CN1487543A - Sol-gel enclosed treatment process for electronic element and device - Google Patents
Sol-gel enclosed treatment process for electronic element and device Download PDFInfo
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- CN1487543A CN1487543A CNA031422853A CN03142285A CN1487543A CN 1487543 A CN1487543 A CN 1487543A CN A031422853 A CNA031422853 A CN A031422853A CN 03142285 A CN03142285 A CN 03142285A CN 1487543 A CN1487543 A CN 1487543A
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- sol
- gel
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- borosilicate
- components
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Abstract
The present invention discloses the method for enclosed processing electronic element and device with sol-gel. Electronic element and device is set inside sealed container, and after vacuum pumping, sol is introduced to soak the electronic element and device before further vacuum pumping and drying at room temperature. The dip coating process is repeated for several times to raise surface gel thickness, and the electronic element and device with coated gel is heat treated in furnace to complete the enclosing treatment. The said process can enclose the cracks and pores, especially the bonding crack between metal inner electrode and ceramic, inside and outside the electronic element and device, form one compact protecting coating on the surface of inner electrode, prevent outer harmful matter from entering inside of the electronic element and device during electroplating and use, and prolong the service life of electronic element and device.
Description
Affiliated technical field
The sealing that the present invention relates to electronic devices and components is handled, specifically a kind of employing colloidal sol-gel sealing processing electronic element and device method.
Background technology
Since the eighties, along with rapid development of surface mount in the world, lamination sheet type device purposes such as multilayer ceramic capacitor, resistor, multi-layer inductor, filter, balanced to unbalanced transformer (Ba Lun), resonator oscillator, frequency discriminator, antenna, duplexer, RF switch module are more and more wide.Facts have proved and to adopt three layers of termination electrode technology, can improve anti-sweating heat and solderability effectively, adapt to the surface mounting technology requirement.The basal electrode of three layers of termination electrode is the fine silver layer, and target is a nickel dam, and outer electrode is tin or tin-lead alloy layer.Form the plating of three layers of termination electrode structure, plating than general machinery, plastic part is more complex, it integrates pottery, electronics, chemical industry technology, should make product when improving anti-sweating heat and solderability, keep every electrical property to be without prejudice, allow again the chemical composition of plating bath does not produce harmful effect to the medium body in the electroplating process.In electroplating process, these devices are in the also charged adverse circumstances of weakly acidic plating bath, because termination electrode, termination electrode and the ceramic dielectric contact zones of laminated device are porous matter, electroplate liquid permeates to device inside by termination electrode and layer electrode defects in electroplating process, make the corrosion of the electroplate liquid that electrode is infiltrated in the device and cause its electrical property to descend, electroplate liquid is stayed also can influence the partial properties of device index in the device, all can cause the deterioration of part electrical performance indexes after electroplating.For preventing the device performance degradation, carried out serial test at device and plating, generally all alleviate the device electrical performance fall at present by the method for raising porcelain body sintered density and the method for adjustment electroplate liquid formulation.
Summary of the invention
The purpose of this invention is to provide a kind of employing colloidal sol-gel sealing processing electronic element and device method; thereby device surface form diaphragm or in hole and crackle the method for decomposition in situ sintering dead-end pore and crackle carry out the device surface sealing and handle and make plating bath can't carry out device inside, thereby prevent the device electrical performance deterioration.
