CN107515149B - Method for detecting granularity and surface characteristics of diamond micropowder by using flow cytometer - Google Patents
Method for detecting granularity and surface characteristics of diamond micropowder by using flow cytometer Download PDFInfo
- Publication number
- CN107515149B CN107515149B CN201710747999.XA CN201710747999A CN107515149B CN 107515149 B CN107515149 B CN 107515149B CN 201710747999 A CN201710747999 A CN 201710747999A CN 107515149 B CN107515149 B CN 107515149B
- Authority
- CN
- China
- Prior art keywords
- solution
- diamond
- flow cytometer
- micro powder
- ultrasonic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 124
- 239000010432 diamond Substances 0.000 title claims abstract description 124
- 238000000034 method Methods 0.000 title claims abstract description 32
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 64
- 238000001514 detection method Methods 0.000 claims abstract description 55
- 239000002245 particle Substances 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 38
- 239000011780 sodium chloride Substances 0.000 claims abstract description 32
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 22
- -1 ethyl phenyl Chemical group 0.000 claims abstract description 22
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 22
- 238000009826 distribution Methods 0.000 claims abstract description 19
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000010586 diagram Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 7
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000005054 agglomeration Methods 0.000 abstract description 10
- 230000002776 aggregation Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 3
- 239000012530 fluid Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003703 image analysis method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
-
- 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
- G01N15/10—Investigating individual particles
- G01N15/14—Optical investigation techniques, e.g. flow cytometry
- G01N15/1404—Handling flow, e.g. hydrodynamic focusing
Landscapes
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)
Abstract
The invention discloses a method for detecting the granularity and surface characteristics of diamond micropowder by using a flow cytometer. Placing diamond micro powder of a detection sample in a container, adding a prepared sodium chloride solution, and stirring to obtain a diamond micro powder solution; putting the container filled with the diamond micropowder solution into an ultrasonic cell crusher for ultrasonic dispersion to obtain a preliminarily dispersed diamond micropowder solution; standing the obtained solution, adding the prepared ethyl phenyl polyethylene glycol solution, and shaking up; then placing the diamond powder into an ultrasonic cell crusher for ultrasonic dispersion again to obtain diamond powder solution to be detected; finally, a flow cytometer is adopted to automatically detect the diamond powder solution to be detected, and data are automatically stored; and finally calling data such as diameter, circularity, width-length ratio, strip ratio, particle size distribution diagram and the like, and analyzing results. The detection method can greatly reduce agglomeration, and has simple operation and obvious effect.
Description
The technical field is as follows:
the invention relates to a method for detecting the granularity and the surface characteristics of diamond micropowder, belongs to the technical field of superhard material micropowder, and particularly relates to a method for detecting the granularity and the surface characteristics of the diamond micropowder by using a flow cytometer.
Secondly, background art:
the diamond micropowder refers to diamond particles with the granularity of less than 36/54 microns, and in the production of the diamond micropowder, the use of the diamond micropowder is greatly influenced by the particle size distribution and the surface characteristics (the crystal form of the diamond micropowder), particularly in the field of diamond wire saw application. Different particle size distributions, different crystal forms, can have a severe impact on diamond wire cutting. In the production of diamond, the powder particles absorb a large amount of mechanical energy and heat energy to ensure that the surface of the powder particles has quite high specific surface energy, so that the particles are in an extremely unstable state and have a tendency of agglomeration, thereby causing pseudo large particles. Therefore, it is required to reduce agglomeration as precisely as possible in the detection of the diamond fine powder. In the existing detection of diamond micropowder, the particle size distribution is usually detected by a laser diffraction method and a resistance method in the industry, and a microscope is used for observing and judging the crystal form. However, because of different individual senses, the crystal form is not easy to describe, and data analysis is difficult to carry out, and the image analysis method of a microscope and a computer is few in detection particles, and the data are unstable. Therefore, it is necessary to develop a simple, efficient and accurate method.
Thirdly, the invention content:
the technical problem to be solved by the invention is as follows: aiming at the defects in the existing diamond micropowder detection technology, the invention provides a method for detecting the granularity and the surface characteristics of diamond micropowder by using a flow cytometer. The technical scheme of the invention is that the particle size distribution and the surface characteristics are directly measured by one-time detection of a fluidity cell instrument on the basis of more reasonable and scientific dispersion of the sample. Therefore, the detection method is simple, practical and efficient.
