CN115235856A - Method for testing cleanliness of magnetic particles extracted by high magnetic force - Google Patents
Method for testing cleanliness of magnetic particles extracted by high magnetic force Download PDFInfo
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- CN115235856A CN115235856A CN202211154721.9A CN202211154721A CN115235856A CN 115235856 A CN115235856 A CN 115235856A CN 202211154721 A CN202211154721 A CN 202211154721A CN 115235856 A CN115235856 A CN 115235856A
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- 239000006249 magnetic particle Substances 0.000 title claims abstract description 64
- 230000003749 cleanliness Effects 0.000 title claims abstract description 42
- 238000012360 testing method Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 66
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000011888 foil Substances 0.000 claims abstract description 57
- 238000003756 stirring Methods 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 42
- 238000000967 suction filtration Methods 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 28
- 238000000605 extraction Methods 0.000 claims abstract description 25
- 238000007789 sealing Methods 0.000 claims abstract description 25
- 239000005060 rubber Substances 0.000 claims abstract description 24
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000004033 plastic Substances 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000004806 packaging method and process Methods 0.000 claims abstract description 9
- 238000004804 winding Methods 0.000 claims abstract description 8
- 238000002604 ultrasonography Methods 0.000 claims abstract description 5
- 239000002985 plastic film Substances 0.000 claims description 40
- 229920006255 plastic film Polymers 0.000 claims description 40
- 238000000498 ball milling Methods 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 24
- 238000005520 cutting process Methods 0.000 claims description 14
- 230000005389 magnetism Effects 0.000 claims description 13
- 238000011010 flushing procedure Methods 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000696 magnetic material Substances 0.000 claims description 5
- 238000005452 bending Methods 0.000 claims description 4
- 239000004677 Nylon Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- 238000009461 vacuum packaging Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims 2
- 238000001514 detection method Methods 0.000 abstract description 10
- 238000011068 loading method Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract 1
- 229920001169 thermoplastic Polymers 0.000 description 10
- 239000004416 thermosoftening plastic Substances 0.000 description 10
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 241001391944 Commicarpus scandens Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 241000689227 Cora <basidiomycete fungus> Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/0606—Investigating concentration of particle suspensions by collecting particles on a support
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/0606—Investigating concentration of particle suspensions by collecting particles on a support
- G01N15/0618—Investigating concentration of particle suspensions by collecting particles on a support of the filter type
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a method for testing the cleanliness of magnetic particles extracted by high magnetic force, which comprises the following steps: step 1, plastic packaging of a magnetic rod; step 2, weighing and stirring; step 3, magnetic extraction and collection; step 4, performing ultrasonic treatment; step 5, magnetic extraction is repeated: sleeving a layer of aluminum foil bag outside the strong magnetic rod, winding and sealing the upper part of the strong magnetic rod by using an O-shaped ring or a rubber band, stirring for more than 1 circle in a first beaker, taking out the strong magnetic rod from the aluminum foil bag, washing the aluminum foil bag, collecting washing liquid into a second beaker, performing secondary ultrasound in the second beaker, performing loading, stirring, taking out, washing and ultrasound actions at least twice, and discarding the aluminum foil bag; step 6, suction filtration and drying are carried out; and 7, testing. The nonmagnetic particles in the particles to be detected placed in the cleanliness meter are reduced as much as possible, so that the dependence of the cleanliness meter on workers is reduced, and the detection result is more accurate.
Description
Technical Field
The invention relates to the technical field of performance detection of nickel-cobalt-manganese ternary materials, in particular to a method for testing the cleanliness of magnetic particles extracted by high magnetic force.
Background
The nickel-cobalt-manganese ternary material is used as a positive electrode material for manufacturing the battery, and the size and the number of magnetic particles contained in the nickel-cobalt-manganese ternary material have great influence on the safety of the battery. The nickel-cobalt-manganese ternary positive electrode material is synthesized by mixing lithium with a nickel-cobalt-manganese ternary precursor and then performing a high-temperature solid phase method, so that the detection of the content of magnetic foreign matters in the nickel-cobalt-manganese ternary material for manufacturing the battery, the precursor and the lithium salt thereof is one of important bases for judging whether the nickel-cobalt-manganese ternary material can manufacture the battery with good performance.
