrangement diagram are arranged side by side in a cross manner, a result 2 is obtained, wherein the result 2 is that the rare earth element effectively purifies the rare earth steel;
if the atoms in the atomic arrangement diagram are arranged in a gathering mode, obtaining a result 1;
step S2 further comprises the steps of: analyzing the distribution condition of each element in the sample to be detected through energy spectrum;
if the atomic distribution of each element is uniform, obtaining a result 1;
if the atomic distribution of each element is not uniform, the result 2 is obtained.
2. The analysis method according to claim 1, wherein the content of the carbon element in the rare earth steel is 0.15wt% to 0.20wt%;
and/or the content of the rare earth element in the rare earth steel is 0.03-0.1 wt%.
3. The method according to claim 1, wherein the rare earth element is at least one of a lanthanoid element, an yttrium element, and a scandium element.
4. The method according to claim 1, wherein the rare earth steel material further contains at least one of manganese element, silicon element, aluminum element, molybdenum element, copper element, nickel, titanium element, and nitrogen element.
5. The analysis method according to claim 4, wherein the rare earth steel contains 1.75wt% to 1.80wt% of manganese, 0.25wt% to 0.30wt% of silicon, 1.50wt% to 1.55wt% of aluminum, 0.00 to 0.05wt% of molybdenum, 0.005wt% to 0.015wt% of copper, 0.005wt% to 0.010wt% of nickel, 0.00 to 0.005wt% of titanium, 0.000 to 0.005wt% of nitrogen, and the balance of iron.
6. The method according to any one of claims 1 to 5, wherein in step S1, the magnification of the electron scanning microscope is such that the observation scale is 1 μm to 10 μm when the rare earth steel is observed.
7. The method according to any one of claims 1 to 5, wherein the thickness of the sample to be measured is 40nm to 80nm.
8. The method according to any one of claims 1 to 5, wherein in step S2, when the sample to be measured is observed, the magnification of the transmission electron microscope is such that the observation scale is 100pm to 1000pm.
9. The use of the analysis method according to any one of claims 1 to 5 for evaluating the purification effectiveness of rare earth elements on rare earth steel.
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