CN115290416A - Magnetic particle cleanliness testing method - Google Patents
Magnetic particle cleanliness testing method Download PDFInfo
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- CN115290416A CN115290416A CN202211169817.2A CN202211169817A CN115290416A CN 115290416 A CN115290416 A CN 115290416A CN 202211169817 A CN202211169817 A CN 202211169817A CN 115290416 A CN115290416 A CN 115290416A
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Abstract
The invention provides a method for testing the cleanliness of magnetic particles, which comprises the following steps: step 1, plastic packaging of a magnetic rod; step 2, weighing and stirring; step 3, magnetism extraction and collection: placing a first external magnetic rod outside a ball milling tank cover to adsorb the magnetic rod in the ball milling tank, and removing the first external magnetic rod to enable the magnetic rod to fall into a beaker; washing the materials on the beaker and the magnetic rod by pure water along the wall of the beaker; cutting off the thermoplastic bag, taking out the magnetic rod, and leaving the thermoplastic bag in the beaker; step 4, ultrasonic treatment: placing the beaker in ultrasonic equipment for ultrasonic treatment, and taking out the thermoplastic bag in the beaker; step 5, magnetic extraction is repeated: adsorbing the second external magnetic bar around the outer wall of the beaker for at least one circle, placing the beaker at the bottom of the beaker, pouring out water in the beaker, adding ethanol, placing the beaker in ultrasonic equipment for ultrasonic treatment, and pouring out the ethanol; step 6, suction filtration and drying; 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 magnetic particle cleanliness testing method.
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 rolling shaft 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. and (3) 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.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the magnetic particle cleanliness testing method is provided, and the magnetic particles in the particles adsorbed by the magnetic rod wrapping the thermoplastic bag are fully extracted, so that the non-magnetic particles in the particles to be detected placed in the cleanliness meter are reduced as much as possible, the dependence of the cleanliness meter on workers 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 magnetic particles, the method comprising:
step 1, plastic packaging of a magnetic rod:
step 1.1, the magnetic rod is arranged in a thermoplastic belt and is completely plastically packaged by a thermoplastic machine;
step 1.2, cutting off the redundant part of the thermoplastic bag 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-sealed magnetic rod, adding pure water into the ball milling tank, and tightly covering the cover of the ball milling tank;
step 2.2, placing the ball milling tank on a roller mixer to automatically stir and mix uniformly;
step 3, magnetism extraction and collection:
step 3.1, taking down the ball milling tank after automatic stirring, placing a first external magnetic rod outside a cover of the ball milling tank to adsorb the magnetic rod in the ball milling tank, opening the cover of the ball milling tank, moving the magnetic rod to the position above a beaker, separating the first external magnetic rod from the cover of the ball milling tank, and dropping the magnetic rod in the beaker;
3.2, washing materials on the beaker and the magnetic rod by pure water along the wall of the beaker;
3.3, cutting off the thermoplastic bag of the magnetic rod, taking out the magnetic rod, and keeping the thermoplastic bag in a beaker;
step 4, ultrasound:
step 4.1, adding pure water into the beaker with the thermoplastic bag, placing the beaker in ultrasonic equipment for water bath ultrasonic treatment, and taking out the beaker after the ultrasonic treatment is finished;
step 4.2, taking out the thermoplastic bag in the beaker, washing the outer surface of the thermoplastic bag by pure water and collecting water into the beaker;
step 5, magnetic extraction is repeated:
step 5.1, adsorbing the second external magnetic bar around the outer wall of the beaker for at least one circle, then placing the magnetic bar at the bottom of the beaker, and slowly washing the magnetic bar along the inner wall of the beaker by using pure water to enable the magnetic substance to be gathered at the bottom of the beaker; pouring out water in the beaker, adding ethanol, putting the beaker in ultrasonic equipment, and pouring out the ethanol after ultrasonic treatment;
step 5.2 repeating the action of step 5.1 at least once;
step 6, suction filtration and drying:
step 6.1, injecting pure water into the beaker;
step 6.2, assembling a suction filtration device, carrying out suction filtration by using a filter membrane, washing the inner wall of the beaker by using a washing bottle, and carrying out suction filtration to obtain the filter membrane attached with particles;
6.3, 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 have metal reflectivity or not and whether the particles are metal reflective magnetic particles or not 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 plastic-packaged magnetic rod, adding pure water to a calibration capacity scale mark of the ball milling tank, discharging air after adding the pure water, covering a cover of the ball milling tank tightly, and sealing tightly by using 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 60min, placing the sealed ball milling tank on the roller mixer, and automatically stirring and mixing after starting the device.
