CN117269219A - Method for acquiring metal information in lubricating grease - Google Patents
Method for acquiring metal information in lubricating grease Download PDFInfo
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- CN117269219A CN117269219A CN202311248407.1A CN202311248407A CN117269219A CN 117269219 A CN117269219 A CN 117269219A CN 202311248407 A CN202311248407 A CN 202311248407A CN 117269219 A CN117269219 A CN 117269219A
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- grease
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- 239000004519 grease Substances 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 39
- 239000002184 metal Substances 0.000 title claims abstract description 36
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 27
- 239000012535 impurity Substances 0.000 claims abstract description 75
- 239000000853 adhesive Substances 0.000 claims abstract description 48
- 230000001070 adhesive effect Effects 0.000 claims abstract description 48
- 239000002923 metal particle Substances 0.000 claims abstract description 38
- 239000002904 solvent Substances 0.000 claims abstract description 34
- 238000001914 filtration Methods 0.000 claims abstract description 28
- 238000004458 analytical method Methods 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims description 46
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 claims description 13
- 229950011008 tetrachloroethylene Drugs 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 12
- 230000003287 optical effect Effects 0.000 claims description 11
- 238000003384 imaging method Methods 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 18
- 238000001514 detection method Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 230000000877 morphologic effect Effects 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 238000010586 diagram Methods 0.000 description 18
- 238000004090 dissolution Methods 0.000 description 15
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000006870 function Effects 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 238000000120 microwave digestion Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QWVMUSBBWGTKML-UHFFFAOYSA-N [Li].[Mo](=S)=S Chemical compound [Li].[Mo](=S)=S QWVMUSBBWGTKML-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000002199 base oil Substances 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- BQKCOFRVVANBNO-UHFFFAOYSA-N chromium manganese Chemical compound [Cr][Mn][Cr] BQKCOFRVVANBNO-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000000209 wet digestion Methods 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The embodiment of the application provides a method for acquiring metal information in lubricating grease, which comprises the following steps: dissolving grease containing impurities with a solvent to obtain a mixture; standing the mixture until layering; filtering the bottom impurities of the layered mixture to obtain filtered impurities; adhering the filtered impurities to the conductive adhesive; placing the conductive adhesive in a scanning electron microscope instrument, and collecting images of the filtered impurities on the conductive adhesive to obtain collected images; and acquiring analysis data of metal particles in the lubricating grease containing impurities according to the acquired image. The metal particles can be directly observed through the scanning electron microscope, the metal particles with various morphological characteristics and sizes can be clearly observed, the solvent is easy to obtain, the experimental conditions are loose compared with the prior art, the testing steps are simple, the detection efficiency is improved, and the morphology of the metal particles is not damaged in the testing process.
Description
Technical Field
The application relates to the technical field of chemical inspection, in particular to a method for acquiring metal information in lubricating grease.
Background
In mechanical equipment, the lubricating grease is an indispensable part, and consists of base oil and a soap base or other thickening agents, and mainly plays roles of lubrication, protection and sealing. Most greases are used for lubrication and are called antifriction greases. The antifriction grease mainly has the functions of reducing mechanical friction and preventing mechanical abrasion, protecting metal corrosion and sealing and dust prevention. After equipment is worn, metal particles are mixed in the lubricating grease, and the lubricating effect of the lubricating grease is affected. By detecting metal particles in the grease, parts of the equipment that are worn out can be found quickly. The existing test method only can test the content of metal elements in the lubricating grease, such as an ASTM D7303 and an NB/SH/T0864 test inductively coupled plasma emission spectrometry, metal particles in the lubricating grease are changed into metal elements to be dissolved in water through wet digestion or microwave digestion, the content of the metal elements in the water is tested by ICP, and according to the result of the content of the elements, whether the specific form of the particles is an iron simple substance or a chromium-manganese mixture or an iron-chromium mixture can not be known, and only the content of the elements can be known.
