CN105001751A - Paint for improving damp heat resistance of precise metal film resistor and preparation method of paint - Google Patents
Paint for improving damp heat resistance of precise metal film resistor and preparation method of paint Download PDFInfo
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- CN105001751A CN105001751A CN201510485875.XA CN201510485875A CN105001751A CN 105001751 A CN105001751 A CN 105001751A CN 201510485875 A CN201510485875 A CN 201510485875A CN 105001751 A CN105001751 A CN 105001751A
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Abstract
The invention discloses paint for improving damp heat resistance of a precise metal film resistor. The paint comprises, by mass, 30-60% of thermoset phenolic resin, 10-40% of epoxy resin, 5-20% of multi p-pi and pi-pi conjugated bond modified material and 25-40% of diluent. Firstly, 9-fluorenone is dissolved in liquid organic ketone according to the mass ratio of 1:1, a 9-fluorenone solution is prepared, or novolac epoxy resin is diluted through the liquid organic ketone, and a novolac epoxy resin solution is prepared; the epoxy resin is diluted through ethylene glycol mono-ether, and an epoxy resin solution is prepared; the epoxy resin solution and the base material thermoset phenolic resin are mixed under the stirring condition, the 9-fluorenone solution or the novolac epoxy resin solution is added, the specific gravity is adjusted to be 0.98 through the diluent, and the paint suitable for coating of the metal film resistor on a production line is prepared. The packaging paint is stable in performance when used for a long time, paint layering can not happen even the paint is stored for two years, and when the paint is applied to resistor protection in the damp heat environment, the resistance change rate meets the technical requirement that deltaR/R is smaller than or equal to 0.4%.
Description
Technical field
This name, about electronic information material, particularly relates to a kind of method improving Mirror Grinding packaged material wet-hot aging performance, specifically the composite coating of a kind of precision metal film resistor resol based high-temp-resistant, resistance to high humidity.
Background technology
Mirror Grinding has a wide range of applications in the field such as precision instrument, Aeronautics and Astronautics, and its reliability effect responsiveness and the stability of the circuit that works long hours.But for the Mirror Grinding be operated in hygrothermal environment, require that it has good wet-hot aging performance, this just proposes superior performance requirement to its packaging protection material.For the finished product of the encapsulation resistance be operated in hygrothermal environment, from reliability perspectives analysis, be mainly subject to thermal stresses and moist stress, and thermal stresses is the main stress causing packaged resistance to lose efficacy.If packaged material is performance degradation because thermal stresses recurring structure changes, then water will increase the rate of permeation of packaged material, galvanic corrosion will occur when the resistance film surface in work has and loses efficacy during water; On the contrary; if there is not performance degradation under heat stress in packaged material; then the rate of permeation of water to packaged material is less; water is difficult to enter resistive film surface through protective membrane; resistance by packaged material protection would not operationally lose efficacy because there is galvanic corrosion, thus showed good wet-hot aging performance.Based on the reason that packaged resistance lost efficacy, so improve the method for Mirror Grinding packaged material wet-hot aging performance at present, mainly pass through nano material (as nano-SiO
2, nano-TiO
2deng) or organosilicon etc. improve the resistance toheat of packaged material, make packaged material not hair tonic performance degradation in hot environment, keep the rate of permeation lower to water molecules, thus make packaged resistance in hygrothermal environment, show good wet-hot aging performance.Although packaging protection coating prepared by aforesaid method can meet the requirement of Mirror Grinding wet-hot aging performance, for the packaged material of modified by nano particles, the problem of existence and stability difference in prolonged storage.Find in the application, for the nano-SiO deposited more than 3 months
2, all can there is nano-SiO in modification composite encapsulating material
2the problem of sedimentation, is separated with macromolecule resin matrix and makes packaged material unstable properties, because which limit the application of prepared resistance composite encapsulating material.
