CN115656149A - Method for detecting element content in nickel-based superalloy - Google Patents
Method for detecting element content in nickel-based superalloy Download PDFInfo
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Abstract
The invention discloses a method for detecting the element content in a nickel-based superalloy. The invention takes chromium particles (powder) with the purity of more than or equal to 99.99wt% and nickel particles (powder) as base stock solutions, and then obtains respective working curve solutions of molybdenum, niobium and titanium by adding respective standard solutions of molybdenum, niobium and titanium on the basis.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for detecting the content of elements in a nickel-based superalloy, in particular to a method for detecting the content of molybdenum, niobium and titanium in the nickel-based superalloy.
Background
Superalloys, also known as hot strength alloys, and also known as "superalloys," include wrought superalloys and cast superalloys, welding superalloy wires, and powdered superalloys. The material is a metal material which takes iron, nickel and cobalt as the base and can work for a long time at a high temperature of more than 600 ℃ and under the action of certain stress; and has high-temperature strength, good oxidation resistance and corrosion resistance, good fatigue performance, good fracture toughness and other comprehensive properties. Based on the performance characteristics, the high-temperature alloy is widely applied to important materials of aviation, aerospace, petroleum, chemical engineering and ships. The high-temperature alloy is divided into iron-based, nickel-based, cobalt-based and other high-temperature alloys according to matrix elements. Iron-based superalloys typically can only be used up to 750-780 ℃, and for heat-resistant components used at higher temperatures, nickel-based and refractory metal-based alloys are used. Nickel-base superalloys have a particularly important position in the entire superalloy field, and are widely used to manufacture the hottest end pieces of aircraft jet engines and various industrial gas turbines.
For the analysis of the basic elements in the nickel superalloy, the method for analyzing the chemical elements of the superalloy is not referred to in international standard ISO, russian national standard TOC, japanese industrial standard JIS, and national standard GB/T. The American society for testing and materials Standard ASTM E2594-09, chemical composition test method in nickel alloy by inductively coupled plasma atomic emission spectrometry, can determine Mo, nb, ti and other elements in the nickel-based superalloy. However, such methods have the disadvantages of large environmental pollution, long time consumption and complicated operation, so that a detection method capable of accurately and rapidly detecting the contents of molybdenum, niobium and titanium in the high-temperature alloy needs to be established.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for detecting the content of elements in a nickel-based high-temperature alloy, which can quickly and accurately detect the content of molybdenum, niobium and titanium in the high-temperature alloy.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a method for detecting the content of elements in a nickel-based superalloy, which is used for detecting the content of molybdenum, niobium and titanium in the nickel-based superalloy, comprises the following steps:
(1) Respectively taking chromium particles (powder) and nickel particles (powder) with the purity of more than or equal to 99.99wt%, and adding hydrochloric acid and nitric acid to dissolve the chromium particles (powder) and the nickel particles (powder) to obtain a matrix stock solution; preparing a mixed solution of the working curves of the molybdenum, the niobium and the titanium by using the base stock solution and respective standard solutions of the molybdenum, the niobium and the titanium; detecting the molybdenum, niobium and titanium working curve mixed solution by using an inductively coupled plasma emission spectrometer to prepare a working curve;
(2) Weighing a nickel-based superalloy sample to be detected, and performing jar-closing digestion to obtain a sample solution to be detected;
(3) And measuring the solution of the sample to be measured by using an inductively coupled plasma emission spectrometer to obtain the contents of molybdenum, niobium and titanium in the nickel-based superalloy sample to be measured.
Because nickel and chromium are main chemical components in the nickel-based superalloy, the content of molybdenum, niobium and titanium to be detected is relatively low, and if a nickel-based superalloy sample is directly adopted to prepare a working curve solution, the spectral intensity of a spectral line of an element to be detected in the working curve is increased, so that the stability and accuracy of a detection result are affected, therefore, chromium particles (powder) and nickel particles (powder) with the purity of more than or equal to 99.99wt% are used as a base stock solution, and then respective working curve solutions of molybdenum, niobium and titanium are obtained by adding respective standard solutions of molybdenum, niobium and titanium on the basis, so that the influence of impurity elements on the detection accuracy is avoided. The method realizes the simultaneous detection of molybdenum, niobium and titanium elements in the nickel-based superalloy by a closed tank dissolution-inductive coupling plasma emission spectrometry, and has high detection efficiency and good accuracy.
