A method for detecting the composition of deposits in a transmission

The method addresses the inaccuracy of existing varistor deposit analysis by using solvent dissolution, thermal analysis, and microwave digestion to accurately measure metal particle content, improving varistor quality assessment and oil performance.

CN115266464BActive Publication Date: 2025-07-15SHAANXI FAST GEAR CO LTD
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Patent Information

Application Number
CN202211060943.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-08-31
Publication Date
2025-07-15
Estimated Expiration
2042-08-31

AI Technical Summary

Technical Problem

The prior art cannot accurately measure the content of metal particles in transmission deposits, especially quantitative analysis of copper and aluminum, resulting in inaccurate detection results and the inaccurate determination of parts wear and lubricating oil performance.

Method used

The combination of dissolution, thermogravimetric analysis, microwave digestion and inductively coupled plasma emission spectrometer is adopted to dissolve the deposits in organic solvents, and the mass of inorganic substances is obtained by selecting metal particles for quantitative analysis of alloy elements. After microwave digestion, quantitative analysis of Fe, Cu, and Al is carried out. Combined with an electron probe X-ray microscope analyzer and an inductively coupled plasma emission spectrometer, accurate quantification detection of the sediment components is achieved.

Benefits of technology

The accurate determination of the content of metal particles in the transmission deposits is achieved, and the metal grade and lubricating oil performance can be accurately judged, providing a reliable basis for improving the transmission quality and gear oil performance, and improving the accuracy and comprehensiveness of the detection.

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Abstract

The present invention discloses a method for detecting the composition of deposits in a transmission, belonging to the technical field of cleanliness evaluation and detection of transmissions. This method collects the deposits in the transmission, removes the organic matter in the deposits, obtains the mass of the inorganic matter in the deposits by thermogravimetric analysis, and accurately obtains the mass of the organic matter by the subtraction method; through the quantitative analysis of the metal deposits, the alloy element content is accurately obtained, providing a reliable basis for tracing the material grade; finally, through microwave digestion and quantitative analysis, the mass of Fe, the mass of Cu, and the mass of Al in the deposits are obtained; and according to the mass of Fe, the mass of Cu, and the mass of Al in the deposits, the mass of the non-metallic inorganic matter is accurately obtained, providing an effective basis for improving the quality of the transmission and the performance of the gear oil. It solves the problems in the prior art such as low accuracy of detection results, inability to accurately determine the content of metal particle elements in the deposits, and inability to perform quantitative analysis on copper and aluminum in the deposits.
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Description

Technical Field

[0001] The present invention belongs to the technical field of transmission cleanliness evaluation and detection, and relates to a method for detecting the composition of deposits in a transmission. Background Art

[0002] During the use of a transmission, due to mechanical wear and oxidation and deterioration of the lubricating oil, various impurities with different particle sizes are generated. Part of the impurities are dispersed in the lubricating oil, and the other part is deposited on the transmission housing and parts. They are classified into inorganic substances and organic substances in general. By analyzing the content of metal elements in the deposited inorganic substances, the wear degree of parts in the transmission can be judged. Among them, the content of iron element reflects the wear degree of steel parts in the whole transmission, such as gears, bearings, shift forks, etc.; the copper content mainly reflects the wear of parts such as bearing cages and shift fork blocks; the aluminum element mainly reflects the wear degree of the transmission housing; by analyzing the elements of large particle grinding metals, the metal grade can be reversely inferred, so as to trace the parts that have suffered wear; through the quantitative analysis of deposited organic substances, the antioxidant capacity and cleaning dispersibility of the lubricating oil can be reflected. Therefore, it is of great significance for improving the quality of the transmission and the performance of gear oil.

