Method for measuring non-destructive corrosion component content of tulip contact copper wafer

Abstract

The invention relates to a method for measuring the non-destructive corrosion component content of a tulip contact copper wafer, which comprises the following steps of: respectively detecting the mass gain quantity before and after corrosion of a tulip contact copper wafer sample in a high-voltage switch cabinet and the energy spectrum of a corrosion product, and then testing the energy spectrum of the corrosion product to obtain the mass of carbon and hydrogen elements; and calculating the verdigris mass in the corrosive based on the mass ratio of the elements in the molecular formula so as to obtain the verdigris reaction loss and the verdigris reaction mass gain, obtaining the mass gain of the oxidation reaction and the copper loss of the oxidation reaction by combining the mass gain before and after corrosion, and finally obtaining the copper oxide content in the corrosive. The corrosion component content can be accurately calculated, and a theoretical basis is provided for operation state evaluation of the tulip contact.

Description

Technical Field

[0001] The invention relates to a technology in the field of chemical detection, in particular to a method for measuring the content of non-destructive corrosion components of copper contact pieces of plum blossom contacts in a high-voltage switch cabinet. Background Art

[0002] When measuring the content of corrosion components in the copper contact of the existing switch cabinet plum blossom contact, a simple and efficient weight method is often used to test, and the degree of corrosion of the material is evaluated by measuring the mass difference of the metal sample exposed to the atmospheric environment before and after the test. Since the composition of the corrosion product is complex and often not a single product (mainly copper green Cu2(OH)2CO3 and copper oxide CuO), the traditional simplified mass difference analysis before and after the test cannot accurately grasp the corrosion state of the sample, especially the content and specific gravity of the corrosion product cannot be determined, which is not conducive to the analysis of the corrosion analysis of the plum blossom contact in the actual switch cabinet. Summary of the invention

[0003] In view of the above-mentioned deficiencies in the prior art, the present invention proposes a method for measuring the content of non-destructive corrosion components in the copper contact piece of a plum blossom contact. By accurately measuring the mass gain of corrosion products and the content of characteristic elements of corrosion products, the contents of corrosion products such as verdigris Cu2(OH)2CO3 and copper oxide CuO are calculated respectively, thereby achieving accurate calculation of the content of corrosion components and providing a theoretical basis for evaluating the operating status of the plum blossom contact.

[0004] The present invention is achieved through the following technical solutions:

[0005] The present invention relates to a method for measuring the content of non-destructive corrosion components in a copper contact piece of a plum blossom contact, comprising:

[0006] Step 1) Detect the mass gain Δm of the plum blossom contact copper contact sample before and after corrosion 总 and the energy spectrum of the corrosion products, specifically: after the plum blossom contact piece in the switch cabinet is removed, it is placed in a vacuum oven as the initial copper contact piece for drying and then its mass and energy spectrum are recorded; then the plum blossom contact is put into normal operation, and its mass and energy spectrum are collected in the same way during the operation and maintenance of the switch cabinet, and the mass gain Δm is obtained. 总 .

[0007] The drying process is as follows: the drying temperature is 70° C. and the duration is 5 hours.

[0008] The mass mentioned above is measured using a precision balance.

[0009] The energy spectrum is measured by an X-ray photoelectron spectrometer.

[0010] Step 2) Select the characteristic elements of copper green corrosion products, carbon C and hydrogen H, and obtain the content m of the two elements through the energy spectrum test of the corrosion products. C and m H , and based on the mass ratio k of the elements in the molecular formula C and k H , calculate the copper green content m in the corrosion product 铜绿 .

[0011] The chemical reaction equation of the copper green reaction is: 2Cu+H2O+CO2+O2=Cu2(OH)2CO3.

[0012] Step 3) Based on the copper content m 铜绿 Calculate the copper green reaction loss m 铜绿铜耗 and the mass gain of the copper green reaction Δm 铜绿反应 , combined with the mass gain Δm before and after corrosion 总 , calculate the mass gain of the oxidation reaction Δm 氧化反应 , and then calculate the copper consumption of oxidation reaction m 氧化铜铜耗 , and finally the copper oxide content m in the corrosion product is obtained 氧化铜 .

[0013] The chemical reaction equation of the oxidation reaction is: 2Cu+O2=2CuO. Technical Effects

[0014] The present invention calculates the content of corrosion products respectively to determine the specific conversion coefficient, thereby realizing the accurate calculation of the corrosion rate, and then realizing the content of characteristic elements (copper) in the corrosion products through chemical analysis methods such as spectral analysis, mass spectrometry, atomic absorption spectroscopy and other technologies.