Further, step 3.2 of step 3 magnetic field extraction and collection further comprises:
3.2, washing materials on the beaker and the magnetic rod by using pure water along the wall of the beaker, attaching the first external magnetic rod to the outer wall of the beaker to adsorb the magnetic rod in the beaker, and slowly rolling the first external magnetic rod for at least one circle along the beaker to pour the water in the beaker; this process is repeated at least once until the water in the beaker is clear and the first external magnetic bar is removed.
Further, step 3, magnetic extraction and collection are specifically as follows:
step 3.1, taking down the ball milling tank after automatic stirring, attaching a first external magnetic rod to the outside of the cover of the ball milling tank to adsorb the magnetic rod in the ball milling tank, opening the cover of the ball milling tank, moving the magnetic rod attached to the cover of the ball milling tank to the upper part of a beaker, pulling the first external magnetic rod upwards to separate the first external magnetic rod from the cover of the ball milling tank, and dropping the magnetic rod in the beaker;
3.2, washing materials on the beaker and the magnetic rod by using pure water along the wall of the beaker, attaching the first external magnetic rod to the outer wall of the beaker to adsorb the magnetic rod in the beaker, slowly rolling the first external magnetic rod for 5 circles along the beaker, and pouring water in the beaker; repeating the process for 3 times until the water in the beaker is clear, and taking away the first external magnetic rod;
and 3.3, cutting off and horizontally flattening one long side of two short sides of the thermoplastic bag of the magnetic rod, bending the obtained edges of the two cut long sides downwards and outwards, taking out the magnetic rod, and leaving the thermoplastic bag in a beaker.
Further, step 4.1 specifically comprises:
and 4.1, adding pure water into the beaker with the thermoplastic bag, sealing the beaker by using a sealing film, placing the beaker in an ultrasonic device for carrying out ultrasonic treatment in ice-water bath for 5min, and taking out the beaker.
Further, step 5 is repeated to carry magnetism, specifically:
step 5.1, adsorbing the second external magnetic bar for two circles around the outer wall of the beaker, then placing the second external magnetic bar at the bottom of the beaker, and slowly flushing the second external magnetic bar along the inner wall of the beaker by using water to enable the magnetic substances to be gathered at the bottom of the beaker; pouring out water in the beaker, adding 10ml of ethanol, and pouring out the ethanol after ultrasonic treatment for 1 min;
step 5.2 the action of step 5.1 is repeated 3 times.
Further, the number of the second outer magnetic rods in the step 5.1 is two, and each second outer magnetic rod is a magnetic rod above 5700 GS.
Further, step 6, suction filtration and drying specifically comprise:
step 6.1, injecting 20ml of pure water into the beaker;
step 6.2, assembling a suction filtration device, carrying out suction filtration by using a nylon mesh filter membrane, simultaneously washing the inner wall of the beaker by using a washing bottle, carrying out 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 6.3, 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: the step of repeatedly carrying out magnetism is added, in the process of repeatedly carrying out magnetism, firstly, the second external magnetic rod is used for adsorbing magnetic particles along the outer wall of the beaker in a surrounding mode, the magnetic particles and the non-magnetic particles in the beaker are fully separated, water containing the non-magnetic particles is poured off, secondly, ethanol is added for carrying out ultrasound, the magnetic particles and the non-magnetic particles are fully dispersed, adhesion is prevented, thirdly, the actions of the second external magnetic rod in the surrounding mode and the ethanol ultrasound adding mode are repeatedly carried out, the effect of maximally dispersing the magnetic particles and the non-magnetic particles is achieved, accordingly, follow-up monitoring on the magnetic particles on a cleanliness meter is facilitated, misjudgment of the cleanliness meter is reduced to the maximum extent, dependence of the cleanliness meter on manual work is reduced, and the accuracy of detection results is higher.
Drawings
FIG. 1 is a flow chart of a magnetic particle cleanliness testing method according to an embodiment of the present invention;
fig. 2 is a drawing of the magnetic bar after plastic encapsulation according to the embodiment of the invention.