Further, the process of preparing the matrix stock solution in step (1) is as follows:
s1, preparing a chromium matrix stock solution: weighing 1.00-4.00 g of the chromium particles (powder) into a glass beaker, adding secondary deionized water, covering a surface dish, adding 20-80 mL of high-grade pure hydrochloric acid to dissolve at 80-100 ℃, heating to boil for 10-20 mins after the chromium particles (powder) are completely dissolved, taking down, cooling to room temperature, diluting and fixing the volume to obtain a matrix stock solution containing 0.02g/mL of chromium.
S2, preparing a matrix nickel stock solution: weighing 3.00-8.00 g of nickel particles (powder) into a glass beaker, adding secondary deionized water, covering a watch glass, adding 20-80 mL of high-grade pure nitric acid to dissolve at 80-100 ℃, adding 5-10 mL of high-grade pure hydrochloric acid after the nickel particles (powder) are completely dissolved, heating to boil for 10-20 mins, taking down, cooling to room temperature, diluting and fixing the volume to obtain a matrix stock solution containing 0.03g/mL of nickel.
The invention uses the superior pure hydrochloric acid and the superior pure nitric acid to dissolve the chromium particles (powder) and the nickel particles (powder), and correspondingly weighs the chromium particles (powder) and the nickel particles (powder) for preparing the base stock solution according to the specific gravity relation of the chromium element and the nickel element in the nickel-based superalloy, so that the chromium particles (powder) and the nickel particles (powder) are basically consistent with the contents of the chromium element and the nickel element in the nickel-based superalloy, thereby ensuring that the prepared working curve solution is matched with the actual sample base body, and further ensuring the preparation of the detection result. In the process of dissolving the chromium particles (powder) and the nickel particles (powder), the invention gradually adds the superior pure hydrochloric acid or the nitric acid in a mode of multiple times to ensure that the chromium particles (powder) and the nickel particles (powder) are evenly and fully dissolved completely, and finally, the superior pure nitric acid or the hydrochloric acid is added to ensure that the amount of the superior pure acid is consistent with the amount of the superior pure acid which must be added when a high-temperature alloy sample is subsequently dissolved, the components of the solution are consistent, and the addition of the superior pure hydrochloric acid or the nitric acid can better ensure that other impurities are not introduced into the matrix solution.
After the violent reaction is stopped after each addition, the high-grade pure hydrochloric acid or nitric acid is dissolved at low temperature until small bubbles are generated, and then the high-grade pure hydrochloric acid or nitric acid is added again for reaction again. Generally, the times of adding the super-grade pure hydrochloric acid or nitric acid for several times are 2-3 times, and the addition is equivalent for each time. The volumes of the superior pure hydrochloric acid, the secondary deionized water and the superior pure nitric acid are the total amount of the superior pure acid added for a plurality of times.
Further, step (1) further comprises:
s3, preparing a working curve solution: mixing 1.00mL of the chromium matrix stock solution, 10.00mL of superior pure hydrochloric acid, 3.00mL of superior pure nitric acid and 5.00mL of superior pure hydrofluoric acid with standard solutions of molybdenum, niobium and titanium respectively to obtain a working curve mixed solution;
wherein the standard solutions of molybdenum, niobium and titanium are added in a gradient manner within 0-10.00 mL respectively;
the concentrations of the molybdenum, niobium and titanium standard solutions were all 1000. Mu.g/mL.
The invention adds superior pure hydrochloric acid, superior pure nitric acid and superior pure hydrofluoric acid into the working curve solution, and aims to keep consistent with acid solution adopted in subsequent sample dissolution, prolong the valid period of molybdenum and niobium elements and ensure the detection accuracy.