To sum up, the existing test methods are ASTM D7303 and NB/SH/T0864, and the grease is digested by acidification or microwaveThe molecular chain is broken, the related elements are dissolved in acid after the molecular chain is broken, and the related element content is detected by diluting with water and placing in ICP. The current testing method can only determine the content of single element, but cannot determine which metal or compound thereof, such as Fe simple substance and Fe 2 O 3 The method can only reflect the content of Fe element, and cannot reflect whether the metal is simple substance or compound. The testing steps are complicated, the metal content is required to be tested after grease is digested, daily detection quantity is low, and the number of samples detected by a single-day microwave digestion instrument is 60.
Disclosure of Invention
An object of the embodiments of the present application is to provide a method for acquiring metal information in grease, which is capable of acquiring a metal species, a metal compound species, a metal content, and a metal compound content in grease containing impurities.
The method for acquiring the metal information in the lubricating grease provided by the embodiment of the application comprises the following steps:
dissolving grease containing impurities with a solvent to obtain a mixture;
standing the mixture until layering;
filtering the bottom impurities of the layered mixture to obtain filtered impurities;
adhering the filtered impurities to the conductive adhesive;
placing the conductive adhesive in a scanning electron microscope instrument, and collecting images of the filtered impurities on the conductive adhesive to obtain collected images;
and acquiring analysis data of metal particles in the lubricating grease containing impurities according to the acquired image.
Further, the filtering the bottom impurity of the layered mixture to obtain filtered impurity includes:
placing the bottom impurities of the layered mixture into a filtering device for filtering;
flushing the beaker and filter funnel of the filter device with the solvent;
and after the filter membrane is dried, obtaining the filtered impurities.
Further, the adhering the filtered impurities to the conductive adhesive includes:
adhering the filter membrane to a glass slide;
placing the slide in an optical microscope;
sticking one corner of the conductive adhesive by using tweezers, tearing the conductive adhesive from the back adhesive, and lightly placing the torn conductive adhesive on the surface of the filtered impurities;
after the filtered impurities are stuck, sticking the other surface of the conductive adhesive on a T-shaped table;
ding Tai was placed in the sample stage and the screw was tightened.
Further, the placing of the conductive adhesive in the scanning electron microscope device, the image acquisition of the filtered impurities on the conductive adhesive, and the acquisition of the acquired images, includes:
placing the sample stage in a scanning electron microscope;
the observation mode is respectively adjusted to a secondary electron mode or a back scattering mode, and the magnification and the focal length are adjusted until clear imaging can be achieved;
and (3) performing image acquisition on the filtered impurities on the conductive adhesive to obtain an acquired image.
Further, the placing of the conductive adhesive in the scanning electron microscope device, the image acquisition of the filtered impurities on the conductive adhesive, and the acquisition of the acquired images, includes: placing the sample stage in a scanning electron microscope; adjusting the observation mode to a back scattering mode, and adjusting the magnification and the focal length until clear imaging can be achieved; and (3) performing image acquisition on the filtered impurities on the conductive adhesive to obtain an acquired image.
Further, the acquiring analysis data of the metal particles in the grease containing impurities according to the acquired image includes:
and when the observation mode is a back scattering mode, selecting particles with brightness exceeding a brightness threshold value from the acquired image for analysis, and obtaining the analysis data.
Further, the selecting particles with brightness exceeding a brightness threshold in the collected image for analysis to obtain the analysis data includes:
and analyzing the image information of the particles with the brightness exceeding the brightness threshold by using an energy spectrometer to obtain analysis data of the particles with the brightness exceeding the brightness threshold.
Further, the solvent is one of 120# solvent gasoline, petroleum ether III, dimethylbenzene and tetrachloroethylene.
Further, the solvent is tetrachloroethylene or 120# solvent gasoline.
Further, the analyzing the image information of the particles with the brightness exceeding the brightness threshold by using the energy spectrometer to obtain the analysis data of the particles with the brightness exceeding the brightness threshold comprises:
quantitatively analyzing the image information of the particles with the brightness exceeding the brightness threshold by using an energy spectrometer to obtain the metal content of the particles with the brightness exceeding the brightness threshold;
acquiring the atomic percentage of the particles with the brightness exceeding a brightness threshold according to the metal content;
and determining the metal type of the particles with the brightness exceeding a brightness threshold according to the atomic percent.