In order to solve the technical problems, the invention adopts the technical scheme that:
the invention provides a method for detecting the granularity and surface characteristics of diamond micropowder by using a flow cytometer, which comprises the following steps:
a. weighing the prepared diamond micropowder as a detection sample at room temperature for later use;
b. adding sodium chloride into water to prepare a sodium chloride solution, and filtering the obtained sodium chloride solution to obtain a sodium chloride solution for later use;
c. placing the diamond micro powder of the detection sample weighed in the step a into a container, adding the sodium chloride solution prepared in the step b, and stirring, wherein the addition amount of the volume of the sodium chloride solution is 200-300 times of the mass of the diamond micro powder, so as to obtain a diamond micro powder solution for later use;
d. c, placing the container filled with the stirred diamond micro powder solution in the step c on a lifting platform in an ultrasonic cell crusher, and lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micro powder solution for ultrasonic dispersion to obtain the preliminarily dispersed diamond micro powder solution;
e. adding ethyl phenyl polyethylene glycol into pure water to prepare an ethyl phenyl polyethylene glycol solution for later use;
f. taking out the container filled with the preliminarily dispersed diamond micro powder solution in the step d, standing, adding the ethyl phenyl polyethylene glycol solution prepared in the step e into the solution, and uniformly shaking for later use;
g. putting the container filled with the diamond micropowder solution obtained in the step f on a lifting platform in an ultrasonic cell crusher, lifting the lifting platform to immerse an ultrasonic probe into the diamond micropowder solution for ultrasonic dispersion to obtain a diamond micropowder solution to be detected;
h. pre-starting the flow cytometer for preheating, and selecting a sheath liquid special for the flow cytometer; in background detection, when background particles are less than 10 particles in high power and low power respectively, the marking liquid is operated to focus light, when the light is successfully focused, the detection is carried out, and SOP parameters are set; and g, adding the diamond micropowder solution to be detected obtained in the step g into a feeding port of a flow cytometer, and automatically detecting; after the detection is finished, automatically storing data, and then calling out a diameter, circularity, width-length ratio, strip ratio and granularity distribution map;
i. and d, analyzing the particle size distribution of the sample according to the diameter and particle size distribution diagram obtained in the step h, and analyzing the crystal form of the material according to the circularity, width-length ratio and strip ratio to obtain an analysis result.
According to the method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer, the mass percentage concentration of the sodium chloride solution prepared in the step b is 0.5-1.0%.
According to the method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer, the stirring time in the step c is 3-5 minutes.
According to the method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer, in the step d, the ultrasonic probe is immersed into the diamond micropowder solution for 1.0-2.0 cm; and during ultrasonic dispersion, the output ultrasonic power of the ultrasonic cell crusher is set to be 300W, and the dispersion time is set to be 3-5 min.
According to the method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer, the mass percentage concentration of the ethyl phenyl polyethylene glycol solution prepared in the step e is 0.05-0.2%.
According to the method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer, the standing time in the step f is 1-2 min; the addition amount of the ethyl phenyl polyethylene glycol solution is 0.05-0.1 mL.
According to the method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer, in the step g, an ultrasonic probe is immersed into the diamond micropowder solution for 1.0-2.0 cm; and during ultrasonic dispersion, the output ultrasonic power of the ultrasonic cell crusher is set to be 300W, and the dispersion time is set to be 3-5 min.
According to the method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer, the preheating time in the step h is 30 minutes; the set SOP parameters are set to be fixed particle values of 1000-5000, the diameter values of detected particles are 0.5-200 um, and the rotating speed is set to be 600-750 r/min; the addition amount of the diamond micro powder solution to be detected is 5 ml.
The invention has the following positive beneficial effects:
1. the invention firstly proposes that the materials are added into the prepared sodium chloride solution, compared with the materials added into pure water, the invention is beneficial to the definition of the material particle images and is not easy to form agglomeration; then, the solid impurities can be effectively removed by adopting a filter flask for filtration.
