CN115993312B - Method for testing organic powder/slurry by using laser particle sizer - Google Patents
Method for testing organic powder/slurry by using laser particle sizer Download PDFInfo
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- CN115993312B CN115993312B CN202310290188.7A CN202310290188A CN115993312B CN 115993312 B CN115993312 B CN 115993312B CN 202310290188 A CN202310290188 A CN 202310290188A CN 115993312 B CN115993312 B CN 115993312B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method for testing organic powder/slurry by a laser particle sizer, relates to the field of organic powder/slurry testing, and aims to solve the problem that bubbles are easy to generate in an ultrasonic process, and the technical scheme is as follows: the method comprises the following steps: the first step: taking a proper amount of alcohol, and placing the alcohol in a vacuum deaeration machine for vacuum deaeration; and a second step of: adding an organic defoaming agent into the alcohol subjected to the defoaming treatment; and a third step of: placing alcohol added with a defoaming agent into an ultrasonic homogenizer, adjusting the power of the ultrasonic homogenizer to be consistent with that of a laser particle analyzer, observing the state after the ultrasonic homogenizer is started, closing the ultrasonic homogenizer after no bubble is generated, and taking out the alcohol for later use; fourth step: adding alcohol into the organic powder or slurry, setting test parameters of a laser particle analyzer, and starting built-in ultrasonic waves for testing. The method for testing the organic powder/slurry by using the laser particle sizer does not generate bubbles or secondary agglomeration.
Description
Technical Field
The invention relates to a method for detecting organic powder slurry, in particular to a method for testing organic powder/slurry by using a laser particle sizer.
Background
The laser particle sizer measures the particle size by using the scattering or diffraction phenomenon of the particles to light, that is, when the light encounters the particles during the traveling process, a part of the light deviates from the original traveling direction: the smaller the particle size, the greater the angle of deviation; the larger the particle size, the smaller the angle of departure. The scattering phenomenon can be described by strict electromagnetic wave theory, i.e. Mie scattering theory.
When the laser particle analyzer tests the powder of a water system, the secondary agglomeration phenomenon of the powder can not occur basically under the combined action of external ultrasound and internal ultrasound, the test data is more accurate, but when the system is tested, the use of alcohol can cause problems, because the alcohol can generate bubbles in the ultrasound and circulation process, especially the bubbles are most serious in the ultrasound process, the ultrasound system needs to be closed when the system is tested, but the closed ultrasound system does not solve the bubble problem, and the circulation system can generate relatively fewer bubbles; the ultrasonic system is turned off to cause another problem, and the external ultrasonic dispersed particles have no built-in ultrasonic effect, so that secondary agglomeration causes errors in the test result.
There is therefore a need to propose a new solution to this problem.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for testing organic powder/slurry by using a laser particle sizer, which aims to solve the problem that bubbles (circulation and ultrasonic systems) are generated due to equipment when the laser particle sizer tests an organic system, and provides a set of flow method of the system, including a method for mixing and utilizing lower vacuum defoaming, an antifoaming agent and high-power ultrasonic defoaming.
The technical aim of the invention is realized by the following technical scheme: a method for testing organic powder/slurry with a laser particle sizer comprising the steps of:
the first step: alcohol is taken and placed in a vacuum deaeration machine for vacuum deaeration;
and a second step of: adding an organic defoaming agent into the alcohol subjected to the defoaming treatment;
and a third step of: placing alcohol added with a defoaming agent into an ultrasonic homogenizer, adjusting the power of the ultrasonic homogenizer to be consistent with that of a laser particle analyzer, observing the state after the ultrasonic homogenizer is started, closing the ultrasonic homogenizer after no bubble is generated, and taking out the alcohol for later use;
fourth step: adding alcohol into the organic powder or slurry, setting test parameters of a laser particle analyzer, and starting built-in ultrasonic waves for testing.
The invention is further provided with: the mass of the proper amount of alcohol is an amount sufficient to test one sample 2-3 times.
The invention is further provided with: in the first step, the vacuum defoaming pressure is 0.4-0.5 mpa, and the time is 20-30 min.
The invention is further provided with: the dosage of the organic defoaming agent is one to two thousandths of alcohol.
The invention is further provided with: in the fourth step, the treated alcohol is taken, organic dispersing agent is added for ultrasonic dispersion, then organic powder or slurry is added, ultrasonic dispersion is carried out again, ultrasonic defoaming is carried out again, and then the test is started after the test parameters of a laser particle sizer are set.