The existing method for detecting the content of magnetic foreign matters in the nickel-cobalt-manganese ternary material, the precursor thereof and the lithium salt comprises the following steps: 1. plastic packaging of the magnetic bar: the magnetic bar is arranged in a thermoplastic bag; 2. weighing and stirring: mixing the magnetic rod wrapped with the thermoplastic bag, the material to be detected and water, and filling the mixture into a ball milling tank, wherein the ball milling tank is placed on a roller mixer, so that the material to be detected in the ball milling tank is fully contacted with the magnetic rod wrapped with the thermoplastic bag, and at the moment, magnetic particles in the material to be detected are adsorbed on the magnetic rod wrapped with the thermoplastic bag; 3. carrying out magnetism extraction and collection: taking out the magnetic rod which adsorbs the magnetic particles and wraps the thermoplastic bag from the ball milling tank, putting the magnetic rod into a beaker, washing the surface of the thermoplastic bag by using water, collecting the water for washing the thermoplastic bag in the beaker, cutting open the thermoplastic bag after washing is finished, taking out the magnetic rod, and leaving the thermoplastic bag in the beaker; 4. ultrasonic: putting the beaker into ultrasonic equipment for ultrasonic treatment, taking out the beaker after the ultrasonic treatment is finished, and taking out the thermoplastic bag in the beaker; 5. suction filtration and drying: carrying out suction filtration and drying on water in the beaker after ultrasonic treatment to obtain particles to be detected; 6. and (3) testing: and (3) putting the particles to be detected into a cleanliness meter for analysis and test, and distinguishing the metal from the nonmetal by utilizing the difference of the reflection of cross polarized light of the metal and the nonmetal, wherein the metal particles detected by the cleanliness meter are the magnetic particles to be detected. Although the existing detection method can detect the magnetic particles adsorbed by the magnetic rod, the plastic packaging bag wrapped outside the magnetic rod contains not only the magnetic particles but also nonmagnetic particles, so that when the cleanliness meter is used for detecting the magnetic particles, the erroneous judgment particles preliminarily judged by the cleanliness meter need to be manually deleted, connected and cut, and then the report is generated by recalculation, so that the cleanliness meter is manually operated too much, and the accuracy of the detection result is low. In addition, the existing method for detecting the content of the magnetic foreign matters in the nickel-cobalt-manganese ternary material, the precursor thereof and the lithium salt is only suitable for adsorbing the magnetic particles in a small sample by a small-sized magnetic bar, when the magnetic particles are extracted from a large sample, the strong magnetic bar is required to be adsorbed for a test due to the large number of the samples, and the existing detection method is not suitable for the existing method because the strong magnetic bar is long and cannot be completely immersed in a beaker.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for testing the cleanliness of the magnetic particles extracted by the high magnetic force is provided, the magnetic particles in the particles adsorbed by the strong magnetic force magnetic rod wrapped by the aluminum-plastic film are fully extracted, and nonmagnetic particles in particles to be detected placed in a cleanliness meter are reduced as much as possible, so that the dependence of the cleanliness meter on manpower is reduced, and the accuracy of a detection result is higher.
In order to solve the technical problems, the invention adopts the technical scheme that:
a method for testing the cleanliness of high-magnetic-force-extraction magnetic particles comprises the following steps:
step 1, plastic packaging of a magnetic rod:
step 1.1, putting a strong magnetic bar into an aluminum-plastic film, vacuumizing by using a vacuum packaging machine and carrying out plastic packaging;
step 1.2, cutting off the redundant part of the aluminum-plastic film by using ceramic scissors;
step 2, weighing and stirring:
step 2.1, weighing a sample, placing the sample in a ball milling tank, placing a plastic-packaged strong magnetic rod, adding pure water, and tightly covering the cover of the ball milling tank;
step 2.2, placing the ball milling tank on a roller mixer for automatic stirring and mixing;
step 3, magnetism extraction and collection:
step 3.1, taking down the ball milling tank after automatic stirring, clamping the ball milling tank by using a non-magnetic tweezers, taking out the strong magnetic bar wrapped with the aluminum-plastic film, and placing the strong magnetic bar in a first beaker;
3.2, flushing the material adsorbed by the strong magnetic bar on the upper part of the aluminum plastic film by using pure water;
3.3, cutting off the aluminum plastic film of the strong magnetic bar by using ceramic scissors, and taking out the strong magnetic bar;
