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Standard of the Ministry of Electronics Industry of the People's Republic of China SJ2253--82
Cathode carbonate
Published on December 29, 1982
Approved by the Ministry of Electronics Industry of the People's Republic of China and implemented on July 1, 1983
Standard of the Ministry of Electronics Industry of the People's Republic of China
Determination method of cathode carbonate particle size (temporary)
This method is applicable to the determination of cathode carbonate particle size. 1 Light transmission powder particle size distribution test method SJ2253-82
This method uses the WID-C301 powder particle size distribution tester to determine the cathode carbonate particle size, and its range is 0 to 100 microns. 1.1 Basic principle
1.1.1 The working principle of the light transmission powder particle size distribution tester is shown in Figure 1. Figure 1
1-light source, 6V, 15W incandescent bulb: 2-half convex lens, converts the light of the bulb into parallel light, 3-slit, the parallel light transmitted by lens "2" passes through this slit and then shines on the sedimentation III-a small beam of light 4-sedimentation dish, containing the suspension containing the sample to be tested, 5-biconvex lens, focuses the transmitted light and irradiates it on the photoelectric tube, 6-phototube, converts the absorbed light into photocurrent and outputs it to the recorder, 1. One person incident light; I-transmitted light: A-phototube anode, K-phototube cathode 1.1.2 Working principle
Put the powder to be tested into the liquid as the dispersion medium, and stir it continuously to make the powder particles evenly dispersed in the liquid medium. When the stirring stops, the sedimentation velocity of the powder particles in the dispersion medium conforms to Stokes' law. The particle size is different, and the sedimentation velocity is also different, so the particle concentration in the suspension is formed with different distributions along the height. Using the principle of particle absorption of light, a parallel light beam is used to automatically scan the entire suspension from bottom to top, and the relationship curve between particles of different particle sizes marked with H (in this instrument, the movement of the recording paper and the movement of the sedimentation blood from top to bottom relative to the light beam are synchronized at the same speed, so the vertical coordinate corresponds to the sedimentation height h from the liquid surface and the time 1 from the beginning of sedimentation) and the transmitted light intensity /. According to Stoke's new law, the particle diameter D is related to the sedimentation height h and the sedimentation time t. After conversion, it can be obtained! The relationship between g/ and D can be calculated from it to calculate the particle size distribution of the measured powder. 1.2 Determination method
1.2.1 Before the measurement of this instrument, the power must be turned on first, and the positions of each knob are as follows! Issued by the Ministry of Electronics Industry of the People's Republic of China on December 29, 1982 and implemented on July 1, 1983
SJ2253--82
1.2.1.1 Set the power switch to "on" and preheat for 30 minutes; 1.2.1.2 Set the optical scanning speed switch to "4 mm/min"; 1.2.1.3 Set the height of the sedimentation tank to "0" cm according to the "scale" on the ruler; 1.2.1.4 Set the optical scanning switch to "manual"; 1.2.1.5 Set the measurement band switch to "off". 1.2.2 Sample preparation
Put the sample to be tested in a small beaker (10 ml), grind the carbonate powder evenly with a glass rod, then add a drop of 1% sodium hexametaphosphate solution, and then add 3 to 4 drops of dispersion medium, i.e. deionized water, and mix the powder into a paste until it is evenly dispersed for use in testing. 1.2.3 Test steps