The invention is further provided with: in the third step, after turning on the ultrasound, an organic defoamer is added in addition.
The invention is further provided with: the amount of the supplementary organic defoamer is less than one thousandth of the mass of the solution.
In summary, the invention has the following beneficial effects:
1. the pretreated alcohol has less gas content and small surface tension, bubbles are not easy to generate, the possibility of bubble generation is reduced from the root, and meanwhile, the defoaming pretreatment method is simpler, more convenient and lower in cost;
2. when testing organic system powder/slurry, the problem that when testing, the alcohol generates a large amount of bubbles due to the starting of ultrasound can be effectively solved by using low surface tension alcohol which is subjected to defoaming pretreatment and dripping an organic defoaming agent in a low-power ultrasonic environment when preparing a test sample solution until the system is stable;
3. by means of the defoaming treatment means, the instrument can be started to be internally provided with low-power ultrasonic waves when the organic system powder/slurry is tested, so that the risk of secondary agglomeration of particles is greatly reduced;
4. the defoaming treatment means can save the test cost and improve the test efficiency and the result accuracy.
Drawings
FIG. 1 is a graph showing the results of the laser grain size test for silicon nitride of example 1;
FIG. 2 is a graph of the results of a normal flow silicon nitride laser grain size test;
FIG. 3 is a graph showing the results of laser particle size testing of the silicon nitride slurry of example 2;
fig. 4 is a graph showing the results of laser granularity testing of a silicon nitride slurry in a normal flow.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
A method for testing organic powder/slurry by using a laser particle sizer adopts the following technical scheme:
the first step: and taking a proper amount of alcohol (the use amount of the alcohol is enough to test one sample for 2-3 times), and placing the sample in a vacuum defoaming machine to perform vacuum defoaming for 20-30 min under the pressure of 0.4-0.5 mpa.
And a second step of: adding an organic defoaming agent into the alcohol subjected to the defoaming treatment, wherein the dosage of the organic defoaming agent is one to two thousandths of the alcohol.
And a third step of: placing alcohol added with the defoaming agent into an ultrasonic homogenizer, adjusting the power of the ultrasonic homogenizer to be consistent with that of a laser particle analyzer, observing the state after starting ultrasonic treatment, properly supplementing the organic defoaming agent, closing the ultrasonic homogenizer after no bubble is generated, and taking out the alcohol for later use.
Fourth step: and adding an organic dispersing agent into the treated alcohol for ultrasonic dispersion, adding organic powder or slurry, performing ultrasonic dispersion again, performing ultrasonic defoaming again to set test parameters of a laser particle analyzer, and starting built-in ultrasonic for testing.
The detailed embodiments of the present invention are given below, but the present invention is not limited thereto.
Example 1 (silicon nitride test)
The first step: an appropriate amount of alcohol (sufficient to test one sample 3 times) was taken, and placed in a vacuum deaerator, and vacuum deaeration was performed at a pressure of 0.5Mpa for 25min.
And a second step of: adding an organic defoaming agent into the alcohol subjected to the defoaming treatment, wherein the dosage of the organic defoaming agent is one thousandth of that of the alcohol.
And a third step of: placing alcohol added with an antifoaming agent into an ultrasonic homogenizer, adjusting the power of the ultrasonic homogenizer to be consistent with that of a laser particle analyzer, observing the state after starting ultrasonic treatment, properly supplementing 5 drops of an organic antifoaming agent, closing the ultrasonic homogenizer after no bubble is generated, and taking out the alcohol.
Fourth step: taking 100ml of treated alcohol, adding 0.8g of organic dispersing agent, dispersing for 1min by using 300w of ultrasonic, adding 0.8g of silicon nitride powder, dispersing for 8min by using 300w of ultrasonic, defoaming for 2min by using 35w of ultrasonic, and starting testing by using the treated alcohol after setting the testing parameters of a laser particle sizer.
The original standard D50 of the silicon nitride powder used in this example is 0.7-0.8 μm, and after the method of the present invention is adopted, the silicon nitride powder is tested by a Bettersize2600 laser particle sizer, the test result is shown in fig. 1, and fig. 1 is a graph of the test result of the silicon nitride laser particle size of example 1.
The test was performed using a Bettersize2600 laser particle sizer using plain alcohol and normal flow of operation, the results are shown in FIG. 2, and FIG. 2 is a graph of the results of the normal flow silicon nitride laser particle size test.