2. In the industry of detecting the diamond micropowder by using the flow cytometer, the invention firstly adopts multiple times of ultrasonic cell crushing and vibrating treatment, adjusts the optimal vibrating power and the optimal treating time, and disperses agglomerated particles of the diamond micropowder in an intermittent manner, thereby maximally reducing the existence of false 'large particles' and improving the detection precision and the detection efficiency.
3. In the detection process, after the diamond micropowder solution is treated in the ultrasonic cell crusher, a certain amount of ethyl phenyl polyethylene glycol solvent is added into the solution again by standing, the ethyl phenyl polyethylene glycol solvent can effectively disperse the diamond micropowder solution again, and then secondary ultrasonic vibration dispersion treatment is carried out on the solution again, so that the diamond micropowder particles agglomerated together are further dispersed, the dispersion effect is improved, and the detection precision is indirectly improved.
4. The detection method is obviously superior to the conventional detection method, because the conventional detection method directly adds the materials into water and has no prior dispersion treatment, a large amount of partial false large particles exist in the diamond micro-powder solution, and the detection precision error is larger; moreover, the detection time is long, and the result difference is large. After the detection method provided by the invention is subjected to dispersion treatment, the detection precision of the diamond particle size is improved, the agglomeration is reduced to the greatest extent, and meanwhile, the detection efficiency is also greatly improved.
5. The detection method of the invention uses less detection equipment, and can accurately detect the particle size distribution and the crystal form surface characteristics of the diamond micropowder by using a machine flow type cytometer and an auxiliary cell crusher in the detection of the diamond micropowder.
6. According to the invention, the surface characteristics of the diamond micro powder can be quantitatively analyzed through the measured related data.
In conclusion, the detection method is simple to operate, the agglomeration of the diamond micropowder in the result image can be reduced to the maximum extent, the detection precision of the diamond particle size and the detection accuracy of the surface characteristics are improved, and meanwhile, the detection efficiency is also greatly improved; the technical scheme of the invention can simultaneously, accurately and quickly detect the particle size distribution and the particle morphology of the diamond micro powder.
Fourthly, the specific implementation mode:
the invention is further illustrated by the following examples, but the technical content of the invention is not limited thereto.
Example 1:
the invention discloses a method for detecting the granularity and the surface characteristics of diamond micropowder by using a flow cytometer, which is characterized by comprising the following steps:
a. weighing 0.2g of prepared diamond micropowder as a detection sample at room temperature for later use;
b. adding sodium chloride into water to prepare a sodium chloride solution with the mass concentration of 0.9%, and filtering the obtained sodium chloride solution by adopting a filter flask to obtain a sodium chloride solution for later use;
c. b, placing 0.2g of the diamond micropowder of the detection sample weighed in the step a into a container, adding 40mL of the sodium chloride solution prepared in the step b, and stirring for 3 minutes to obtain a diamond micropowder solution for later use;
d. c, placing the container filled with the stirred diamond micropowder solution in the step c on a lifting platform in an ultrasonic cell crusher, lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micropowder solution for 1.6cm, setting the output ultrasonic power of the ultrasonic cell crusher to be 300W, and then carrying out ultrasonic dispersion on the diamond micropowder solution for 5min to obtain the preliminarily dispersed diamond micropowder solution;
e. adding an ethyl phenyl polyethylene glycol solvent into pure water to prepare an ethyl phenyl polyethylene glycol solution with the mass percentage concentration of 0.1% for later use;
f. taking out the container filled with the preliminarily dispersed diamond micro powder solution in the step d, standing for 2min, adding 0.1mL of ethyl phenyl polyethylene glycol solution prepared in the step e into the solution, and uniformly shaking for later use;
g. putting the container filled with the diamond micropowder solution obtained in the step f on a lifting platform in an ultrasonic cell crusher, lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micropowder solution for 1.6cm, setting the output ultrasonic power of the ultrasonic cell crusher to be 300W, and then carrying out ultrasonic dispersion on the diamond micropowder solution for 5min to obtain the diamond micropowder solution to be detected;
h. preheating by starting a flow cytometer in advance, wherein the preheating time is 30 minutes, selecting a special sheath fluid for the flow cytometer, in background detection, operating the standard fluid to perform light alignment when background particles are less than 10 particles in high power and low power respectively, and detecting when the light alignment is successful; setting SOP parameters, namely setting 1000-5000 fixed particle values, 0.5-200 um diameter values of detected particles and 600-750 r/min rotation speed; then adding 5 ml of the diamond micro powder solution to be detected obtained in the step g through a feeding port of the flow cytometer, and automatically detecting; after the detection is finished, automatically storing the data; the data results are detailed in table 1;
i. and d, analyzing the particle size distribution of the sample according to the diameter and particle size distribution diagram obtained in the step h, and analyzing the crystal form of the material according to the circularity, width-length ratio and strip ratio to obtain an analysis result.