Further, the specific preparation process of the sample solution to be tested in the step (2) is as follows: weighing a nickel-based superalloy sample to be detected, placing the nickel-based superalloy sample into a sealed pressure container, sequentially adding 1-10 mL of secondary deionized water, 1-20 mL of high-grade pure hydrochloric acid, 0.3-5 mL of high-grade pure nitric acid and 1-5 mL of high-grade pure hydrofluoric acid, covering and screwing the sealed pressure container after the phenomenon of violent reaction stops, sealing the sealed pressure container, placing the sealed pressure container into an electric heating plate or a corrosion-resistant oven at 80-150 ℃, preserving heat for 0.5-6 h, taking out and cooling to room temperature, diluting the obtained solution, and fixing the volume to 100mL to obtain a sample solution to be detected. When the content of the element to be detected is 10-30 wt%, accurately taking 20mL of sample solution, diluting to constant volume to 100mL to obtain the sample solution to be detected
According to the invention, the superior pure hydrochloric acid, the superior pure nitric acid and the superior pure hydrofluoric acid are used as hydrofluoric acid systems for dissolving the nickel-based high-temperature alloy sample, the introduction of the nitric acid basically realizes the complete digestion of the low-carbon sample, and simultaneously the digestion is carried out in a sealed environment at a specific temperature of 80-150 ℃, so that molybdenum, niobium and titanium elements to be detected in the sample can be completely dissolved at one time, and the dissolving efficiency is improved. Meanwhile, the dissolution time of the invention is 0.5 to 6 hours, the dissolution speed is high, the sample dissolution process can be unattended, and the rest time of the staff is fully utilized. The mode of dissolving the sample in a sealed manner can effectively avoid pollution caused by the environment.
Further, the nickel-base superalloy sample was weighed as follows:
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 0.10-1.00 wt%, the weighed sample amount is 0.15g, and the accuracy is 0.0001g;
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 1.00-7.00 wt%, the weighed sample amount is 0.1g, and the accuracy is 0.0001g;
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 7.00-10.0 wt%, the weighed sample amount is 0.08g, and the accuracy is 0.0001g.
When the content of the element to be detected in the nickel-based superalloy sample to be detected is 10.0-30.0 wt%, the weighed sample amount is 0.1g, and the accuracy is 0.0001g.
Further, when the content of the molybdenum element in the nickel-based superalloy to be detected is more than 10.0-30.0 wt% and the content of the niobium and titanium elements is 0.1-10 wt%, 0.10g of a sample is weighed to detect the content of the molybdenum element, and 0.08-0.15 g of the sample is weighed to detect the niobium and titanium.
The invention establishes the sample weighing standard in the test evaluation of actual national standard substances, and the weighing quantity is helpful for obtaining the best data. In the working curve, the content of the element to be measured is not recommended to be at the lowest end or the highest end of the working curve, but the data at the two ends do not exceed the allowable difference, only in the middle part of the working curve, the optimal data can be obtained, and the error is minimum. Therefore, the invention aims at nickel-based superalloy samples with different element contents, and proper sample mass is weighed, so that more accurate detection data is obtained, and the weighing standard is also verified in the following table. And for the nickel-based superalloy sample with the molybdenum element content of 10.0-30.0 wt% and the niobium and titanium element content of 0.1wt% -1 wt%, the invention establishes a mode of respectively weighing and carrying out sample dissolution twice, and the test is carried out in a separate-taking and testing mode, although the sample dissolution is carried out once more than the sample dissolution mode once, the detection result is more accurate, and meanwhile, compared with the prior art, the sample dissolution times are obviously saved once when one element is detected, the acid consumption is obviously reduced, the cost is reduced, and the environment protection is facilitated.
Further, the sealed pressure container is a sample dissolving bottle or a digestion tank made of polytetrafluoroethylene or PFA plastic.