Example 2 (silicon nitride slurry test)
The first step: an appropriate amount of alcohol (enough to test one sample 2 times) was taken, and placed in a vacuum deaerator, and vacuum deaeration was performed at a pressure of 0.4Mpa for 20min.
And a second step of: adding an organic defoaming agent into the alcohol subjected to the defoaming treatment, wherein the dosage of the organic defoaming agent is two thousandths of that of the alcohol.
And a third step of: placing alcohol added with an antifoaming agent into an ultrasonic homogenizer, adjusting the power of the ultrasonic homogenizer to be consistent with that of a laser particle analyzer, observing the state after starting ultrasonic treatment, properly supplementing 7 drops of an organic antifoaming agent, closing the ultrasonic homogenizer after no bubble is generated, and taking out the alcohol.
Fourth step: taking 100ml of treated alcohol, dripping 4 drops of silicon nitride slurry by drip irrigation, performing ultrasonic dispersion for 2min at 300w, performing ultrasonic defoaming for 1min at 35w, setting the test parameters of a laser particle sizer, and starting the test by using the treated alcohol.
The original standard D50 of the silicon nitride powder used in this example is 0.5-0.6 μm, and after the method of the present invention is adopted, the silicon nitride powder is tested by a Bettersize2600 laser particle sizer, the test result is shown in fig. 3, and fig. 3 is a graph showing the laser particle size test result of the silicon nitride slurry of example 2.
The test was performed using a Bettersize2600 laser particle sizer using plain alcohol and a normal flow of operation, the results are shown in FIG. 4, and FIG. 4 is a graph of the results of the normal flow laser particle size test of the silicon nitride slurry.
The surface tension of the alcohol is much smaller than that of water, so bubbles are easier to generate due to the circulation and the effect of ultrasound in the particle size test process, the method provided by the invention solves the problem of bubbles through the mutual complementation of each flow, and the vacuum defoaming in the first step can remove most of air contained in the alcohol and reduce the generation of bubbles; the defoaming agent added in the second step can improve the surface tension of alcohol and increase the difficulty of bubble generation; and thirdly, ultrasonic defoaming can enable the treated alcohol to adapt to the power of ultrasonic built-in a laser particle sizer, so that the possibility of bubble generation is reduced.
The invention provides a method for solving the problem of bubbles generated by alcohol by a method combining vacuum defoaming, defoaming agent addition and ultrasonic defoaming during testing of organic system powder/slurry by a laser particle sizer.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (6)
1. A method for testing organic powder/slurry using a laser particle sizer, comprising the steps of:
the first step: alcohol is taken and placed in a vacuum deaeration machine for vacuum deaeration;
and a second step of: adding an organic defoaming agent into the alcohol subjected to the defoaming treatment;
and a third step of: placing alcohol added with an organic defoaming agent into an ultrasonic homogenizer, adjusting the power of the ultrasonic homogenizer to be consistent with that of a laser particle analyzer, observing the state after the ultrasonic homogenizer is started, closing the ultrasonic homogenizer after no bubbles are generated, and taking out the alcohol for later use;
fourth step: adding alcohol into the organic powder or slurry, setting test parameters of a laser particle analyzer, and starting built-in ultrasonic waves for testing.
2. A method of testing organic powders/slurries with a laser particle sizer as claimed in claim 1, wherein: in the first step, the vacuum defoaming pressure is 0.4-0.5 mpa, and the time is 20-30 min.
3. A method of testing organic powders/slurries with a laser particle sizer as claimed in claim 1, wherein: the dosage of the organic defoamer is one to two thousandths of the mass of the alcohol.
4. A method of testing organic powders/slurries with a laser particle sizer as claimed in claim 1, wherein: in the fourth step, the treated alcohol is taken, organic dispersing agent is added for ultrasonic dispersion, then organic powder or slurry is added, ultrasonic dispersion is carried out again, ultrasonic defoaming is carried out again, and then the test is started after the test parameters of a laser particle sizer are set.
5. A method of testing organic powders/slurries with a laser particle sizer as claimed in claim 1, wherein: in the third step, after turning on the ultrasound, an organic defoamer is added in addition.
6. The method for testing organic powder/slurry with a laser particle sizer according to claim 5, wherein: the amount of the supplementary organic defoamer is less than one thousandth of the mass of the solution.
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