First, adjust the sedimentation III containing pure dispersion medium to "zero" and full scale (the recording pen indicates between 80 and 90 on the recording paper), take it out after adjustment, slowly drip a little of the prepared paste of the powder to be tested into the sedimentation dish, and stir it up and down with a stick until it is uniform. Put the sedimentation dish immediately into the dark box of the analysis room (note: do not let the solution overflow), then set the band switch to the "measurement" position, and check whether the recording pen indicates between 10 and 20 on the recording paper (around 15 is the best). If the concentration of the suspension is appropriate, start the test. Set the measurement band switch to "off"; the scanning switch to "manual": the paper feed speed of the recorder is adjusted to 16 mm/min, and the recording pen starts to move. Stir the suspension, cover the dark room immediately after stirring, and quickly set the measurement band switch to the dry measurement position. At this time, the sedimentation blood seat automatically descends from the top with the sedimentation III, and at the same time the recorder records the relationship curve of H and. When the test is completed, turn the paper feed speed switch back to "off"; turn the measurement band switch back to "off"; open the cover of the analysis chamber, put a 0-50℃ mercury thermometer into the sedimentation blood, measure the actual temperature of the suspension, and record it. 1.3 Data Processing
1.3.1 The HI curve recorded by the recorder is shown in Figure 2. H
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1-transmitted light intensity, 11-curve ordinate (meter); K-the total length of the curve ordinate H (mm). Because the paper feeding speed is 16 m/min, the whole test time is 15 minutes, so K = 16 × 15 = 240 mm, n is the starting point of the curve; n is the straight line segment, one corresponds to the transmitted light intensity at the place where the particle with the maximum particle size D)max is completely settled: 5--corresponds to the transmitted light intensity when the light scans to the highest position: H-the vertical coordinate of point a (mm) corresponds to the sedimentation height at the place where the maximum particle is completely settled 2
1.3.2 Calculation
SJ2253-82
1.3.2.1 According to Stokes' law, the particle diameter is calculated according to the following formula: D-175||tt| |Where: D
particle diameter (micrometer);
(PP)-t
viscosity of the sedimentation medium at the test temperature (poise); true density of the sample powder to be tested (g, cm3); density of the sedimentation medium at the test temperature (g/cm3); sedimentation height (i.e. the distance from the liquid surface to the point where the light beam scans the suspension) (cm); sedimentation time (i.e. the time after which all particles with a diameter of D have fallen below the position of the light beam) (minutes) (1)
According to actual needs, the particle size can be divided into several intervals, i.e. D1, D2, D..….Dmax, etc., and various calculations can be performed according to the table below. D, (micron)
H (micrometer)
Igla-Igl
Da-agl
Wmx100%
x100%+
Ig/,-Ig12
Dmigl,
Igl 2-Igls
Dm-Jigl
Wm+wm.+Wwm,+wmax
Wa×100%
Wmx100%
Ig max
Ig/3-1g/max
D,+Dmax
Daigl,
Wm×100%
Wm×100%+Dm
m3*100%
m*Total
SJ2253--82
Table: 1h---corresponding to the ordinate of each particle size on the curve (mm), its value is equal to 240→+1), where 2 is a constant
Cz=175/(PP)J
! ,1,! , the transmitted light intensity corresponding to each particle size (found out from the curve); Imax
the transmitted light intensity corresponding to the maximum particle size;),)2D,..Dma--particle size of each level (micrometer); Dm--the mean of two adjacent particle sizes (micrometer); m
is proportional to the weight of the powder particles in the sample between two adjacent particle sizes; ten thousand
1.4 Notes
the arithmetic mean diameter of the powder sample (micrometer). 1.4.1 The concentration of the cathode carbonate sample should be appropriately selected, otherwise it will affect the results of the powder particle size distribution. Therefore, when using this instrument, the concentration of the suspended sample must be controlled to be between 10 and 20 on the recording paper. 1.4.2 The accuracy of the particle distribution results measured by this instrument is closely related to the length of the sample dispersion time. Therefore, the sample dispersion time should be strictly controlled, generally 2 to 5 minutes is appropriate. 1.4.3 In order to make the sample dispersed evenly, when measuring the cathode carbonate particle size distribution, the sedimentation medium should be added with a proper amount of dispersant using distilled water, otherwise the powder will aggregate in the liquid and cause errors. 1.4.4. If the curve recorded during the test is distorted, the test should be stopped, and the various factors causing the curve distortion should be checked and corrected before retesting.