Further, the determination process in the step (3) comprises: atomizing a sample solution to be detected through a hydrofluoric acid resistant atomizer and a sample introduction system, introducing the atomized sample solution into an inductively coupled plasma emission spectrometer, measuring the spectral intensity of a working curve in a sequence from low to high in mass fraction at the selected wavelength of an element to be detected, determining the sample solution when the working curve r is more than or equal to 0.9995, checking the background of spectral lines of molybdenum, niobium and titanium determining elements, performing background correction at a proper position, and calculating the mass concentration of the molybdenum, niobium and titanium determining elements;
the measurement conditions of the inductively coupled plasma emission spectrometer include: the power was 1200W, the auxiliary gas flow was 1L/min, the atomizer flow was 0.7L/min, the pump speed was 12rpm and the integration time was 10s.
Further, the mass fractions W (x) of molybdenum, niobium and titanium were calculated according to the following formula, and the values are expressed in%:
in the formula:
C 0 : the mass concentration of the working curve solution is in the unit of mu g/mL;
C 1 : the unit of the mass concentration of the sample solution to be detected is mu g/mL;
v: the total volume of the sample solution to be detected is mL;
m: mass of sample in g;
r: dilution factor.
The invention has the beneficial effects that:
1. the invention provides a closed-tank digestion-inductively coupled plasma emission spectrometry-based method for simultaneously detecting the contents of molybdenum, niobium and titanium in a nickel-based high-temperature alloy, and can achieve the effects of one-time sample dissolution and multi-element simultaneous determination. The method can quickly and accurately detect the contents of molybdenum, niobium and titanium in the nickel-based high-temperature alloy, the detection ranges are that the contents of niobium and titanium are 0.10-10.00% and the content of molybdenum is 0.10-30.0%, and meanwhile, the use amount of chemical reagents can be reduced, so that the method is more environment-friendly.
2. The invention adopts the polytetrafluoroethylene or PFA plastic material as the sealed pressure container, so that the acid for digesting the sample is not easy to volatilize into the environment, and the utilization rate of the acid can be effectively improved. Hydrofluoric acid is introduced in the digestion process, so that the digestion efficiency of the nickel-based superalloy sample can be effectively improved, indissolvable elements in the nickel-based superalloy sample can be completely digested, and the detection accuracy of each element is improved; meanwhile, the nickel-based high-temperature alloy sample is dissolved at the temperature of 80-150 ℃ by heating through an electric heating plate or a corrosion-resistant oven. The corrosion-resistant oven heating mode enables the consistency of temperatures at different positions to be excellent in the traditional electric heating plate, and the precision of data is improved. In addition, the invention prepares a working curve after dissolving the pure chromium particles (powder) and the nickel particles (powder), thereby realizing matrix matching and improving the accuracy of the method.
Detailed Description
The following description of the embodiments of the present invention is provided to facilitate the understanding of the present invention by those skilled in the art, but it should be understood that the present invention is not limited to the scope of the embodiments, and it will be apparent to those skilled in the art that various changes may be made without departing from the spirit and scope of the invention as defined and defined in the appended claims, and all matters produced by the invention using the inventive concept are protected.
Example 1
A method for detecting the content of elements in a nickel-based superalloy comprises the following steps:
(1) Making working curves
S1, preparing a matrix chromium stock solution: weighing 2.00g to 600mL of chromium particles in a glass beaker, adding secondary deionized water, then adding 40mL of high-grade pure hydrochloric acid, covering a watch glass, dissolving at 100 ℃, heating to boil for 10min after the chromium particles are completely dissolved, taking down, cooling to room temperature, diluting and fixing the volume to 100mL to obtain a matrix stock solution containing 0.02g/mL of chromium. When adding acid, the speed is moderate; the adding amount of the secondary deionized water is added according to the concentration of the matrix stock solution required to be prepared.
S2, preparing a matrix nickel stock solution: weighing 3.00g to 600mL of nickel particles in a glass beaker, adding secondary deionized water, covering a watch glass, adding 40mL of high-grade pure nitric acid to dissolve at 100 ℃, adding 5mL of high-grade pure hydrochloric acid after the nickel particles are completely dissolved, heating to boil for 20min, taking down, cooling to room temperature, diluting and fixing the volume to 100mL to obtain a matrix stock solution containing 0.03g/mL of nickel. When adding acid, the speed is moderate; when adding acid, the speed is moderate; the adding amount of the secondary deionized water is added according to the concentration of the matrix stock solution required to be prepared.