In wet environment; when carrying out reliability consideration to the Mirror Grinding in work; find that there is gas evolution on phenolic aldehyde (PF)-epoxy (EP) the resin compounded protective membrane surface at resistance cap two ends, think that the gas of separating out is hydrogen (H
2) and oxygen (O
2).This failtests be by encapsulation after 2.2M Ω (± 0.5%) Cr – Si – Ni – Mo membrane resistance immerse in deionized water; then under voltage rating, carry out experiment 120 seconds, and the part that water is immersed at resistance lead two ends also protects with packaged material.By scanning electron microscope, surface observation is carried out to the resistance after experiment, finds the vestige that the PF-EP composite protection film (comprising the cap place at resistance two ends) of resistive surface is excellent, be not corroded, and resistance value on pretreatment after also do not change.Therefore, can infer that gas that resistance cap two ends are separated out is not that metallic corrosion in resistance film produces.But, according to chemical knowledge, only have conducting metal or organic conductive polymer that water decomposition can be made to produce H
2and O
2.And PF-EP composite protection film used in this experiment is insulating material, be impossible make water decomposition produce H with regard to electroconductibility
2and O
2.With infrared spectra, structural analysis is carried out to PF-EP complex protection material used, find this material contain some p-π and π-pi-conjugated key group (as
).In addition, the electronics in p-π and π-pi-conjugated key is when without being locality when electric field or weak electric field, and electronics can not move, thus makes PF-EP polymer composites macroscopically show as insulativity.But under strong electric field, the local electronic in these p-π and π-pi-conjugated key can be subject to electric field influence, becomes moveable delocalized electron.According to H in above-mentioned failtests
2and O
2the position (resistance cap two ends place, electric field is stronger) produced and packaging protection mould material structure used, think produced H
2and O
2should be PF-EP composite protection film under highfield effect, local electronic in p-π and π-pi-conjugated key occurs delocalized, becomes unbound electron, and with water molecules generation electron exchange, thus the water of resistive surface is decomposed.Based on to H in above-mentioned failtests
2and O
2the analysis of producing cause, thus create the present invention, for the reliability improving Mirror Grinding in hygrothermal environment provides a kind of novel method.
Summary of the invention
Object of the present invention, is to provide a kind of accurate high-accuracy metal film resistor wet-heat resisting coating and preparation method thereof.
The present invention adopts the material containing more p-π and π-pi-conjugated key in a kind of molecular structure, modification is carried out to PF-EP matrix material, p-π and π in formed composite polymeric film-pi-conjugated bond number is increased, to improve it under strong electric field to the capacity of decomposition of water, improve the reliability of Mirror Grinding hygrothermal environment from elimination moisture source side face.
The present invention is achieved by following technical solution.
Improve a coating for Mirror Grinding wet-hot aging performance, raw material and mass percentage content thereof are: thermoset phenolic resin 30 ~ 60%, epoxy resin 10 ~ 40%, many p-π and π-pi-conjugated key material modified 5 ~ 20%, and thinner is 25 ~ 40%;
The number-average molecular weight scope of described thermoset phenolic resin is 200 ~ 1000;
Described epoxy resin is liquid bisphenol A type, and oxirane value scope is 0.44 ~ 0.56Eq/100g;
The material modified organic materials for having insulativity of described many p-π and π-pi-conjugated key;
Described thinner is the mixture of a kind of ethylene glycol mono-ether and liquid organic ketone, and wherein the mass ratio of organic ketone and ethylene glycol mono-ether is m
organic ketone/ m
ethylene glycol mono-ether=1:5 ~ 1:2;
The preparation method of this coating is as follows:
(1) by 1:1 mass ratio, 9-Fluorenone is dissolved in liquid organic ketone, mixes and make 9-Fluorenone solution, or the liquid organic ketone of novolac epoxy is diluted, mix and make novolac epoxy solution; Ethylene glycol mono-ether used for epoxy resin is diluted, mixes and make epoxy resin solution;
(2) according to raw material and mass percentage content batching thereof: thermoset phenolic resin 30 ~ 60%, epoxy resin 10 ~ 40%, many p-π and π-pi-conjugated key material modified 5 ~ 20%, thinner is 25 ~ 40%;
The epoxy resin solution of step (1) is mixed under agitation with body material thermoset phenolic resin, add 9-Fluorenone solution or novolac epoxy solution again, regulate proportion to be 0.98 with thinner, prepare the coating being suitable for metal film resistor and applying on a production line.