In order to achieve the above object, the technical solution used in the present invention is as follows:
Scheme 1:
1) electronic devices and components are placed in the vacuum tank, introduce colloidal sol then and vacuumized 30～300 minutes, dry under room temperature, atmospheric conditions; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
2) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
Scheme 2:
1) electronic devices and components are vacuumized processing, the pumpdown time is between 10～60 minutes; 2) in vacuum tank, introduce colloidal sol, continued then to vacuumize 30～300 minutes, dry under room temperature, atmospheric conditions; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
3) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
Scheme 3:
1) electronic devices and components are vacuumized processing, the pumpdown time is between 10～60 minutes;
2) in vacuum tank, introduce colloidal sol, continued then to vacuumize 30～300 minutes, dry under room temperature, atmospheric conditions; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
3) to passing through immersion process through vacuum treated electronic devices and components, dry under room temperature, the atmospheric conditions, carry out one or many on the electronic devices and components surface and apply, form silicon gel, alumina gel, titanium gel, zirconium gel, zinc borosilicate gel, barium borosilicate gel, borosilicate gel, plumbous borosilicate gel or the plural gel layer of 0.1～2 μ m on the electronic devices and components surface;
4) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
Scheme 4:
1) electronic devices and components is adopted the dip-coating mode in filling the container of colloidal sol, form silicon gel, alumina gel, titanium gel, zirconium gel, zinc borosilicate gel, barium borosilicate gel, borosilicate gel, plumbous borosilicate gel or the plural gel layer of 0.1～2 μ m on the electronic devices and components surface; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
2) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
The present invention compares with background technology, and the useful effect that has is:
Adopt process of the present invention can effectively seal electronic device surface and inside holes and slit; and the flawless protective finish that the metal inner electrode surface that has the slit forms one deck densification can combined with pottery; can effectively prevent in plating or the use; extraneous harmful substance is carried out electronic devices and components inside; even enter the inner corrosion that also can reduce internal electrode metal; keep original electrical property constant simultaneously, can prolong electronic devices and components useful life or reduce device electrical performance deterioration in the electroplating process.
Observe through electronic scanner microscope, above-mentioned Ludox is handled can form the fatal noncrystalline membrane of one deck, effectively shutoff electronic devices and components crizzle and hole at device surface; Adopt zinc borosilicate and barium borosilicate sol to handle, can further promote the sintering between the surface microstructure, thereby the micro-crack of device surface and hole are disappeared.Sealing was handled before the present invention can be used for lamination sheet type electronic devices and components plating such as multilayer ceramic capacitor, resistor, multi-layer inductor, filter, balanced to unbalanced transformer (Ba Lun), resonator oscillator, frequency discriminator, antenna, duplexer, RF switch module, also can be used for the protection against the tide of electronic devices and components, damp proof and anticorrosive property gas sealing processing.
Embodiment
Embodiment 1
Vacuumize 0.3 hour in the airtight container with holding the filter that prints after silver ink firing is finished to be placed on, adopt suction pipe to utilize the container pull of vacuum to introduce Ludox then, continued to vacuumize 2 hours, get rid of gas in the laminated filter, it is inner that colloidal sol enters pottery, stop to vacuumize, take out filter in room temperature, atmosphere is put into box type furnace after dry 2 hours down, and 80 ℃ are incubated 1 hour, are warming up to 600 ℃ with 4 ℃/min speed, be incubated 2 hours, cool to room temperature then with the furnace, obtain sealing the filter of processing, electroplate back device differential loss degradation 0.1～0.2dB, the device differential loss that is untreated reduces by 3～4dB, effectively reduces the electrical property deterioration.
Embodiment 2
Vacuumize 0.3 hour in the airtight container with holding the filter that prints after silver ink firing is finished to be placed on, adopt suction pipe to utilize the container pull of vacuum to introduce aluminium colloidal sol then, continued to vacuumize 2 hours, get rid of gas in the laminated filter, it is inner that colloidal sol enters pottery, stop to vacuumize, take out filter in room temperature, atmosphere is put into box type furnace after dry 2 hours down, and 80 ℃ are incubated 1 hour, are warming up to 900 ℃ with 4 ℃/min speed, be incubated 2 hours, cool to room temperature then with the furnace, obtain sealing the filter of processing, electroplate back device differential loss degradation 0.1～0.2dB, the device differential loss that is untreated reduces by 3～4dB, effectively reduces the electrical property deterioration.
Embodiment 3
Carry out the preparation of zinc borosilicate sol earlier, its proportioning is as follows: Zn (AC)
2: H
3BO
3: Si (OCH
2-CH
3)
4: H
2O=1: 2: 7: 30 (mol ratio), adopt C
2H
5As catalyst, bath temperature is 60 ℃ to OH as solvent, HCl, depositing 1 hour.