S3, preparing a working curve solution: 2.00mL of chromium matrix stock solution, 2.00mL of nickel matrix solution, 10.0mL of high-grade pure hydrochloric acid, 2.00mL of high-grade pure nitric acid and 5.00mL of high-grade pure hydrofluoric acid are respectively mixed with the standard solutions of molybdenum, niobium and titanium to obtain a working curve mixed solution. Adding the standard solutions of molybdenum, niobium and titanium in 0-7.00 mL according to a gradient manner, and referring to Table 1; wherein the concentrations of the molybdenum, niobium and titanium standard solutions are all 1000 mug/mL.
TABLE 1
S4, measuring the working curve solution by using an inductively coupled plasma emission spectrometer, wherein the measuring conditions of the inductively coupled plasma emission spectrometer comprise: the power was 1200W, the auxiliary gas flow was 1L/min, the atomizer flow was 0.7L/min, the pump speed was 12rpm and the integration time was 10s.
(2) Preparing a sample solution to be tested
Weighing a stainless steel sample to be detected, placing the stainless steel sample into a sealed pressure container, then sequentially adding 5mL of secondary deionized water, 10mL of high-grade pure hydrochloric acid, 3mL of high-grade pure nitric acid and 5mL of high-grade pure hydrofluoric acid, after the phenomenon of severe reaction stops, sealing the sealed pressure container, placing the sealed pressure container into a 120-DEG C corrosion-resistant oven, preserving heat for 2.0h, then taking out and cooling to room temperature, diluting the obtained solution, and fixing the volume to obtain a sample solution to be detected.
The nickel-based superalloy sample is weighed according to the following method:
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 0.10-1.00 wt%, the weighed sample amount is 0.15g, and the accuracy is 0.0001g;
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 1.00-7.00 wt%, the weighed sample amount is 0.1g, and the accuracy is 0.0001g;
when the contents of molybdenum and niobium elements in the nickel-based superalloy to be detected are 1.00-7.0 wt% and the content of titanium element is 0.10-1 wt%, weighing 0.10g of sample for detecting the contents of the molybdenum and niobium elements, and weighing 0.15g of sample for detecting the content of the titanium element
(3) Determination of sample solution to be tested
Atomizing a sample solution to be detected by a hydrofluoric acid resistant atomizer, introducing the atomized sample solution into an inductively coupled plasma emission spectrometer, measuring the spectral intensity of a working curve in the sequence of low-to-high mass fraction at the selected wavelength of an element to be detected, when the working curve r is more than or equal to 0.9995, determining the sample solution, checking the background of molybdenum and niobium determination element spectral lines, performing background correction at a proper position (correcting by referring to a recommended analysis line in table 2), and calculating the mass concentration of the molybdenum and niobium determination elements.
The measurement conditions of the inductively coupled plasma emission spectrometer include: the power was 1200W, the auxiliary gas flow was 1L/min, the atomizer flow was 0.7L/min, the pump speed was 12rpm and the integration time was 10s.
The mass fraction w (x) of molybdenum and niobium, expressed in%, is calculated according to the following formula:
in the formula:
C 0 : the mass concentration of the working curve solution is in the unit of mu g/mL;
C 1 : the unit of the mass concentration of the sample solution to be detected is mu g/mL;
v: the total volume of the sample solution to be detected is mL;
m: mass of sample in g;
r: and (5) the dilution times of the solutions to be tested.
TABLE 2
Example 2
The method for detecting the content of the nickel-base superalloy in the embodiment is the same as that in embodiment 1, except that the detection conditions in the steps (1) and (2) are different, and comprises the following steps:
(1) Making working curves
S1, preparing a matrix chromium stock solution: weighing 2.00g of the chromium particles to 600mL of a glass beaker, adding secondary deionized water, then adding 40mL of high-grade pure hydrochloric acid, covering a watch glass, dissolving at 100 ℃, heating to boil for 10mins after the chromium particles are completely dissolved, taking down, cooling to room temperature, diluting and fixing the volume to 100mL to obtain a matrix stock solution containing 0.02g/mL of chromium. When adding acid, the speed is moderate; the adding amount of the secondary deionized water is added according to the concentration of the matrix stock solution required to be prepared.