Described thermoset phenolic resin is that P-F sets the thermoset alcohol resite be polymerized.
Described epoxy resin is E51 type epoxy resin.
Described many p-π and π-pi-conjugated key is material modified is 9-Fluorenone, novolac epoxy F44 or F51, wherein 9-Fluorenone and novolac epoxy structural formula as follows, all containing a large amount of p-π and π-pi-conjugated key.
Described ethylene glycol mono-ether is ethylene glycol monomethyl ether or ethylene glycol ethyl ether.
Described liquid state is organic ketone is acetone, butanone, cyclopentanone or pimelinketone.
Coating 60 ~ 120s internal surface solidification at 160 ~ 180 DEG C prepared by described step (2), uses to be suitable for the encapsulation of Mirror Grinding production line; Solidify completely in 60 ~ 120min at 160 ~ 180 DEG C, to be suitable for the Mirror Grinding with wet-hot aging performance.
After the present invention carries out damp and hot experiment by GJB360A-96, the change in resistance of Mirror Grinding is less, and resistance change rate all meets technical requirement (Δ R/R≤0.4%).The present invention is specially adapted to the packaging protection of high performance precision metalster, stable performance during life-time service, within 2 years, also coating layering can not occur even if deposit.In addition, due to the wet-hot aging performance of its excellence, the aspects such as the encapsulation of such as electrical condenser also can be applied to.
Accompanying drawing explanation
Fig. 1 is the PF-EP composite coating wet-hot aging performance figure of p-π and π-pi-conjugated key material modification.
Embodiment
Below by specific embodiment, the invention will be further described.
The present invention adopts the material containing more p-π and π-pi-conjugated key in a kind of molecular structure, modification is carried out to PF-EP matrix material, p-π and π in formed composite polymeric film-pi-conjugated bond number is increased, to improve it under strong electric field to the capacity of decomposition of water, improve the reliability of Mirror Grinding hygrothermal environment from elimination moisture source side face.The object of the invention is to, a kind of accurate high-accuracy metal film resistor wet-heat resisting coating and preparation method thereof is provided.
High-accuracy metal film resistor wet-heat resisting coating of the present invention, raw material and mass percentage content thereof are:
Thermoset phenolic resin 30 ~ 60%, epoxy resin 10 ~ 40%, many p-π and π-pi-conjugated key material modified 5 ~ 20%, thinner is 25 ~ 40%.
The number-average molecular weight scope of thermoset phenolic resin of the present invention is 200 ~ 1000, for P-F sets the thermoset alcohol resite be polymerized.
Described epoxy resin is liquid bisphenol A type, and oxirane value scope is 0.44 ~ 0.56Eq/100g.Preferred epoxy resin is E51.
The organic materials of the material modified selection insulativity of many p-π and π-pi-conjugated key, in order to avoid affect the insulating property of packaged material.Preferred 9-Fluorenone, novolac epoxy F44 and F51, wherein 9-Fluorenone and novolac epoxy structural formula as follows, all containing a large amount of p-π and π-pi-conjugated key.
Thinner is the mixture of a kind of ethylene glycol mono-ether (as ethylene glycol monomethyl ether, ethylene glycol ethyl ether etc.) and liquid organic ketone (as acetone, butanone, cyclopentanone, pimelinketone etc.), and wherein the mass ratio of organic ketone and ethylene glycol mono-ether is 1:5 ~ 1:2.
