CN115807257A - Dynamic monitoring method for micro-arc ceramic oxidation electroplating process - Google Patents
Dynamic monitoring method for micro-arc ceramic oxidation electroplating process Download PDFInfo
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Abstract
The invention discloses a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process, which comprises the following steps: 1) Sampling the micro-arc ceramic oxidation tank liquid in real time to obtain a solution to be detected; 2) Ionizing the molecules of the solution to be detected by using an ion source, converging the obtained ions into ion beams, and inputting the ion beams into a high-resolution mass spectrometer; 3) Carrying out mass analysis on the ion beam by using a built-in mass analyzer to obtain characteristic ions and mass-to-charge ratios of components of the micro-arc ceramic oxidation bath solution in the solution to be detected, and inputting the characteristic ions and the mass-to-charge ratios into a dynamic monitoring module in the electroplating process; 4) And the dynamic electroplating process monitoring module inputs the characteristic ions and the mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution in the solution to be detected into the dynamic electroplating process monitoring model to obtain the real-time concentration of each component of the micro-arc ceramic oxidation bath solution. The micro-arc ceramic oxidation electroplating process is dynamically monitored, and technical support is provided for the micro-arc ceramic oxidation production process.
Description
Technical Field
The invention relates to the field of monitoring of an electroplating process, in particular to a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process.
Background
Aluminum and its alloys are widely used in aerospace, aviation and other civil and military industries because of their light weight, but have the disadvantages of low surface hardness and no wear resistance. Micro-arc oxidation is a new ceramic treatment technology for the surface of a material, and is a new technology for growing ceramic membranes on the surfaces of nonferrous metals such as Al, mg, ti and the like in situ, which is developed on the basis of the traditional anodic oxidation. After micro-arc oxidation treatment, a layer of crystalline or amorphous Al with large thickness, high hardness and high insulation resistance can be generated on the surface of the material 2 O 3 A ceramic membrane. The film has good wear resistance, corrosion resistance, high temperature impact resistance and thermal stability, and the comprehensive performance is obviously superior to that of the traditional anodic oxide film, so the film has wide application prospect in the industrial fields of aviation, aerospace, automobiles, machinery, light industry and the like.
Because the superiority of the ceramic film performance is closely related to the quality in the electroplating process, in order to obtain the ceramic film with superior performance, the micro-arc ceramic oxidation electroplating process needs to be monitored in real time, and then the electroplating quality is strictly controlled. However, the prior art does not have a means for effectively monitoring the quality change in the micro-arc ceramic oxidation electroplating process.
Therefore, a method for comprehensively controlling the variables and the influencing factors of the factors in the micro-arc ceramic oxidation electroplating process and further controlling the quality of the micro-arc ceramic oxidation electroplating process is needed.
Disclosure of Invention
The invention aims to provide a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process, which comprises the following steps:
1) Sampling micro-arc ceramic oxidation bath solution in the micro-arc ceramic oxidation electroplating process in real time, and performing pretreatment to obtain solution to be detected;
2) Ionizing the molecules of the solution to be detected by using an ion source, and inputting particles obtained by ionization into a high-resolution mass spectrometer;
3) The high-resolution mass spectrometer performs mass analysis on the ion beam by using a built-in mass analyzer to obtain characteristic ions and mass-to-charge ratios thereof of components of the micro-arc ceramic oxidation bath solution in the solution to be detected, and inputs the characteristic ions and the mass-to-charge ratios into an electroplating process dynamic monitoring module in which an electroplating process dynamic monitoring model is stored;
4) The dynamic electroplating process monitoring module inputs characteristic ions and mass-to-charge ratios of components of the micro-arc ceramic oxidation bath solution in the solution to be detected into the dynamic electroplating process monitoring model to obtain real-time concentrations of the components of the micro-arc ceramic oxidation bath solution so as to reflect the real-time state of the micro-arc ceramic oxidation electroplating process.
Further, the pretreatment includes filtration and dilution.
Further, when diluting the micro-arc ceramic oxidation bath solution, dissolving the micro-arc ceramic oxidation bath solution in a sodium hydroxide or potassium hydroxide solution.
Further, the ion source comprises an electrospray ionization source.