S2, preparing a matrix nickel stock solution: weighing 3.00g to 600mL of nickel particles in a glass beaker, adding secondary deionized water, covering a watch glass, adding 40mL of high-grade pure nitric acid to dissolve at 100 ℃, adding 5mL of high-grade pure hydrochloric acid after the nickel particles are completely dissolved, heating to boil for 20min, taking down, cooling to room temperature, diluting and fixing the volume to 100mL to obtain a matrix stock solution containing 0.03g/mL of nickel. When adding acid, the speed is moderate; when adding acid, the speed is moderate; the addition amount of the secondary deionized water is added according to the concentration of the matrix stock solution required to be prepared.
S3, preparing a working curve solution: 2.00mL of chromium matrix stock solution, 2.00mL of nickel matrix solution, 10.0mL of high-grade pure hydrochloric acid, 2.00mL of high-grade pure nitric acid and 5.00mL of high-grade pure hydrofluoric acid are mixed with the standard solutions of molybdenum and niobium respectively to obtain a working curve mixed solution. Adding the standard solutions of molybdenum and niobium in 0-10.00 mL according to gradient, and showing in Table 3; wherein the concentration of the molybdenum standard solution and the niobium standard solution is 1000 mug/mL.
TABLE 3
And S4, measuring the solution of the sample to be measured by using an inductively coupled plasma emission spectrometer to obtain the contents of molybdenum and niobium in the nickel-based superalloy sample to be measured. The measurement conditions of the inductively coupled plasma emission spectrometer include: the power was 1200W, the auxiliary gas flow was 1L/min, the atomizer flow was 0.7L/min, the pump speed was 12rpm and the integration time was 10s.
(2) Preparing a sample solution to be tested
Weighing a nickel-based superalloy sample to be detected, placing the nickel-based superalloy sample into a sealed pressure container, then sequentially adding 5mL of secondary deionized water, 15mL of high-grade pure hydrochloric acid, 0.5mL of high-grade pure nitric acid and 5mL of high-grade pure hydrofluoric acid, after the phenomenon of violent reaction stops, sealing the sealed pressure container, placing the sealed pressure container into a 120-DEG C corrosion-resistant oven, preserving heat for 4 hours, then taking out and cooling to room temperature, diluting the obtained solution, and fixing the volume to obtain a sample solution to be detected.
The nickel-based superalloy sample is weighed according to the following method:
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 1.00-7.00 wt%, the weighed sample amount is 0.1g, and the accuracy is 0.0001g;
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 7.00-10.0 wt%, the weighed sample amount is 0.08g, and the accuracy is 0.0001g.
Example 3
The method for detecting the content of the elements in the nickel-base superalloy of the present embodiment is the same as that of embodiment 1, except that the detection conditions in the steps (1) and (2) are different, and the method for detecting the content of the elements in the nickel-base superalloy of the present embodiment includes:
(1) Making working curves
S1, preparing a matrix nickel stock solution: weighing 3.00g to 600mL of nickel particles in a glass beaker, adding secondary deionized water, covering a watch glass, adding 40mL of high-grade pure nitric acid to dissolve at 100 ℃, adding 5mL of high-grade pure hydrochloric acid after the nickel particles are completely dissolved, heating to boil for 20min, taking down, cooling to room temperature, diluting and fixing the volume to 100mL to obtain a matrix stock solution containing 0.03g/mL of nickel. When adding acid, the speed is moderate; when adding acid, the speed is moderate; the adding amount of the secondary deionized water is added according to the concentration of the matrix stock solution required to be prepared.
S2, preparing a working curve solution: 2.5mL of nickel matrix solution, 2.00mL of super-pure hydrochloric acid, 10.00mL of super-pure nitric acid and 5.00mL of super-pure hydrofluoric acid are respectively mixed with the standard solutions of molybdenum and titanium to obtain a working curve mixed solution. Adding the standard solutions of molybdenum and titanium in a gradient manner within 0-10.00 mL respectively, and the contents are shown in Table 4; wherein the concentration of the molybdenum standard solution and the titanium standard solution is 1000 mu g/mL.