step 3.4, washing the lower part of the aluminum-plastic film for multiple times by using pure water until the aluminum-plastic film is washed cleanly, and discarding the aluminum-plastic film;
step 4, ultrasound:
step 4.1, placing the first beaker after magnetism is increased in ultrasonic equipment for ultrasonic treatment;
step 4.2, uniformly stirring the solution in the first beaker after ultrasonic treatment by using a glass rod;
step 5, magnetic extraction is repeated:
sleeving a layer of aluminum foil bag on the strong magnetic rod, winding and sealing the upper part of the strong magnetic rod by using an O-shaped ring or a rubber band, putting the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for more than 1 circle, taking out the strong magnetic rod from an opening above the aluminum foil bag, and washing materials on the O-shaped ring or the rubber band and the aluminum foil bag into a second beaker; the step is executed at least twice;
after the end, discarding the aluminum foil bag, the O-shaped ring or the rubber band;
step 5, placing the second beaker in ultrasonic equipment for at least one ultrasonic treatment;
step 6, suction filtration and drying:
step 6.1, assembling a suction filtration device, carrying out suction filtration by using a filter membrane, washing the inner wall of the second beaker by using a washing bottle, and carrying out suction filtration to obtain the filter membrane attached with particles;
step 6.2, translating the filter membrane subjected to suction filtration to an object carrying sheet by using tweezers, and drying the object carrying sheet in a drying oven;
and 7, testing:
and detecting whether the particles on the filter membrane are magnetic particles by using a cleanliness meter, and counting the number of the magnetic particles with different particle sizes.
Further, step 2, weighing and stirring, specifically:
step 2.1, weighing a sample, placing the sample in a ball milling tank, placing a strong magnetic rod which is subjected to plastic sealing and pure water washing, adding pure water to a scale mark of the ball milling tank with the marked volume, adding water while pressing the tank body, and exhausting air; after adding water, tightly covering the cover of the ball milling tank and tightly sealing the cover with a sealing film;
and 2.2, inserting the roller mixer into a socket, adjusting a rotating speed switch on an operation screen to enable the rotating speed of the roller mixer to be 60rpm, setting the stirring time to be 15min, placing the sealed ball milling tank on the roller mixer, and automatically stirring and mixing after starting the device.
Further, step 3.3 specifically comprises:
and 3.3, horizontally cutting and flattening the upper part of the aluminum-plastic film of the strong magnetic bar by using ceramic scissors, cutting an opening on the side edge of the upper part, outwards and downwards bending the edges of the two cut upper parts, and taking out the strong magnetic bar.
Further, step 4.1 specifically includes:
and 4.1, sealing the first beaker after magnetic extraction by using a sealing film, and carrying out water bath ultrasonic treatment for 10min in ultrasonic equipment.
Further, step 5 repeats the magnetic extraction, specifically:
presetting an execution time threshold, wherein the execution time threshold is more than 1;
step 5.1, sheathing a layer of aluminum foil bag outside the strong magnetic bar, and winding and sealing the upper part of the strong magnetic bar by using an O-shaped ring or a rubber band;
step 5.2, placing the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for more than 1 circle, taking out the strong magnetic rod from an opening above the aluminum foil bag, and flushing materials on an O-shaped ring or a rubber band and the aluminum foil bag into a second beaker;
step 5.3, adding 1 to the current execution times, judging whether the current execution times is larger than an execution time threshold, if not, turning to the step 5.1 for execution, if so, discarding the aluminum foil bag, the O-shaped ring or the rubber band, and turning to the step 5.4 for execution;
and 5.4, putting the second beaker into ultrasonic equipment for ultrasonic action.
Or, further, step 5 repeats the magnetic extraction, specifically:
presetting an execution time threshold, wherein the execution time threshold is more than 1;
step 5.10, sheathing a layer of aluminum foil bag outside the strong magnetic bar, and winding and sealing the upper part of the strong magnetic bar by using an O-shaped ring or a rubber band;
step 5.20, placing the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for more than 1 circle, taking out the strong magnetic rod from an opening above the aluminum foil bag, and flushing materials on an O-shaped ring or a rubber band and the aluminum foil bag into a second beaker;
step 5.30, putting the second beaker into ultrasonic equipment for ultrasonic action;
and 5.40, adding 1 to the current execution times, judging whether the current execution times is greater than the execution time threshold, if not, turning to the step 5.10 to execute, and if so, discarding the aluminum foil bag, the O-shaped ring or the rubber band.