[0015] Compared with the existing corrosion product analysis methods, the present invention can provide higher precision results, ensure accurate calculation of the corrosion product content, and monitor and analyze the corrosion process in real time without the need for complex sample collection processes, thereby improving the real-time assessment of the corrosion degree of the copper contact of the plum blossom contact. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a flow chart of the present invention.

[0017] Figure 2 is the schematic diagram of the measurement system;

[0018] In the figure: 1 sample, 2 X-ray source, 3 vacuum chamber, 4 filter, 5 ion gun, 6 electron energy analyzer, 7 electron multiplier, 8 first data acquisition card, 9 weighing sensor, 10 measurement circuit, 11 second data acquisition card, 12 control unit;

[0019] Figure 3 Spectra of different element contents in the examples. DETAILED DESCRIPTION

[0020] like Figure 1 As shown, this embodiment relates to a method for measuring the corrosion component content of copper contact pieces of plum blossom contacts in a high-voltage switch cabinet, which specifically includes:

[0021] Step 1) Use a precision balance to measure the mass gain Δm of the plum blossom contact copper contact sample before and after commissioning 总 , the energy spectrum of corrosion products is measured by the detection system, including:

[0022] 1.1) Use a precision balance to obtain the mass of the plum blossom contact copper contact sample before and after corrosion: the difference Δm after processing the data obtained from two measurements by a precision balance 总 is the total mass gain of copper contact corrosion, which satisfies: Δm 总 =Δm 铜绿反应 +Δm 氧化反应 , where: Δm 铜绿反应 and Δm 氧化反应 They are the mass gains of the copper contact sample after patina reaction and oxidation reaction, respectively.

[0023] 1.2) The energy spectrum of corrosion products is measured by the detection system: the electrons inside the atoms escape after being irradiated by the X-ray source to the surface area, and then pass through the filter and ion gun to reduce the photon energy dispersion and clean the sample surface and achieve depth analysis. After that, the energy distribution of the electrons emitted from the sample is measured by the electron energy analyzer, and after being converted into electrical signals and amplified by the electron multiplier, the data is collected and recorded by the data acquisition card, so as to determine the energy spectrum of the corrosion products, that is, the content spectrum of different elements, such as Figure 3 shown.

[0024] like Figure 2 As shown, the detection system comprises: a weighing sensor 9 connected to the test sample 1 in sequence, a measuring circuit 10, a second data acquisition card 11, a control unit 12, and an X-ray source 2, an ion gun 5 and an electron energy analyzer 6 respectively arranged in an independent vacuum chamber 3, wherein: the X-ray source 2 faces the test sample 1 in the high-voltage switch cabinet, and the output end of the electron energy analyzer 6 is connected to the control unit 12 through an electron multiplier 7 and a first data acquisition card 8.

[0025] Step 2) Select the characteristic elements C and H of the copper green reaction corrosion product, and obtain the content m of the two elements through the energy spectrum test of the corrosion product. C and m H , and based on the mass ratio k of the elements in the molecular formula C and k H , calculate the copper green content m in the corrosion product 铜绿Specifically, the contents of the two elements m are obtained according to the phase analysis results of the photoelectron spectrometer. C and m H , respectively combined with their mass ratio k in the molecular formula C and k H Calculate the quality of the patina Among them: the mass ratio of C and H elements in Cu2(OH)2CO3 is: M r铜绿 is the relative molecular mass of copper green, A rCu is the relative atomic mass of copper, A RC and A rH is the relative atomic mass of C and H. Therefore, the mass gain of the copper green reaction can be calculated according to the content of the selected elements, and the mass gain of the oxidation reaction can be obtained by combining the total mass gain. Considering the influence of the H element in the water molecule, the mass gain of the copper green reaction calculated according to the two characteristic elements is m 铜绿C and m 铜绿H m 铜绿C If the error between the two is not less than 1%, further dehydration and drying are required before the above operation; if the error between the two is less than 1%, the average value is taken as the mass gain of the copper green reaction.

[0026] The error is judged by

[0027] The mass gain of the aeruginous reaction

[0028] Step 3) Based on the copper content m 铜绿 Calculate the copper green reaction loss m 铜绿铜耗 and the mass gain of the copper green reaction Δm 铜绿反应 , combined with the mass gain Δm before and after corrosion 总 Calculate the mass gain of the oxidation reaction Δm 氧化反应 , and then calculate the copper consumption of oxidation reaction m 氧化铜铜耗 , and finally the copper oxide content m in the corrosion product is obtained 氧化铜 , that is, the content of corrosion components in the copper contact, specifically: copper green reaction loss Verdigris reaction mass gain Among them: A rCu is the relative atomic mass of copper. The mass gain of the oxidation reaction Δm 氧化反应 =Δm 总 -Δm 铜绿反应 , and then the copper consumption of oxidation reaction can be calculated and the copper oxide content in the corrosion products Where: M r氧化铜 is the relative molecular mass of copper oxide.