Further, the built-in mass analyzer of the high resolution mass spectrometer comprises a time-of-flight mass analyzer, an electrostatic field orbitrap mass analyzer and a Fourier transform ion cyclotron resonance mass analyzer.
Further, the micro-arc ceramic oxidation bath solution comprises sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate.
Further, the characteristic ion of sodium hexametaphosphate comprises a hexametaphosphate ion P 6 O 18 6- ；
The characteristic ions of the sodium metavanadate comprise metavanadate radical ions VO 3 - ；
The characteristic ion of the sodium molybdate comprises molybdate ion HMoO 4 - ；
The characteristic ions of sodium tungstate comprise tungstate radical ions HWO 4 - ；
The characteristic ions of the sodium silicate comprise silicate ions HSiO 3 - 。
Further, the dynamic monitoring model of the electroplating process stores the linear relation between the characteristic ion mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution and the real-time concentration of each component of the micro-arc ceramic metaphosphate oxidation bath solution.
Further, the linear relationship between the characteristic ion mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution and the real-time concentration of each component of the micro-arc ceramic metaphosphate oxidation bath solution is as follows:
y1＝617.62x1+7150； (1)
y2＝3862x2+39540； (2)
y3＝806.62x3+2750.3； (3)
y4＝596.27x4+4537.4； (4)
y5＝995.4x5+27247； (5)
in the formula, y1, y2, y3, y4 and y5 respectively represent the mass-to-charge ratios of characteristic ions of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate; x1, x2, x3, x4 and x5 respectively represent the real-time concentration of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate in the micro-arc ceramic oxidation bath solution of metaphosphoric acid.
The method has the advantages that the method does not doubt explore the migration and conversion rules of various substance components in the micro-arc ceramic oxidation electroplating process, further dynamically monitors the micro-arc ceramic oxidation electroplating process, and provides technical support for the micro-arc ceramic oxidation production process.
The method can carry out qualitative and quantitative analysis on the substances of each component used in the micro-arc ceramic oxidation electroplating process without separating the components of each substance, and has the advantages of simple operation, short analysis time, convenience and rapidness.
The method has important significance for monitoring the quality of the micro-arc ceramic oxidation process.
Drawings
FIG. 1 shows Na 6 P 6 O 18 ESI-mode mass spectrum and characteristic ion of the ion beam;
FIG. 2 shows NaVO 3 ESI-mode mass spectrum and characteristic ion of the ion beam;
FIG. 3 is Na 2 MoO 4 ESI-mode mass spectrum and characteristic ion of the ion;
FIG. 4 shows Na 2 WO 4 ESI-mode mass spectrum and characteristic ion of the ion beam;
FIG. 5 shows Na 2 SiO 3 ESI-mode mass spectrum and characteristic ion of the ion;
FIG. 6 shows Na 6 P 6 O 18 A standard curve of (a);
FIG. 7 shows NaVO 3 A standard curve of (a);
FIG. 8 shows Na 2 MoO 4 A standard curve of (a);
FIG. 9 shows Na 2 WO 4 The standard curve of (2);
FIG. 10 shows Na 2 SiO 3 The standard curve of (2).
Detailed Description
The present invention is further illustrated by the following examples, but it should not be construed that the scope of the above-described subject matter is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.
Example 1:
referring to fig. 1 to 10, a dynamic monitoring method for micro-arc ceramic oxidation electroplating process includes the following steps:
1) Sampling micro-arc ceramic oxidation bath solution in the micro-arc ceramic oxidation electroplating process in real time, and performing pretreatment to obtain solution to be detected;
2) Ionizing the molecules of the solution to be detected by using an ion source to obtain a plurality of ions, converging the obtained ions into ion beams, and inputting the ion beams into a high-resolution mass spectrometer;
3) The high-resolution mass spectrometer performs mass analysis on the ion beam by using a built-in mass analyzer to obtain characteristic ions and mass-to-charge ratios thereof of components of the micro-arc ceramic oxidation bath solution in the solution to be detected, and inputs the characteristic ions and the mass-to-charge ratios into an electroplating process dynamic monitoring module in which an electroplating process dynamic monitoring model is stored;
4) The dynamic monitoring module for the electroplating process inputs characteristic ions and mass-to-charge ratios of all components of the micro-arc ceramic oxidation bath solution in the solution to be detected into the dynamic monitoring model for the electroplating process to obtain the real-time concentration of all components of the micro-arc ceramic oxidation bath solution so as to reflect the real-time state of the micro-arc ceramic oxidation electroplating process.