[0003] At present, the analysis of deposits in transmissions in the industry belongs to the field of cleanliness detection technology. Generally, QC / T572 "Automobile Cleanliness Work Guide - Determination Method", QC / T575 "Automobile Cleanliness Work Guide - Analysis Method of Impurities" or QC / T983 "Automobile Mechanical Transmission Assembly Cleanliness Detection Method" are selected for analysis and detection. However, in the above methods, the method of membrane filtration is adopted. No matter what pore size membrane is selected, all deposits cannot be collected completely, resulting in inaccurate analysis data. Secondly, the above methods do not mention the accurate quantitative detection of impurity components. Only in QC / T575, they are divided into iron-containing substances, inorganic substances, and organic substances. The detection method of iron-containing substances is to use magnet adsorption + balance weighing. However, since in the transmission deposits, the iron-containing substances and organic substances are in a wrapped state, when the iron-containing substances are adsorbed by the magnet, a large amount of organic substances will be adsorbed at the same time, resulting in serious deviation of the analysis results. At the same time, this method cannot accurately measure the content of metal particle elements in the deposits, so the metal impurity material grade cannot be determined. The above methods can only roughly analyze iron-containing substances and cannot quantitatively analyze copper and aluminum in the deposits.

[0004] Therefore, there is an urgent need for a measurement method that can accurately measure the content of metal particle elements and can quantitatively analyze copper and aluminum in the deposits to meet the requirements of the current transmission cleanliness evaluation and detection technology field. Summary of the Invention

[0005] The object of the present invention is to solve the problems in the prior art, such as low accuracy of detection results, inability to accurately determine the content of metal particle elements in sediments, and inability to quantitatively analyze copper and aluminum in sediments. A method for detecting the composition of transmission sediments is provided. This method can effectively collect sediments, accurately determine the content of metal particle elements in sediments, trace the material grades, and quantitatively analyze copper, aluminum, etc. in sediments, providing an effective basis for improving the quality of transmissions and the performance of gear oils.

[0006] To achieve the above object, the present invention adopts the following technical solutions:

[0007] The present invention provides a method for detecting the composition of transmission sediments, including the following steps:

[0008] S1: Obtain the total mass of the sediments, dissolve the sediments in an organic solvent, and remove part of the organic matter;

[0009] S2: Wash, dry the dissolved sediments, and perform thermogravimetric analysis to obtain the mass of inorganic substances in the sediments;

[0010] S3: Obtain the mass of organic substances in the sediments based on the total mass and the mass of inorganic substances;

[0011] S4: Select the metal particle sediments in the sediments after thermogravimetric analysis, perform quantitative analysis of alloy elements, and obtain the alloy element content;

[0012] S5: Perform microwave digestion on the sediments after thermogravimetric analysis, and perform quantitative analysis to obtain the mass of Fe, the mass of Cu, and the mass of Al in the sediments respectively;

[0013] S6: Obtain the mass of non-metallic inorganic substances in the sediments based on the mass of inorganic substances obtained in S2 and the mass of Fe, the mass of Cu, and the mass of Al obtained in S5.

[0014] Further, the specific operation for obtaining the total mass of the sediments in S1 is as follows:

[0015] Use NY-120 solvent gasoline to wash the parts of the transmission and the inner wall of the transmission housing at a pressure greater than 150 KPa, and collect the washing liquid;

[0016] Evaporate and concentrate the collected washing liquid;

[0017] Centrifuge, dry, and weigh the concentrated washing liquid to obtain the mass of the total sediments.

[0018] Preferably, the conditions for evaporation and concentration are: water bath temperature is 85 - 95 °C, vacuum degree ≤ -0.08 MPa, rotation speed is 90 - 110 r / min.

[0019] Preferably, the organic solvent is one or more of chloroform, acetone and dimethyl sulfoxide.

[0020] Preferably, the conditions for thermogravimetric analysis in S2 are as follows: under nitrogen, at a heating rate of 10-20 °C / min, heated to 800 °C, held for 3 h, cooled to room temperature at a rate of 50 °C / min, and kept constant at room temperature for 40 min.

[0021] Further, the method for obtaining the mass of the organic matter in S3 is as follows:

[0022] M6 = M - M5 (1)

[0023] Wherein, M is the total mass, M6 is the mass of the organic matter, and M5 is the mass of the inorganic matter.

