CN115615784A - Sample processing method for representing MLCC barium titanate ceramic grains - Google Patents
Sample processing method for representing MLCC barium titanate ceramic grains Download PDFInfo
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- CN115615784A CN115615784A CN202211424363.9A CN202211424363A CN115615784A CN 115615784 A CN115615784 A CN 115615784A CN 202211424363 A CN202211424363 A CN 202211424363A CN 115615784 A CN115615784 A CN 115615784A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 60
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 41
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000003672 processing method Methods 0.000 title claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 46
- 238000005498 polishing Methods 0.000 claims abstract description 28
- 238000005530 etching Methods 0.000 claims abstract description 23
- 238000000992 sputter etching Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims description 13
- 230000007797 corrosion Effects 0.000 abstract description 22
- 238000005260 corrosion Methods 0.000 abstract description 22
- 238000004458 analytical method Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- 239000003985 ceramic capacitor Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000003486 chemical etching Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- HLLSOEKIMZEGFV-UHFFFAOYSA-N 4-(dibutylsulfamoyl)benzoic acid Chemical compound CCCCN(CCCC)S(=O)(=O)C1=CC=C(C(O)=O)C=C1 HLLSOEKIMZEGFV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- 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
-
- 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
- G01N1/32—Polishing; Etching
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a sample processing method for representing MLCC barium titanate ceramic grains, and relates to a ceramic grain analysis method. The method comprises the steps of fixedly sealing the MLCC on a grinding table along a long axis or a short axis, and mechanically polishing and grinding the MLCC to an effective electrode area; carrying out ion etching on the obtained sample; then soaking the substrate in acid solution for acid etching; taking out and washing the surface of the grinding table with water. The invention provides a sample processing method for representing MLCC barium titanate ceramic grains, compared with the traditional method for representing the ceramic grains by simple acid corrosion or hot corrosion, the method carries out ion etching treatment on the polished surface of a sample in advance, effectively removes N i internal electrodes and the barium titanate ceramic grains which extend due to polishing and grinding by ion etching, fully exposes the grain boundary of the barium titanate grains before acid corrosion, improves the effect of subsequent acid corrosion, has obvious ceramic grain outline and complete grain boundary corrosion, and solves the defects of analyzing the morphology and the grain size of the MLCC barium titanate ceramic grains at present.
Description
Technical Field
The invention relates to the field of ceramic grain analysis methods, in particular to a sample processing method for representing MLCC barium titanate ceramic grains.
Background
A multi-layer ceramic capacitor (MLCC) is an indispensable passive component in the electronic industry field. The development of smart phones, ioT, EV of automobiles, unmanned technologies, and the like, has pushed the development of MLCCs toward miniaturization, high capacity, high reliability, and low price. The high capacity of MLCCs is mainly achieved by multilayer dielectric ceramics and electrode stacking, wherein barium titanate is the most commonly used matrix ceramic material for high capacity MLCCs, and high performance MLCCs promote nanocrystallization of barium titanate.
In the process of realizing high capacity of MLCC, the reliability and capacity of products are influenced by the barium titanate which is a base material, and the dielectric constant of the barium titanate below micron level is reduced along with the reduction of the grain diameter. The insulation performance of the MLCC is related to the number of crystal boundaries of single-layer ceramic dielectric barium titanate, and the flatness of the Ni inner electrode is influenced by the shape of the barium titanate, so that the reliability of the MLCC is influenced. Therefore, the morphology and size analysis of barium titanate ceramic grains is critical to MLCCs.
The most commonly used sample processing methods for ceramic grain morphology analysis include: chemical etching and thermal etching. The chemical etching is carried out by strong acid such as HF, HCl or HNO 3 The solution or the mixed solution thereof is soaked on the surface of the sample, and the corrosion effects of the crystal boundary and the crystal grains are different, thereby achieving the purpose of analysis. Its advantages are easy operation, and high corrosion resistance, but it has poor effect on the ceramic dielectric of I I class high-capacity MLCC with small grain size and high corrosion resistance. The hot corrosion is that the sample is put in a high temperature furnace, the high temperature volatilizes the crystal boundary element, and then the analysis purpose is achieved, but the efficiency is low, the small grain size barium titanate is easy to grow up again at the high temperature, and the accuracy of the analysis result is influenced.