Detailed Description
In order to explain technical contents, achieved objects, and 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 and fig. 2, an embodiment of the present invention is:
a magnetic particle cleanliness testing method selects a magnetic rod with the length of 5 cm and the bottom surface diameter of 1.8 cm, and a 400g sample is tested by the following specific steps:
step 1, plastic packaging of a magnetic rod:
step 1.1, arranging a magnetic rod into a thermoplastic belt, and completely plastically packaging the thermoplastic belt by using a thermoplastic machine, wherein the sealing position of the thermoplastic belt is upward, and the non-magnetic end of the magnetic rod is upward; in the step, the thermoplastic bag is thin, and has small influence on the magnetic force of the magnetic bar;
step 1.2, cutting off redundant parts of the thermoplastic bag by using ceramic scissors, wherein the pattern after the magnetic bar is sealed and molded is specifically shown in figure 2;
step 2, weighing and stirring:
step 2.1, weighing 400g +/-2.00 g of sample, placing the sample in a 500ml ball milling tank, placing a plastic-sealed magnetic rod, adding pure water to 500ml 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 a sample in the ball milling tank is in full contact with the magnetic rod wrapping the thermoplastic bag;
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 60min, placing the sealed ball milling tank on the roller mixer, and automatically stirring and mixing after starting the device; the step ensures that the sample is fully contacted with the magnetic rod wrapping the thermoplastic bag, the magnetic rod can adsorb magnetic particles in the sample to the maximum extent in the ball milling tank, the automatic stirring time is long, and the effect is good;
step 3, magnetism extraction and collection:
step 3.1, taking down the ball milling tank which rolls for 60min, attaching a first external magnetic rod to the outside of a cover of the ball milling tank to adsorb the magnetic rod in the ball milling tank, opening the cover of the ball milling tank, moving the magnetic rod attached to the cover of the ball milling tank to the upper part of a beaker, pulling the first external magnetic rod upwards to separate the first external magnetic rod from the cover of the ball milling tank, and dropping the magnetic rod into a 150ml beaker; the step ensures that no other article is contacted with the magnetic bar wrapping the thermoplastic bag, and prevents the magnetic bar wrapping the thermoplastic bag from being mixed with other articles;
3.2, washing materials on the beaker and the magnetic rod by using pure water along the wall of the beaker, attaching the first external magnetic rod to the outer wall of the beaker to adsorb the magnetic rod in the beaker, slowly rolling the first external magnetic rod for 5 circles along the beaker, and pouring water in the beaker; repeating the process for 3 times until the water in the beaker is clear, and taking away the first external magnetic bar; the step is that before the magnetic bar in the thermoplastic bag is taken out, the magnetic particles and the nonmagnetic particles in the beaker are separated for the first time, and the nonmagnetic particles are discharged out of the beaker, so that the nonmagnetic particles in the beaker are reduced as much as possible, and the influence on the detection of a cleanliness meter is reduced; the first external magnetic rod can not only increase the adsorption force on magnetic particles in the beaker, but also effectively prevent the magnetic rod wrapping the thermoplastic bag from falling out of the beaker in the process of pouring water;
3.3, cutting off and horizontally flattening two short edges and a long edge of the thermoplastic bag of the magnetic rod, bending the edges of the two cut long edges downwards and outwards, taking out the magnetic rod, and leaving the thermoplastic bag in a beaker; the bending state of the thermoplastic bag in the step can effectively prevent the magnetic bar from taking away the magnetic particles outside the thermoplastic bag;
step 4, ultrasound:
step 4.1, adding 60ml of pure water into the beaker with the thermoplastic bag, sealing the beaker by a sealing film, placing the beaker in an ultrasonic device for 5min by ice-water bath ultrasound, and taking out the beaker; the step is to disperse the magnetic particles and the non-magnetic particles in the beaker and separate the particles from the thermoplastic bag;
step 4.2, taking out the thermoplastic bag in the beaker, washing the outer surface of the thermoplastic bag by pure water and collecting the water into the beaker;
step 5, magnetic extraction is repeated:
