CN113848105A

CN113848105A - Sample processing method convenient for analyzing MLCC ceramic grains

Info

Publication number: CN113848105A
Application number: CN202111430181.8A
Authority: CN
Inventors: 黄翔; 黄卫钢
Original assignee: Guangdong Weirong Electronic Technology Co ltd
Current assignee: Guangdong Weirong Electronic Technology Co ltd
Priority date: 2021-11-29
Filing date: 2021-11-29
Publication date: 2021-12-28
Anticipated expiration: 2041-11-29
Also published as: CN113848105B

Abstract

The application relates to the field of MLCC ceramic grain analysis, and discloses a sample processing method convenient for analyzing MLCC ceramic grains, which is used for analyzing the appearance of the ceramic grains and the sintering compactness of ceramics and comprises the following steps: s1, preparing equipment: selecting a rapid sintering furnace which can run at a high belt speed up to 180mm/min and has a highest heating rate up to 8000 ℃/h; s2, sample treatment: slicing along the long axis or short axis of the electrode of the sample; s3, sample temperature rising: feeding the sample into a rapid sintering furnace and adjusting the temperature rise rate to 3000-8000 ℃/min; s4, sample heat preservation: preserving the heat for 1-60 min when the temperature reaches 800-1300 ℃; s5, cooling the sample: and (4) cooling the sample after the step S4, and adjusting the cooling rate to 3000-8000 ℃/min. By the mode, the problems that the real appearance of ceramic grains and the sintering compactness of ceramic are not easy to analyze in the prior art are solved.

Description

Sample processing method convenient for analyzing MLCC ceramic grains

Technical Field

The application relates to the field of MLCC ceramic grain analysis, in particular to a sample processing method convenient for analyzing MLCC ceramic grains.

Background

A multilayer chip ceramic capacitor (MLCC) is a small-sized, high-specific-volume, high-precision electronic component suitable for Surface Mount Technology (SMT), and the MLCC is currently mainly developed in the direction of miniaturization, high-capacity, high-frequency, high-temperature, and high-voltage.

The ceramic powder accounts for the higher production cost of the MLCC, and particularly, the production of the high-capacity MLCC has strict requirements on the purity, the particle size, the granularity and the morphology of the ceramic powder. The number of ceramic grains contained in the single-layer medium in the MLCC is closely related to the electrical property and the reliability of the MLCC, so that the grain appearance and the size of the ceramic medium layer can reflect the suitability of the selected ceramic powder.

The existing processing method commonly used for analyzing the morphology of the ceramic crystal comprises the following steps: chemical etching and thermal etching. The chemical etching is generally carried out using strong acids, such as HF, HCl or HNO₃The mixed solution is used for processing the surface of a ceramic sample, and a morphology phase is formed through the difference of corrosion degrees of strong acid to a grain boundary and grains. Its advantages are simple process, high efficiency, and treating a lot of samples at the same time, and no obvious effect to powder with small particle size and high resistance to acid corrosion. The hot corrosion is to place the sample in a high temperature furnace and to realize the development of crystal grains through the volatilization of crystal boundary elements. Its disadvantages are low productivity, not easy to find out the corrosion condition, but capable of processing the sample with small grain size.

Therefore, it is necessary to explore the hot etching technique.

Disclosure of Invention

In view of the above problems, the present application provides a sample processing method for analyzing MLCC ceramic grains conveniently, and aims to solve the problem that the real morphology of the ceramic grains and the sintering compactness of the ceramic are not easy to analyze in the prior art.

In order to solve the technical problems, the sample processing method for conveniently analyzing the MLCC ceramic grains is used for analyzing the appearance of the ceramic grains and the sintering compactness of the ceramic, and is characterized by comprising the following steps of:

s1, preparing equipment: opening a rapid sintering furnace which runs at a high belt speed up to 180mm/min and has a highest heating rate up to 8000 ℃/h, and maintaining the nitrogen environment of the rapid sintering furnace;

s2, sample treatment: slicing along the long axis or short axis of the electrode of the sample;

s3, sample temperature rising: feeding the sample into a rapid sintering furnace and adjusting the temperature rise rate to 3000-8000 ℃/min;

s4, sample heat preservation: preserving the heat for 1-60 min when the temperature reaches 800-1300 ℃;

s5, cooling the sample: and adjusting the cooling rate to 3000-8000 ℃/min, cooling the sample subjected to the step S4 to below 100 ℃, and taking out.

The beneficial effect of this application is: different from the prior art, the sample processing method convenient for analyzing the MLCC ceramic grains adopts equipment capable of rapidly increasing and decreasing the temperature and a proper corrosion process to meet the thermal corrosion requirement of the fine-grained ceramic. So as to volatilize the grain boundaries without causing excessive corrosion of the grains. By the mode, the problems that the real appearance of ceramic grains and the sintering compactness of ceramic are not easy to analyze in the prior art are solved.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.