TABLE 4
(2) Preparing a sample solution to be tested
Weighing a nickel-based superalloy sample to be detected, placing the nickel-based superalloy sample into a sealed pressure container, then sequentially adding 5mL of secondary deionized water, 3mL of superior pure hydrochloric acid, 10mL of superior pure nitric acid and 5mL of superior pure hydrofluoric acid, after the phenomenon of severe reaction stops, sealing the sealed pressure container, placing the sealed pressure container into a corrosion-resistant oven at 100 ℃ for heat preservation for 5 hours, then taking out and cooling to room temperature, diluting the obtained solution and fixing the volume to obtain a titanium element sample solution to be detected. And (3) transferring 20mL of the solution to be tested containing the titanium element to a 100mL plastic volumetric flask, continuously adding 2mL of high-grade pure hydrochloric acid, 7mL of high-grade pure nitric acid and 4mL of high-grade pure hydrofluoric acid, diluting the obtained solution and fixing the volume to obtain the solution of the sample to be tested containing the molybdenum element.
Working curves were established and a sample solution to be measured was prepared according to the above-described steps (1) and (2) of this example. The selected sample solution to be tested was tested according to the requirements described in example 1 above, and the results of the tests for the tested nickel-base superalloys are shown in tables 5, 6 and 7 below.
TABLE 5
TABLE 6
TABLE 7
As can be seen from tables 5, 6 and 7, the contents of the elements determined by the detection method are almost consistent with the reference values, and the actual detection error is far lower than the allowable error, so that the detection method can be used for rapidly and accurately determining the contents of molybdenum, niobium and titanium in the nickel-based superalloy, has a wide detection range, and can realize accurate detection within the method range.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The method for detecting the element content in the nickel-based superalloy is characterized by comprising the following steps:
(1) Respectively weighing metal chromium and nickel with the purity of more than or equal to 99.99wt%, and dissolving the metal chromium and nickel with acid liquor to obtain chromium matrix stock solution and nickel matrix stock solution;
(2) Mixing the chromium matrix stock solution, the nickel matrix stock solution and the acid solution, then respectively mixing the mixed solutions with the standard solutions of molybdenum, niobium and titanium to prepare mixed solutions of working curves of molybdenum, niobium and titanium, and respectively preparing the working curves of molybdenum, niobium and titanium based on the mixed solutions of the working curves;
(3) Dissolving a nickel-based superalloy sample to be detected, then measuring the nickel-based superalloy sample, and calculating the contents of molybdenum, niobium and titanium in the nickel-based superalloy sample according to a working curve, wherein the calculation formula is as follows:
wherein, C 0 The mass concentration of the solution is the working curve, and the unit is mu g/mL; c 1 The unit is the mass concentration of the sample solution to be detected, and the unit is mu g/mL; v is the total volume of the sample solution to be detected, and the unit is mL; m is the mass of the sample, and is expressed in g, and R is the dilution factor.
2. The detection method according to claim 1, wherein the specific processes for preparing the chromium matrix stock solution and the nickel matrix stock solution are as follows:
s1, weighing 1.00-4.00 g of chromium particles or chromium powder, adding secondary deionized water, then adding 20-80 mL of pure hydrochloric acid, dissolving at 80-100 ℃, heating to boil and keeping for 10-20 min after complete dissolution, cooling to room temperature, diluting and fixing the volume to obtain chromium matrix stock solution containing 0.02g/mL of chromium;
s2, weighing 3.00-8.00 g of nickel particles or nickel powder, adding secondary deionized water, then adding 20-80 mL of pure nitric acid, dissolving at 80-100 ℃, adding 5-10 mL of hydrochloric acid after complete dissolution, heating to boil and keeping for 10-20 min, cooling to room temperature, diluting and fixing the volume to obtain nickel matrix stock solution containing 0.03g/mL of nickel.