According to the method for acquiring the metal information in the lubricating grease, the metal particles are directly observed through the scanning electron microscope, the metal particles with various morphological characteristics and sizes can be clearly observed, the solvent is easy to acquire, the experimental conditions are loose compared with the prior art, the testing steps are simple, the detection efficiency is improved, and the morphology of the metal particles is not damaged in the testing process.
Additional features and advantages of the disclosure will be set forth in the description which follows, or in part will be obvious from the description, or may be learned by practice of the techniques disclosed herein.
In order to make the above objects, features and advantages of the present application more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of a method for obtaining metal information in grease according to an embodiment of the present application;
fig. 2 is a first schematic diagram of the grease provided in the embodiment of the present application after dissolution;
fig. 3 is a second schematic diagram of the grease provided in the embodiment of the present application after dissolution;
fig. 4 is a third schematic diagram of the grease provided in the embodiment of the present application after dissolution;
FIG. 5 is a schematic illustration of filtered impurities provided in an embodiment of the present application;
FIG. 6 is a schematic view of metal particles in secondary electron mode according to an embodiment of the present disclosure;
fig. 7 is a schematic view of metal particles in a backscattering mode according to an embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be described below with reference to the drawings in the embodiments of the present application.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures. Meanwhile, in the description of the present application, the terms "first", "second", and the like are used only to distinguish the description, and are not to be construed as indicating or implying relative importance.
The instruments and reagents used in the examples of this application include: scanning electron microscope, energy spectrometer, optical microscope, petroleum ether iii: analytically pure, tetrachloroethylene: analytically pure, 120# solvent gasoline: analytically pure, xylenes: analytically pure; polytetrafluoroethylene stirring rod, glass cup: 150mL, 1.2 μm acetate filter membrane.
Referring to fig. 1, a method for obtaining metal information in grease provided in an embodiment of the present application includes:
s1: dissolving grease containing impurities with a solvent to obtain a mixture;
in some embodiments, the solvent is one of 120# solvent gasoline, petroleum ether iii, xylene, tetrachloroethylene.
Preferably, the solvent is tetrachloroethylene.
Illustratively, after stirring the sample (grease containing impurities) uniformly, a representative 0.5g sample was taken in a beaker, 4 parts each. 100mL of 120# solvent gasoline, petroleum ether III, xylene and tetrachloroethylene are added respectively for dissolution, and are stirred uniformly. After standing for 1h, the samples were layered. The sample dissolution effect is shown in fig. 2, 3 and 4, the grease in fig. 2 is complex lithium-based grease, the grease in fig. 3 is urea grease, and the grease in fig. 4 is molybdenum disulfide lithium-based grease.
In the steps, the lubricating grease contains abrasion metal particles, and the solvent disintegrates the soap base in the lubricating grease, so that the subsequent extraction of the metal particles is facilitated.
S2: standing the mixture until layering;
s3: filtering the bottom impurities of the layered mixture to obtain filtered impurities;
s4: adhering the filtered impurities to the conductive adhesive;
s5: placing the conductive adhesive in a scanning electron microscope instrument, and collecting images of the filtered impurities on the conductive adhesive to obtain collected images;
s6: and acquiring analysis data of metal particles in the lubricating grease containing impurities according to the acquired image.
In the scanning electron microscope, the specific form of the metal particles can be directly observed, and meanwhile, the method for destroying the form of the metal particles by microwaves and the like is not used, so that the method can accurately detect the specific content of the metal particles in the lubricating grease.
According to the method for acquiring the metal information in the lubricating grease, the metal particles are directly observed through the scanning electron microscope, the metal particles with various morphological characteristics and sizes can be clearly observed, the solvent is easy to acquire, the experimental conditions are loose compared with the prior art, the testing steps are simple, the detection efficiency is improved, and the morphology of the metal particles is not damaged in the testing process.
In some embodiments, the filtering the bottom impurity of the layered mixture to obtain a filtered impurity comprises:
placing the bottom impurities of the layered mixture into a filtering device for filtering;
in some embodiments, filtration is performed using a suction filtration device. Filtration was performed using a 1.2 μm acetate membrane.