[0029] After a specific actual experiment, the copper contact was placed in an environment with a temperature of 25°C and a relative humidity of 90% and exposed for 6 hours. Then, the copper contact after corrosion was measured using a precision balance and an X-ray photoelectron spectrometer according to the above steps. According to the method for measuring the content of corrosion components of the present invention, the experimental data that can be obtained are:

[0030] Step 1) using a precision balance and an X-ray photoelectron spectrometer, respectively measuring the mass gain Δm of the copper contact piece sample of the plum blossom contact before and after commissioning and the energy spectrum of the corrosion products, including:

[0031] 1.1 Precision balance measurement: mass before corrosion (m0) = 13.64g, mass after corrosion (m1) = 13.8415g, Δm 总 =m1-m0=0.01g;

[0032] 1.2 Corrosion product spectrum measurement: element wt% C 0.149 H 0.025

[0033] Step 2) Select characteristic elements of the corrosion products of the copper green reaction, obtain the contents of the two elements through the energy spectrum test of the corrosion products, and calculate the copper green content in the corrosion products based on the mass ratio of the elements in the molecular formula, including:

[0034] 2.1 Calculation of the mass of the corrosion products of copper green reaction: Through the energy spectrum test of the corrosion products, the values ​​of the two element contents are obtained as m C = 0.02032g and m H =0.00341g, from which the copper green mass is calculated:

[0035] 2.2 Calculation error criteria and patina quality: According to the above calculation results, the error between the two is: Therefore, the mass of the copper green generated by the copper green reaction is:

[0036] Step 3) based on the copper green content, the copper green reaction loss and the copper green reaction mass gain are calculated, and the mass gain of the oxidation reaction is calculated by combining the total mass gain before and after corrosion, and then the copper loss of the oxidation reaction is calculated to obtain the copper oxide content in the corroded product, including:

[0037] 3.1 Calculation of the mass gain of the copper green reaction: According to the above calculation results, the copper green reaction loss From this, the mass gain of the copper green reaction can be calculated as:

[0038] 3.2 Calculation of the mass gain of the oxidation reaction and the mass of the corrosion products of the oxidation reaction: According to the above calculation results, the mass gain of the oxidation reaction is: Δm 氧化反应 =Δm总 -Δm 铜绿反应 =0.04177g, the copper consumption of oxidation reaction is: Therefore, the mass of copper oxide generated by the oxidation reaction is:

[0039] Compared with the prior art, the present invention can more accurately determine the corrosion of copper contacts and the composition of corrosion products by measuring the mass gain and the energy spectrum of corrosion products, thereby improving the accuracy of performance indicators. The present invention can collect data during the normal operation of the equipment and realize the measurement of real-time corrosion components. This helps to find problems in time and take necessary maintenance measures, thereby improving the reliability and safety of the equipment; in addition, the present invention ensures the normal operation of the equipment through a non-destructive detection process, reducing maintenance costs and downtime.

[0040] The above-mentioned specific implementation can be partially adjusted in different ways by those skilled in the art without departing from the principle and purpose of the present invention. The protection scope of the present invention shall be based on the claims and shall not be limited by the above-mentioned specific implementation. Each implementation scheme within its scope shall be subject to the constraints of the present invention.

Claims

1. A method for measuring the content of non-destructive corrosion components in copper contact pieces of plum blossom contacts, characterized in that: By detecting the mass gain of the copper contact piece sample of the plum blossom contact in the high-voltage switch cabinet before and after corrosion and the energy spectrum of the corrosion product, the mass of carbon and hydrogen elements was obtained through the energy spectrum test of the corrosion product, and the mass of the verdigris in the corrosion product was calculated based on the mass ratio of the elements in the molecular formula, and then the verdigris reaction loss and the verdigris reaction mass gain were obtained. Combined with the mass gain before and after corrosion, the mass gain of the oxidation reaction and the copper loss of the oxidation reaction were obtained, and finally the copper oxide content in the corrosion product was obtained.

2. The measuring method according to claim 1, characterized in that include: Step 1) Detect the mass gain Δm of the plum blossom contact copper contact sample before and after corrosion 总 and the energy spectrum of the corrosion products, specifically: after the plum blossom contact piece in the switch cabinet is removed, it is placed in a vacuum oven as the initial copper contact piece for drying and then its mass and energy spectrum are recorded; then the plum blossom contact is put into normal operation, and its mass and energy spectrum are collected in the same way during the operation and maintenance of the switch cabinet, and the mass gain Δm is obtained. 总 . Step 2) Select the characteristic elements of copper green corrosion products, carbon C and hydrogen H, and obtain the content m of the two elements through the energy spectrum test of the corrosion products. C and m H , and based on the mass ratio k of the elements in the molecular formula C and k H , calculate the copper green content m in the corrosion product 铜绿 ; Step 3) Based on the copper content m 铜绿 Calculate the copper green reaction loss m 铜绿铜耗 and the mass gain of the copper green reaction Δm 铜绿反应 , combined with the mass gain Δm before and after corrosion 总 , calculate the mass gain of the oxidation reaction Δm 氧化反应 , and then calculate the copper consumption of oxidation reaction m 氧化铜铜耗 , and finally the copper oxide content m in the corrosion product is obtained 氧化铜 .