Further, in step 5, in the step of repeatedly carrying out magnetism extraction, the step 5.2 specifically comprises the following steps:
and 5.2, placing the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for 30 circles for about 1min, stirring for 5 times, and flushing the magnetic material adsorbed by the strong magnetic rod wrapped with the aluminum foil bag into a second beaker.
Further, step 6, suction filtration and drying specifically comprise:
step 6.1, assembling a suction filtration device, performing suction filtration by using a nylon mesh filter membrane, simultaneously washing the inner wall of the second beaker by using a washing bottle, performing suction filtration for 3min after no visible water drops exist on the filter paper, and obtaining the filter membrane attached with particles after suction filtration;
and 6.2, translating the filter membrane subjected to suction filtration to an object slide by using tweezers, and drying the object slide in a drying oven at 60 ℃ for 30min.
The invention has the beneficial effects that:
1. the strong magnetic bar is wrapped by the aluminum-plastic film in a vacuumizing mode, so that the aluminum-plastic film is in close contact with the strong magnetic bar, the influence on the magnetic force of the strong magnetic bar is small, the aluminum-plastic film is firm, and the aluminum-plastic film is not easy to break in the using process;
2. transferring the magnetic particles in the first beaker to a second beaker by adopting a repeated magnetism-lifting mode after ultrasonic treatment, filling a strong magnetic rod for multiple times and stirring, taking out the strong magnetic rod for multiple times and washing an aluminum foil bag in the repeated magnetism-lifting process, so that the first beaker is not easy to adhere, the magnetic particles are fully extracted, and performing ultrasonic treatment on the second beaker for multiple times so that the magnetic particle materials in the second beaker are relatively dispersed and easy to identify;
3. in the repeated magnetic extraction process, an O-shaped ring or a rubber band is wound at the sealing position of the aluminum foil bag, so that magnetic particles on the aluminum foil bag are prevented from being taken away when the high-intensity magnetic bar is taken out;
therefore, the magnetic particle and the nonmagnetic particle can be fully separated on the whole, the nonmagnetic particle is discharged, the magnetic particle is dispersed, the misjudgment condition of the cleanliness meter during detection is reduced, the dependence degree of the cleanliness meter on manual work is reduced, and the accuracy and the efficiency of the cleanliness meter detection are improved.
Drawings
Fig. 1 is a flow chart of a high magnetic force extraction magnetic particle cleanliness testing method of an embodiment of the invention.
Detailed Description
In order to explain the technical contents, the objects and the effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
Referring to fig. 1, one embodiment of the present invention is:
a method for testing the cleanliness of magnetic particles extracted by high magnetic force selects a high-magnetic-force magnetic rod with the length of 25cm, the diameter of the bottom surface of 2.5 cm and the magnetic force of 12000GS, and a specific embodiment of the test by selecting 1000g of samples is as follows:
step 1, plastic packaging of a magnetic rod:
step 1.1, a strong magnetic rod with the magnetic force of about 12000GS is filled into an aluminum plastic film, and the aluminum plastic film is vacuumized and sealed by a vacuum packaging machine, wherein the magnetic force of the strong magnetic rod is about 10000 to 11000GS; the step leads the aluminum-plastic film to be closely contacted with the strong magnetic bar, has small influence on the magnetic force of the strong magnetic bar, and is firm, durable and not easy to break;
step 1.2, cutting off the redundant part of the aluminum-plastic film by using ceramic scissors;
step 2, weighing and stirring:
step 2.1, weighing 1000g +/-2.00 g of sample, placing the sample in a 2000ml ball milling tank, placing a strong magnetic rod which is subjected to plastic sealing and pure water washing, adding pure water to 2000ml of scale mark, extruding the tank body, and exhausting air; after adding water, tightly covering the cover of the ball milling tank, tightly sealing the cover with a sealing film, and shaking up manually; the step ensures that air in the ball milling tank is as little as possible, and the sample in the ball milling tank is in full contact with the strong magnetic bar wrapping the aluminum-plastic film;