Vacuumize 0.5 hour in the airtight container with holding the filter that prints after silver ink firing is finished to be placed on, adopt suction pipe to utilize the container pull of vacuum to introduce the zinc borosilicate sol then, continued to vacuumize 2 hours, get rid of gas in the laminated filter, it is inner that colloidal sol enters pottery, stop to vacuumize, take out the filter room temperature, atmosphere is put into box type furnace after dry 2 hours down, and 80 ℃ are incubated 1 hour, are warming up to 500 ℃ with 4 ℃/min speed, be incubated 2 hours, cool to room temperature then with the furnace, obtain sealing the filter of processing, electroplate back device differential loss degradation 0.1～0.2dB, the device differential loss that is untreated reduces by 3～4dB, effectively reduces the electrical property deterioration.
Embodiment 4
Carry out the preparation of zinc borosilicate sol earlier, its proportioning is as follows: Zn (AC)
2: H
3BO
3: Si (OCH
2-CH
3)
4: H
2O=1: 2: 7: 30 (mol ratio), adopt C
2H
5As catalyst, bath temperature is 60 ℃ to OH as solvent, HCl, depositing 1 hour.
Vacuumize 0.5 hour in the airtight container with holding the filter that prints after silver ink firing is finished to be placed on, adopt suction pipe to utilize the container pull of vacuum to introduce the zinc borosilicate sol then, continued to vacuumize 2 hours, get rid of gas in the laminated filter, it is inner that colloidal sol enters pottery, stop to vacuumize, take out the filter room temperature, atmosphere is dry down, repeatedly dip-coating then, form 0.8 μ m gel coat at device surface, put into 80 ℃ of insulations of box type furnace 1 hour, be warming up to 500 ℃ with 4 ℃/min speed, be incubated 2 hours, cool to room temperature then with the furnace, obtain sealing the filter of processing, electroplate in the device differential loss degradation 0.1dB of back, the device differential loss that is untreated reduces by 3～4dB, effectively reduces the electrical property deterioration.
Embodiment 5
Carry out the preparation of zinc borosilicate sol earlier, its proportioning is as follows: Zn (AC)
2: H
3BO
3: Si (OCH
2-CH
3)
4: H
2O=1: 2: 7: 30 (mol ratio), adopt C
2H
5As catalyst, bath temperature is 60 ℃ to OH as solvent, HCl, depositing 1 hour.
Adopt repeatedly dip-coating after will holding the seal silver ink firing to finish, form 1 μ m gel coat at device surface, put into 80 ℃ of insulations of box type furnace 1 hour, be warming up to 500 ℃ with 4 ℃/min speed, be incubated 2 hours, cool to room temperature then with the furnace, obtain sealing the filter of processing, electroplate in the device differential loss degradation 0.1～0.3dB of back, the device differential loss that is untreated reduces by 3～4dB, effectively reduces the electrical property deterioration.
Embodiment 6
Carry out the preparation of zinc borosilicate sol earlier, its proportioning is as follows: Ba (AC)
2: H
3BO
3: Si (OCH
2-CH
3)
4: H
2O=1: 2: 7: 30 (mol ratio), adopt C
2H
5As catalyst, bath temperature is 60 ℃ to OH as solvent, HCl, depositing 1 hour.
Adopt repeatedly dip-coating after will holding the seal silver ink firing to finish, form 0.8 μ m gel coat at device surface, put into 80 ℃ of insulations of box type furnace 1 hour, be warming up to 500 ℃ with 4 ℃/min speed, be incubated 2 hours, cool to room temperature then with the furnace, obtain sealing the filter of processing, electroplate in the device differential loss degradation 0.1～0.2dB of back, the device differential loss that is untreated reduces by 3～4dB, effectively reduces the electrical property deterioration.