2 Digital display microscope measurement method
2.1 Basic Principle
Digital Display Microscope Particle Size Tester is a test system composed of a digital display micrometer and a measuring microscope. The digital display micrometer is a precision measuring device that uses a converter that converts mechanical displacement into an electrical signal and directly displays the measurement result in digital form. Its basic structure is: connect the micrometer with a precision multi-turn wire-wound potentiometer so that the particle diameter measured by the micrometer is expressed by changing the resistance of the micrometer into voltage. The corresponding relationship between the length and the display voltage, the K value, can be calibrated using a micrometer scale. Finally, the true diameter of the particle in each gear can be obtained by multiplying the
electrical grade count value by the human value. The block diagram of the digital display particle size tester is shown in Figure 3. 2.2 Measurement method 2.2.1 Sample preparation Digital ammeter SYA type Digital printer Counter Command print SJ2253--82 The powder particles should be evenly dispersed so that they are dispersed in the surrounding medium as single particles. 2.2.1.1 Dispersant Photosensitive Adhesive Formula
2.2.1.2 Powder Dispersion
68g of dimethyl phosphite
32g of benzophenone
32g of phthalic acid epoxy resin (photosensitizer)
6121, 5 parts
Choose a glass slide and cover glass with good transparency, use silk to wipe the glass slide clean; use a glass rod to add some photosensitive adhesive, drop it on the glass slide, then grab an appropriate amount of photosensitizer on the drop of photosensitive adhesive, and then add a few milligrams of the powder to be tested on the adhesive. Finally, use a glass column to squeeze the powder into the adhesive, and then pull up the glass column, repeat squeezing and pulling for many times, so that the powders are separated from each other and evenly distributed in the adhesive: cover the cover glass, and pay attention to eliminate bubbles. 2.2.1.3 Sample solidification
The purpose of sample solidification is: ②, to prevent re-aggregation during "ebb". ③, to fix the particles and eliminate Brownian motion. ③, to make it easier to store.
The method of sample internalization is to place the test piece under ultraviolet light for about 10 minutes, and the sample can be solidified. The circuit diagram of the ultraviolet lamp used for illumination is shown in Figure 4.
Ballast
Oil-immersed capacitor:
2.2.2 Measurement steps
2.2.2.1K value calibration
Push button switch
GGZ.300 type
Linear ultraviolet high-pressure mercury lamp
K value is the ratio of length and voltage display (length unit is micrometer, display voltage unit is millivolt). The calibration method is: the selected micrometer eyepiece is fixed on the graticule, a certain graticule is taken as the zero point line, the hand wheel of the micrometer eyepiece is rotated to make the right one of the two parallel graticules on the graticule coincide with the zero line, and then the microscope platform is moved to make the two coincident lines coincide with the third graticule on the micrometer scale; adjust the zero adjustment potentiometer W2 to make the digital voltmeter display zero; rotate the hand wheel of the micrometer eyepiece to make the selected graticule on the movable graticule travel 100 microns on the micrometer scale, and adjust the potentiometer W to make the digital voltage representation value an integer, such as 500 millivolts. The ratio of length to voltage K=100
=0.2 microns, millivolts is obtained.
2.2.2.2 Measurement of particle diameter
When the two parallel lines of the movable graticule sweep across the field of view, the long diameter is measured when the long diameter of the particle is encountered, the short diameter is measured when the short diameter is encountered, and the oblique diameter is measured when the residual diameter is encountered. The specific method of measuring the diameter is:
Move the microscope platform so that the right side of the particle is tangent to the zero line, and rotate the microscope hand wheel. Make the line on any side of the movable graticule tangent to the left side of the particle 5
SJ2253—82
. The voltage change caused by this length change is displayed by the voltage, and the counter counts in steps. The voltage value multiplied by the K value is the diameter of the particle.
2.3 Data processing
Digital display The measurement of particle size by microscope is to measure the specific diameter of the particle or a range of particle diameters. The particle size is expressed as the percentage of the number of particles in a certain range of particle diameters. In order to facilitate statistical analysis, a cumulative curve of particles can be drawn and the arithmetic average particle size can be calculated.
2.3.1 Cumulative curve - a curve showing the relationship between the diameter of particles smaller than a certain value and the cumulative percentage. The cumulative curve of ternary carbonate particle size is shown in Figure 5.