step 2.2, inserting the roller mixer into a socket, adjusting a rotating speed switch on an operation screen to enable the rotating speed of the roller mixer to be 60rpm, setting the stirring time to be 15min, placing the sealed ball milling tank on the roller mixer, and automatically stirring and mixing after starting the device; the step makes the sample fully contact with the strong magnetic bar wrapping the aluminum plastic film, and the strong magnetic bar can adsorb magnetic particles in the sample to the maximum extent in the ball milling tank;
step 3, magnetism extraction and collection:
step 3.1, taking down the ball milling tank after automatic stirring, clamping the ball milling tank by using a non-magnetic tweezers, taking out the strong magnetic bar wrapped with the aluminum-plastic film, and placing the strong magnetic bar in a 3000ml first beaker (the height of the first beaker is 25 cm); the non-magnetic tweezers are plastic tweezers or ceramic tweezers;
3.2, flushing the material adsorbed by the strong magnetic bar on the upper part of the aluminum plastic film by using pure water;
3.3, horizontally cutting and flattening the upper part of the aluminum-plastic film of the strong magnetic bar by using a ceramic scissors, cutting an opening on the side edge of the upper part, bending the edges of the two cut upper parts outwards and downwards, and taking out the strong magnetic bar; in the step, the bending state of the aluminum-plastic film can effectively prevent the strong magnetic bar from taking away the magnetic particles outside the aluminum-plastic film;
step 3.4, washing the lower part of the aluminum-plastic film for multiple times by using pure water until the aluminum-plastic film is washed cleanly, and discarding the aluminum-plastic film;
step 4, ultrasonic treatment:
step 4.1, sealing the first beaker after magnetism is extracted tightly by using a sealing film, and placing the beaker in ultrasonic equipment for water bath ultrasonic treatment for 10min; this step disperses the magnetic particles from the non-magnetic particles in the first beaker;
step 4.2, uniformly stirring the solution in the first beaker after ultrasonic treatment by using a glass rod;
step 5, magnetic extraction is repeated:
the preset execution time threshold is equal to 8;
step 5.100, sheathing a layer of aluminum foil bag outside the high-intensity magnetic rod, and winding and sealing the upper part of the high-intensity magnetic rod by using an O-shaped ring or a rubber band; the O-shaped ring or the rubber band is used, so that magnetic particles can be effectively prevented from being taken out of the aluminum foil bag when the high-intensity magnetic rod is taken out, and the high-intensity magnetic rod can be conveniently loaded and taken out;
step 5.200, placing the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for 30 circles for about 1min, stirring for 5 times totally, taking out the strong magnetic rod from an opening above the aluminum foil bag, and washing the O-shaped ring or rubber band and the material on the aluminum foil bag into a second beaker with the capacity of 3000ml and the height of 25 cm; in the step, a stirring action with a certain speed is carried out, so that the strong magnetic bar wrapping the aluminum foil bag fully adsorbs the magnetic particles in the first beaker, and non-magnetic particles can be prevented from being stuck on the aluminum foil bag to the maximum extent;
step 5.300 adds 1 to the current execution times;
judging whether the current execution times is an even number, if so, putting the second beaker into ultrasonic equipment for ultrasonic treatment; the step is that the solution in the second beaker is subjected to ultrasonic treatment for a plurality of times to disperse the particles in the second beaker;
judging whether the current execution times is greater than the execution time threshold value, if not, turning to the step 5.100 for execution, if so, discarding the aluminum foil bag, the O-shaped ring or the rubber band, and turning to the step 5.400 for execution; the operations of loading the strong magnetic bar, stirring, taking out the strong magnetic bar and washing the aluminum foil bag are carried out for multiple times, so that the situation that the strong magnetic bar is difficult to adsorb magnetic particles again due to the fact that magnetic particle materials wrap the surface of the aluminum foil bag because of more magnetic particle materials when magnetic extraction and stirring are carried out for one time is avoided, and finally, the magnetic particle materials in the first beaker are fully extracted;
step 5.400, judging whether the current execution times is odd, if so, putting the second beaker into ultrasonic equipment for ultrasonic action, and if not, executing step 6; this step ensures that the second beaker can be ultrasonically activated before step 6 is performed;
step 6, suction filtration and drying:
step 6.1, assembling a suction filtration device, performing suction filtration by using a 10-micron nylon mesh filter membrane, simultaneously washing the inner wall of the second beaker by using a washing bottle, performing suction filtration for 3min after no visible water drops exist on the filter paper, and obtaining the filter membrane attached with particles after suction filtration;
step 6.2, translating the filter membrane after suction filtration to an object carrying sheet by using a pair of tweezers, and drying the object carrying sheet in a drying oven at 60 ℃ for 30min (ensuring that the object carrying sheet has no water vapor);
and 7, testing:
detecting whether the particles on the filter membrane are metal magnetic particles by using a cleanliness meter, specifically, judging whether the particles are metal magnetic particles according to the reflectivity of the particles, and counting the number of the magnetic particles with different particle sizes, wherein the following specific steps of detecting the magnetic particles by using the cleanliness meter are described by reading an HFD 4 cleanliness meter:
step 7.1 preparation before testing:
step 7.1.1, sequentially opening a JMC Motor Controller (wherein JMC is an abbreviation of Jomesas Motor Controller and means the Jomesas Motor Controller, and JMC is a term special for a reading cleanliness instrument), a computer and 'PicEd Cora' test software;
7.1.2, ensuring that controllers of the JMC motor and the polarization unit are in an open state, and shifting the optical splitter to a Photo/Bino position;
step 7.2 standard block measurement:
step 7.2.1, parameters (< program > - < import parameters >) are imported into software, and particle standard block parameters (particle standard) are selected;
step 7.2.2 in the process of starting scanning, clicking < document > - < automatic scanning >, placing the particle standard block into the groove of the filter membrane bracket, adjusting the multiplying power to be 1.0, focusing to the maximum FOC (the FOC is a focusing button on a reading cleanliness meter and is an abbreviation of Focus in English words), scanning until the number of the particle sizes from large to small is 20/20/20/20/12/12/12, otherwise, the result does not accord with the standard value, wiping off dust and pollutants on the standard block by using dust-free paper or soft clean dust-free cloth, re-scanning, and judging data until the number of the particle sizes from large to small is 20/20/20/12/12/12;
step 7.3 sample analysis:
step 7.3.1 import parameters (< program > - < import parameters >), select test parameters, start scanning, click < document > - < automatic scanning >, the scanning platform will automatically move to the loading position, and place the filter membrane bracket or the objective lens with the filter membrane at the test position;
step 7.3.2, automatic scanning is clicked, and batch information, sample preparation date, analysis date, sample preparation mode and other information are written in the sample number;
7.3.3 clicking 'continue', after automatically calibrating the polarizer, checking whether the position of the zoom knob 3.0 is consistent with the software display, focusing until FOC is approximately equal to max, clicking 'continue', automatically scanning light and polarized light, and analyzing particles on a filter membrane;
step 7.4 confirmation of results:
7.4.1 after the scanning is finished, clicking three types of clickable metal particles, non-metal particles containing no fibers and fibers, checking and analyzing large-size particles, observing an original image and an analyzed image, judging whether misjudgment occurs or not, if not, turning to the step 7.5 for execution, and if so, turning to the step 7.4.2 for execution;
and 7.4.2, deleting, connecting and segmenting the misjudged particles:
step 7.4.2.1 delete: other pollutants on the filter membrane can be mixed with fibers and the like, the other pollutants are considered as a whole by software and are judged as a large particle, and the single particle is artificially deleted as the size of the single particle is very small;
step 7.4.2.2 connection: after one fiber is shielded, judging the fiber into a plurality of fibers by software, and manually connecting the fibers into one fiber;
step 7.4.2.3 cutting: the distance between the two particles is very small, and when the two particles are judged to be a large particle by software, the two particles are manually cut apart;
step 7.4.3 click the recalculate button, recalculate the results of the deleting, cutting, connecting and other steps, generate a report, and save the path and mode as follows: d, analyzing result, year, month, date and batch number;
step 7.5 sample marker preservation:
after the cleanliness meter is analyzed, the sample is recovered and kept, and can be kept in a clean filter membrane box or a slide, and batch information is noted.