[0024] Further, in S4, the specific operation for obtaining the alloy element content is as follows:

[0025] After the thermogravimetric analysis is completed, select metal particle deposits with a particle size greater than 200 μm from the crucible;

[0026] Stick the selected metal particle deposits on the conductive tape, and use an electron probe X-ray microanalyzer to perform quantitative analysis of the alloy elements to obtain the alloy element content.

[0027] Preferably, the analysis conditions for the quantitative analysis of alloy elements are: acceleration voltage 15 ± 5 kV, electron beam current 100 ± 10 nA, beam spot 10-20 μm.

[0028] Further, the specific operation of S5 is as follows:

[0029] After the thermogravimetric analysis is completed, transfer all the deposits in the thermogravimetric analysis crucible into a microwave digestion tank, add nitric acid and hydrogen peroxide, and perform microwave digestion;

[0030] Volume-fix the digestion solution with deposits after microwave digestion;

[0031] Use an inductively coupled plasma emission spectrometer to perform quantitative analysis on the digestion solution with deposits after volume-fixing, and obtain the mass of Fe, the mass of Cu, and the mass of Al in the deposits respectively;

[0032] Among them, the conditions for microwave digestion are: heating ramp time 20-30 min, heating to 190-210 °C and holding for 20 min, digestion power 1500-1700 W; the conditions for quantitative analysis are: RF power 1100-1200 W, atomizing gas flow rate 0.60-0.80 L / min, pump speed 50-80 r / min.

[0033] Further, in S6, the method for obtaining the mass of non-metallic inorganic substances in the sediment is as follows:

[0034] M7 = M5 - (M Fe + M Cu + M Al )(2)

[0035] where M7 is the mass of non-metallic inorganic substances, M5 is the mass of inorganic substances, M Fe is the mass of Fe, M Cu is the mass of Cu, and M Al is the mass of Al.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] The present invention provides a method for detecting the composition of transmission sediment. The method collects the sediment in the transmission to obtain the mass of the total sediment; performs thermogravimetric analysis on the sediment to obtain the mass of the inorganic substances in the sediment; obtains the mass of the organic substances in the sediment according to the mass of the total sediment and the mass of the inorganic substances in the sediment; uses thermogravimetric analysis to perform quantitative analysis of alloy elements on the metal particle sediment in the sediment to obtain the alloy element content; performs quantitative analysis on the sediment after thermogravimetric analysis by microwave digestion to realize quantitative analysis of elements such as Fe, Cu, and Al in the sediment, and the analysis range is increased; finally, according to the mass of Fe, Cu, and Al in the sediment and the mass of the inorganic substances in the sediment, the mass of non-metallic inorganic substances is obtained. The method is simple and easy to operate, can accurately measure the mass of organic substances in the transmission sediment, analyze the metal element content, and perform quantitative analysis on copper, aluminum, etc. in the sediment, realize accurate speculation of the metal grade, and accurate judgment of the part wear degree. Through the mass analysis of non-metallic inorganic substances, accurate judgment of the oxidation ability and cleaning dispersibility of the lubricating oil can be realized, providing a reliable basis for improving the quality of the transmission and the performance of the gear oil.

[0038] Secondly, the method adopts the method of concentrating the cleaning solution by a rotary evaporator and collecting the precipitate by a high-speed centrifuge, avoiding the disadvantage that when collecting sediment by the filter membrane filtration method in the automotive industry standard, there is always part of the sediment distributed in the filter residue and cannot be completely collected, further improving the accuracy of the test.

[0039] Furthermore, by dissolving the precipitate with an organic solvent, most of the organic matter is removed, effectively reducing the total amount of the subsequent precipitate to be measured. Then, the precipitate is calcined under nitrogen protection using a thermogravimetric analyzer, and the total amount of organic matter is obtained through calculation, avoiding the disadvantage of the QC / T 575 automotive industry standard that it is impossible to accurately quantify due to the iron-containing substances and organic matter in the precipitate being in a wrapped state. At the same time, the precipitate is calcined under nitrogen protection by the thermogravimetric analyzer, avoiding the oxidation of metal impurities caused by directly calcining the sediment in the air, thereby ensuring better accuracy of the test results.