Flushing the beaker and filter funnel of the filter device with the solvent;
and after the filter membrane is dried, obtaining the filtered impurities.
Referring to fig. 5, a schematic diagram of filtered impurities obtained by filtering after dissolving different greases with different solvents is shown, and in fig. 5, the first row represents a schematic diagram of filtered impurities obtained by filtering after dissolving different greases with tetrachloroethylene; line 2 shows a schematic diagram of filtered impurities obtained by filtering after dissolving different greases in gasoline; line 3 shows a schematic diagram of filtered impurities obtained by dissolving different greases in xylene and then filtering; line 4 shows a schematic diagram of filtered impurities obtained by filtering petroleum ether iii after dissolving different greases; a schematic diagram of filtered impurities obtained by dissolving general lithium-based grease with different dissolving agents and then filtering the solution is shown in the 1 st column; a schematic diagram of the filtered impurities obtained by filtering the calcium sulfonate base grease after being dissolved by different dissolving agents; 3, a schematic diagram of filtered impurities obtained by filtering after dissolving molybdenum disulfide lithium-based grease with different dissolving agents; column 4 shows a schematic diagram of filtered impurities obtained by filtering after dissolution of the composite lithium-based lipid with different dissolution agents; column 5 shows a schematic diagram of filtered impurities obtained by filtering after dissolution of urea resin with different dissolution agents; as can be seen from fig. 5, the general lithium-based grease, the complex lithium-based grease and the urea-based grease do not have the condition of film formation and curling of the filter material after suction filtration, the extraction of the particles depends on the dissolution condition of the grease, the dissolution effect of tetrachloroethylene is the best, the 120# solvent is gasoline-secondary, and the calcium sulfonate-based grease and the molybdenum disulfide lithium-based grease have the condition of film formation and curling after dissolution and filtration of the four solvents. The combination of the dissolution effect and the effect after filtration may select tetrachloroethylene or 120# solvent gasoline as the diluting solvent.
In some embodiments, the adhering the filtered impurities to the conductive adhesive comprises:
adhering the filter membrane to a glass slide;
placing the slide in an optical microscope;
sticking one corner of the conductive adhesive by using tweezers, tearing the conductive adhesive from the back adhesive, and lightly placing the torn conductive adhesive on the surface of the filtered impurities;
after the filtered impurities are stuck, sticking the other surface of the conductive adhesive on a T-shaped table;
ding Tai was placed in the sample stage and the screw was tightened.
Illustratively, the filtered membrane is adhered to a slide, the slide is placed in an optical microscope, and the location of the metal particles is generally observed by the optical microscope. When using an optical microscope, the observed area will have white light. When metal particles appear in the optical microscope, the white light position on the membrane is the target area, at the moment, forceps are used for lightly sticking one corner of the conductive adhesive, the conductive adhesive is torn out from the back adhesive, the torn conductive adhesive is lightly placed on the surface of a sample (filtered impurities), and after enough samples are stuck, the other surface of the conductive adhesive is stuck on the T-shaped table. Ding Tai was placed in the sample stage and the screw was tightened.
In some embodiments, the placing the conductive adhesive in the scanning electron microscope device, and performing image acquisition on the filtered impurities on the conductive adhesive to obtain an acquired image, includes:
placing the sample stage in a scanning electron microscope;
the observation mode is respectively adjusted to a secondary electron mode or a back scattering mode, and the magnification and the focal length are adjusted until clear imaging can be achieved;
and (3) performing image acquisition on the filtered impurities on the conductive adhesive to obtain an acquired image.
The sample stage was placed in a scanning electron microscope, evacuated, and the observation mode was adjusted to secondary electron mode and Back Scattering (BSD) mode, respectively, and the pitch was adjusted to 8.5mm. And adjusting the magnification and the focal length according to the scanning electron microscope imaging until clear imaging can be achieved. Referring to fig. 6, an acquired image in the secondary electron mode, referring to fig. 7, an acquired image in the back scattering mode.