By using the method for testing the cleanliness of the magnetic particles, samples of different batches are tested, the weight of each sample is 1kg, and the obtained test results are shown in table 1:
TABLE 1 data of test results of magnetic particle cleanliness tests
In summary, the method for testing the cleanliness of the magnetic particles extracted by the high magnetic force provided by the invention has the beneficial effects that:
1. the strong magnetic bar adopts a vacuumizing mode for plastic sealing, so that the strong magnetic bar is tightly attached to the aluminum-plastic film, and the influence of magnetic force is small;
2. the strong magnetic bar cannot completely enter the beaker due to the long length of the strong magnetic bar, so the magnetic field is lifted by adopting a mode of flushing the upper part firstly and then flushing the lower part;
3. repeatedly performing repeated circulating actions of loading the strong magnetic bars into the aluminum foil bag, stirring the strong magnetic bars in the first beaker, taking the strong magnetic bars out of the aluminum foil bag and washing the aluminum foil bag, fully extracting the magnetic particles in the first beaker and transferring the magnetic particles into the second beaker, wherein the stirring action avoids the non-magnetic particles from being stuck outside the aluminum foil bag as much as possible, so that the magnetic particles and the non-magnetic particles in the first beaker are separated to the greatest extent; performing ultrasonic treatment on the second beaker for multiple times to disperse the magnetic particle materials as much as possible;
in conclusion, the strong magnetic bar wrapped by the aluminum-plastic film is used for automatically stirring and adsorbing magnetic materials in a large sample, the strong magnetic bar wrapped by the aluminum-plastic film is used for stirring and adsorbing the magnetic materials in the first beaker for multiple times, sufficient magnetism extraction is carried out, the magnetic particles in the second beaker are subjected to ultrasound for multiple times, the magnetic particles are extracted and dispersed to the maximum extent, the nonmagnetic particles in the particles to be detected placed in the cleanliness instrument are reduced as much as possible, the magnetic particles are dispersed as much as possible, the dependence of the cleanliness instrument on workers is reduced, and the accuracy of detection results is higher.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.
Claims (9)
1. A method for testing the cleanliness of magnetic particles extracted by high magnetic force is characterized by comprising the following steps:
step 1, plastic packaging of a magnetic rod:
step 1.1, putting a strong magnetic bar into an aluminum-plastic film, vacuumizing by using a vacuum packaging machine and carrying out plastic packaging;
step 1.2, cutting off the redundant part of the aluminum-plastic film by using a ceramic scissors;
step 2, weighing and stirring:
step 2.1, weighing a sample, placing the sample in a ball milling tank, placing a plastic-packaged strong magnetic rod, adding pure water, and tightly covering a cover of the ball milling tank;
step 2.2, placing the ball milling tank on a roller mixer for automatic stirring and mixing;
step 3, magnetism extraction and collection:
step 3.1, taking down the ball milling tank after automatic stirring, clamping the ball milling tank by using a non-magnetic tweezers, taking out the strong magnetic bar wrapped with the aluminum-plastic film, and placing the strong magnetic bar in a first beaker;
3.2, flushing the material adsorbed by the strong magnetic bar on the upper part of the aluminum plastic film by using pure water;
3.3, cutting off the aluminum plastic film of the strong magnetic bar by using ceramic scissors, and taking out the strong magnetic bar;
step 3.4, washing the lower part of the aluminum-plastic film for multiple times by using pure water until the aluminum-plastic film is washed cleanly, and discarding the aluminum-plastic film;
step 4, ultrasound:
step 4.1, placing the first beaker after magnetic extraction in ultrasonic equipment for ultrasonic treatment;
step 4.2, uniformly stirring the solution in the first beaker after ultrasonic treatment by using a glass rod;
step 5, magnetic extraction is repeated:
sleeving a layer of aluminum foil bag on the strong magnetic rod, winding and sealing the upper part of the strong magnetic rod by using an O-shaped ring or a rubber band, putting the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for more than 1 circle, taking out the strong magnetic rod from an opening above the aluminum foil bag, and washing materials on the O-shaped ring or the rubber band and the aluminum foil bag into a second beaker; the step is executed at least twice;
after the end, discarding the aluminum foil bag, the O-shaped ring or the rubber band;
in the step 5, the second beaker is placed in ultrasonic equipment for at least one time;
step 6, suction filtration and drying:
step 6.1, assembling a suction filtration device, carrying out suction filtration by using a filter membrane, washing the inner wall of the second beaker by using a washing bottle, and carrying out suction filtration to obtain the filter membrane attached with particles;
step 6.2, translating the filter membrane after suction filtration to an object carrying sheet by using tweezers, and drying the object carrying sheet in a drying oven;
and 7, testing:
and detecting whether the particles on the filter membrane are magnetic particles by using a cleanliness meter, and counting the number of the magnetic particles with different particle sizes.
2. The method for testing the cleanliness of magnetic particles extracted by high magnetic force according to claim 1, wherein the step 2 comprises the following steps:
step 2.1, weighing a sample, placing the sample in a ball milling tank, placing a strong magnetic rod which is subjected to plastic packaging and is washed by pure water, adding the pure water to a scale mark of the ball milling tank with the marked capacity, adding water while pressing a tank body, and exhausting air; after adding water, tightly covering the cover of the ball milling tank and tightly sealing the cover with a sealing film;
and 2.2, inserting the roller mixer into a socket, adjusting a rotating speed switch on an operation screen to enable the rotating speed of the roller mixer to be 60rpm, setting the stirring time to be 15min, placing the sealed ball milling tank on the roller mixer, and automatically stirring and mixing after starting the device.
