CN112179958A - Novel characterization method for slurry stability - Google Patents
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- CN112179958A CN112179958A CN202011006000.4A CN202011006000A CN112179958A CN 112179958 A CN112179958 A CN 112179958A CN 202011006000 A CN202011006000 A CN 202011006000A CN 112179958 A CN112179958 A CN 112179958A
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Abstract
The invention discloses a novel characterization method of slurry stability, which comprises the following steps: the method comprises the steps of sample preparation and test position selection, interdigital electrode sensor selection and preparation, slurry capacitance change value test along with time, sedimentation and stability analysis, and slurry storage period calculation and prediction. The invention relates to the technical field of slurry detection, and particularly provides a novel slurry stability characterization method which solves the technical problems that in the prior art, a slurry storage stability characterization method is not clear, the continuous change relation of the slurry stability along with time cannot be obtained, and the storage period cannot be accurately calculated.
Description
Technical Field
The invention relates to the technical field of slurry detection, in particular to a novel characterization method of slurry stability.
Background
The slurry is a relatively complex system, generally comprising porcelain powder, a solvent, a dispersant, a binder, a plasticizer and an antifoaming agent, and if the added additives can generate steric hindrance effect on particles and make the particles difficult to accumulate, the added solvent can overcome van der waals force between the particles and maintain certain spatial stability. Although the prepared slurry has better stability in a short time, the phenomena of precipitation, agglomeration and the like can be generated if the mixture ratio of the slurry components is not proper during the storage process, thereby obviously influencing the performance of the slurry. In addition, the uneven performance of the slurry can lead to the stable performance of the product, which is not favorable for producing qualified high-performance products. For example, the dispersibility and storage stability of ceramic slurry for MLCC (chip multilayer ceramic capacitor) casting are very important for the performance of the finished product.
Today, the characterization of slurry stability is mostly measured by using a rotational viscometer and a sedimentation method, but the method has the difficulties of long test period and unpredictable storage period. For example, the zhouhafeng team at gillin university tests the influence of the types and contents of additives in ceramic slurry for MLCC casting on the slurry stability by using a traditional sedimentation method (study on toluene substitution solvent in zhang. MLCC [ D ]. gilin university, 2010), that is, ceramic powder solid particles with the same mass are put into a colorimetric tube with the same volume, a mixed solvent is added, then, the particles are fully dispersed in liquid by using ultrasound and are kept still for one week, and the slurry stability is tested by testing the height of suspension liquid in the suspension liquid. Besides, precipitation weighing and some modified precipitation methods are also common methods for characterizing the stability of the slurry. However, it is obvious that the above method cannot obtain continuous data, takes long time and causes more errors in the experimental process.
At present, in the existing standard and related patents, the representation of the real-time stability of the slurry and the accurate calculation of the storage period are lacked, in addition, the representation of the stability of the slurry cannot be scientifically and clearly represented by the existing means, in addition, the calculation basis of the storage period of the slurry is not very clear, so that a novel representation method is required to be found to shorten the detection period and preferably achieve the characteristic of real-time monitoring, and meanwhile, a method which can simply and scientifically represent the stability of the slurry and calculate the storage period is found, so that the method is particularly important for outputting stable and high-quality products.
Disclosure of Invention
In order to solve the existing problems, the invention provides a novel slurry stability characterization method which solves the technical problems that in the prior art, a slurry storage stability characterization method is not clear, the continuous change relation of the slurry stability along with time cannot be obtained, and the storage period cannot be accurately calculated.
The technical scheme adopted by the invention is as follows: the invention discloses a novel characterization method of slurry stability, which comprises the following steps:
the method comprises the following steps: sample preparation and test site selection:
preparing slurry and a clean columnar container, extracting a slurry sample from the slurry, placing the slurry sample in the columnar container, and selecting positions with different depths as test points of slurry stability;
step two: selecting and preparing an interdigital electrode sensor:
selecting an interdigital electrode with a proper material and size, and connecting an external device for testing the capacitance to manufacture an interdigital electrode sensor system;
step three: testing the capacitance change value of the slurry along with time:
fixing the interdigital electrode at a certain position in the slurry sample in the first columnar container, and detecting the relation of the capacitance of the slurry sample changing along with time;
step four: sedimentation and stability analysis:
drawing a curve relation graph according to the relation of the capacitance of the slurry sample at a certain position in the columnar container, which is obtained in the third step, along with the change of time, and analyzing the sedimentation condition of the slurry according to the curve relation graph so as to judge the stability of the slurry;
step five: calculating and predicting the storage period of the slurry:
and obtaining the optimal slurry storage period according to the change relation of the curve relation diagram in the fourth step, and fitting a curve through data processing software to predict the settling condition of the slurry in a longer time.
