CN112316844A - Surface modification solution and application thereof - Google Patents

Surface modification solution and application thereof Download PDF

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Publication number
CN112316844A
CN112316844A CN202011200078.XA CN202011200078A CN112316844A CN 112316844 A CN112316844 A CN 112316844A CN 202011200078 A CN202011200078 A CN 202011200078A CN 112316844 A CN112316844 A CN 112316844A
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solution
surface modification
modification solution
emulsifier
modifier
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CN202011200078.XA
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Inventor
曹秀华
黄�俊
付振晓
任海东
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Guangdong Fenghua Advanced Tech Holding Co Ltd
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Guangdong Fenghua Advanced Tech Holding Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C09K23/017Mixtures of compounds
    • C09K23/018Mixtures of two or more different organic oxygen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/018Dielectrics
    • H01G4/06Solid dielectrics
    • H01G4/08Inorganic dielectrics
    • H01G4/12Ceramic dielectrics
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/228Terminals
    • H01G4/252Terminals the terminals being coated on the capacitive element

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Capacitors (AREA)

Abstract

The invention discloses a surface modification solution which comprises the following components in parts by weight: 10-20 parts of surface modifier, 0.5-1 part of emulsifier and 0.5-1 part of defoaming agent; the surface modifier is siloxane. The surface modification solution is adopted to carry out surface treatment on the chip component, so that the hydrophobicity of the surface of the chip component can be improved, the surface tension is increased, the end-capping appearance of the end electrode of the chip component is effectively improved, the end-capping defects are reduced, the end electrode of the chip component is good in appearance, the bad phenomena of sagging, crescent and the like are avoided, and the reliability of a product is improved. Meanwhile, the invention also discloses the application of the surface modification solution in the surface treatment of electronic components.