The pretreatment comprises filtration and dilution.
When the micro-arc ceramic oxidation tank liquid is diluted, the micro-arc ceramic oxidation tank liquid is dissolved in a sodium hydroxide or potassium hydroxide solution.
The ion source comprises an electrospray ionization source.
The built-in mass analyzer of the high-resolution mass spectrometer comprises a time-of-flight mass analyzer, an electrostatic field orbitrap mass analyzer and a Fourier transform ion cyclotron resonance mass analyzer.
The micro-arc ceramic oxidation bath solution comprises the components of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate.
The characteristic ion of sodium hexametaphosphate comprises hexametaphosphate ion P 6 O 18 6- ；
The characteristic ions of the sodium metavanadate comprise metavanadate radical ions VO 3 - ；
The characteristic ions of the sodium molybdate comprise molybdate ions HMoO 4 - ；
The characteristic ions of sodium tungstate comprise tungstate radical ions HWO 4 - ；
The characteristic ions of the sodium silicate comprise silicate ions HSiO 3 - 。
The dynamic monitoring model for the electroplating process stores the linear relation between the characteristic ion mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution and the real-time concentration of each component of the micro-arc ceramic metaphosphate oxidation bath solution.
The linear relationship between the characteristic ion mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution and the real-time concentration of each component of the metaphosphoric acid micro-arc ceramic oxidation bath solution is as follows:
y1＝617.62x1+7150； (1)
y2＝3862x2+39540； (2)
y3＝806.62x3+2750.3； (3)
y4＝596.27x4+4537.4； (4)
y5＝995.4x5+27247； (5)
in the formula, y1, y2, y3, y4 and y5 respectively represent the mass-to-charge ratios of characteristic ions of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate; x1, x2, x3, x4 and x5 respectively represent the real-time concentration of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate in the micro-arc ceramic oxidation bath solution of metaphosphoric acid.
Example 2:
a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process comprises the following steps:
1) Sampling micro-arc ceramic oxidation bath solution in the micro-arc ceramic oxidation electroplating process in real time, and performing pretreatment to obtain solution to be detected;
2) Ionizing the molecules of the solution to be detected by using an ion source to obtain a plurality of ions, converging the obtained ions into ion beams, and inputting the ion beams into a high-resolution mass spectrometer;
3) The high-resolution mass spectrometer performs mass analysis on the ion beam by using a built-in mass analyzer to obtain characteristic ions and mass-to-charge ratios thereof of components of the micro-arc ceramic oxidation bath solution in the solution to be detected, and inputs the characteristic ions and the mass-to-charge ratios thereof into an electroplating process dynamic monitoring module in which an electroplating process dynamic monitoring model is stored;
4) The dynamic monitoring module for the electroplating process inputs characteristic ions and mass-to-charge ratios of all components of the micro-arc ceramic oxidation bath solution in the solution to be detected into the dynamic monitoring model for the electroplating process to obtain the real-time concentration of all components of the micro-arc ceramic oxidation bath solution so as to reflect the real-time state of the micro-arc ceramic oxidation electroplating process.
Example 3:
a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process is disclosed in an embodiment 2, wherein pretreatment comprises filtration and dilution.
Example 4:
a dynamic monitoring method for micro-arc ceramic oxidation electroplating process is disclosed in example 3, wherein the micro-arc ceramic oxidation bath solution is dissolved in sodium hydroxide or potassium hydroxide solution when the micro-arc ceramic oxidation bath solution is diluted.
Example 5:
the main content of the dynamic monitoring method for the micro-arc ceramic oxidation electroplating process is shown in embodiment 2, wherein the ion source comprises an electrospray ionization source.
Example 6:
a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process mainly comprises the following steps of embodiment 2, wherein a built-in mass analyzer of a high-resolution mass spectrometer comprises a flight time mass analyzer, an electrostatic field orbitrap mass analyzer and a Fourier transform ion cyclotron resonance mass analyzer.