Preferably, the placing the conductive adhesive in a scanning electron microscope instrument, and collecting the filtered impurities on the conductive adhesive to obtain a collected image, including:
placing the sample stage in a scanning electron microscope;
adjusting the observation mode to a back scattering mode, and adjusting the magnification and the focal length until clear imaging can be achieved;
and (3) performing image acquisition on the filtered impurities on the conductive adhesive to obtain an acquired image.
In some embodiments, the acquiring analysis data of metal particles in the grease containing impurities from the acquired image includes:
and when the observation mode is a back scattering mode, selecting particles with brightness exceeding a brightness threshold value from the acquired image for analysis, and obtaining the analysis data.
As can be seen from fig. 6 and 7, the grease easily accumulates charges in the secondary electron mode, and assumes an exposed state in which metal particles are less likely to be found than in the back scattering mode. The grease and the metal particles have obvious light and shade differences in the back scattering mode, the grease presents darker color, the metal particles present brighter color, and the brighter particles are selected for focusing, analysis and quantification.
In some embodiments, the analyzing, by using a spectrometer, the image information of the particles with the brightness exceeding the brightness threshold to obtain the analysis data of the particles with the brightness exceeding the brightness threshold includes:
quantitatively analyzing the image information of the particles with the brightness exceeding the brightness threshold by using an energy spectrometer to obtain the metal content of the particles with the brightness exceeding the brightness threshold;
acquiring the atomic percentage of the particles with the brightness exceeding a brightness threshold according to the metal content;
and determining the metal type of the particles with the brightness exceeding a brightness threshold according to the atomic percent.
Illustratively, particle 1, particle 2 and particle 3 were selected for spectroscopic quantitative analysis, and the metal particle content for the different modes was compared as shown in the following table:
as can be seen from the data in Table 1, the quantitative results of the metal particles are not greatly different in the back scattering mode and the secondary electron mode, but are greatly different in the test time, the test time of the single metal particle in the secondary electron mode is about half an hour, the test time of the metal particle in the back scattering mode is only required to be not more than 5 minutes, and the efficiency is improved by 83%.
And switching the analysis result to atomic percent after the quantitative analysis of the energy spectrum, and determining the metal type according to the atomic percent. As shown in Table 1, the sample was elemental iron, the Fe content in the pellets 2 was 98.15% and the Cr content was 1.85%, and the Cr content was less than 10% (88:12 ratio of iron-chromium alloy to stainless steel) so that only a small amount of chromium was mixed in the elemental iron. The atomic percentage content should be consistent with the atomic ratio in the chemical formula, such as Fe2O3 and Fe3O4, and iron atoms: oxygen atoms are 2:3 and 3:4, respectively.
The method of the embodiment of the application has the following advantages:
in the prior art, 8mL of concentrated nitric acid is added into grease for grease digestion, the grease is heated for 30min at 120 ℃ for pre-digestion, so that the grease is preliminarily dissolved, and after the grease is sealed, the pre-digestion product is digested by setting the heating parameter of a microwave digestion instrument. Concentrated nitric acid which is an easy-to-explode reagent is used in the test process, so that the concentrated nitric acid is not easy to purchase, has great harm to human bodies, and is troublesome in acid liquor treatment. After improvement, the lubricating grease containing impurities is dissolved by adopting solvents such as 120# solvent gasoline or tetrachloroethylene, the solvents belong to conventional reagents, the purchase is convenient, and the subsequent treatment is only carried out according to the normal reagents. Meanwhile, dissolution by using 120# solvent gasoline or tetrachloroethylene is only carried out at normal temperature, and after dissolution is completed, the scanning electron microscope-energy spectrum analysis can be carried out by only carrying out a simple filtering step, so that the testing step is simpler.