TABLE 1 relevant data obtained by examining samples according to example 1 of the present invention
| Diameter of | Degree of circularity | Width to length ratio | Ratio of strips |
| 7.546 | 0.94 | 0.764 | 1.81 |
The direct detection by the existing method has more particle agglomeration, and the detection result is detailed in table 2.
TABLE 2 relevant data obtained from prior art testing of samples
| Diameter of | Degree of circularity | Width to length ratio | Ratio of strips |
| 7.604 | 0.93 | 0.753 | 2.69 |
Example 2:
the invention discloses a method for detecting the granularity and the surface characteristics of diamond micropowder by using a flow cytometer, which is characterized by comprising the following steps:
a. weighing 0.2g of prepared diamond micropowder as a detection sample at room temperature for later use;
b. adding sodium chloride into water to prepare a sodium chloride solution with the mass concentration of 0.6%, and filtering the obtained sodium chloride solution by adopting a filter flask to obtain a sodium chloride solution for later use;
c. b, placing 0.2g of the diamond micropowder of the detection sample weighed in the step a into a container, adding 50mL of the sodium chloride solution prepared in the step b, and stirring for 4 minutes to obtain a diamond micropowder solution for later use;
d. c, placing the container filled with the stirred diamond micropowder solution in the step c on a lifting platform in an ultrasonic cell crusher, lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micropowder solution for 1.0cm, setting the output ultrasonic power of the ultrasonic cell crusher to be 300W, and then carrying out ultrasonic dispersion on the diamond micropowder solution for 5min to obtain the preliminarily dispersed diamond micropowder solution;
e. adding an ethyl phenyl polyethylene glycol solvent into pure water to prepare an ethyl phenyl polyethylene glycol solution with the mass percentage concentration of 0.08% for later use;
f. taking out the container filled with the preliminarily dispersed diamond micro powder solution in the step d, standing for 2min, adding 0.1mL of ethyl phenyl polyethylene glycol solution prepared in the step e into the solution, and uniformly shaking for later use;
g. putting the container filled with the diamond micropowder solution obtained in the step f on a lifting platform in an ultrasonic cell crusher, lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micropowder solution for 1.2cm, setting the output ultrasonic power of the ultrasonic cell crusher to be 300W, and then carrying out ultrasonic dispersion on the diamond micropowder solution for 5min to obtain the diamond micropowder solution to be detected;
h. preheating by starting a flow cytometer in advance, wherein the preheating time is 30 minutes, selecting a special sheath fluid for the flow cytometer, in background detection, operating the standard fluid to perform light alignment when background particles are less than 10 particles in high power and low power respectively, and detecting when the light alignment is successful; setting SOP parameters, namely setting 1000-5000 fixed particle values, 0.5-200 um diameter values of detected particles and 600-750 r/min rotation speed; then adding 5 ml of the diamond micro powder solution to be detected obtained in the step g through a feeding port of the flow cytometer, and automatically detecting; after the detection is finished, automatically storing the data; the data results are detailed in table 3;
i. and d, analyzing the particle size distribution of the sample according to the diameter and particle size distribution diagram obtained in the step h, and analyzing the crystal form of the material according to the circularity, width-length ratio and strip ratio to obtain an analysis result.