step 5.1, adsorbing two second external magnetic rods more than 5700GS around the outer wall of the beaker for two circles, then placing the magnetic rods at the bottom of the beaker, and slowly washing the magnetic rods along the inner wall of the beaker by pure water to ensure that magnetic substances are gathered at the bottom of the beaker, wherein about 30ml of water is used; pouring out water in the beaker, adding 10ml of ethanol, and pouring out the ethanol after ultrasonic treatment for 1 min; the step enables the magnetic particles and the non-magnetic particles in the beaker to be fully separated, the non-magnetic particles to be fully discharged, and the magnetic particles and the non-magnetic particles to be fully dispersed and not easy to adhere; the two magnetic rods above 5700GS enable the second external magnetic rod to have larger magnetic force and stronger adsorption capacity on magnetic particles on one hand, and enable the whole action area of the second external magnetic rod to be large on the other hand;
step 5.2 repeat the action of step 5.1 for 3 times; this step maximizes the extraction of the magnetic particles;
step 6, suction filtration and drying:
step 6.1, injecting 20ml of pure water into the beaker;
step 6.2, assembling a suction filtration device, performing suction filtration by using a 5-micron nylon mesh filter membrane, washing the inner wall of the 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 6.3, translating the filter membrane after suction filtration to an object slide by using tweezers, and drying the object slide in a drying oven at 60 ℃ for 30min (ensuring that the object slide has no water vapor);
and 7, testing:
detecting whether the particles on the filter membrane have reflectivity or not and whether the particles are metal magnetic particles or not by using a cleanliness meter, and counting the number of the magnetic particles with different particle sizes, wherein the specific steps of detecting the magnetic particles by using the cleanliness meter are described in the following by reading the 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 beginning of scanning, clicking < document > - < automatic scanning >, horizontally placing the particle standard block into a groove of a filter membrane bracket, adjusting the multiplying factor to be 1.0, focusing to the maximum FOC (FOC is a focusing button on a reading and beautifying cleanliness meter and is an abbreviation of an English word of Focus), 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, scanning again, 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, clicking automatic scanning, and writing batch information, sample preparation date, analysis date, sample preparation mode and other information in the sample number;
7.3.3 clicking 'continue', automatically calibrating the polarizer, checking whether the position of the zooming 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 the filter membrane;
step 7.4 confirmation of results:
7.4.1 after the scanning is finished, clicking three types of metal particles, non-metal particles containing no fibers and fibers, checking and analyzing the 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 ligation: 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 steps of deleting, cutting, connecting and the like, generate a report, and save the path and the 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, 400g of the samples are weighed each time for testing, 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 provided by the invention has the beneficial effects that:
1. the sample in the ball milling tank can be fully contacted with the outer surface of the magnetic rod wrapping the thermoplastic bag, and the magnetic particles in the sample can be adsorbed to the maximum extent;
2. before the thermoplastic bag is cut open, the magnetic particles and the nonmagnetic particles adsorbed by the magnetic bar are separated for the first time, so that the influence of the nonmagnetic particles on the misjudgment of the detection result of the cleanliness meter is reduced;
3. after the magnetic bar is taken out, carrying out ultrasonic treatment on the thermoplastic bag to ensure that particles on the thermoplastic bag fall off as much as possible and the particles in the beaker are dispersed as much as possible;
4. carrying out secondary separation on the magnetic particles and the nonmagnetic particles in the beaker by using two second external magnetic rods with strong magnetic force, and adding ethanol for carrying out ultrasonic treatment for multiple times to disperse the particles as much as possible;
in conclusion, magnetic particles and nonmagnetic particles are separated for many times, and are subjected to ultrasonic treatment for many times, so that the magnetic particles are extracted to the maximum extent, the nonmagnetic particles are discharged, and the nonmagnetic particles in the particles to be detected placed in the cleanliness instrument are reduced as much as possible, so that the dependence of the cleanliness instrument on manpower is reduced, and the accuracy of a detection result is higher.
The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention and the contents of the accompanying drawings, which are directly or indirectly applied to the related technical fields, are included in the scope of the present invention.