Description

Surface modification solution and application thereof
Technical Field
The invention belongs to the technical field of electronic components, and particularly relates to a surface modification solution and application thereof in electronic components.
Background
Electronic components are important supports of the electronic information industry, are essential important components of electronic equipment, electronic information systems and weapon equipment control systems, are smaller and smaller in size, higher and higher in circuit density and higher in transmission speed, and are developing towards chip type, miniaturization, high frequency, high reliability, green and environment protection and the like. Chip electronic components are generally prepared by the processes of material preparation, tape casting, lamination, sintering, end sealing, end burning and the like, and each process link is closely related to the performance and reliability of the components except the performance of the materials.
Early researches on the reliability of the chip components mainly focused on the ceramic body and the internal electrode part, and with the continuous improvement of the reliability requirements of the chip components and the deep research, the influence of the terminal electrode on the reliability is increasingly concerned. How to obtain a good terminal electrode becomes one of common technical problems to be overcome by the industry, and the processes of end capping, end burning and the like get attention of technicians. The end capping is one of the important process steps of the chip electronic component, namely, the conductive slurry encapsulates two ends of the component in a dip coating mode, and the end electrode is formed after sintering. Because the chip of the chip type electronic component is made of inorganic ceramic materials and the surface of the chip is hydrophilic, the slurry after end capping is easy to generate poor appearances such as sagging, crescent moon and the like, and the performance of the electronic component is influenced. In order to solve the problem, besides the adjustment of the rheological property of the conductive paste, technical experts in the chip component industry also make various attempts, and pioneers and others report a plasma treatment process, namely before the end-capping process of the multilayer ceramic capacitor, the surface of the multilayer ceramic capacitor is subjected to plasma hydrophobic treatment, so that the surface of the electronic component reaches a better hydrophobic state, and the problem of product sagging is solved. However, the method requires special plasma treatment equipment, which is expensive and needs to be imported, and is not easy to operate. The Yangyi seal and the like invent that the surface hydrophobic solution soaks and dries the chip component to improve the surface hydrophobicity of the chip component, but the processes of soaking, drying and the like are added, the production period is prolonged, and the hydrophobic solution is not beneficial to environmental protection and safe production because of adding the hydrochloric acid by using an isopropanol solvent.
Disclosure of Invention
Based on this, the object of the present invention is to overcome the above-mentioned disadvantages of the prior art and to provide a surface modification solution. The surface modifier solution is directly added into the chamfering liquid, chamfering and surface treatment of the chip component are simultaneously completed, the end sealing effect of the chip component after the surface treatment is good, and the product performance is obviously improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a surface modification solution comprises the following components in parts by weight: 10-20 parts of surface modifier, 0.5-1 part of emulsifier and 0.5-1 part of defoaming agent; the surface modifier is siloxane.
Preferably, the emulsifier is alkylphenol ethoxylates.
Preferably, the antifoaming agent is n-butanol.
The alkylphenol polyoxyethylene has good emulsifying effect, can form stable emulsion, has good defoaming effect, and is beneficial to reducing bubbles generated in the chamfering process; the n-butyl alcohol is used as a solvent, and has good defoaming effect, so that bubbles generated in the chamfering process of the element can be reduced.
Preferably, the surface modification solution comprises the following components in parts by weight: 12-15 parts of surface modifier, 0.5-0.8 part of emulsifier and 0.5-0.8 part of defoaming agent.
Meanwhile, the invention also provides a preparation method of the surface modification solution, which comprises the following steps:
s1: stirring and dispersing an emulsifier in an aqueous solution to obtain a mixed solution A;
s2: adding a surface modifier into the mixed solution A, and stirring until the surface modifier is uniformly dispersed to obtain a mixed solution B;
s3: and adding a defoaming agent into the mixed solution B, and stirring until the mixture is uniformly dispersed to obtain a surface modified solution.
In addition, the invention also discloses an application of the surface modification solution in surface treatment of electronic components.
Further, the invention also discloses a surface treatment method of the chip electronic component, which comprises the following steps: and (3) directly adding the surface modification solution into a chamfering tank, carrying out surface modification in the chamfering process, and uniformly coating the surface modifier on the surface of the sheet element after drying.
Preferably, the weight percentage content of the surface modification solution in the chamfering solution is 5-10%.
More preferably, the surface modification solution is present in the chamfering fluid in an amount of 8% by weight.
Compared with the prior art, the invention has the beneficial effects that:
the surface modification solution is adopted to carry out surface treatment on the chip component, so that the hydrophobicity of the surface of the chip component is improved, the surface tension is increased, the end-capping appearance of the terminal electrode of the chip component can be effectively improved, the end-capping defects are reduced, the terminal electrode of the chip component is good in appearance, the poor phenomena of sagging, crescent and the like are avoided, and the reliability of a product is improved.
The surface modification solution is directly added into the chamfering tank, the surface treatment of the electronic component is completed by utilizing the chamfering process, and compared with the original process and method, the process has the advantages of no increase of equipment investment and production period, simple process, safety, environmental protection and easy operation.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The invention is provided with embodiments 1-4, and the surface modification solution formula in the specific embodiments 1-4 is shown in table 1:
TABLE 1 EXAMPLES 1 TO 4 surface modification solution formulations
Figure BDA0002751681910000031
The surface treatment solution in table 1 is used for surface treatment of electronic components, and the specific method comprises the following steps:
s1: firstly, dispersing an emulsifier alkylphenol polyoxyethylene ether in an aqueous solution under stirring at room temperature;
s2: adding surface modifier siloxane into S1, and stirring until the surface modifier siloxane is uniformly dispersed;
s3: finally adding the defoaming agent n-butyl alcohol, and stirring until the mixture is uniformly dispersed to prepare a surface treating agent solution;
s4: and (4) adding the surface treating agent solution in the step (S3) into a chamfering tank, wherein the mass amount of the surface treating agent solution accounts for 8% of that of the chamfering solution, and chamfering and surface treating are carried out. The end-capped chip after chamfering was end-capped, and the appearance of the end-capped chip was observed with a microscope to see whether the edge of the end electrode was straight (sagging), whether the end electrode fell off (porcelain exposed), and whether there were air holes (pinholes), and the test results are shown in table 2 (wherein the comparative example is an electronic component that was not treated with a surface modification solution);
s5: the capped chips were subjected to termination burning and plating to prepare MLCCs, which were subjected to reliability testing, and the test results are shown in table 3 (wherein the comparative examples are electronic components not treated with the surface modification solution).
Wherein, the heating aging test: and (3) sealing the ceramic body, burning the end, electroplating, preparing into MLCC, placing into a reflow oven for three times at the temperature of 250 ℃ for 5min, and testing the IR value of the sample without reduction, namely, the sample is qualified.
Accelerated aging test: the method comprises the steps of carrying out end sealing, end burning and electroplating on a ceramic body, preparing the ceramic body into the MLCC, placing the MLCC into a chip experiment board, placing the MLCC into an aging box, and testing the capacity (C), loss (DF) and Insulation Resistance (IR) before and after the MLCC enters the box under the conditions of 8Ur, 150 +/-5 ℃ and 8-8.5 h, wherein the conditions that | delta C/C | is less than or equal to 20%, DF is less than or equal to 2 times of an initial value, and IR is more than or equal to 2000 MOmega are met.
And (3) life test: the method comprises the steps of sealing a ceramic body, burning the end and electroplating the ceramic body to prepare the MLCC, placing the MLCC into a chip experiment board, placing the MLCC into a life test box, testing the capacity (C), loss (DF) and Insulation Resistance (IR) before and after the MLCC enters the box under the conditions of 25V +/-10%, 125 +/-5 ℃ and 100 +/-2 h, wherein the content of delta C/C is less than or equal to 20%, the DF is less than or equal to 2 times of an initial value, and the IR is more than or equal to 2000M omega.
TABLE 2 end-capping morphology test results
Figure BDA0002751681910000041
As can be seen from table 2, in the electronic component subjected to surface modification treatment, the sagging defects on the surface of the end-capped electrode are greatly reduced, mainly the surface modification liquid improves the hydrophobicity of the surface of the component, and the external electrode slurry is not easy to diffuse on the surface to cause the sagging defects. Too little siloxane content in the surface modification liquid can cause insufficient surface hydrophobicity, and the diffusion of the external electrode slurry can not be effectively prevented; the siloxane content is too high and when the outer electrode is sintered, the sintering may cause porcelain exposure or pinhole defects.
TABLE 3 reliability test results
Figure BDA0002751681910000051
As can be seen from the reliability test results in Table 3, the reliability of the element can be significantly improved due to the defect-free morphology of the terminal electrode, and the reliability of the element can be affected due to the fact that the terminal electrode has appearance defects and is permeated by electroplating solution in the subsequent electroplating process.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (8)