TABLE 3 data relating to the examination of samples by the method of the invention and the prior art
| Diameter of | Degree of circularity | Width to length ratio | Ratio of strips | Comparison of the methods |
| 8.510 | 0.943 | 0.781 | 1.09 | Existing methods |
| 8.345 | 0.947 | 0.786 | 0.69 | Inventive example 2 |
Example 3:
the invention discloses a method for detecting the granularity and the surface characteristics of diamond micropowder by using a flow cytometer, which is characterized by comprising the following steps:
a. weighing 0.2g of prepared diamond micropowder as a detection sample at room temperature for later use;
b. adding sodium chloride into water to prepare a sodium chloride solution with the mass concentration of 0.8%, and filtering the obtained sodium chloride solution by adopting a filter flask to obtain a sodium chloride solution for later use;
c. b, placing 0.2g of the diamond micropowder of the detection sample weighed in the step a into a container, adding 60mL of the sodium chloride solution prepared in the step b, and stirring for 4 minutes to obtain a diamond micropowder solution for later use;
d. c, placing the container filled with the stirred diamond micropowder solution in the step c on a lifting platform in an ultrasonic cell crusher, lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micropowder solution for 1.8cm, setting the output ultrasonic power of the ultrasonic cell crusher to be 300W, and then carrying out ultrasonic dispersion on the diamond micropowder solution for 5min to obtain the preliminarily dispersed diamond micropowder solution;
e. adding an ethyl phenyl polyethylene glycol solvent into pure water to prepare an ethyl phenyl polyethylene glycol solution with the mass percentage concentration of 0.15% for later use;
f. taking out the container filled with the preliminarily dispersed diamond micro powder solution in the step d, standing for 2min, adding 0.08mL of ethyl phenyl polyethylene glycol solution prepared in the step e into the solution, and uniformly shaking for later use;
g. putting the container filled with the diamond micropowder solution obtained in the step f on a lifting platform in an ultrasonic cell crusher, lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micropowder solution for 1.8cm, setting the output ultrasonic power of the ultrasonic cell crusher to be 300W, and then carrying out ultrasonic dispersion on the diamond micropowder solution for 5min to obtain the diamond micropowder solution to be detected;
h. preheating by starting a flow cytometer in advance, wherein the preheating time is 30 minutes, selecting a special sheath fluid for the flow cytometer, in background detection, operating the standard fluid to perform light alignment when background particles are less than 10 particles in high power and low power respectively, and detecting when the light alignment is successful; setting SOP parameters, namely setting 1000-5000 fixed particle values, 0.5-200 um diameter values of detected particles and 600-750 r/min rotation speed; then adding 5 ml of the diamond micro powder solution to be detected obtained in the step g through a feeding port of the flow cytometer, and automatically detecting; after the detection is finished, automatically storing the data; the data results are detailed in table 4;
i. and d, analyzing the particle size distribution of the sample according to the diameter and particle size distribution diagram obtained in the step h, and analyzing the crystal form of the material according to the circularity, width-length ratio and strip ratio to obtain an analysis result.
TABLE 4 data relating to the examination of samples by the method of the present invention and the prior art
| Diameter of | Degree of circularity | Width to length ratio | Ratio of strips | Comparison of the methods |
| 9.443 | 0.901 | 0.689 | 10.32 | Existing methods |
| 9.094 | 0.907 | 0.701 | 9.83 | Inventive example 3 |
In summary, the comparison between the data obtained by the detection method of the present invention and the data obtained by the detection in the prior art shows that: the diamond micro powder is detected by the invention, the particle agglomeration is obviously reduced, and the diameter is reduced by 0.1 um. As agglomeration is reduced, the circularity aspect ratio increases and the strip ratio decreases. Therefore, the detection method can greatly reduce agglomeration, and has simple operation and obvious effect.