The preparation method of precision metal film resistor wet-heat resisting coating is as follows:
By 1:1 mass ratio, 9-Fluorenone is dissolved in liquid organic ketone, mixes and make 9-Fluorenone solution, or the liquid organic ketone of novolac epoxy is diluted, mix and make novolac epoxy solution; Ethylene glycol mono-ether used for epoxy resin is diluted, mixes and make epoxy resin solution; Epoxy resin solution is mixed under agitation with body material resol, add 9-Fluorenone solution (or novolac epoxy solution) again, and reach 0.98 with the proportion of thinner adjusting coating, apply on a production line to be suitable for metal film resistor, wherein thermoset phenolic resin is 30 ~ 60%, epoxy resin is 10 ~ 40%, and 9-Fluorenone or novolac epoxy are 5 ~ 20%, and thinner is 25 ~ 40%.Prepared coating can at 160 ~ 180 DEG C 60 ~ 120s internal surface solidification (surface drying), use to be suitable for production line encapsulation; (doing solid work) is solidified completely in 60 ~ 120min, to prepare the resistance with wet-hot aging performance at 160 ~ 180 DEG C.
Embodiment 1
Proportioning raw materials is:
Wherein m
cyclopentanone/
ethylene glycol ethyl ether=1:2
Embodiment 2
Prepare by following masses proportioning:
Wherein m
cyclopentanone/
ethylene glycol ethyl ether=1:2.7
Embodiment 3
Prepare by following masses proportioning:
Wherein m
cyclopentanone/
ethylene glycol ethyl ether=1:2.5
Resistance used in embodiment is the Cr – Si – Ni – Mo membrane resistance of 2.2M Ω (± 0.5%).Resistance after often kind of encapsulation gets 30, and carry out wet-heat resisting experiment by GJB360A-96, actual conditions is: relative humidity is 85% ~ 98%, adds at full capacity, and temperature circulates three times from-10 DEG C to+80 DEG C, and total time continues 240 hours continuously.After experiment terminates, require resistance change rate Δ R/R≤0.4%.Experimental result as shown in Figure 1.
As shown in Figure 1, when the PF-EP composite coating (containing more p-π and π-pi-conjugated key) of modification is protected for Mirror Grinding, the resistance of three kinds of material package all has good performance in hygrothermal environment.After damp and hot experiment, the change in resistance of 2.2M Ω Mirror Grinding is less, and resistance change rate all meets technical requirement (Δ R/R≤0.4%).This shows, the 9-Fluorenone containing more p-π and π-pi-conjugated key and novolac epoxy all can make prepared PF-EP composite coating wet-hot aging performance be greatly improved.In addition, the PF-EP composite coating wet-hot aging performance of novolac epoxy modification is better than the material of 9-Fluorenone modification, and this may can form interpenetrating(polymer)networks with PF-EP with novolac epoxy, make the polymer network compactness of matrix material increase relevant.It is more stable that the present invention encapsulates coating performance when life-time service, within 2 years, also coating layering can not occur even if deposit.
Claims (7)
1. improve a coating for Mirror Grinding wet-hot aging performance, raw material and mass percentage content thereof are: thermoset phenolic resin 30 ~ 60%, epoxy resin 10 ~ 40%, many p-π and π-pi-conjugated key material modified 5 ~ 20%, and thinner is 25 ~ 40%;
The number-average molecular weight scope of described thermoset phenolic resin is 200 ~ 1000;
Described epoxy resin is liquid bisphenol A type, and oxirane value scope is 0.44 ~ 0.56Eq/100g;
The material modified organic materials for having insulativity of described many p-π and π-pi-conjugated key;
Described thinner is the mixture of a kind of ethylene glycol mono-ether and liquid organic ketone, and wherein the mass ratio of organic ketone and ethylene glycol mono-ether is m
organic ketone/ m
ethylene glycol mono-ether=1:5 ~ 1:2;
The preparation method of this coating is as follows:
(1) by 1:1 mass ratio, 9-Fluorenone is dissolved in liquid organic ketone, mixes and make 9-Fluorenone solution, or the liquid organic ketone of novolac epoxy is diluted, mix and make novolac epoxy solution; Ethylene glycol mono-ether used for epoxy resin is diluted, mixes and make epoxy resin solution;
(2) according to raw material and mass percentage content batching thereof: thermoset phenolic resin 30 ~ 60%, epoxy resin 10 ~ 40%, many p-π and π-pi-conjugated key material modified 5 ~ 20%, thinner is 25 ~ 40%;
The epoxy resin solution of step (1) is mixed under agitation with body material thermoset phenolic resin, add 9-Fluorenone solution or novolac epoxy solution again, regulate proportion to be 0.98 with thinner, prepare the coating being suitable for metal film resistor and applying on a production line.