1. The surface modification solution is characterized by comprising the following components in parts by weight: 10-20 parts of surface modifier, 0.5-1 part of emulsifier and 0.5-1 part of defoaming agent; the surface modifier is siloxane.
2. The surface modification solution of claim 1, wherein the emulsifier is an alkylphenol ethoxylate.
3. The surface modification solution of claim 1, wherein the anti-foaming agent is n-butanol.
4. The surface modification solution of any one of claims 1 to 3, comprising the following components in parts by weight: 12-15 parts of surface modifier, 0.5-0.8 part of emulsifier and 0.5-0.8 part of defoaming agent.
5. A method for preparing the surface modification solution according to any one of claims 1 to 4, comprising the steps of:
s1: stirring and dispersing an emulsifier in an aqueous solution to obtain a mixed solution A;
s2: adding a surface modifier into the mixed solution A, and stirring until the surface modifier is uniformly dispersed to obtain a mixed solution B;
s3: and adding a defoaming agent into the mixed solution B, and stirring until the mixture is uniformly dispersed to obtain a surface modified solution.
6. Use of the surface modification solution according to any one of claims 1 to 4 in surface treatment of electronic components.
7. A surface treatment method for a chip electronic component is characterized by comprising the following steps: directly adding the surface modification solution as described in any one of claims 1 to 4 into a chamfering tank, carrying out surface modification in the chamfering process, and uniformly coating the surface modification agent on the surface of the sheet element after drying.
8. The surface treatment method for chip electronic components as claimed in claim 7, wherein the weight percentage of the surface modification solution in the chamfering solution is 8%.
CN202011200078.XA 2020-10-30 2020-10-30 Surface modification solution and application thereof Pending CN112316844A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113552419A (en) * 2021-09-18 2021-10-26 广东微容电子科技有限公司 Method for indirectly detecting MLCC medium ceramic lattice defect

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01208848A (en) * 1988-02-17 1989-08-22 Hitachi Ltd Resin sealed type semiconductor device
CN1487123A (en) * 2003-08-13 2004-04-07 浙江大学 Pre-electroplating treatment process of electronic element and device to prevent electrical performance degradation
CN103773226A (en) * 2013-12-20 2014-05-07 深圳顺络电子股份有限公司 Hydrophobic solution and method for solving slurry sagging of chip element outer electrode
WO2017046017A1 (en) * 2015-09-14 2017-03-23 Wacker Chemie Ag Process for continuous production of stable silicone emulsions
CN107099237A (en) * 2017-05-31 2017-08-29 青岛海信电器股份有限公司 A kind of coating and preparation method thereof, dual-component coating and component containing the coating
CN108752590A (en) * 2018-04-25 2018-11-06 中科广化(重庆)新材料研究院有限公司 A kind of long-chain siloxy flucride siloxane lotion and its modified inorganic silicate coating and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01208848A (en) * 1988-02-17 1989-08-22 Hitachi Ltd Resin sealed type semiconductor device
CN1487123A (en) * 2003-08-13 2004-04-07 浙江大学 Pre-electroplating treatment process of electronic element and device to prevent electrical performance degradation
CN103773226A (en) * 2013-12-20 2014-05-07 深圳顺络电子股份有限公司 Hydrophobic solution and method for solving slurry sagging of chip element outer electrode
WO2017046017A1 (en) * 2015-09-14 2017-03-23 Wacker Chemie Ag Process for continuous production of stable silicone emulsions
CN107099237A (en) * 2017-05-31 2017-08-29 青岛海信电器股份有限公司 A kind of coating and preparation method thereof, dual-component coating and component containing the coating
CN108752590A (en) * 2018-04-25 2018-11-06 中科广化(重庆)新材料研究院有限公司 A kind of long-chain siloxy flucride siloxane lotion and its modified inorganic silicate coating and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113552419A (en) * 2021-09-18 2021-10-26 广东微容电子科技有限公司 Method for indirectly detecting MLCC medium ceramic lattice defect
CN113552419B (en) * 2021-09-18 2022-06-14 广东微容电子科技有限公司 Method for indirectly detecting MLCC medium ceramic lattice defect

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