Disclosure of Invention
The invention provides a sample processing method for representing MLCC barium titanate ceramic grains, which is used for truly reflecting the true appearance of the ceramic grains and has an obvious ceramic grain outline.
In order to solve the above technical problems, the present invention provides a sample processing method for characterizing MLCC barium titanate ceramic grains, comprising the steps of:
(1) Fixedly sealing the MLCC on a grinding table along a long axis or a short axis, and mechanically polishing and grinding the MLCC to an effective electrode area;
(2) Carrying out ion etching on the sample obtained in the step (1);
(3) Immersing the sample obtained in the step (2) in an acid solution for acid etching;
(4) And (4) taking out the sample obtained in the step (3), and then washing the surface of the grinding table by using water.
Preferably, in the step (1), the mechanical polishing comprises polishing by using 200-300 mesh, 1000-1500 mesh, 2000-3000 mesh and 3500-4500 mesh sandpaper in sequence.
Preferably, in the step (2), the ion gun angle of the ion etching is 1-10 degrees, the voltage is 2-8 kv, and the time is 2-4 h.
Preferably, in the step (3), the acid solution comprises HC i and/or HNO 3 。
Preferably, in step (3), the acid solution comprises HC i, HNO 3 And water in a volume ratio of 1:1: (1-5).
Preferably, in the step (3), the acid solution includes HC 1 at an initial concentration of 37% and HNO 3 Was 68%.
Preferably, in the step (3), the acid etching time is 5 to 20min.
Preferably, in the step (1), the mechanical polishing comprises polishing with 200-mesh, 1200-mesh, 2400-mesh and 4000-mesh sandpaper in sequence;
in the step (2), the angle of an ion gun of the ion etching is 5 degrees, the voltage is 5kV, and the time is 2h;
in step (3), the acid solution comprises HC l, HNO 3 And water in a volume ratio of 1:1:1, and the acid etching time is 10min.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a sample processing method for representing MLCC barium titanate ceramic grains, compared with the traditional method for representing the ceramic grains by simple acid corrosion or hot corrosion, the method carries out ion etching treatment on the polished surface of a sample in advance, effectively removes N i internal electrodes and the barium titanate ceramic grains which extend due to polishing and grinding by ion etching, fully exposes the grain boundary of the barium titanate grains before acid corrosion, improves the effect of subsequent acid corrosion, can truly reflect the real morphology of the ceramic grains, has obvious ceramic grain outline and complete grain boundary corrosion, solves the defects of analyzing the morphology and the grain size of the MLCC barium titanate ceramic grains at present, has simple processing steps and improves the processing efficiency.
Drawings
FIG. 1: is a flow schematic diagram of a sample processing method for characterizing MLCC barium titanate ceramic grains;
FIG. 2: the invention discloses a ceramic grain shape graph after the treatment of a sample representing MLCC barium titanate ceramic grains in embodiment 1;
FIG. 3: the invention is a comparative example 1 which is a ceramic grain shape chart for representing the processed MLCC barium titanate ceramic grain sample;
FIG. 4: the invention is a comparative example 2 which is a ceramic grain shape chart for representing the processed MLCC barium titanate ceramic grain sample;
FIG. 5: the invention is a comparative example 3 which is a graph representing the morphology of ceramic grains after being processed by an MLCC barium titanate ceramic grain sample.
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 obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1
A sample processing method for characterizing MLCC barium titanate ceramic grains comprises the following steps:
(1) Polishing and grinding a long shaft grinding table of the sample: curing a chip multilayer ceramic capacitor (MLCC) sample in the center of an epoxy resin grinding table along the long axis direction, and mechanically polishing and grinding the MLCC sample to an effective electrode area by using 200-mesh, 1200-mesh, 2400-mesh and 4000-mesh abrasive paper in sequence;
(2) And (3) performing ion polishing on a polished surface of the sample: performing ion etching on the sample obtained in the step (1), wherein the angle of an ion gun is 5 degrees, the voltage is 5kV, and the time is 2h;
(3) Acid corrosion of the sample: immersing the sample of step (2) in HC l and HNO 3 Mixing aqueous solution of HC l and HNO 3 And water in a volume ratio of 1:1:1, acid etching time is 10 min;
(4) Cleaning a sample after acid etching: and (4) taking out the sample in the step (3), and washing the surface of the grinding table by using ultrapure water.
