CN118290899A - Zinc oxide piezoresistor encapsulation material and preparation method thereof - Google Patents
Zinc oxide piezoresistor encapsulation material and preparation method thereof Download PDFInfo
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- CN118290899A CN118290899A CN202410392357.2A CN202410392357A CN118290899A CN 118290899 A CN118290899 A CN 118290899A CN 202410392357 A CN202410392357 A CN 202410392357A CN 118290899 A CN118290899 A CN 118290899A
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- zinc oxide
- encapsulating material
- oxide varistor
- flame retardant
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 45
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 32
- 238000005538 encapsulation Methods 0.000 title abstract description 15
- 238000002360 preparation method Methods 0.000 title description 6
- 239000003063 flame retardant Substances 0.000 claims abstract description 19
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003365 glass fiber Substances 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000007822 coupling agent Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010330 laser marking Methods 0.000 claims abstract description 8
- 239000003550 marker Substances 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003822 epoxy resin Substances 0.000 claims abstract description 6
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000945 filler Substances 0.000 claims abstract description 3
- 239000005350 fused silica glass Substances 0.000 claims abstract description 3
- 239000000049 pigment Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 3
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 3
- 239000004843 novolac epoxy resin Substances 0.000 claims abstract 2
- 238000001125 extrusion Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 239000008393 encapsulating agent Substances 0.000 claims description 9
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 239000011265 semifinished product Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical class OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims description 6
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical class CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 150000004982 aromatic amines Chemical class 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- QYCVHILLJSYYBD-UHFFFAOYSA-L copper;oxalate Chemical compound [Cu+2].[O-]C(=O)C([O-])=O QYCVHILLJSYYBD-UHFFFAOYSA-L 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006355 external stress Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
Landscapes
- Thermistors And Varistors (AREA)
Abstract
The invention discloses a zinc oxide piezoresistor encapsulation material, which comprises the following components in parts by mass: 15-25 parts of bisphenol F type epoxy resin; 10-15 parts of novolac epoxy resin; 10-15 parts of bisphenol A type epoxy resin; 6-8 parts of a composite curing agent; 20-30 parts of glass fiber; 2-4 parts of a laser marking agent; 5-10 parts of a flame retardant; 1-2 parts of a composite coupling agent; 2-4 parts of pigment and filler; 5-8 parts of titanium dioxide; 5-10 parts of fused quartz powder. The invention solves a series of problems of the conventional insulating encapsulating material in the application of the zinc oxide piezoresistor, and improves the high-temperature and high-humidity resistance and breakdown resistance of the encapsulating material.
Description
Technical Field
The invention belongs to the technical field of paint, and particularly relates to a zinc oxide piezoresistor encapsulation material.
Background
The zinc oxide piezoresistor is a special electronic component, has nonlinear resistance characteristic, and can provide high resistance when the voltage exceeds the rated value, so that the circuit is protected from overvoltage and current damage, and is widely applied to various electronic equipment and circuits in the fields of power supplies, communication equipment, household appliances and the like. Because of the electrical insulation and electrical breakdown resistance and different environmental requirements of the use, a protective coating needs to be encapsulated on the surface of the zinc oxide varistor so as to play a role in mechanical protection and electrical insulation.
At present, the zinc oxide varistor encapsulating material widely adopted in the industry is solvent type insulating paint or conventional insulating encapsulating material. But the solvent type insulating paint has large VOC emission and high environmental protection pressure. The conventional insulation encapsulant has the following problems due to its own characteristics and limitations of encapsulation construction: 1. the conventional insulating encapsulating material has poor adhesive force on the zinc oxide piezoresistor; 2. the conventional insulating encapsulating material has quick degradation of insulating property under a high-temperature and high-humidity environment, is easy to break down when being used under the high-temperature and high-humidity environment, and has rapid increase of leakage current; 3. the explosion phenomenon of the encapsulating material easily occurs in the conventional insulating encapsulating material circulating cold and hot impact test. The above problems result in a significant limitation in the application of conventional insulating encapsulants.
Disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a zinc oxide varistor encapsulating material and a preparation method thereof, solves a series of problems of the conventional insulating encapsulating material in the application of the zinc oxide varistor, and improves the high-temperature and high-humidity resistance and breakdown resistance of the encapsulating material.