Particle size (μ)
Figure 5 Cumulative curve of ternary carbonate particle size
cp - coarseness. The diameter of the particle when the cumulative number of particles reaches 99%, expressed in microns less than: dme - median diameter. The diameter of the particle on the cumulative curve that is equivalent to (intersects) the central cumulative value; d. - 1st quartile diameter. The diameter of the particles on the cumulative curve that accumulate to 25%: d. - 3rd quartile diameter. The diameter of the particles on the cumulative curve that accumulate to 75% 2.3.2 Distribution curve - a curve showing the relationship between the particle diameter and its percentage. The distribution curve of ternary carbonate particle size is shown in Figure 6.
SJ2253-82
dmoa particle size (u)
Figure 6 Particle size distribution curve of ternary carbonate
dmoa is a modal diameter, a majority diameter. The diameter where the highest peak of the particle size distribution is located 2.3.3 Calculation of arithmetic mean particle size:
Where: - average particle size (micrometer);
- number of particles with diameter d;
d, the diameter of the ith particle.
2.4 Measurement error
2.4.1 Instrument error
(2)
2.4.1.1 The error caused by the stability of the measurement power supply and the output ripple voltage. When measuring 1 micrometer, the error is 1±0.10 micrometer. The error caused by the linear accuracy of the precision multi-turn wirewound potentiometer. When measuring 1 micrometer, the error is 1±0.16 micrometer. 2.4.1.2
2.4.1.3 The accuracy of the digital voltmeter is 0.03%. When measuring 1 micron, the error is 1±0.003 micron. 2.4.1.4 Error of the micrometer eyepiece. When measuring 1 micron, the error is 1±0.003 micron. 2.4.2 Accidental error
2.4.2.1 When preparing samples, false particles should be prevented, particles should be prevented from breaking, and uneven distribution of coarse and fine powders should be prevented. 2.4.2.2 Before testing, the sample should be fully observed and a representative field of view should be selected for testing. The number of test particles should be more than 2000.2 microns, millivolts.
2.2.2.2 Measurement of particle diameter
When the two parallel lines of the movable graticule sweep across the field of view, the long diameter is measured when the long diameter of the particle is encountered, the short diameter is measured when the short diameter is encountered, and the oblique diameter is measured when the residual diameter is encountered. The specific method of measuring the diameter is:
Move the microscope platform so that the right side of the particle is tangent to the zero line, and rotate the microscope hand wheel. Make the line on any side of the movable graticule tangent to the left side of the particle 5
SJ2253—82
. The voltage change caused by this length change is displayed by the voltage, and the counter counts in steps. The voltage value multiplied by the K value is the diameter of the particle.
2.3 Data processing
Digital display The measurement of particle size by microscope is to measure the specific diameter of the particle or a range of particle diameters. The particle size is expressed as the percentage of the number of particles in a certain range of particle diameters. In order to facilitate statistical analysis, a cumulative curve of particles can be drawn and the arithmetic average particle size can be calculated.
2.3.1 Cumulative curve - a curve showing the relationship between the diameter of particles smaller than a certain value and the cumulative percentage. The cumulative curve of ternary carbonate particle size is shown in Figure 5.
Particle size (μ)
Figure 5 Cumulative curve of ternary carbonate particle size
cp - coarseness. The diameter of the particle when the cumulative number of particles reaches 99%, expressed in microns less than: dme - median diameter. The diameter of the particle on the cumulative curve that is equivalent to (intersects) the central cumulative value; d. - 1st quartile diameter. The diameter of the particles on the cumulative curve that accumulate to 25%: d. - 3rd quartile diameter. The diameter of the particles on the cumulative curve that accumulate to 75% 2.3.2 Distribution curve - a curve showing the relationship between the particle diameter and its percentage. The distribution curve of ternary carbonate particle size is shown in Figure 6.
SJ2253-82
dmoa particle size (u)
Figure 6 Particle size distribution curve of ternary carbonate
dmoa is a modal diameter, a majority diameter. The diameter where the highest peak of the particle size distribution is located 2.3.3 Calculation of arithmetic mean particle size:
Where: - average particle size (micrometer);
- number of particles with diameter d;
d, the diameter of the ith particle.