Claims (5)
1. A method for detecting the granularity and surface characteristics of diamond micropowder by using a flow cytometer is characterized in that
Characterized in that the detection method comprises the following steps:
a. weighing the prepared diamond micropowder as a detection sample at room temperature for later use;
b. adding sodium chloride into water to prepare sodium chloride solution, and filtering the obtained sodium chloride solution to obtain the sodium chloride
The sodium chloride solution is ready for use;
the mass percentage concentration of the prepared sodium chloride solution is 0.5-1.0%;
c. placing the diamond micro powder of the detection sample weighed in the step a into a container, adding the sodium chloride solution prepared in the step b, and stirring, wherein the addition amount of the volume of the sodium chloride solution is 200-300 times of the mass of the diamond micro powder, so as to obtain a diamond micro powder solution for later use;
d. c, placing the container filled with the stirred diamond micro powder solution in the step c on a lifting platform in an ultrasonic cell crusher, and lifting the lifting platform to enable an ultrasonic probe to be immersed into the diamond micro powder solution for ultrasonic dispersion to obtain the preliminarily dispersed diamond micro powder solution;
e. adding ethyl phenyl polyethylene glycol into pure water to prepare an ethyl phenyl polyethylene glycol solution for later use;
the mass percentage concentration of the prepared ethyl phenyl polyethylene glycol solution is 0.05-0.2%;
f. taking out the container filled with the diamond micro powder solution after the primary dispersion in the step d, standing, and then adding the diamond micro powder solution into the container
E, adding the ethyl phenyl polyethylene glycol solution prepared in the step e into the solution, and uniformly shaking for later use;
g. putting the container filled with diamond micropowder solution obtained in step f into an ultrasonic cell crusher
On the lifting platform, the lifting platform is lifted to immerse the ultrasonic probe into the diamond micropowder solution for ultrasonic dispersion to obtain
A diamond micro powder solution to be detected;
h. pre-starting the flow cytometer for preheating, and selecting a sheath liquid special for the flow cytometer; in background detection, when background particles are less than 10 particles in high power and low power respectively, the marking liquid is operated to focus light, when the light is successfully focused, the detection is carried out, and SOP parameters are set; and g, adding the diamond micropowder solution to be detected obtained in the step g into a feeding port of a flow cytometer, and automatically detecting; after the detection is finished, automatically storing data, and then calling out a diameter, circularity, width-length ratio, strip ratio and granularity distribution map;
the preheating time is 30 minutes; the set SOP parameters are set to be fixed particle values of 1000-5000, the diameter values of detected particles are 0.5-200 um, and the rotating speed is set to be 600-750 r/min; the adding amount of the diamond micro powder solution to be detected is 5 ml;
i. and d, analyzing the particle size distribution of the sample according to the diameter and particle size distribution diagram obtained in the step h, and analyzing the crystal form of the material according to the circularity, width-length ratio and strip ratio to obtain an analysis result.
2. The method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer as claimed in claim 1, wherein: and c, stirring for 3-5 minutes.
3. The method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer as claimed in claim 1, wherein: d, immersing the ultrasonic probe into the diamond micro powder solution for 1.0-2.0 cm; and during ultrasonic dispersion, the output ultrasonic power of the ultrasonic cell crusher is set to be 300W, and the dispersion time is set to be 3-5 min.
4. The method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer as claimed in claim 1, wherein: standing for 1-2 min in the step f; the addition amount of the ethyl phenyl polyethylene glycol solution is 0.05-0.1 mL.
5. The method for detecting the granularity and the surface characteristics of the diamond micropowder by using the flow cytometer as claimed in claim 1, wherein: step g, immersing the ultrasonic probe into the diamond micro powder solution for 1.0-2.0 cm; and during ultrasonic dispersion, the output ultrasonic power of the ultrasonic cell crusher is set to be 300W, and the dispersion time is set to be 3-5 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710747999.XA CN107515149B (en) | 2017-08-28 | 2017-08-28 | Method for detecting granularity and surface characteristics of diamond micropowder by using flow cytometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710747999.XA CN107515149B (en) | 2017-08-28 | 2017-08-28 | Method for detecting granularity and surface characteristics of diamond micropowder by using flow cytometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107515149A CN107515149A (en) | 2017-12-26 |
| CN107515149B true CN107515149B (en) | 2020-08-21 |
Family