Comparative example 1
A sample processing method for characterizing MLCC barium titanate ceramic grains comprises the following steps:
(1) Polishing and grinding a long shaft grinding table of the sample: curing a chip multilayer ceramic capacitor (MLCC) sample in the center of an epoxy resin grinding table along the long axis direction, and mechanically polishing and grinding the sample to an effective electrode area by using 200-mesh, 1200-mesh, 2400-mesh and 4000-mesh abrasive paper in sequence;
(2) Acid corrosion of the sample: immersing the sample of step (1) in HC l and HNO 3 Mixing aqueous solution of HC l and HNO 3 And water in a volume ratio of 1:1:1, acid etching time is 10 min;
(3) Cleaning a sample after acid etching: taking out the sample in the step (2), and washing the surface of the grinding table by using ultrapure water.
Comparative example 2
A sample processing method for characterizing MLCC barium titanate ceramic grains comprises the following steps:
(1) Polishing and grinding a long shaft grinding table of the sample: curing a chip multilayer ceramic capacitor (MLCC) sample in the center of an epoxy resin grinding table along the long axis direction, and mechanically polishing and grinding the MLCC sample to an effective electrode area by using 200-mesh, 1200-mesh, 2400-mesh and 4000-mesh abrasive paper in sequence;
(2) And (3) performing ion polishing on a polished surface of the sample: performing ion etching on the sample obtained in the step (1), wherein the angle of an ion gun is 5 degrees, the voltage is 5kV, and the time is 2h;
(3) Acid corrosion of the sample: immersing the sample of step (2) in HC l and HNO 3 Mixing aqueous solution of HC l and HNO 3 And water in a volume ratio of 1:1:10, acid etchingInterval is 30mi n;
(4) Cleaning a sample after acid etching: and (4) taking out the sample in the step (3), and washing the surface of the grinding table by using ultrapure water.
Comparative example 3
A sample processing method for characterizing MLCC barium titanate ceramic grains comprises the following steps:
(1) Polishing and grinding a long shaft grinding table of the sample: curing a chip multilayer ceramic capacitor (MLCC) sample in the center of an epoxy resin grinding table along the long axis direction, and mechanically polishing and grinding the MLCC sample to an effective electrode area by using 200-mesh, 1200-mesh, 2400-mesh and 4000-mesh abrasive paper in sequence;
(2) And (3) performing ion polishing on the polished surface of the sample: performing ion etching on the sample obtained in the step (1), wherein the angle of an ion gun is 5 degrees, the voltage is 5kV, and the time is 2h;
(3) Acid corrosion of the sample: immersing the sample of step (2) in HC l and HNO 3 Mixing aqueous solution of HC l and HNO 3 And water in a volume ratio of 2:2:1, acid etching time is 5 min;
(4) Cleaning a sample after acid etching: and (4) taking out the sample in the step (3), and washing the surface of the grinding table by using ultrapure water.