The technical aim of the invention is realized by the following technical scheme:
The zinc oxide varistor encapsulating material comprises the following components in parts by weight:
Preferably, the compound curing agent is a mixture of modified aromatic amine, dimethyl imidazole and trimellitic anhydride.
Preferably, the mass ratio of the modified aromatic amine, the dimethyl imidazole and the trimellitic anhydride in the composite curing agent is as follows: 2-3:0.5-1:1-5.
Preferably, the laser marking agent is a mixture of copper oxalate and calcium carbonate.
Preferably, the mass ratio of the copper oxalate to the calcium carbonate in the laser marking agent is 2-4:1-2.
Preferably, the mixed glass fiber is a mixture of glass fibers with different lengths, and the mixing mass ratio of the glass fibers with different lengths is as follows: 800 um-1000 um: 400-600 um:100-200 um = 3-5:2-3:1-3.
Preferably, the flame retardant is a mixture of an organic phosphorus-nitrogen flame retardant and an electrodeless aluminum hydroxide flame retardant, and the mass ratio of the organic phosphorus-nitrogen flame retardant to the electrodeless aluminum hydroxide flame retardant is 2-3:1-2.
Preferably, the composite coupling agent is a mixture of a silane coupling agent and a titanate coupling agent, and the mass ratio of the silane coupling agent to the titanate coupling agent is 1-2:1-2.
The preparation method of the zinc oxide piezoresistor encapsulating material comprises the following specific steps:
s1: sequentially adding the weighed component materials into a mixing tank according to the proportion, firstly stirring and mixing for 5min at a low speed of 200-300rpm, and then stirring and mixing for 6min at a high speed of 1000-1200rpm to obtain a premix;
S2, adding the premix into an extruder for melt extrusion to obtain a semi-finished product, wherein the extrusion temperature is set in a partitioned manner;
S3, adding the extruded semi-finished product into a grinder for grinding and grading, and controlling the grain size distribution of the finished product to meet the D50 of 30-40um to obtain the target product.
Preferably, in the step S2, a zone of extrusion temperature is set to 60-70 ℃ in sequence from the material conveying end; the extrusion temperature of the second area is 70-80 ℃; the extrusion temperature of the three zones is 80-90 ℃.
The beneficial effects are that: the invention discloses a zinc oxide piezoresistor encapsulation material and a preparation method thereof, and the zinc oxide piezoresistor encapsulation material has the following advantages:
(1) The zinc oxide piezoresistor encapsulating material prepared by the invention has high coating crosslinking density in reaction due to the use of the composite curing agent, and can effectively prevent invasion of water molecules to the encapsulating material for a long time, thereby ensuring continuous and effective operation of the zinc oxide piezoresistor in a high-temperature and high-humidity environment, not reducing the upper limit of breakdown voltage, and reducing the generation of leakage current.
(2) The bisphenol F type epoxy and the composite coupling agent can be combined with the surface of the zinc oxide varistor in a chain manner when the encapsulating material is melted and solidified, so that the encapsulating material is closely combined with the zinc oxide varistor, the adhesive force between the encapsulating material and the zinc oxide varistor is enhanced, and compared with the conventional encapsulating material, the adhesive force performance of the encapsulating material is obviously improved.
(3) In the invention, glass fibers with different lengths form an interpenetration network structure in the organic coating in the melting and solidifying stages, and when the encapsulating layer receives impact and external stress, the glass fibers with different lengths can reduce the influence of the impact and the stress on the encapsulating layer by dispersing energy. The structure can effectively increase the strength and the rigidity of the coating, and the formed complete encapsulation layer can bear external stress and impact, so that the encapsulation layer is prevented from being broken in cold-heat exchange impact, and meanwhile, the electronic components are effectively prevented from being scratched in the process of circulation installation.
Drawings
FIG. 1 is a microscopic view of the encapsulation effect (x 100) of the comparative example;
Fig. 2 is a microscopic image of the encapsulation effect (x 100) of example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
The preparation method of the zinc oxide piezoresistor encapsulating material comprises the following specific steps:
s1, sequentially adding the materials of the components weighed according to the proportion into a mixing tank, firstly stirring and mixing for 5min at a low speed of 200-300rpm, and then stirring and mixing for 6min at a high speed of 1000-1200rpm to obtain a premix;
S2, adding the premix into an extruder for melt extrusion to obtain a semi-finished product, wherein the extrusion temperature is set in a partition mode, and a region of extrusion temperature is set to be 60-70 ℃ from a material conveying end in sequence; the extrusion temperature of the second area is 70-80 ℃; the extrusion temperature of the three zones is 80-90 ℃.