ID=60724299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710747999.XA Active CN107515149B (en) | 2017-08-28 | 2017-08-28 | Method for detecting granularity and surface characteristics of diamond micropowder by using flow cytometer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107515149B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111982763B (en) * | 2020-08-17 | 2021-05-14 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5238202B2 (en) * | 2007-08-29 | 2013-07-17 | ビジョン開発株式会社 | Contact member and manufacturing method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009017734A1 (en) * | 2007-07-31 | 2009-02-05 | Aspt, Inc. | Slurry containing multi-oxidizer and nano-sized diamond abrasive for tungsten cmp |
| CN103018142B (en) * | 2012-12-05 | 2016-03-16 | 平顶山易成新材料有限公司 | A kind of electric-resistivity method detects the method for silicon carbide micro-powder granularity |
| CN105865988A (en) * | 2015-01-23 | 2016-08-17 | 中国科学院重庆绿色智能技术研究院 | Detection and analysis method for cell size distribution of phytoplankton |
| CN105865990B (en) * | 2016-03-28 | 2018-08-28 | 河南省人造金刚石微粉质量监督检验中心 | A kind of diadust grain size analysis sampling quantitative approach |
-
2017
- 2017-08-28 CN CN201710747999.XA patent/CN107515149B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5238202B2 (en) * | 2007-08-29 | 2013-07-17 | ビジョン開発株式会社 | Contact member and manufacturing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Development of nano diamond particles composite plating and evaluation of their tribological property;M.Koizumi;<Abstract of China 6th International Symposium on Tribology>;20110819;第5-6页 * |
| Experimental and theoretical values of the ultrasonic properties of dispersions: effect of particle state and size distribution;Javanaud C.;《Elsevier》;19910701;第331-337页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107515149A (en) | 2017-12-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI403714B (en) | Determination of Particle Size Distribution of Microparticles in Metallic Materials | |
| CN105004643B (en) | The assay method of Solid content particle diameter distribution in a kind of catalytic cracked oil pulp | |
| CN1755348A (en) | Method, apparatus, reagent kit and reagent for distinguishing erythrocytes in a biological specimen | |
| Capelo et al. | Ultrasound-assisted extraction of cadmium from slurried biological samples for electrothermal atomic absorption spectrometry | |
| CN107515149B (en) | Method for detecting granularity and surface characteristics of diamond micropowder by using flow cytometer | |
| CN112557429A (en) | Quantitative determination method for all minerals in graphite ore and sample preparation method | |
| CN103018142A (en) | Method for detecting granularity of silicon carbide micro powder by resistance method | |
| JP5277906B2 (en) | Measuring method of particle size distribution of fine particles | |
| CN109115575B (en) | Method for detecting inclusions in metal 3D printing nickel-based superalloy | |
| CN106568764A (en) | Inductively coupled plasma emission spectroscopy analysis method of acid soluble aluminum and acid insoluble aluminum | |
| JP4972784B2 (en) | Analysis method of fine particles in steel | |
| CN110672577A (en) | Method for measuring selenium content in rice | |
| CN103604678A (en) | Sample preparation method for uniformly distributing trace components in solid block matrix | |
| CN106932377B (en) | Method for detecting pathogenic bacteria in food by using Raman enhanced spectrum | |
| CN108663497A (en) | A method of measuring Dissolved H in Liquid Al-Si Alloy content | |
| CN112730379B (en) | Nano Au film surface enhanced Raman sensing array substrate and preparation method thereof | |
| JP2018130670A (en) | Dispersant, dispersant for field flow fractionation, fractionation method of fine particle in steel material and analysis method of fine particle in steel material | |
| CN113640084B (en) | Detection method of farmland soil micro-plastics | |
| JP2009155155A (en) | Methods for manufacturing and evaluating metal oxide particulate and the metal oxide particulate | |
| CN106814062A (en) | The method for determining various chemical element contents in slag simultaneously | |
| CN111551533A (en) | Surface enhanced substrate, preparation method thereof and detection method of methanol in insulating oil | |
| Zhang et al. | Improving and controlling the drug loading capacity of seven quinolones in minced fish matrix based on microfluidics | |
| CN103063550B (en) | Method for accurately measuring dimension distribution of TiB2 particles in Al-Ti-B intermediate alloy | |
| TWI790793B (en) | Detection method of lithium in liquid sample | |
| CN114381262B (en) | Carbon quantum dot fluorescent probe and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200817 Address after: 476200, Henan, Shangqiu Zhecheng County Industrial Zone North Sea Road Patentee after: ZHECHENG HUIFENG DIAMOND TECHNOLOGY Co.,Ltd. Address before: 476200 Guangzhou Road, Zhecheng County, Shangqiu City, Henan Province, No. 12 Patentee before: HENAN KELA DIAMOND Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 476200 Beihai Road, Zhecheng County, Shangqiu City, Henan Province Patentee after: Huifeng Dimond Co.,Ltd. Address before: 476200 Beihai Road, Zhecheng County, Shangqiu City, Henan Province Patentee before: ZHECHENG HUIFENG DIAMOND TECHNOLOGY CO.,LTD. |
|
| CP01 | Change in the name or title of a patent holder |