Claims (8)
1. A method for testing the cleanliness of magnetic particles is characterized by comprising the following steps:
step 1, plastic packaging of a magnetic rod:
step 1.1, the magnetic rods are arranged in a thermoplastic belt and are completely plastically packaged by a thermoplastic machine;
step 1.2, cutting off the redundant parts of the thermoplastic bag 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-sealed magnetic rod, adding pure water into the ball milling tank, 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, placing a first external magnetic rod outside a cover of the ball milling tank to adsorb the magnetic rod in the ball milling tank, opening the cover of the ball milling tank, moving the magnetic rod to the upper part of a beaker, separating the first external magnetic rod from the cover of the ball milling tank, and dropping the magnetic rod in the beaker;
3.2, washing the materials on the beaker and the magnetic rod by using pure water along the wall of the beaker;
3.3, cutting off the thermoplastic bag of the magnetic rod, taking out the magnetic rod, and keeping the thermoplastic bag in the beaker;
step 4, ultrasonic treatment:
step 4.1, adding pure water into the beaker with the thermoplastic bag, placing the beaker in ultrasonic equipment for water bath ultrasonic treatment, and taking out the beaker after the ultrasonic treatment is finished;
step 4.2, taking out the thermoplastic bag in the beaker, washing the outer surface of the thermoplastic bag by pure water and collecting water into the beaker;
step 5, magnetic extraction is repeated:
step 5.1, adsorbing the second external magnetic bar around the outer wall of the beaker for at least one circle, then placing the magnetic bar at the bottom of the beaker, and slowly washing the magnetic bar along the inner wall of the beaker by using pure water to enable the magnetic substance to be gathered at the bottom of the beaker; pouring out water in the beaker, adding ethanol, putting the beaker in ultrasonic equipment, and pouring out the ethanol after ultrasonic treatment;
step 5.2 repeating the action of step 5.1 at least once;
step 6, suction filtration and drying:
step 6.1, injecting pure water into the beaker;
step 6.2, assembling a suction filtration device, carrying out suction filtration by using a filter membrane, washing the inner wall of the beaker by using a washing bottle, and carrying out suction filtration to obtain the filter membrane attached with particles;
6.3, 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.
2. The method for testing the cleanliness of magnetic particles according to claim 1, wherein the step 2 comprises the steps of weighing and stirring:
step 2.1, weighing a sample, placing the sample in a ball milling tank, placing a plastic-packaged magnetic rod, adding pure water to a calibrated capacity scale mark of the ball milling tank, discharging air after adding the 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 60min, placing the sealed ball milling tank on the roller mixer, and automatically stirring and mixing after starting the device.
3. The magnetic particle cleanliness test method according to claim 1, wherein step 3.2 of step 3, magnetic field extraction and collection, further comprises:
3.2, washing materials on the beaker and the magnetic rod by using pure water along the wall of the beaker, attaching the first external magnetic rod to the outer wall of the beaker to adsorb the magnetic rod in the beaker, and slowly rolling the first external magnetic rod for at least one circle along the beaker to pour the water in the beaker; this process is repeated at least once until the water in the beaker is clear and the first external magnetic bar is removed.
4. The magnetic particle cleanliness test method according to claim 3, wherein step 3 comprises magnetic extraction and collection, specifically:
step 3.1, taking down the ball milling tank after automatic stirring, attaching a first external magnetic rod to the outside of a cover of the ball milling tank to adsorb the magnetic rod in the ball milling tank, opening the cover of the ball milling tank, moving the magnetic rod attached to the cover of the ball milling tank to the upper part of a beaker, pulling the first external magnetic rod upwards to separate the first external magnetic rod from the cover of the ball milling tank, and dropping the magnetic rod in the beaker;
3.2, washing materials on the beaker and the magnetic rod by using pure water along the wall of the beaker, attaching the first external magnetic rod to the outer wall of the beaker to adsorb the magnetic rod in the beaker, slowly rolling the first external magnetic rod for 5 circles along the beaker, and pouring water in the beaker; repeating the process for 3 times until the water in the beaker is clear, and taking away the first external magnetic rod;
and 3.3, cutting off and horizontally flattening one long side of two short sides of the thermoplastic bag of the magnetic rod, bending the obtained edge of the two cut long sides downwards and outwards, taking out the magnetic rod, and leaving the thermoplastic bag in a beaker.
5. The magnetic particle cleanliness test method according to claim 1, wherein step 4.1 specifically comprises:
and 4.1, adding pure water into the beaker with the thermoplastic bag, sealing the beaker by using a sealing film, placing the beaker in an ultrasonic device for carrying out ultrasonic treatment in ice-water bath for 5min, and taking out the beaker.