[0040] By picking out the metal sediment larger than 200 μm in the crucible and using an electron probe for quantitative chemical composition analysis, the metal material grade can be reversely inferred and judged, thus overcoming the disadvantage in QC / T 575 that only the iron content can be analyzed and the metal material grade cannot be analyzed.

[0041] Through the combination of microwave digestion and inductively coupled plasma optical emission spectrometer, quantitative analysis of elements such as Fe, Cu, and Al in the sediment is achieved, with an increased analysis range and more accurate results. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as limiting the scope. For those of ordinary skill in the art, other related drawings can be obtained based on these drawings without creative efforts.

[0043] Figure 1 It is a flowchart of the method for detecting the composition of the transmission sediment of the present invention.

[0044] Figure 2 It is a secondary electron image of the large particle metal sediment in the embodiment of the present invention.

[0045] Figure 3 It is a diagram of the quantitative analysis results of the elements of the metal sediment in the embodiment of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0046] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. Usually, the components of the embodiments of the present invention described and illustrated in the drawings here can be arranged and designed in various different configurations.

[0047] Accordingly, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts fall within the scope of protection of the present invention.

[0048] It should be noted that like reference numerals and letters denote like items in the following drawings, and thus, once an item is defined in one drawing, it does not require further definition and explanation in subsequent drawings.

[0049] In the description of the embodiments of the present invention, it should be noted that if terms such as "upper", "lower", "horizontal", "inner", etc. are used to indicate the orientation or positional relationship, it is based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship in which the product of the invention is usually placed during use. This is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation of the present invention. In addition, terms such as "first", "second", etc. are only used for distinguishing descriptions and cannot be understood as indicating or implying relative importance.

[0050] In addition, if the term "horizontal" appears, it does not mean that the component is required to be absolutely horizontal, but it can be slightly inclined. For example, "horizontal" only means that its direction is more horizontal relative to "vertical", and does not mean that the structure must be completely horizontal, but it can be slightly inclined.

[0051] In the description of the embodiments of the present invention, it should also be noted that unless otherwise clearly specified and limited, if terms such as "set", "installed", "connected", "coupled" are used, they should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0052] The following further describes the present invention in detail with reference to the accompanying drawings:

[0053] See Figure 1 , the present invention provides a method for detecting the composition of transmission deposits, including the following steps:

[0054] S1: Obtain the total mass of the deposits and dissolve the deposits in an organic solvent to remove part of the organic matter. The specific operation is as follows:

[0055] Remove the transmission from the whole vehicle and disassemble it;

[0056] Use NY-120 solvent gasoline to wash the disassembled parts and the inner wall of the transmission housing at a pressure greater than 150 KPa, and collect the washing liquid;

[0057] For the collected washing liquid, perform evaporation and concentration under the conditions of a water bath temperature of 85-95 °C, a vacuum degree ≤ -0.08 MPa, and a rotation speed of 90-110 r / min;

[0058] Centrifuge, dry, and weigh the concentrated washing liquid to obtain the total mass of the sediment;

[0059] Add an organic solvent to the collected sediment and perform ultrasonic oscillation to completely dissolve the organic matter in the sediment; among them, the organic solvent is one or more of chloroform, acetone, and dimethyl sulfoxide.