FIG. 1 is a flow chart of a sample processing method provided herein to facilitate analysis of MLCC ceramic grains;

FIG. 2 is a graph illustrating the effect of the prior art acid etching technique provided herein;

FIG. 3 is a graph illustrating the effect of the prior art hot etching technique provided herein;

FIG. 4 is a graph illustrating the effect of a sample processing method provided herein to facilitate analysis of MLCC ceramic grains.

Detailed Description

The technical solutions in the embodiments of the present application will be described clearly and completely with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, 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 application.

It should be noted that all the directional indications such as up, down, left, right, front and rear … … in the embodiment of the present application are only used to explain the relative positional relationship, movement, etc. between the components in a specific posture as shown in the drawings, and if the specific posture is changed, the directional indication is changed accordingly.

In addition, the descriptions referred to as "first", "second", etc. in this application are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicit ly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present application.

The technical scheme provided by the application is to provide a sample processing method convenient for analyzing MLCC ceramic grains.

Referring to fig. 1, fig. 1 is a flow chart of a sample processing method for analyzing MLCC ceramic grains according to the present invention.

The flow chart comprises the following steps:

s5, cooling the sample: and (4) adjusting the cooling rate to be 3000-8000 ℃/min, and cooling the sample subjected to the step S4 to be below 100 ℃.

The samples were under nitrogen throughout the treatment. It will be understood that the effect of nitrogen on the sample is on the one hand to isolate the oxidizing environment from the reducing environment: the ceramic crystal grains can grow for the second time in the oxidizing environment, so that the real appearance of the ceramic crystal grains cannot be obtained; the electrode can agglomerate in a reducing environment, and the surface appearance is influenced. On the other hand, the nitrogen gas flow can be used as purge gas to take away the thermally corroded gaseous substances, so that the phenomenon that the gaseous substances are condensed on the surface of the ceramic again to influence the appearance observation during the temperature reduction is prevented.

To facilitate understanding of the technology of the present application, the effect is compared with the existing acid etching technology and the existing hot etching technology.

Referring to fig. 2, fig. 2 is a diagram illustrating an effect of a conventional acid etching technique provided in the present application.

The prior acid corrosion effect can be seen in fig. 2: the corrosion time is short, and crystal grains cannot be shown; the corrosion time is long, the crystal grains are over-corroded, and the actual conditions of the crystal grains cannot be reflected.

Referring to fig. 3, fig. 3 is a diagram illustrating the effect of the conventional hot etching technique provided in the present application.

The prior art uses the corrosion effect of a common sintering furnace: the heating rate is too slow, the ceramic crystal grains are sintered for the second time, the internal electrode is seriously shrunk, and the real size of the ceramic crystal grains cannot be obtained.

Further, the techniques provided herein are used to process samples. Please see table one, which is four preferred embodiments of the present application.

Table one:

examples	Rate of temperature rise (. degree. C./min)	Holding temperature (C)℃）	Incubation time (min)
				1	5000	950	10
2	5000	1000	10
				3	5000	1050	10
4	5000	1100	10

Preferably, the temperature increase rate in the step S3 is 5000 deg.C/min.

Wherein the flow rate of the nitrogen is 100-300L/min.

Preferably, the flow rate of the nitrogen is 150L/min or 200L/min.

Referring to fig. 4, fig. 4 is a diagram illustrating the effect of a sample processing method for analyzing MLCC ceramic grains according to the present invention.

The results of fig. 4 were obtained by the 4 examples described above under the same nitrogen atmosphere conditions. It can be understood that the real morphology of the ceramic grains can be obtained by adopting the rapid sintering furnace for hot corrosion and reasonably controlling the conditions of each step according to the technical scheme of the application.

Different from the prior art, the technical method provided by the application solves the problem that the real morphology of the ceramic crystal grains and the sintering compactness of the ceramic are not easy to analyze in the prior art.

In the embodiments provided in the present application, it should be understood that the disclosed method can be implemented in other ways. For example, the above-described embodiments are merely illustrative, and other values may be obtained in actual implementations.

The above embodiments are merely examples, and not intended to limit the scope of the present application, and all equivalent changes, direct or indirect applications, which are made by using the contents of the specification and drawings of the present application, and other related technical fields, are included in the scope of the present application.

Claims

1. A sample processing method convenient for analyzing MLCC ceramic grains is used for analyzing the appearance of the ceramic grains and the sintering compactness of ceramics and is characterized by comprising the following steps:

2. The process according to claim 1, wherein the temperature increase rate in the step of S3 is preferably 5000 ℃/min.

3. The process according to claim 1, characterized in that the incubation temperature of the step S4 is preferably 950 ℃ or 1000 ℃ or 1050 ℃.

4. The treatment method according to claim 3, wherein the holding time in the step S4 is preferably 10 min.

5. The method according to any one of claims 1 to 4, wherein the flow rate of the nitrogen gas is 100 to 300L/min.

6. The process according to claim 5, characterized in that the flow rate of nitrogen is preferably 150L/min or 200L/min.