2. a kind of coating improving Mirror Grinding wet-hot aging performance according to claim 1, is characterized in that, described thermoset phenolic resin is that P-F sets the thermoset alcohol resite be polymerized.
3. a kind of coating improving Mirror Grinding wet-hot aging performance according to claim 1, is characterized in that, described epoxy resin is E51 type epoxy resin.
4. a kind of coating improving Mirror Grinding wet-hot aging performance according to claim 1, it is characterized in that, described many p-π and π-pi-conjugated key is material modified is 9-Fluorenone, novolac epoxy F44 or F51, wherein 9-Fluorenone and novolac epoxy structural formula as follows, all containing a large amount of p-π and π-pi-conjugated key.
。
5. a kind of coating improving Mirror Grinding wet-hot aging performance according to claim 1, is characterized in that, described ethylene glycol mono-ether is ethylene glycol monomethyl ether or ethylene glycol ethyl ether.
6. a kind of coating improving Mirror Grinding wet-hot aging performance according to claim 1, is characterized in that, described liquid organic ketone is acetone, butanone, cyclopentanone or pimelinketone.
7. a kind of coating improving Mirror Grinding wet-hot aging performance according to claim 1, it is characterized in that, coating 60 ~ 120s internal surface solidification at 160 ~ 180 DEG C prepared by described step (2), uses to be suitable for the encapsulation of Mirror Grinding production line; Solidify completely in 60 ~ 120min at 160 ~ 180 DEG C, to be suitable for the Mirror Grinding with wet-hot aging performance; When applying resistance protection in hygrothermal environment, resistance change rate meets the technical requirements of Δ R/R≤0.4%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510485875.XA CN105001751B (en) | 2015-08-07 | 2015-08-07 | A kind of coating for improving Mirror Grinding wet-hot aging performance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510485875.XA CN105001751B (en) | 2015-08-07 | 2015-08-07 | A kind of coating for improving Mirror Grinding wet-hot aging performance and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN105001751A true CN105001751A (en) | 2015-10-28 |
| CN105001751B CN105001751B (en) | 2017-03-29 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0834768A (en) * | 1994-07-25 | 1996-02-06 | Mitsubishi Rayon Co Ltd | New dimethacrylate |
| CN101570662A (en) * | 2009-03-26 | 2009-11-04 | 天津大学 | High-temperature and high-moisture resistant coating for metalster and preparation method thereof |
| CN101724330A (en) * | 2009-12-02 | 2010-06-09 | 天津大学 | Heat and humidity resistant acrylic acid/phenolic resin/nano-SiO2 coating for metal film resistor and preparation method thereof |
| CN102633990A (en) * | 2012-04-05 | 2012-08-15 | 广东生益科技股份有限公司 | Epoxy resin composition, prepreg made of epoxy resin composition and copper-coated laminate made of epoxy resin composition |
-
2015
- 2015-08-07 CN CN201510485875.XA patent/CN105001751B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0834768A (en) * | 1994-07-25 | 1996-02-06 | Mitsubishi Rayon Co Ltd | New dimethacrylate |
| CN101570662A (en) * | 2009-03-26 | 2009-11-04 | 天津大学 | High-temperature and high-moisture resistant coating for metalster and preparation method thereof |
| CN101724330A (en) * | 2009-12-02 | 2010-06-09 | 天津大学 | Heat and humidity resistant acrylic acid/phenolic resin/nano-SiO2 coating for metal film resistor and preparation method thereof |
| CN102633990A (en) * | 2012-04-05 | 2012-08-15 | 广东生益科技股份有限公司 | Epoxy resin composition, prepreg made of epoxy resin composition and copper-coated laminate made of epoxy resin composition |
Non-Patent Citations (1)
| Title |
|---|
| 胡玉静等: "酚醛树脂耐湿热老化性能研究进展", 《塑料工业》 * |
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| CN105001751B (en) | 2017-03-29 |
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Granted publication date: 20170329 Termination date: 20210807 |