Existing test methods ASTM D7303 and NB/SH/T0864 have two pretreatment methods, one is to bake the grease into ash by using a muffle furnace, and then add an acid to dissolve the elements in the grease with nitric acid or hydrochloric acid. The other is to put the acid and grease in a closed microwave digestion tank, and the molecular chains of the base oil and soap base in the grease are broken by a pressure-increasing heating mode, so that the base oil and the grease can be dissolved in the acid. After the pretreatment is finished, the sample is diluted by deionized water, and ICP detection is used, wherein the two methods can only test the element content in the lubricating grease, and only can primarily judge which element content is higher, for example, the Fe content is higher, and only iron in the lubricating grease can be confirmed, and whether the lubricating grease is elemental iron or other compounds of the iron can not be confirmed. According to the method, the lubricating grease is dissolved by using the solvent, solid particles in the lubricating grease can be deposited in the filter membrane after vacuum suction filtration, the region of the metal particles on the membrane is observed by an optical microscope, the corresponding metal particles are adhered to a sample stage, the morphology of the particles is analyzed by a scanning electron microscope, the atomic proportion of the particles is analyzed by an energy spectrometer, and the chemical formula of the metal can be deduced according to the atomic proportion after the atomic proportion is given by the energy spectrometer, so that the types and the content of the metal particles are accurately distinguished, and the defect that the existing testing method can only test the content of elements is overcome.
The method provided by the embodiment of the application improves the detection efficiency, the number of single-day sample detection can reach 180, and compared with the existing test method, the efficiency is improved by 200%.
The scanning electron microscope has high magnification and long focal depth, can clearly inspect abrasive particles with various morphological characteristics and sizes, can determine the element types and the element contents of the abrasive particles by combining an X-ray energy spectrum analyzer, and can accurately judge the composition of the abrasive particles by adopting the scanning electron microscope and energy spectrum analysis for unknown abrasive particles with optical characteristics which are not known. Particles such as abrasion particles and pollution particles are separated from equipment lubricating oil, and qualitative and quantitative analysis is carried out on the morphology, the size, the composition, the particle size distribution and the like of the particles by means of equipment such as an electron microscope, so that the abrasion type, the abrasion degree and the external pollution particle sources of the surfaces of equipment parts are judged, and further important information such as the working states of friction pairs and lubricating systems of mechanical equipment is obtained.
In the several embodiments provided in this application, it should be understood that the disclosed apparatus and method may be implemented in other manners as well. The apparatus embodiments described above are merely illustrative, for example, flow diagrams and block diagrams in the figures illustrate the architecture, functionality, and operation of possible implementations of apparatus, methods and computer program products according to various embodiments of the present application. In this regard, each block in the flowchart or block diagrams may represent a module, segment, or portion of code, which comprises one or more executable instructions for implementing the specified logical function(s). It should also be noted that in some alternative implementations, the functions noted in the block may occur out of the order noted in the figures. For example, two blocks shown in succession may, in fact, be executed substantially concurrently, or the blocks may sometimes be executed in the reverse order, depending upon the functionality involved. It will also be noted that each block of the block diagrams and/or flowchart illustration, and combinations of blocks in the block diagrams and/or flowchart illustration, can be implemented by special purpose hardware-based systems which perform the specified functions or acts, or combinations of special purpose hardware and computer instructions.
In addition, the functional modules in the embodiments of the present application may be integrated together to form a single part, or each module may exist alone, or two or more modules may be integrated to form a single part.
The functions, if implemented in the form of software functional modules and sold or used as a stand-alone product, may be stored in a computer-readable storage medium. Based on such understanding, the technical solution of the present application may be embodied essentially or in a part contributing to the prior art or in a part of the technical solution, in the form of a software product stored in a storage medium, including several instructions for causing a computer device (which may be a personal computer, a server, or a network device, etc.) to perform all or part of the steps of the methods described in the embodiments of the present application. And the aforementioned storage medium includes: a U-disk, a removable hard disk, a Read-Only Memory (ROM), a random access Memory (RAM, random Access Memory), a magnetic disk, or an optical disk, or other various media capable of storing program codes.
The foregoing is merely exemplary embodiments of the present application and is not intended to limit the scope of the present application, and various modifications and variations may be suggested to one skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
The foregoing is merely specific embodiments of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art can easily think about changes or substitutions within the technical scope of the present application, and the changes and substitutions are intended to be covered by the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
Claims (10)
1. A method for obtaining metal information in grease, comprising:
dissolving grease containing impurities with a solvent to obtain a mixture;
standing the mixture until layering;
filtering the bottom impurities of the layered mixture to obtain filtered impurities;
adhering the filtered impurities to the conductive adhesive;
placing the conductive adhesive in a scanning electron microscope instrument, and collecting images of the filtered impurities on the conductive adhesive to obtain collected images;
and acquiring analysis data of metal particles in the lubricating grease containing impurities according to the acquired image.