Example 7:
the main content of the dynamic monitoring method for the micro-arc ceramic oxidation electroplating process is shown in an embodiment 2, wherein the micro-arc ceramic oxidation bath solution comprises the components of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate.
Example 8:
a dynamic monitoring method for micro-arc ceramic oxidation electroplating process is disclosed in embodiment 2, wherein characteristic ions of sodium hexametaphosphate comprise hexametaphosphate ion P 6 O 18 6- ；
The characteristic ions of the sodium metavanadate comprise metavanadate radical ions VO 3 - ；
The characteristic ion of the sodium molybdate comprises molybdate ion HMoO 4 - ；
The characteristic ions of sodium tungstate comprise tungstate radical ions HWO 4 - ；
The characteristic ion of the sodium silicate comprises silicate ionHSiO 3 - 。
Example 9:
the main content of the dynamic monitoring method for the micro-arc ceramic oxidation electroplating process is shown in an embodiment 2, wherein a linear relation between the characteristic ion mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution and the real-time concentration of each component of the micro-arc ceramic oxidation bath solution metaphosphate is stored in the dynamic monitoring model for the electroplating process.
Example 10:
a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process mainly comprises the following steps of (1) embodiment 2, wherein the linear relations between the characteristic ion mass-to-charge ratios of all components of the micro-arc ceramic oxidation bath solution and the real-time concentrations of all components of the micro-arc ceramic metaphosphate oxidation bath solution are respectively as follows:
y1＝617.62x1+7150； (1)
y2＝3862x2+39540； (2)
y3＝806.62x3+2750.3； (3)
y4＝596.27x4+4537.4； (4)
y5＝995.4x5+27247； (5)
in the formula, y1, y2, y3, y4 and y5 respectively represent the mass-to-charge ratios of characteristic ions of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate; x1, x2, x3, x4 and x5 respectively represent the real-time concentration of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate in the micro-arc metaphosphoric acid ceramic oxidation bath solution.
Example 11:
a dynamic monitoring method for micro-arc ceramic oxidation electroplating process comprises the following steps:
(1) Pretreating the obtained micro-arc ceramic oxidation bath solution;
(2) Determining the solution to be detected by adopting a high-resolution mass spectrometry;
(3) Obtaining 5 component characteristic ions and response strength of the micro-arc ceramic oxidation tank liquid;
(4) And calculating the concentration of each component in the solution to be detected according to the response intensity of the characteristic ions of each component.
The micro-arc ceramic oxidation bath solution comprises sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate, and the components are dissolved in a sodium hydroxide or potassium hydroxide solution.
The ion source of high resolution mass spectrometry is electrospray ionization (ESI), and detection is performed in a negative ion mode.
The mass analyzer of the high-resolution mass spectrum can be a time of flight mass analyzer (TOF), an electrostatic field orbit trap mass analyzer (Obitrap) or a Fourier transform ion cyclotron resonance mass analyzer (FTICR).
The characteristic ions and mass-to-charge ratio (m/z) of the components of the micro-arc ceramic oxidation bath solution are as follows, and the characteristic ion of sodium hexametaphosphate is P 6 O 18 6- M/z is 78.9580, and the characteristic ion of sodium metavanadate is VO 3 - M/z is 98.9282; the characteristic ion of sodium molybdate is HMoO 4 - M/z is 162.8923; sodium tungstate characterized by an ion HWO 4 - M/z is 248.9379; the characteristic ion of sodium silicate is HSiO 3 And m/z is 76.9689.