3. The method for detecting the content of the elements in the nickel-base superalloy as claimed in claim 1, wherein the process for preparing the working curve solution is as follows:
mixing a chromium matrix stock solution, a nickel matrix stock solution, pure hydrochloric acid, pure nitric acid and pure hydrofluoric acid according to the volume ratio of 0.5-1:1-2:5-10 and then mixing the mixture with a standard solution of molybdenum, niobium and titanium respectively to obtain a working curve mixed solution, wherein the volume ratio of the chromium matrix stock solution to the nickel matrix stock solution to the pure nitric acid to the pure hydrofluoric acid is 1.5-3:3-5;
wherein the standard solutions of molybdenum, niobium and titanium are added in a gradient manner within 0-10.00 mL respectively; the concentrations of the molybdenum, niobium and titanium standard solutions were all 1000. Mu.g/mL.
4. The method for detecting the element content in the nickel-base superalloy according to claim 3, wherein the volume ratio of the chromium-base stock solution to the nickel-base stock solution to the pure hydrochloric acid to the pure nitric acid to the pure hydrofluoric acid is 1.
5. The method for detecting the content of the elements in the nickel-based superalloy according to claim 1, wherein a sample of the nickel-based superalloy to be detected is dissolved to prepare a sample solution to be detected, and a specific preparation process is as follows:
weighing a nickel-based superalloy sample to be detected, placing the nickel-based superalloy sample into a sealed pressure container, sequentially adding 1-10 mL of secondary deionized water, 1-20 mL of pure hydrochloric acid, 0.3-5 mL of pure nitric acid and 1-5 mL of pure hydrofluoric acid, covering and screwing the sealed pressure container tightly after the phenomenon of violent reaction stops, sealing the sealed pressure container, placing the sealed pressure container into an electric heating plate or a corrosion-resistant oven at the temperature of 80-150 ℃, preserving heat for 0.5-6 h, taking out and cooling to room temperature, diluting the obtained solution, and fixing the volume in a 100mL plastic volumetric flask to obtain a sample solution to be detected.
6. The method for detecting the content of the elements in the nickel-base superalloy according to claim 5, wherein the sealed pressure vessel is a sample dissolving bottle or a digestion tank made of polytetrafluoroethylene or PFA plastic.
7. The method for detecting the content of the elements in the nickel-base superalloy as claimed in claim 1, wherein the sample of the nickel-base superalloy is weighed as follows:
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 0.1wt% -1 wt%, the weighed sample amount is 0.15g, and the accuracy is 0.0001g;
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 1wt% -7 wt%, the weighed sample amount is 0.1g, and the accuracy is 0.0001g;
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 7wt% -10 wt%, the weighed sample amount is 0.08g, and the accuracy is 0.0001g;
when the content of the element to be detected in the nickel-based superalloy sample to be detected is 10wt% -30 wt%, the weighed sample amount is 0.1g, and the accuracy is 0.0001g;
when the content of the molybdenum element in the nickel-based superalloy to be detected is more than 10wt% and the content of the niobium and titanium elements is 0.1wt% -10 wt%, 0.10g of a sample is weighed to detect the content of the molybdenum element, and 0.08-0.15 g of the sample is weighed to detect the niobium and titanium.
8. The method for detecting the content of elements in the nickel-base superalloy according to any of claims 1 to 7, wherein the determination in step (3) is as follows:
atomizing a sample solution to be detected through a hydrofluoric acid resistant atomizer and a sample introduction system, introducing the atomized sample solution into an inductively coupled plasma emission spectrometer, measuring the spectral intensity of a working curve in the sequence from low to high according to mass fraction at the selected wavelength of an element to be detected, determining the sample solution when the working curve r is more than or equal to 0.9995, checking the background of spectral lines of molybdenum, niobium and titanium determining elements, correcting the background, and calculating the mass concentration of the molybdenum, niobium and titanium determining elements according to a formula;
the measuring conditions of the inductively coupled plasma emission spectrometer comprise: the power was 1200W, the auxiliary gas flow was 1L/min, the atomizer flow was 0.7L/min, the pump speed was 12rpm and the integration time was 10s.
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