Further, the interdigital electrode material in the second step comprises a substrate material and an electrode material, wherein the substrate material is a silicon substrate, a glass substrate inorganic substrate or a polymer substrate such as PET, PI and the like, and the electrode material is a metal such as gold, silver, copper, aluminum and the like or a conductive fabric.
Furthermore, the line width and the line distance of the interdigital electrode in the second step can be controlled within 5-200 μm, and can be properly selected and adjusted according to specific precision requirements and cost.
Further, the fixed position of the interdigital electrode in the third step can be any position within the same height, but the fixed position cannot be freely moved in the test process.
Further, the slurry in the first step may be any liquid or viscous sample such as ceramic slurry, metal slurry or emulsion.
Furthermore, the external connection device of the interdigital electrode in the second step can be a testing device capable of measuring capacitance, such as an LCR tester.
Further, the cylindrical container in the first step is preferably a cylindrical container, preferably with a diameter of 5-15 cm, and the height of the slurry in the container is 10-20 cm.
Furthermore, in the first step, a plurality of interdigital electrodes can be fixed at different positions of the slurry to detect the change of the slurry capacitance at different positions along with time, so that a plurality of groups of data can be acquired.
Further, the capacitance/time change curve is used in the first step to reflect the sedimentation rate/time change relationship, and the stability in the fourth step is expressed by the sedimentation rate/time change relationship.
Furthermore, in the fifth step, an inflection point on the curve is found according to the change relation of the capacitance along with the time to judge the change condition of the slurry stability, so that the slurry storage period is accurately calculated.
The invention with the structure has the following beneficial effects: compared with the traditional sedimentation method, the method for characterizing the stability of the slurry does not need to repeatedly extract the slurry at different positions, dry, weigh and the like, can realize full automation, therefore, the operation difficulty can be greatly simplified, the labor cost in actual production can be reduced, the technical problems that the characterization method of the storage stability of the slurry in the prior art is not clear, the continuous change relation of the stability of the slurry along with time cannot be obtained and the storage period cannot be accurately calculated are solved, the stability of the slurry is reflected by using the continuous relation of capacitance change of a certain position of the slurry along with time through testing the interdigital electrode, the method has the advantages of simple and accurate operation, real-time monitoring and realization of full automation, and the purpose of accurately monitoring the stability of the slurry in real time is achieved, can meet a plurality of requirements of real-time monitoring, screening, detecting, evaluating and the like in the process of producing and storing the slurry.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a novel method for characterizing slurry stability according to the present invention;
FIG. 2 is a graph of capacitance versus time for an alumina ceramic slurry without any additives at a location in accordance with a novel method of characterizing slurry stability in accordance with the present invention;
FIG. 3 is a graph of capacitance versus time for a ceramic slurry with added thickener and dispersant at a location in accordance with a novel method of characterizing slurry stability in accordance with the present invention;
FIG. 4 is a graph of capacitance versus time for an oil-in-water emulsion at a location for a novel method of characterizing slurry stability of the present invention.