Example 12:
a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process comprises the following steps:
(1) Pretreating the obtained micro-arc ceramic oxidation bath solution;
(2) Determining the solution to be detected by adopting a high-resolution mass spectrometry;
(2-1) apparatus: a high-resolution LC-MS instrument with an ESI (electronic spray ionization) source; an ultrapure water meter; an electronic balance;
(2-2) reagents: ultrapure water, sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate, sodium silicate and potassium hydroxide;
(2-3) in one embodiment, the apparatus: quadrupole time-of-flight mass spectrometer (Q-TOF), with the conditions: ESI source negative ion mode, gasTemp:350 ℃, dryingGas:12L/min, nebulizer:35psi, sheathgastemp:350 ℃, sheathGasFlow:12L/min; vcap:3000V, nozleVoltage: 1500V; fragment: -170V, skimmer-65V, oct 1RFVpp:750V; sample introduction flow rate: 0.1mL/min;
(3) Obtaining 5 component characteristic ions and response strength of the micro-arc ceramic oxidation tank liquid;
the characteristic ion of sodium hexametaphosphate is P 6 O 18 6- M/z is 78.9580, and the characteristic ion of sodium metavanadate is VO 3 - M/z is 98.9282; the characteristic ion of sodium molybdate is HMoO 4 - M/z is 162.8923; sodium tungstate characterized by an ion HWO 4 - M/z is 248.9379; the characteristic ion of sodium silicate is HSiO 3 And m/z is 76.9689.
(4) According to the response intensity of the characteristic ions, the concentration of each component in the solution to be detected is calculated, and in the concentration range of 20-200 mg/L, the concentration of 5 components and the response intensity of the characteristic ions are in a linear relation:
the linear relationship between the sodium hexametaphosphate concentration x and the corresponding characteristic ion (m/z 78.9580) response intensity y is as follows: y =617.62x C +7150 2 ＝0.9937；
The linear relation between the sodium metavanadate concentration x and the corresponding characteristic ion (m/z 98.9315) response intensity y is as follows: y =3862x+39540 2 ＝0.9995；
The linear relationship between the sodium molybdate concentration x and the corresponding characteristic ion (m/z 162.8923) response intensity y is: y =806.62x +2750.3 2 ＝0.9999；
The linear relation between the sodium tungstate concentration x and the corresponding characteristic ion (m/z 248.9379) response intensity y is as follows: y = y =596.27x +4537.4 2 ＝0.9999；
The linear relationship between the sodium silicate concentration x and the corresponding characteristic ion (m/z 76.9689) response intensity y is as follows: y =995.4x +27247 2 ＝0.9992；
Wherein the unit of the concentration x is mg/L;
the ion source of the high-resolution mass spectrum is electrospray ionization (ESI) and is used for detecting in a negative ion mode.
The mass analyzer of the high resolution mass spectrum can be a time of flight mass analyzer (TOF), an electrostatic field orbit trap mass analyzer (Obitrap) or a Fourier transform ion cyclotron resonance mass analyzer (FTICR).
Example 13:
a dynamic monitoring method for a micro-arc ceramic oxidation electroplating process comprises the following steps:
1. instruments and reagents:
(1) The instrument comprises the following steps: QTOF 6545XT model high resolution LC MS (Agilent, USA), matching ESI electrospray source and injection pump; an Ellga Chorus 1Complete ultrapure water meter; sartorious Quintix213 electronic balance.
(2) Reagent: sodium hexametaphosphate (Na) 6 P 6 O 18 ) Sodium metavanadate (NaVO) 3 ) Sodium molybdate (Na) 2 MoO 4 ) Sodium tungstate (Na) 2 MoO 4 ) Sodium silicate (Na) 2 SiO 3 ) Potassium hydroxide (KOH) guaranteed reagent grade was obtained from Sigma reagent company. The micro-arc ceramic oxidation bath solution comes from a certain company.
2. Method and results
(1) Solution preparation
a. Potassium hydroxide solution: 2.0g of potassium hydroxide was weighed and dissolved in 1L of water at a concentration of 2g/L.
b. Preparing a standard solution stock solution: respectively and accurately weighing Na 6 P 6 O 18 、NaVO 3 、Na 2 MoO 4 、Na 2 MoO 4 、Na 2 SiO 3 0.1g of each was dissolved in a potassium hydroxide solution (2 g/L) to a constant volume of 100mL, and the concentration was 1g/L.