3. The measuring method according to claim 2, characterized in that: The drying process is as follows: the drying temperature is 70° C. and the duration is 5 hours.

4. The measuring method according to claim 2, characterized in that: The mass is measured by a precision balance; the energy spectrum is measured by an X-ray photoelectron spectrometer.

5. The measuring method according to any one of claims 1 to 4, characterized in that include: Step 1) Use a precision balance to measure the mass gain Δm of the plum blossom contact copper contact sample before and after commissioning 总 , the energy spectrum of corrosion products is measured by the detection system, including: 1.1) Use a precision balance to obtain the mass of the plum blossom contact copper contact sample before and after corrosion: the difference Δm after processing the data obtained from two measurements by a precision balance 总 is the total mass gain of copper contact corrosion, which satisfies: Δm 总 =Δm 铜绿反应 +Δm 氧化反应 , where: Δm 铜绿反应 and Δm 氧化反应 are the mass gains of the copper contact sample after patina reaction and oxidation reaction respectively; 1.2) The energy spectrum of the corrosion product is measured by the detection system: the electrons inside the atom escape after being irradiated by the X-ray source to the surface area, and are irradiated by the filter and ion gun respectively. The energy distribution of the electrons emitted from the sample is measured by the electron energy analyzer, and after being converted into electrical signals and amplified by the electron multiplier, the data is collected and recorded by the data acquisition card, thereby determining the energy spectrum of the corrosion product, that is, the content spectrum of different elements; Step 2) Select the characteristic elements C and H of the copper green reaction corrosion product, and obtain the content m of the two elements respectively through the energy spectrum test of the corrosion product C and m H , and based on the mass ratio k of the elements in the molecular formula C and k H , calculate the copper green content m in the corrosion product 铜绿 Specifically, the contents of the two elements m are obtained according to the phase analysis results of the photoelectron spectrometer. C and m H , respectively combined with their mass ratio k in the molecular formula C and k H Calculate the quality of the patina Among them: the mass ratio of C and H elements in Cu2(OH)2CO3 is: M r铜绿 is the relative molecular mass of copper green, A rCu is the relative atomic mass of copper, A RC and A rH is the relative atomic mass of C and H elements. The mass gain of the copper green reaction is calculated according to the content of the selected elements. The mass gain of the oxidation reaction is obtained by combining the total mass gain. The mass gain of the copper green reaction calculated according to the two characteristic elements is m 铜绿C and m 铜绿H m 铜绿C As a benchmark, the mass gain of the copper green reaction Step 3) Based on the copper content m 铜绿 Calculate the copper green reaction loss m 铜绿铜耗 and the mass gain of the copper green reaction Δm 铜绿反应 , combined with the mass gain Δm before and after corrosion 总 Calculate the mass gain of the oxidation reaction Δm 氧化反应 , and then calculate the copper consumption of oxidation reaction m 氧化铜铜耗 , and finally the copper oxide content m in the corrosion product is obtained 氧化铜 , that is, the content of corrosion components in the copper contact, specifically: copper green reaction loss Verdigris reaction mass gain Among them: A rCu is the relative atomic mass of copper; the mass gain of the oxidation reaction Δm 氧化反应 =Δm 总 -Δm 铜绿反应 , and then the copper consumption of oxidation reaction can be calculated and the copper oxide content in the corrosion products Where: M r氧化铜 is the relative molecular mass of copper oxide.

6. The measuring method according to claim 5, characterized in that: When the two characteristic elements calculate the copper green reaction mass gain m 铜绿C and m 铜绿H If the error of the two is not less than 1%, the above operation is performed after further dehydration and drying; if the error of the two is less than 1%, the average value is taken as the mass gain of the copper green reaction; The error is judged by 7. The measuring method according to claim 5, characterized in that: The detection system comprises: a weighing sensor connected to the sample to be tested in sequence, a measuring circuit, a second data acquisition card, a control unit, and an X-ray source, an ion gun and an electron energy analyzer respectively arranged in an independent vacuum chamber, wherein: the X-ray source faces the sample to be tested in the high-voltage switch cabinet, and the output end of the electron energy analyzer is connected to the control unit through an electron multiplier and a first data acquisition card.

Images