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
The device comprises a computer 1, an LCR tester 2, a slurry sample 3, a columnar container 4, an interdigital electrode 5.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 to 3, the novel method for characterizing slurry stability of the present invention comprises the following steps:
the method comprises the following steps: sample preparation and test site selection:
preparing slurry and a clean columnar container, extracting a slurry sample from the slurry, placing the slurry sample in the columnar container, and selecting positions with different depths as test points of slurry stability;
step two: selecting and preparing an interdigital electrode sensor:
selecting an interdigital electrode with a proper material and size, and connecting an external device for testing the capacitance to manufacture an interdigital electrode sensor system;
step three: testing the capacitance change value of the slurry along with time:
fixing the interdigital electrode at a certain position in the slurry sample in the first columnar container, and detecting the relation of the capacitance of the slurry sample changing along with time;
step four: sedimentation and stability analysis:
drawing a curve relation graph according to the relation of the capacitance of the slurry sample at a certain position in the columnar container, which is obtained in the third step, along with the change of time, and analyzing the sedimentation condition of the slurry according to the curve relation graph so as to judge the stability of the slurry;
step five: calculating and predicting the storage period of the slurry:
and obtaining the optimal slurry storage period according to the change relation of the curve relation diagram in the fourth step, and fitting a curve through data processing software to predict the settling condition of the slurry in a longer time.
The interdigital electrode material in the second step comprises a substrate material and an electrode material, wherein the substrate material is a silicon substrate, a glass substrate inorganic substrate or a polymer substrate such as PET, PI and the like, and the electrode material is metal such as gold, silver, copper, aluminum and the like or conductive fabric. In the second step, the line width and the line distance of the interdigital electrode can be controlled to be 5-200 mu m, and the interdigital electrode can be properly selected and adjusted according to specific precision requirements and cost. The fixed position of the interdigital electrode in the third step can be any position within the same height, but the fixed position cannot be freely moved in the test process. The slurry in the first step can be any liquid or viscous sample such as ceramic slurry, metal slurry or emulsion. And in the second step, external equipment of the interdigital electrode can be testing equipment capable of measuring capacitance, such as an LCR tester. The cylindrical container in the first step is preferably a cylindrical container, the preferred diameter is 5-15 cm, and the height of the slurry in the container is 10-20 cm. In the first step, a plurality of interdigital electrodes can be fixed at different positions of the slurry to detect the change of the capacitance of the slurry at different positions along with time, so that a plurality of groups of data can be acquired. And in the first step, a capacitance/time change curve is used for reflecting the relation of sedimentation rate/time change, and in the fourth step, the stability is expressed by the relation of sedimentation rate/time change. And fifthly, searching an inflection point on the curve according to the change relation of the capacitance along with the time to judge the change condition of the slurry stability, thereby accurately calculating the slurry storage period.
Example 1, a novel method of characterizing slurry stability according to the present invention comprises the steps of:
the method comprises the following steps: sample preparation and test site selection:
mixing micron-grade alumina ceramic powder and deionized water according to the weight ratio of 5: 5, preparing a slurry sample No. 1, then placing the slurry sample in a cylindrical beaker, and selecting the uppermost layer of the slurry sample as a test point of slurry stability;
step two: selecting and preparing an interdigital electrode sensor:
selecting an interdigital electrode with a substrate material of alumina ceramic and an electrode material of metallic silver, inserting the interdigital electrode into the upper layer of the slurry, fixing and connecting the interdigital electrode with an LCR tester to form a capacitance sensor;
step three: testing the capacitance change value of the slurry along with time:
fixing the interdigital electrode on the position in the step one, and detecting the relation of the capacitance of the slurry sample changing along with time;
step four: sedimentation and stability analysis:
and analyzing the sedimentation condition of the slurry according to the relation curve of the capacitance of the slurry sample at a certain position in the columnar container, which is obtained in the third step, along with the change of time, so as to judge the stability of the slurry.
Example 2, a novel method of characterizing slurry stability of the present invention comprises the steps of:
the method comprises the following steps: sample preparation and test site selection:
mixing alumina ceramic powder and deionized water according to the weight ratio of 3: 7, adding 0.1 wt% of thickening agent methylcellulose and 0.1 wt% of dispersant polyethylene glycol, marking as a sample No. 2, then placing the slurry sample in a cylindrical beaker, and selecting the uppermost layer of the slurry sample as a test point of slurry stability;
step two: selecting and preparing an interdigital electrode sensor:
selecting an interdigital electrode with a substrate material of alumina ceramic and an electrode material of metallic silver, inserting the interdigital electrode into the upper layer of the slurry, fixing and connecting the interdigital electrode with an LCR tester to form a capacitance sensor;
step three: testing the capacitance change value of the slurry along with time:
fixing the interdigital electrode on the position in the step one, and detecting the relation of the capacitance of the slurry sample changing along with time;
step four: sedimentation and stability analysis:
and analyzing the sedimentation condition of the slurry according to the relation curve of the capacitance of the slurry sample at a certain position in the columnar container, which is obtained in the third step, along with the change of time, so as to judge the stability of the slurry.