[0060] S2: Wash, dry, and perform thermogravimetric analysis on the dissolved sediment to obtain the mass of inorganic matter in the sediment. The specific operation is as follows: Centrifuge the dissolved sediment at 10000 ± 100 r / min and a centrifugal force of 90000 N for 10-30 min, discard the supernatant, and place it in a drying condition at 95-105 °C; Weigh the total mass of the crucible of the thermogravimetric analyzer, place the dried sediment in the crucible, and pass nitrogen at a rate of 50-80 mL / min;

[0061] Raise the temperature to 800 °C at a rate of 10-20 °C / min, hold for 3 h, cool to room temperature at a rate of 50 °C / min, and keep it at a constant temperature for 40 min; Weigh the total mass of the crucible together with the sintered precipitate, and the mass of inorganic matter in the sediment is:

[0062] M5 = M4 - M3 (1)

[0063] Among them, M5 is the mass of inorganic matter, M4 is the total mass of the crucible together with the sintered precipitate, and M3 is the total mass of the crucible.

[0064] S3: Obtain the mass of organic matter in the sediment according to the total mass and the mass of inorganic matter. The method is:

[0065] M6 = M - M5 (2)

[0066] Among them, M is the total mass of the sediment, M6 is the mass of organic matter, and M5 is the mass of inorganic matter.

[0067] S4: Select the metal particle sediment in the sediment after thermogravimetric analysis and perform quantitative analysis of alloy elements to obtain the alloy element content. The specific operation is as follows:

[0068] After the thermogravimetric analysis, select the metal particle sediment with a particle size greater than 200 μm from the crucible;

[0069] The selected metal particle deposits are adhered to the conductive tape, and the alloy element quantitative analysis is carried out by using an electron probe X-ray microanalyzer to obtain the alloy element content; among them, the analysis conditions for the alloy element quantitative analysis are: acceleration voltage 15±5 kV, electron beam current 100±10 nA, beam spot 10-20 μm.

[0070] S5: For the deposits after thermogravimetric analysis, perform microwave digestion and quantitative analysis to obtain the mass of Fe, the mass of Cu, and the mass of Al in the deposits respectively. The specific operation is as follows:

[0071] After the thermogravimetric analysis is completed, transfer all the deposits in the thermogravimetric analysis crucible into the microwave digestion tank, add nitric acid and hydrogen peroxide, and perform microwave digestion; the conditions for microwave digestion are: temperature rise ramp time 20-30 min, rise to 190-210 °C and hold for 20 min, digestion power 1500-1700 W;

[0072] Make the volume of the digestion solution with deposits after microwave digestion constant;

[0073] Use an inductively coupled plasma emission spectrometer to perform quantitative analysis on the digestion solution with deposits after constant volume. The quantitative analysis conditions are: RF power 1100-1200 W, atomizing gas flow rate 0.60-0.80 L / min, pump speed 50-80 r / min, and obtain the mass of Fe, the mass of Cu, and the mass of Al in the deposits respectively.

[0074] S6: According to the mass of inorganic substances obtained in S2 and the mass of Fe, the mass of Cu, and the mass of Al obtained in S5, obtain the mass of non-metallic inorganic substances in the deposits. The specific operation is as follows:

[0075] M7 = M5 - (M Fe + M Cu + M Al )(3)

[0076] Among them, M7 is the mass of non-metallic inorganic substances, M5 is the mass of inorganic substances, M Fe is the mass of Fe in the deposits, M Cu is the mass of Cu in the deposits, M Al is the mass of Al in the deposits.

[0077] Taking the transmission of a certain tractor truck that has run 150,000 km as an example, perform component detection on the deposits inside it.

[0078] Remove the transmission from the whole vehicle and disassemble it;

[0079] Use NY-120 solvent gasoline to rinse the disassembled parts and the inner wall of the transmission housing under a pressure greater than 150 KPa, and collect the rinsing liquid; note that when rinsing the inner wall of the transmission housing, use a brush to rinse while brushing, and collect the rinsing liquid.

[0080] For the collected rinsing liquid, perform evaporation and concentration under the conditions of a water bath temperature of 85 - 95 °C, a vacuum degree ≤ -0.08 MPa, and a rotation speed of 90 - 110 r / min;

[0081] Centrifuge, dry, and weigh the concentrated rinsing liquid to obtain a total sediment mass of 2796.0 mg.