Embodiment 7
Carry out the preparation of zinc borosilicate sol earlier, its proportioning is as follows: Zn (AC)
2: H
3BO
3: Si (OCH
2-CH
3)
4: H
2O=1: 2: 7: 30 (mol ratio), adopt C
2H
5As catalyst, bath temperature is 60 ℃ to OH as solvent, HCl, depositing 1 hour.
Vacuumize 0.5 hour in the airtight container with holding the capacitor that prints after silver ink firing is finished to be placed on, adopt suction pipe to utilize the container pull of vacuum to introduce the zinc borosilicate sol then, continued to vacuumize 2 hours, get rid of gas in the stacked capacitor, it is inner that colloidal sol enters pottery, stop to vacuumize, take out the filter room temperature, atmosphere is dry down, repeatedly dip-coating then, form 0.8 μ m gel coat at device surface, put into 80 ℃ of insulations of box type furnace 1 hour, be warming up to 500 ℃, be incubated 2 hours with 4 ℃/min speed, cool to room temperature then with the furnace, obtain sealing the capacitor of processing, (loss angle tangent of 0.1PF～0.22uF) is less than 1.0% (20, IMHz IVDC for plating back NPO capacitor, 75%), being untreated, (loss angle tangent of 0.1PF～0.22uF) is less than 3.5% (20, IMHz IVDC, 75%) for the NPO capacitor.
Embodiment 8
Carry out the preparation of zinc borosilicate sol earlier, its proportioning is as follows: Zn (AC)
2: H
3BO
3: Si (OCH
2-CH
3)
4: H
2O=1: 2: 7: 30 (mol ratio), adopt C
2H
5As catalyst, bath temperature is 60 ℃ to OH as solvent, HCl, depositing 1 hour.
Introduce colloidal sol and vacuumized then 2 hours in filling the vacuum tank of filter, get rid of gas in the laminated filter, it is inner that colloidal sol enters pottery, stops to vacuumize, and takes out drying for standby under filter room temperature, the atmosphere.Be warming up to 500 ℃ with 4 ℃/min speed, be incubated 2 hours, cool to room temperature then with the furnace, obtain sealing the filter of processing, electroplate in the device differential loss degradation 0.1～0.3dB of back, the device differential loss that is untreated reduces by 3～4dB, effectively reduces the electrical property deterioration.
Claims (4)
1. one kind is adopted colloidal sol-gel method to handle the method for sealing electronic devices and components, and it is characterized in that: it comprises following each step:
1) electronic devices and components are placed in the vacuum tank, introduce colloidal sol then and vacuumized 30～300 minutes, dry under room temperature, atmospheric conditions; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
2) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
2. a kind of employing colloidal sol according to claim 1-gel method is handled the method for sealing electronic devices and components, and it is characterized in that: it comprises following each step:
1) electronic devices and components are vacuumized processing, the pumpdown time is between 10～60 minutes;
2) in vacuum tank, introduce colloidal sol, continued then to vacuumize 30～300 minutes, dry under room temperature, atmospheric conditions; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
3) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
3. a kind of employing colloidal sol according to claim 1-gel method is handled the method for sealing electronic devices and components, and it is characterized in that: it comprises following each step:
1) electronic devices and components are vacuumized processing, the pumpdown time is between 10～60 minutes;
2) in vacuum tank, introduce colloidal sol, continued then to vacuumize 30～300 minutes, dry under room temperature, atmospheric conditions; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
3) to passing through immersion process through vacuum treated electronic devices and components, dry under room temperature, the atmospheric conditions, carry out one or many on the electronic devices and components surface and apply, form silicon gel, alumina gel, titanium gel, zirconium gel, zinc borosilicate gel, barium borosilicate gel, borosilicate gel, plumbous borosilicate gel or the plural gel layer of 0.1～2 μ m on the electronic devices and components surface;
4) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