Example 3, a novel method of characterizing slurry stability of the present invention comprises the steps of:
the method comprises the following steps: sample preparation and test site selection:
weighing octane according to the volume ratio: methyl hydrogen silicone oil: TEOS 10: 8: 1, fully stirring for 10min at 10000rpm of a nano milk homogenizing machine to fully mix the components to obtain an oil phase A; weighing an oil phase A in a weight ratio: anhydrous ethanol: stirring tween 80 at 15:1:1 in a nano homogenizer at 10000rpm for 10min, and fully mixing to obtain a mixed solution B; adding deionized water, wherein the weight ratio of the mixed solution B to the deionized water is 3: 1, stirring for 10min at 10000rpm of a nano emulsion homogenizing machine to uniformly disperse a mixed oil phase into a water phase to obtain an oil-in-water emulsion; placing the oil-in-water emulsion as a slurry sample in a cylindrical beaker, and selecting the uppermost layer of the slurry as a test point of slurry stability;
step two: selecting and preparing an interdigital electrode sensor:
selecting an interdigital electrode with a substrate material of alumina ceramic and an electrode material of metallic silver, inserting the interdigital electrode into the upper layer of the oil-in-water emulsion, fixing the interdigital electrode and connecting the interdigital electrode with an LCR tester to form a capacitance sensor;
step three: measurement of the capacitance of oil-in-water emulsions over time:
fixing the interdigital electrode on the position in the step one, and detecting the capacitance change relation of the oil-in-water emulsion along with time;
step four: and (3) stability analysis:
analyzing the stability of the oil-in-water emulsion according to the capacitance-time change curve of the oil-in-water emulsion at a certain position obtained in the third step;
step five: oil-in-water emulsion shelf life calculation and prediction:
and obtaining the optimal oil-in-water emulsion storage period according to the variation relation of the curve relation diagram in the fourth step.
The graphs obtained in example 1, example 2 and example 3 are shown in fig. 2, fig. 3 and fig. 4, respectively.
Based on the curve of fig. 2, it can be seen that the alumina ceramic slurry without any additive has a large capacitance change within 0-2000 s, i.e., the sedimentation phenomenon is severe, and the capacitance/time curve after 2000s has a gentle change, i.e., the sedimentation speed is slow, the slurry is still in an unstable state, and since the dielectric constant of water is much higher than that of the ceramic particles, the capacitance of the upper layer slurry is gradually increased with the increase of time, and the overall trend of the curve is also in line with expectations.
Based on the graph of fig. 3, it can be seen that the capacitance/time curve of the ceramic slurry with the thickener and the dispersant added is more gradual, indicating that the stability of the slurry containing the additive is improved, the slurry settles more slowly within 2400s, indicating that the stability of the slurry at this stage is better, and the stability transition point of the slurry occurs at 2400 s.
Based on the graph of fig. 4, it can be seen that the capacitance of the oil-in-water emulsion is substantially unchanged within 6000s with only very small jumps, indicating that the oil-in-water emulsion is very stable at this time point and no separation occurs, while after 6000s the capacitance gradually increases, indicating that the emulsion becomes unstable and separation occurs and is not yet usable.
The storage period of the slurry and the emulsion can be accurately obtained on the curve, the testing time can be accurate to seconds, the real-time monitoring can be realized, the automatic detection can be continuously carried out, and the regular curve can be fitted to predict the stability change of the subsequent slurry.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Claims (10)
1. A novel characterization method of slurry stability is characterized in that: the method comprises the following steps:
the method comprises the following steps: sample preparation and test site selection:
preparing slurry and a clean columnar container, extracting a slurry sample from the slurry, placing the slurry sample in the columnar container, and selecting positions with different depths as test points of slurry stability;
step two: selecting and preparing an interdigital electrode sensor:
selecting an interdigital electrode with a proper material and size, and connecting an external device for testing the capacitance to manufacture an interdigital electrode sensor system;
step three: testing the capacitance change value of the slurry along with time:
fixing the interdigital electrode at a certain position in the slurry sample in the first columnar container, and detecting the relation of the capacitance of the slurry sample changing along with time;
step four: sedimentation and stability analysis:
drawing a curve relation graph according to the relation of the capacitance of the slurry sample at a certain position in the columnar container, which is obtained in the third step, along with the change of time, and analyzing the sedimentation condition of the slurry according to the curve relation graph so as to judge the stability of the slurry;
step five: calculating and predicting the storage period of the slurry:
and obtaining the optimal slurry storage period according to the change relation of the curve relation diagram in the fourth step, and fitting a curve through data processing software to predict the settling condition of the slurry in a longer time.