3. The high magnetic force extraction magnetic particle cleanliness test method according to claim 1, wherein step 3.3 specifically comprises:
and 3.3, horizontally cutting the upper part of the aluminum plastic film of the strong magnetic bar by using ceramic scissors, cutting an opening on the side edge of the upper part, outwards and downwards bending the edges of the two cut upper parts, and taking out the strong magnetic bar.
4. The high magnetic force extraction magnetic particle cleanliness test method according to claim 1, wherein step 4.1 specifically comprises:
and 4.1, sealing the first beaker sealing film after magnetism is increased tightly, and placing the first beaker sealing film in ultrasonic equipment for water bath ultrasonic treatment for 10min.
5. The method for testing the cleanliness of the high-magnetic-force-extraction magnetic particles according to claim 1, wherein the step 5 of repeatedly extracting magnetism comprises:
presetting an execution time threshold, wherein the execution time threshold is more than 1;
step 5.1, sheathing a layer of aluminum foil bag outside the high-intensity magnetic rod, and winding and sealing the upper part of the high-intensity magnetic rod by using an O-shaped ring or a rubber band;
step 5.2, placing the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for more than 1 circle, taking out the strong magnetic rod from an opening above the aluminum foil bag, and flushing materials on an O-shaped ring or a rubber band and the aluminum foil bag into a second beaker;
step 5.3, adding 1 to the current execution times, judging whether the current execution times is greater than an execution time threshold, if not, turning to the step 5.1 for execution, if so, discarding the aluminum foil bag, the O-shaped ring or the rubber band, and turning to the step 5.4 for execution;
and 5.4, putting the second beaker into ultrasonic equipment for ultrasonic action.
6. The method for testing the cleanliness of the high-magnetic-force-extraction magnetic particles according to claim 5, wherein in the step 5 of repeatedly extracting magnetism, the step 5.2 is specifically as follows:
and 5.2, placing the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for 30 circles for about 1min, stirring for 5 times, and flushing the magnetic material adsorbed by the strong magnetic rod wrapped with the aluminum foil bag into a second beaker.
7. The method for testing the cleanliness of the high-magnetic-force-extraction magnetic particles according to claim 1, wherein the step 5 of repeatedly extracting magnetism comprises:
presetting an execution time threshold, wherein the execution time threshold is more than 1;
step 5.10, sheathing a layer of aluminum foil bag outside the high-intensity magnetic rod, and winding and sealing the upper part of the high-intensity magnetic rod by using an O-shaped ring or a rubber band;
step 5.20, placing the strong magnetic rod wrapped with the aluminum foil bag into a first beaker, stirring for more than 1 circle, taking out the strong magnetic rod from an opening above the aluminum foil bag, and flushing materials on an O-shaped ring or a rubber band and the aluminum foil bag into a second beaker;
step 5.30, putting the second beaker into ultrasonic equipment for ultrasonic action;
and 5.40, adding 1 to the current execution times, judging whether the current execution times is greater than an execution time threshold, if not, turning to the step 5.10 to execute, and if so, discarding the aluminum foil bag, the O-shaped ring or the rubber band.
8. The method for testing the cleanliness of the high-magnetic-force-extraction magnetic particles according to claim 7, wherein in the step 5 of repeatedly extracting magnetism, the step 5.20 is specifically as follows:
and 5.20, placing the strong magnetic bar wrapped with the aluminum foil bag into a first beaker, stirring for 30 circles for 5 times, controlling the time to be about 1min, and washing the magnetic material adsorbed by the strong magnetic bar wrapped with the aluminum foil bag into a second beaker.
9. The method for testing the cleanliness of the magnetic particles extracted by the high magnetic force according to claim 1, wherein the step 6 of suction filtration and drying comprises the following specific steps:
step 6.1, assembling a suction filtration device, performing suction filtration by using a nylon mesh filter membrane, simultaneously washing the inner wall of the second beaker by using a washing bottle, performing suction filtration for 3min after no visible water drops exist on the filter paper, and obtaining the filter membrane attached with particles after suction filtration;
and 6.2, translating the filter membrane subjected to suction filtration to an object slide by using tweezers, and drying the object slide in a drying oven at 60 ℃ for 30min.
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