[0082] Add the collected sediment to an organic solvent and perform ultrasonic oscillation to completely dissolve the organic matter in the sediment; among them, the organic matter is one or more of chloroform, acetone, and dimethyl sulfoxide.

[0083] Centrifuge the dissolved sediment at 10000 ± 100 r / min and a centrifugal force of 90000 N for 10 - 30 min, discard the supernatant, and place it in an oven at 95 - 105 °C for drying.

[0084] Weigh the total mass of the crucible of the thermogravimetric analyzer as 2280.52 mg, place the dried sediment in the crucible, and pass nitrogen at a rate of 50 - 80 mL / min;

[0085] Heat it at a rate of 10 - 20 °C / min to 800 °C, hold for 3 h, cool it to room temperature at a rate of 50 °C / min, and keep it at a constant temperature for 40 min; weigh the total mass of the crucible together with the sintered precipitate as 3152.72 mg, then the mass of the inorganic matter in the sediment is:

[0086]

[0087] Among them, M5 is the mass of the inorganic matter in the sediment, M4 is the total mass of the crucible together with the sintered precipitate, and M3 is the total mass of the crucible.

[0088] Based on the total mass of the sediment and the mass of the inorganic matter in the sediment, the mass of the organic matter in the sediment is:

[0089]

[0090] Among them, M is the total mass of the sediment, M6 is the mass of the organic matter in the sediment, and M5 is the mass of the inorganic matter in the sediment.

[0091] After the thermogravimetric analysis is completed, select metal particle sediments with a particle size greater than 200 μm from the crucible;

[0092] The selected metal particle deposits are adhered to the conductive tape, and the alloying elements are quantitatively analyzed using an electron probe X-ray microanalyzer to obtain the alloying element content. Among them, the analysis conditions for the quantitative analysis of alloying elements are: acceleration voltage 15 ± 5 kV, electron beam current 100 ± 10 nA, and beam spot 10 - 20 μm.

[0093] See Figure 2 and Figure 3 , it can be seen that the elemental contents of the metal deposit are 0.20% for C, 0.31% for Si, 0.48% for Cr, 1.05% for Mn, 0.58% for Ni, and 0.13% for Mo, which meet the chemical composition range of the 8620H alloy steel grade in the SAE J1268 standard, and are presumably generated from the normal wear of gear parts in the transmission during use.

[0094] After the thermogravimetric analysis, all the deposits in the thermogravimetric analysis crucible are transferred into a microwave digestion tank, nitric acid and hydrogen peroxide are added, and microwave digestion is carried out. The conditions for microwave digestion are: temperature rise ramp time 20 - 30 min, raise the temperature to 190 - 210 °C and hold for 20 min, and digestion power 1500 - 1700 W.

[0095] The digestion solution with deposits after microwave digestion is made up to a constant volume.

[0096] The digestion solution with deposits after volume making is quantitatively analyzed using an inductively coupled plasma optical emission spectrometer. The quantitative analysis conditions are: RF power 1100 - 1200 W, atomizing gas flow rate 0.60 - 0.80 L / min, pump speed 50 - 80 r / min, and the masses of Fe, Cu, and Al in the deposit are obtained respectively as 558.08 mg for Fe, 15.48 mg for Cu, and l 56.25 mg for Al. Then the mass of non-metallic inorganic substances in the deposit is:

[0097]

[0098] Among them, M7 is the mass of non-metallic inorganic substances in the deposit, M5 is the mass of inorganic substances in the deposit, M Fe is the mass of Fe in the deposit, M Cu is the mass of Cu in the deposit, M Al is the mass of Al in the deposit.