2. The novel method for characterizing slurry stability according to claim 1, wherein: in the second step, the interdigital electrode material comprises a substrate material and an electrode material, the substrate material comprises any one of an inorganic substrate and a polymer substrate, and the electrode material is any one of metal and conductive fabric.
3. The novel method for characterizing slurry stability according to claim 1, wherein: and in the second step, the line width and the line distance of the interdigital electrode are controlled to be 5-200 mu m.
4. The novel method for characterizing slurry stability according to claim 1, wherein: the fixed position of the interdigital electrode in the third step can be any position within the same height, but the fixed position cannot be freely moved in the test process.
5. The novel method for characterizing slurry stability according to claim 1, wherein: the slurry in the first step includes, but is not limited to, ceramic slurry, metal slurry, and emulsion.
6. The novel method for characterizing slurry stability according to claim 1, wherein: and in the second step, external equipment of the interdigital electrode is an LCR tester.
7. The novel method for characterizing slurry stability according to claim 1, wherein: the cylindrical container in the first step is a cylindrical container with the diameter of 5-15 cm, and the height of the slurry in the cylindrical container is 10-20 cm.
8. The novel method for characterizing slurry stability according to claim 1, wherein: in the first step, a plurality of interdigital electrodes can be fixed at different positions of the slurry sample to detect the change of the slurry capacitance at different positions along with time.
9. The novel method for characterizing slurry stability according to claim 1, wherein: and in the first step, a capacitance/time change curve is used for reflecting the relation of sedimentation rate/time change, and in the fourth step, the stability is expressed by the relation of sedimentation rate/time change.
10. The novel method for characterizing slurry stability according to claim 1, wherein: and fifthly, searching an inflection point on the curve according to the change relation of the capacitance along with the time to judge the change condition of the slurry stability, thereby accurately calculating the slurry storage period.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101486836A (en) * | 2008-01-18 | 2009-07-22 | 郑州泰达电子材料科技有限公司 | Conductive macromolecular solution, preparation thereof, conductive polymer coated film and solid electrolyte capacitor |
| CN104181208A (en) * | 2014-07-25 | 2014-12-03 | 河南科技大学 | Battery paste testing device |
| CN107167739A (en) * | 2017-05-17 | 2017-09-15 | 力信（江苏）能源科技有限责任公司 | A kind of electrokinetic cell life-span prediction method |
| CN107271386A (en) * | 2017-06-12 | 2017-10-20 | 常州第六元素材料科技股份有限公司 | A kind of method for setting up graphene Stability of Slurry characterization model |
| CN109817382A (en) * | 2017-11-21 | 2019-05-28 | 山东欧铂新材料有限公司 | A kind of preparation method of high-stability graphene electrocondution slurry |
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2020
- 2020-09-23 CN CN202011006000.4A patent/CN112179958A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486836A (en) * | 2008-01-18 | 2009-07-22 | 郑州泰达电子材料科技有限公司 | Conductive macromolecular solution, preparation thereof, conductive polymer coated film and solid electrolyte capacitor |
| CN104181208A (en) * | 2014-07-25 | 2014-12-03 | 河南科技大学 | Battery paste testing device |
| CN107167739A (en) * | 2017-05-17 | 2017-09-15 | 力信（江苏）能源科技有限责任公司 | A kind of electrokinetic cell life-span prediction method |
| CN107271386A (en) * | 2017-06-12 | 2017-10-20 | 常州第六元素材料科技股份有限公司 | A kind of method for setting up graphene Stability of Slurry characterization model |
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