6. The magnetic particle cleanliness testing method according to claim 1, wherein step 5 comprises repeating the magnetic lifting, specifically:
step 5.1, adsorbing the second external magnetic rod for two circles around the outer wall of the beaker, placing the second external magnetic rod at the bottom of the beaker, and slowly washing the second external magnetic rod along the inner wall of the beaker by using water to enable magnetic substances to be gathered at the bottom of the beaker; pouring out water in the beaker, adding 10ml of ethanol, and pouring out the ethanol after ultrasonic treatment for 1 min;
step 5.2 the action of step 5.1 is repeated 3 times.
7. The magnetic particle cleanliness test method according to claim 6, wherein the number of the second external magnetic rods in step 5.1 is two, and each of the second external magnetic rods is a magnetic rod of 5700GS or more.
8. The method for testing the cleanliness of the magnetic particles according to claim 1, wherein the step 6 of suction filtration and drying comprises the following specific steps:
step 6.1, injecting 20ml of pure water into the beaker;
step 6.2, assembling a suction filtration device, carrying out suction filtration by using a nylon mesh filter membrane, simultaneously washing the inner wall of the beaker by using a washing bottle, carrying out 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 6.3, 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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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016058561A1 (en) * | 2014-10-13 | 2016-04-21 | 中国环境科学研究院 | Magnetic nanomaterial solid phase extraction agent, and preparation method and use therefor |
| WO2018109075A1 (en) * | 2016-12-15 | 2018-06-21 | Qiagen Gmbh | Method for isolating highly pure nucleic acid with magnetic particles |
| WO2019088106A1 (en) * | 2017-10-31 | 2019-05-09 | 大研医器株式会社 | Magnetic particle collection method and test set |
| CN110333168A (en) * | 2019-08-02 | 2019-10-15 | 江苏塔菲尔新能源科技股份有限公司 | A kind of detection method of magnetic-particle |
| CN110398402A (en) * | 2019-07-22 | 2019-11-01 | 中国科学院地球环境研究所 | A purification method suitable for different mineral composition rocks or sand sample quartz |
| CN111889077A (en) * | 2019-05-06 | 2020-11-06 | 北京化工大学 | Preparation of Modified Magnetic Zeolite Imidazole Framework Materials and Adsorption of Trace Ceftazidime in Water |
| CN113376063A (en) * | 2021-05-24 | 2021-09-10 | 合肥国轩高科动力能源有限公司 | Detection method of magnetic foreign matter |
| CN114361378A (en) * | 2021-12-14 | 2022-04-15 | 宁德厦钨新能源材料有限公司 | Electrochemical performance detection method of ternary material |
| CN114966121A (en) * | 2022-06-09 | 2022-08-30 | 浙江南都电源动力股份有限公司 | Method for identifying magnetic foreign matters in lithium battery material |
-
2022
- 2022-09-26 CN CN202211169817.2A patent/CN115290416A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016058561A1 (en) * | 2014-10-13 | 2016-04-21 | 中国环境科学研究院 | Magnetic nanomaterial solid phase extraction agent, and preparation method and use therefor |
| WO2018109075A1 (en) * | 2016-12-15 | 2018-06-21 | Qiagen Gmbh | Method for isolating highly pure nucleic acid with magnetic particles |
| WO2019088106A1 (en) * | 2017-10-31 | 2019-05-09 | 大研医器株式会社 | Magnetic particle collection method and test set |
| CN111889077A (en) * | 2019-05-06 | 2020-11-06 | 北京化工大学 | Preparation of Modified Magnetic Zeolite Imidazole Framework Materials and Adsorption of Trace Ceftazidime in Water |
| CN110398402A (en) * | 2019-07-22 | 2019-11-01 | 中国科学院地球环境研究所 | A purification method suitable for different mineral composition rocks or sand sample quartz |
| CN110333168A (en) * | 2019-08-02 | 2019-10-15 | 江苏塔菲尔新能源科技股份有限公司 | A kind of detection method of magnetic-particle |
| CN113376063A (en) * | 2021-05-24 | 2021-09-10 | 合肥国轩高科动力能源有限公司 | Detection method of magnetic foreign matter |
| CN114361378A (en) * | 2021-12-14 | 2022-04-15 | 宁德厦钨新能源材料有限公司 | Electrochemical performance detection method of ternary material |
| CN114966121A (en) * | 2022-06-09 | 2022-08-30 | 浙江南都电源动力股份有限公司 | Method for identifying magnetic foreign matters in lithium battery material |
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