2.4 Measurement error
2.4.1 Instrument error
(2)
2.4.1.1 The error caused by the stability of the measurement power supply and the output ripple voltage. When measuring 1 micrometer, the error is 1±0.10 micrometer. The error caused by the linear accuracy of the precision multi-turn wirewound potentiometer. When measuring 1 micrometer, the error is 1±0.16 micrometer. 2.4.1.2
2.4.1.3 The accuracy of the digital voltmeter is 0.03%. When measuring 1 micron, the error is 1±0.003 micron. 2.4.1.4 Error of the micrometer eyepiece. When measuring 1 micron, the error is 1±0.003 micron. 2.4.2 Accidental error
2.4.2.1 When preparing samples, false particles should be prevented, particles should be prevented from breaking, and uneven distribution of coarse and fine powders should be prevented. 2.4.2.2 Before testing, the sample should be fully observed and a representative field of view should be selected for testing. The number of test particles should be more than 2000.2 microns, millivolts.
2.2.2.2 Measurement of particle diameter
When the two parallel lines of the movable graticule sweep across the field of view, the long diameter is measured when the long diameter of the particle is encountered, the short diameter is measured when the short diameter is encountered, and the oblique diameter is measured when the residual diameter is encountered. The specific method of measuring the diameter is:
Move the microscope platform so that the right side of the particle is tangent to the zero line, and rotate the microscope hand wheel. Make the line on any side of the movable graticule tangent to the left side of the particle 5
SJ2253—82
. The voltage change caused by this length change is displayed by the voltage, and the counter counts in steps. The voltage value multiplied by the K value is the diameter of the particle.
2.3 Data processing
Digital display The measurement of particle size by microscope is to measure the specific diameter of the particle or a range of particle diameters. The particle size is expressed as the percentage of the number of particles in a certain range of particle diameters. In order to facilitate statistical analysis, a cumulative curve of particles can be drawn and the arithmetic average particle size can be calculated.
2.3.1 Cumulative curve - a curve showing the relationship between the diameter of particles smaller than a certain value and the cumulative percentage. The cumulative curve of ternary carbonate particle size is shown in Figure 5.
Particle size (μ)
Figure 5 Cumulative curve of ternary carbonate particle size
cp - coarseness. The diameter of the particle when the cumulative number of particles reaches 99%, expressed in microns less than: dme - median diameter. The diameter of the particle on the cumulative curve that is equivalent to (intersects) the central cumulative value; d. - 1st quartile diameter. The diameter of the particles on the cumulative curve that accumulate to 25%: d. - 3rd quartile diameter. The diameter of the particles on the cumulative curve that accumulate to 75% 2.3.2 Distribution curve - a curve showing the relationship between the particle diameter and its percentage. The distribution curve of ternary carbonate particle size is shown in Figure 6.
SJ2253-82
dmoa particle size (u)
Figure 6 Particle size distribution curve of ternary carbonate
dmoa is a modal diameter, a majority diameter. The diameter where the highest peak of the particle size distribution is located 2.3.3 Calculation of arithmetic mean particle size:
Where: - average particle size (micrometer);
- number of particles with diameter d;
d, the diameter of the ith particle.
2.4 Measurement error
2.4.1 Instrument error
(2)
2.4.1.1 The error caused by the stability of the measurement power supply and the output ripple voltage. When measuring 1 micrometer, the error is 1±0.10 micrometer. The error caused by the linear accuracy of the precision multi-turn wirewound potentiometer. When measuring 1 micrometer, the error is 1±0.16 micrometer. 2.4.1.2
2.4.1.3 The accuracy of the digital voltmeter is 0.03%. When measuring 1 micron, the error is 1±0.003 micron. 2.4.1.4 Error of the micrometer eyepiece. When measuring 1 micron, the error is 1±0.003 micron. 2.4.2 Accidental error
2.4.2.1 When preparing samples, false particles should be prevented, particles should be prevented from breaking, and uneven distribution of coarse and fine powders should be prevented. 2.4.2.2 Before testing, the sample should be fully observed and a representative field of view should be selected for testing. The number of test particles should be more than 2000.
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