[0099] The above are only the preferred embodiments of the present invention and are not used to limit the present invention. For those skilled in the art, the present invention can have various changes and modifications. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for detecting the composition of transmission deposits, characterized in that, It includes the following steps: S1: Obtain the total mass of the sediment, dissolve the sediment in an organic solvent, and remove part of the organic matter; S2: Wash, dry, and perform thermogravimetric analysis on the dissolved sediment to obtain the mass of inorganic substances in the sediment; among them, the conditions for thermogravimetric analysis are: under nitrogen conditions, with a heating rate of 10 - 20 °C / min, raise the temperature to 800 °C, keep it warm for 3 h, cool it to room temperature at a rate of 50 °C / min, and keep it at a constant temperature for 40 min; S3: Obtain the mass of organic substances in the sediment according to the total mass and the mass of inorganic substances; S4: Select the metal particle sediment in the sediment after thermogravimetric analysis, perform quantitative analysis of alloy elements, and obtain the alloy element content. Specifically: After the thermogravimetric analysis is completed, select the metal particle sediment with a particle size greater than 200 μm from the crucible; Stick the selected metal particle sediment on the conductive tape, and use an electron probe X-ray microanalyzer to perform quantitative analysis of alloy elements to obtain the alloy element content; S5: Perform microwave digestion on the sediment after thermogravimetric analysis, and perform quantitative analysis to obtain the mass of Fe, the mass of Cu, and the mass of Al in the sediment respectively; S6: Obtain the mass of non-metallic inorganic substances in the sediment according to the mass of inorganic substances obtained in S2 and the mass of Fe, the mass of Cu, and the mass of Al obtained in S5.

2. The method for detecting the composition of deposits in a transmission according to claim 1, wherein The specific operation for obtaining the total mass of the sediment in S1 is: Use NY-120 solvent gasoline to rinse the parts of the transmission and the inner wall of the transmission housing under a pressure greater than 150 KPa, and collect the rinsing liquid; Perform evaporation and concentration on the collected rinsing liquid; Centrifuge, dry, and weigh the concentrated rinsing liquid to obtain the mass of the total sediment.

3. The method for detecting the composition of the transmission deposit according to claim 2, wherein The conditions for the evaporation and concentration are: the water bath temperature is 85 - 95 °C, the vacuum degree ≤ -0.08 MPa, and the rotation speed is 90 - 110 r / min.

4. The method for detecting the composition of transmission deposits according to claim 1, wherein The organic solvent is one or more of chloroform, acetone, and dimethyl sulfoxide.

5. The method for detecting the composition of transmission deposits according to claim 1, wherein The method for obtaining the mass of organic substances in S3 is: Among them, M is the total mass, M6 is the mass of organic substances, and M5 is the mass of inorganic substances.

6. The method for detecting the composition of the transmission deposit according to claim 1, wherein The analysis conditions for quantitative analysis of alloy elements are: the acceleration voltage is 15 ± 5 kV, the electron beam current is 100 ± 10 nA, and the beam spot is 10 - 20 μm.

7. The method for detecting the composition of transmission deposits according to claim 1, characterized in that, The specific operation of S5 is: After the thermogravimetric analysis is completed, transfer all the sediment in the thermogravimetric analysis crucible into a microwave digestion tank, add nitric acid and hydrogen peroxide, and perform microwave digestion; Make the volume of the digestion solution with sediment after microwave digestion constant; Use an inductively coupled plasma emission spectrometer to perform quantitative analysis on the digestion solution with sediment after constant volume to obtain the mass of Fe, the mass of Cu, and the mass of Al in the sediment respectively; Among them, the conditions for microwave digestion are: the heating ramp time is 20 - 30 min, raise the temperature to 190 - 210 °C and keep it for 20 min, and the digestion power is 1500 - 1700 W; the quantitative analysis conditions are: the RF power is 1100 - 1200 W, the atomizing gas flow rate is 0.60 - 0.80 L / min, and the pump speed is 50 - 80 r / min.

8. The method for detecting the composition of transmission deposits according to any one of claims 1-7, characterized in that, In S6, the method for obtaining the mass of non-metallic inorganic substances in the sediment is as follows: Among them, M7 is the mass of non-metallic inorganic substances, M5 is the mass of inorganic substances, M Fe is the mass of Fe, M Cu is the mass of Cu, M Al is the mass of Al.

Citation Information

Patent Citations

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