2. The method for obtaining metal information in grease according to claim 1, wherein filtering the bottom impurities of the layered mixture to obtain filtered impurities comprises:
placing the bottom impurities of the layered mixture into a filtering device for filtering;
flushing the beaker and filter funnel of the filter device with the solvent;
and after the filter membrane is dried, obtaining the filtered impurities.
3. The method for acquiring metal information in grease according to claim 2, wherein the adhering the filtered impurities to the conductive paste comprises:
adhering the filter membrane to a glass slide;
placing the slide in an optical microscope;
sticking one corner of the conductive adhesive by using tweezers, tearing the conductive adhesive from the back adhesive, and lightly placing the torn conductive adhesive on the surface of the filtered impurities;
after the filtered impurities are stuck, sticking the other surface of the conductive adhesive on a T-shaped table;
ding Tai was placed in the sample stage and the screw was tightened.
4. The method for obtaining metal information in grease according to claim 3, wherein the placing the conductive paste in a scanning electron microscope, and collecting the filtered impurities on the conductive paste to obtain a collected image, comprises:
placing the sample stage in a scanning electron microscope;
the observation mode is respectively adjusted to a secondary electron mode or a back scattering mode, and the magnification and the focal length are adjusted until clear imaging can be achieved;
and (3) performing image acquisition on the filtered impurities on the conductive adhesive to obtain an acquired image.
5. The method for obtaining metal information in grease according to claim 4, wherein the placing the conductive paste in a scanning electron microscope, and collecting the filtered impurities on the conductive paste to obtain a collected image, comprises:
placing the sample stage in a scanning electron microscope;
adjusting the observation mode to a back scattering mode, and adjusting the magnification and the focal length until clear imaging can be achieved;
and (3) performing image acquisition on the filtered impurities on the conductive adhesive to obtain an acquired image.
6. The method for acquiring metal information in grease according to claim 5, wherein the acquiring analysis data of metal particles in the grease containing impurities from the acquired image includes:
and when the observation mode is a back scattering mode, selecting particles with brightness exceeding a brightness threshold value from the acquired image for analysis, and obtaining the analysis data.
7. The method of claim 6, wherein selecting particles having a brightness exceeding a brightness threshold in the captured image for analysis to obtain the analysis data comprises:
and analyzing the image information of the particles with the brightness exceeding the brightness threshold by using an energy spectrometer to obtain analysis data of the particles with the brightness exceeding the brightness threshold.
8. The method for acquiring metal information in grease according to claim 1, wherein the solvent is one of 120# solvent gasoline, petroleum ether iii, xylene, tetrachloroethylene.
9. The method for acquiring metal information in grease according to claim 1, wherein the solvent is tetrachloroethylene or 120# solvent gasoline.
10. The method for acquiring metal information in grease according to claim 7, wherein analyzing image information of particles having a luminance exceeding a luminance threshold by using an energy spectrometer to obtain analysis data of the particles having the luminance exceeding the luminance threshold comprises:
quantitatively analyzing the image information of the particles with the brightness exceeding the brightness threshold by using an energy spectrometer to obtain the metal content of the particles with the brightness exceeding the brightness threshold;
acquiring the atomic percentage of the particles with the brightness exceeding a brightness threshold according to the metal content;
and determining the metal type of the particles with the brightness exceeding a brightness threshold according to the atomic percent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311248407.1A CN117269219A (en) | 2023-09-25 | 2023-09-25 | Method for acquiring metal information in lubricating grease |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311248407.1A CN117269219A (en) | 2023-09-25 | 2023-09-25 | Method for acquiring metal information in lubricating grease |
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| CN117269219A true CN117269219A (en) | 2023-12-22 |
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| CN202311248407.1A Pending CN117269219A (en) | 2023-09-25 | 2023-09-25 | Method for acquiring metal information in lubricating grease |
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