c. Mixing standard solutions: taking each standard stock solution with corresponding volume to prepare mixed standard solutions with the concentrations of 20, 50, 100 and 200 mg/L;
d. preparing a sample solution of a sample to be tested: taking the solution to be detected, filtering the solution through a 0.22um filter membrane, and continuously diluting the solution to a proper concentration by using a potassium hydroxide solution (2 g/L) according to the response intensity;
(2) Conditions of the apparatus
Mass spectrum conditions: ESI source negative ion mode, gasTemp:350 ℃, dryingGas:12L/min, nebulizer:35psi, sheathgastemp:350 ℃, sheathGasFlow:12L/min; vcap:3000V, nozleVoltage: 1500V; fragment: -170V, skimmer-65V, oct 1RFVpp:750V; sample introduction flow rate: 0.1mL/min;
(3) Characteristic ion and mass-to-charge ratio (m/z)
According to the mass spectrum response condition of each standard solution, the characteristic ions and mass-to-charge ratios of 5 components are determined as follows: characteristic ions are respectively P 6 O 18 6- 、VO 3 - 、HMoO 4 - 、HWO 4 - 、HSiO 3 - And m/z is 78.9580, 98.9282, 162.8923, 248.9379 and 76.9689 respectively.
(4) Standard curve
Within the concentration range of 20-200 mg/L, the concentrations of the four substances and the sum of the characteristic ionic strength thereof present a linear relationship, and the fitting parameters of the relevant standard curve are shown in Table 1.
TABLE 1 Standard Curve parameters of the five formulation components
(5) Measurement results
And calculating the concentration of the formula components in the solution according to the characteristic ionic strength of each substance in the sample to be detected and the standard curve, and calculating the content of each component in the micro-arc ceramic oxidation formula according to the dilution multiple. The results were as follows:
the content of sodium hexametaphosphate is 0.61g/L, the content of sodium metavanadate is 0.59g/L, the content of sodium molybdate is 1.56g/L, the content of sodium tungstate is 0, the content of sodium silicate is 0.29g/L,
the invention aims to provide a method for measuring the component content of micro-arc ceramic oxidation bath solution. Comprises the steps of pretreating the obtained micro-arc ceramic oxidation bath solution; determining the solution to be detected by adopting an electrospray high-resolution mass spectrometry method to obtain the characteristic ion intensity in the solution to be detected; and calculating the concentration of each component in the solution to be detected according to the characteristic ion intensity. Compared with the traditional detection method, the method disclosed by the invention is simple to operate, short in analysis time, convenient and quick, good in method specificity and high in sensitivity, and can be used for carrying out qualitative and quantitative analysis on various components without separating the components of the micro-arc ceramic oxidation tank solution.
Claims (9)
1. A dynamic monitoring method for a micro-arc ceramic oxidation electroplating process is characterized by comprising the following steps:
1) And sampling the micro-arc ceramic oxidation bath solution in the micro-arc ceramic oxidation electroplating process in real time, and performing pretreatment to obtain the solution to be detected.
2) And (3) ionizing the molecules of the solution to be detected by using an ion source, and inputting the particles obtained by ionization into a high-resolution mass spectrometer.
3) The high-resolution mass spectrometer performs mass analysis on the ion beam by using a built-in mass analyzer to obtain characteristic ions and mass-to-charge ratios thereof of components of the micro-arc ceramic oxidation bath solution in the solution to be detected, and inputs the characteristic ions and the mass-to-charge ratios into an electroplating process dynamic monitoring module in which an electroplating process dynamic monitoring model is stored;
4) The dynamic electroplating process monitoring module inputs characteristic ions and mass-to-charge ratios of components of the micro-arc ceramic oxidation bath solution in the solution to be detected into the dynamic electroplating process monitoring model to obtain real-time concentrations of the components of the micro-arc ceramic oxidation bath solution so as to reflect the real-time state of the micro-arc ceramic oxidation electroplating process.
2. The method for dynamically monitoring the micro-arc ceramic oxidation plating process according to claim 1, characterized in that: the pretreatment comprises filtration and dilution.
3. The method for dynamically monitoring the micro-arc ceramic oxidation plating process according to claim 2, characterized in that: when the micro-arc ceramic oxidation tank liquid is diluted, the micro-arc ceramic oxidation tank liquid is dissolved in a sodium hydroxide or potassium hydroxide solution.
4. The method for dynamically monitoring the micro-arc ceramic oxidation plating process according to claim 1, characterized in that: the ion source comprises an electrospray ionization source.