Performance test
The surface topography of the treated MLCC samples of example 1 and comparative examples 1-3 was characterized and the results are shown in FIGS. 2-5. Fig. 2 is a morphology diagram of the ceramic grains subjected to ion polishing and acid etching in example 1, which is provided by the present application, and shows that the ceramic grains have an obvious profile and complete grain boundary corrosion, which indicates that the actual morphology of the sample ceramic grains can be truly reflected by the acid etching after ion polishing. Fig. 3 is a morphology diagram of a ceramic grain of comparative example 1, which is not subjected to ion etching but acid etching, provided by the application, the ceramic grain has an unobvious profile, grain adhesion exists, and the grain boundary is not completely corroded, which indicates that the actual morphology of the sample ceramic grain cannot be truly reflected only by acid etching. Compared with the comparative example 1, the ion polishing before the acid corrosion fully proves that the Ni inner electrode and the barium titanate ceramic grains expanded by the polishing can be effectively removed, so that the grain boundary of the barium titanate grains is fully exposed, and the subsequent acid corrosion effect is improved. FIG. 4 is a morphology of ceramic grains etched by low-concentration acid for a long time in comparative example 2, which shows that the ceramic grains have an unobvious outline and the grain boundaries are not completely etched, and thus the concentration of the acid used in acid etching is too low, and even if the acid etching is carried out for a long time, the sample etching effect is still poor, and the real morphology of the sample ceramic grains cannot be truly reflected. FIG. 5 is a graph showing the morphology of ceramic grains obtained by ion etching in comparative example 3, which shows a high acid concentration and a short etching time, and shows excessive grain corrosion and a reduced ceramic grain size, which do not correspond to the actual morphology of the sample ceramic grains.
The above-mentioned embodiments are provided to further explain the objects, technical solutions and advantages of the present invention in detail, and it should be understood that the above-mentioned embodiments are only examples of the present invention and are not intended to limit the scope of the present invention. It should be understood that any modifications, equivalents, improvements and the like, which come within the spirit and principle of the invention, may occur to those skilled in the art and are intended to be included within the scope of the invention.
Claims (8)
1. A sample processing method for characterizing MLCC barium titanate ceramic grains is characterized by comprising the following steps:
(1) Fixedly sealing the MLCC on a grinding table along a long axis or a short axis, and mechanically polishing and grinding the MLCC to an effective electrode area;
(2) Carrying out ion etching on the sample obtained in the step (1);
(3) Immersing the sample obtained in the step (2) in an acid solution for acid etching;
(4) And (4) taking out the sample obtained in the step (3), and then washing the surface of the grinding table by using water.
2. The sample processing method for characterizing MLCC barium titanate ceramic grains according to claim 1, wherein in step (1), the mechanical polishing comprises polishing with 200-300 mesh, 1000-1500 mesh, 2000-3000 mesh, 3500-4500 mesh sandpaper in sequence.
3. The sample processing method for characterizing MLCC barium titanate ceramic grains according to claim 1, wherein in step (2), the ion gun angle of the ion etching is 1 ° to 10 °, the voltage is 2kv to 8kv, and the time is 2h to 4h.
4. The sample processing method for characterizing MLCC barium titanate ceramic grains according to claim 1, wherein in step (3), the acid solution comprises HCl and HNO 3 。
5. The sample processing method for characterizing MLCC barium titanate ceramic grains according to claim 4, wherein in step (3), the acid solution comprises HCl, HNO 3 And water in a volume ratio of 1:1: (1-5).
6. The sample processing method for characterizing MLCC barium titanate ceramic grains according to claim 5, wherein in step (3), the initial concentration comprising HCl 37% and HNO 3 68% of the initial concentration.
7. The sample processing method for characterizing MLCC barium titanate ceramic grains according to claim 1, wherein in step (3), the acid etching time is 5-20min.
8. The sample processing method for characterizing MLCC barium titanate ceramic grains according to claim 1, wherein in step (1), the mechanical polishing comprises polishing with 200 mesh, 1200 mesh, 2400 mesh, 4000 mesh sandpaper in sequence;
in the step (2), the angle of an ion gun of the ion etching is 5 degrees, the voltage is 5kv, and the time is 2h;
in the step (3), the acid solution comprises HCl, HNO 3 And water in a volume ratio of 1:1:1, and the acid etching time is 10min.
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Cited By (2)
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| CN116660303A (en) * | 2023-07-31 | 2023-08-29 | 广东微容电子科技有限公司 | Analysis method of ceramic grains of multilayer ceramic capacitor |
| CN117073548A (en) * | 2023-08-15 | 2023-11-17 | 广东微容电子科技有限公司 | Method for detecting thickness of inner electrode of chip type multilayer ceramic capacitor |
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| CN117073548A (en) * | 2023-08-15 | 2023-11-17 | 广东微容电子科技有限公司 | Method for detecting thickness of inner electrode of chip type multilayer ceramic capacitor |
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