4. one kind is adopted colloidal sol-gel method to handle the method for sealing electronic devices and components, and it is characterized in that: it comprises following each step:
1) electronic devices and components is adopted the dip-coating mode in filling the container of colloidal sol, form silicon gel, alumina gel, titanium gel, zirconium gel, zinc borosilicate gel, barium borosilicate gel, borosilicate gel, plumbous borosilicate gel or the plural gel layer of 0.1～2 μ m on the electronic devices and components surface; Said colloidal sol is Ludox, aluminium colloidal sol, titanium colloidal sol, zirconium colloidal sol, zinc borosilicate sol, barium borosilicate sol, borosilicate sol, plumbous borosilicate sol or complex sol;
2) after under room temperature, the atmospheric conditions dry 1～3 hour; the electronic devices and components that are coated with gel are placed box type furnace, chain-conveyer furnace or atmosphere protection stove; be warming up to 350～950 ℃ to be not more than 50 ℃/min speed; temperature retention time was heat-treated in 0.5～6 hour; cool to room temperature then with the furnace, promptly finish the sealing of electronic devices and components is handled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031422853A CN1287398C (en) | 2003-08-13 | 2003-08-13 | Sol-gel enclosed treatment process for electronic element and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031422853A CN1287398C (en) | 2003-08-13 | 2003-08-13 | Sol-gel enclosed treatment process for electronic element and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1487543A true CN1487543A (en) | 2004-04-07 |
| CN1287398C CN1287398C (en) | 2006-11-29 |
Family
ID=34155685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031422853A Expired - Fee Related CN1287398C (en) | 2003-08-13 | 2003-08-13 | Sol-gel enclosed treatment process for electronic element and device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1287398C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102751090A (en) * | 2012-07-09 | 2012-10-24 | 合肥华耀电子工业有限公司 | Impregnation process of metal foil type capacitor with dry type high-pressure polypropylene film |
| CN104726030A (en) * | 2015-04-03 | 2015-06-24 | 叶峰 | Welding mud for novel high temperature resistant insulation lamp as well as preparation method and application of welding mud |
| CN105689833A (en) * | 2016-03-24 | 2016-06-22 | 株洲天微技术有限公司 | Brazing sealing covering method and structure for shell and cover plate of microcircuit module |
| CN108441923A (en) * | 2018-03-23 | 2018-08-24 | 长沙小新新能源科技有限公司 | A kind of hole-sealing technology of magnesium alloy |
| CN109449013A (en) * | 2018-10-19 | 2019-03-08 | 福建火炬电子科技股份有限公司 | A method of prevent electroplate liquid from invading terminal electrode of multi-layer ceramic capacitor |
-
2003
- 2003-08-13 CN CNB031422853A patent/CN1287398C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102751090A (en) * | 2012-07-09 | 2012-10-24 | 合肥华耀电子工业有限公司 | Impregnation process of metal foil type capacitor with dry type high-pressure polypropylene film |
| CN104726030A (en) * | 2015-04-03 | 2015-06-24 | 叶峰 | Welding mud for novel high temperature resistant insulation lamp as well as preparation method and application of welding mud |
| CN104726030B (en) * | 2015-04-03 | 2016-11-23 | 叶峰 | A kind of high-temperature insulation lamp weldering mud and its preparation method and application |
| CN105689833A (en) * | 2016-03-24 | 2016-06-22 | 株洲天微技术有限公司 | Brazing sealing covering method and structure for shell and cover plate of microcircuit module |
| CN105689833B (en) * | 2016-03-24 | 2018-02-23 | 株洲天微技术有限公司 | A kind of the sealed with brazing capping method and structure of microcircuit module housing and cover plate |
| CN108441923A (en) * | 2018-03-23 | 2018-08-24 | 长沙小新新能源科技有限公司 | A kind of hole-sealing technology of magnesium alloy |
| CN109449013A (en) * | 2018-10-19 | 2019-03-08 | 福建火炬电子科技股份有限公司 | A method of prevent electroplate liquid from invading terminal electrode of multi-layer ceramic capacitor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1287398C (en) | 2006-11-29 |
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Granted publication date: 20061129 |