5. The method for dynamically monitoring the micro-arc ceramic oxidation plating process according to claim 1, characterized in that: the built-in mass analyzer of the high-resolution mass spectrometer comprises a time-of-flight mass analyzer, an electrostatic field orbitrap mass analyzer and a Fourier transform ion cyclotron resonance mass analyzer.
6. The method for dynamically monitoring the micro-arc ceramic oxidation plating process according to claim 1, characterized in that: the micro-arc ceramic oxidation bath solution comprises the components of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate.
7. The method for dynamically monitoring the micro-arc ceramic oxidation electroplating process according to claim 6, wherein the method comprises the following steps: the characteristic ion of sodium hexametaphosphate comprises hexametaphosphate ion P 6 O 18 6- ；
The characteristic ions of the sodium metavanadate comprise metavanadate radical ions VO 3 - ；
The characteristic ions of the sodium molybdate comprise molybdate ions HMoO 4 - ；
The characteristic ions of sodium tungstate comprise tungstate radical ions HWO 4 - ；
The characteristic ions of the sodium silicate comprise silicate ions HSiO 3 - 。
8. The method for dynamically monitoring the micro-arc ceramic oxidation plating process according to claim 7, wherein the method comprises the following steps: the dynamic monitoring model of the electroplating process stores the linear relationship between the characteristic ion mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution and the real-time concentration of each component of the metaphosphoric acid micro-arc ceramic oxidation bath solution.
9. The method for dynamically monitoring the micro-arc ceramic oxidation plating process according to claim 8, wherein the method comprises the following steps: the linear relationship between the characteristic ion mass-to-charge ratio of each component of the micro-arc ceramic oxidation bath solution and the real-time concentration of each component of the metaphosphoric acid micro-arc ceramic oxidation bath solution is as follows:
y1＝617.62x1+7150； (1)
y2＝3862x2+39540； (2)
y3＝806.62x3+2750.3； (3)
y4＝596.27x4+4537.4； (4)
y5＝995.4x5+27247； (5)
in the formula, y1, y2, y3, y4 and y5 respectively represent the mass-to-charge ratios of characteristic ions of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate; x1, x2, x3, x4 and x5 respectively represent the real-time concentration of sodium hexametaphosphate, sodium metavanadate, sodium molybdate, sodium tungstate and sodium silicate in the micro-arc metaphosphoric acid ceramic oxidation bath solution.
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Citations (4)
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| US6878932B1 (en) * | 2003-05-09 | 2005-04-12 | John D. Kroska | Mass spectrometer ionization source and related methods |
| CN1749749A (en) * | 2004-09-13 | 2006-03-22 | 安捷伦科技有限公司 | Sampling device for mass spectrometer ion source with multiple inlets |
| US20110162969A1 (en) * | 2010-01-07 | 2011-07-07 | BZ Plating Process Solution | Intelligent control system for electrochemical plating process |
| CN111058077A (en) * | 2020-01-19 | 2020-04-24 | 常州大学 | Electrolyte for micro-arc oxidation of black ceramic membrane, preparation method of electrolyte and micro-arc oxidation method |
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Patent Citations (4)
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|---|---|---|---|---|
| US6878932B1 (en) * | 2003-05-09 | 2005-04-12 | John D. Kroska | Mass spectrometer ionization source and related methods |
| CN1749749A (en) * | 2004-09-13 | 2006-03-22 | 安捷伦科技有限公司 | Sampling device for mass spectrometer ion source with multiple inlets |
| US20110162969A1 (en) * | 2010-01-07 | 2011-07-07 | BZ Plating Process Solution | Intelligent control system for electrochemical plating process |
| CN111058077A (en) * | 2020-01-19 | 2020-04-24 | 常州大学 | Electrolyte for micro-arc oxidation of black ceramic membrane, preparation method of electrolyte and micro-arc oxidation method |
Non-Patent Citations (1)
| Title |
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| QIN, SHI-JIANG等: ""Simultaneous Determination of Twenty Amino Acids in In Vitro Fertilization Medium by the HPLC-MS/MS Method"", 《CHROMATOGRAPHIA》, vol. 85, no. 7, pages 643 - 654, XP037907922, DOI: 10.1007/s10337-022-04169-5 * |
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