S3, adding the extruded semi-finished product into a grinder for grinding and grading, and controlling the grain size distribution of the finished product to meet the requirement that D 50 is 50-70 mu m, thus obtaining the target product.
Examples 1, 2, 3 and comparative examples were prepared according to the formulations shown in table 1, respectively.
Table 1 shows the formulation of each sample
| Components (parts by weight) | Example 1 | Example 2 | Example 3 | Comparative example |
| Bisphenol F type epoxy resin | 25 | 20 | 15 | / |
| Epoxy novolac resin | 10 | 10 | 20 | 25 |
| Bisphenol A type epoxy resin | 10 | 15 | 10 | 20 |
| Composite curing agent | 2.5 | 2.3 | 2.1 | / |
| Anhydride curing agent | / | / | / | 3 |
| Glass fiber (different length) | 22 | 25 | 27 | / |
| Glass fiber | / | / | / | 25 |
| Laser marking agent | 3 | 3 | 3 | 3 |
| Flame retardant | 6 | 6 | 6 | / |
| Organic phosphorus-nitrogen flame retardant | / | / | / | 6 |
| Composite coupling agent | 2 | 2 | 2 | / |
| Coupling agent | / | / | 2 | |
| Pigment and filler | 3 | 3 | 3 | 3 |
| Titanium dioxide | 6 | 6 | 6 | 6 |
| Fused silica powder | 10.5 | 7.7 | 5.9 | 7 |
In examples 1-3, in the composite curing agent, the aromatic amine was modified: dimethylimidazole: trimellitic anhydride=1.5:0.5:2; in the laser marking agent, copper oxalate: calcium carbonate = 3:2; the mixing mass ratio of the glass fibers with different lengths in the mixed glass fibers is as follows: 800 um-1000 um: 400-600 um:100-200 um=4:2.5:1.5; among the flame retardants, an organic phosphorus nitrogen flame retardant: electrodeless aluminum hydroxide flame retardant = 3:2; among the composite coupling agents, silane coupling agents: titanate coupling agent = 2:1.
In the comparative example, the coupling agent used was a single silane coupling agent; the length of the glass fiber is 400-600 um; the curing agent adopts trimellitic anhydride; the flame retardant is a single organic phosphorus-nitrogen flame retardant.
(1) Comparative performance test
The encapsulants of examples 1,2, 3 and comparative examples, each having a coating thickness of 250-350 μm, were tested, respectively, and the specific test results are shown in table 2:
table 2 shows the results of performance tests for each sample
From the above results, it is clear that the coating water resistance, high temperature and high humidity resistance, high temperature load performance and cold and hot impact performance of the encapsulants prepared by the formulations of examples 1, 2 and 3 are significantly superior to those of the conventional encapsulants, compared with the comparative examples.
In addition, the adhesive force between the encapsulating material of the embodiment 1-3 and the piezoresistor is obviously better than that of the conventional encapsulating material at high temperature, so that the phenomenon that the encapsulating material is separated from the piezoresistor in a high-temperature use environment can be avoided, the voltage-sensitive voltage change rate is increased, the leakage current is increased, and the loss of the piezoresistor is caused. The adhesive force can also be enhanced to cope with the stability of the encapsulation layer of the piezoresistor when the piezoresistor expands with heat and contracts with cold. Therefore, the performance stability of the encapsulants of examples 1-3 is significantly better than that of conventional encapsulants, and particularly the rate of change of the voltage-sensitive voltage and leakage current among the performance indexes of example 2 are excellent.
(2) Encapsulation test under microscope (×100)
The encapsulation effect of the encapsulants of example 2 and comparative example on the surface of zinc oxide varistor was examined by using a microscope (x 100), respectively. As can be seen from fig. 1, the density of the encapsulation layer in the comparative example is loose, the distribution of glass fibers is uneven, and uneven particle bumps exist. In fig. 2, the packing layer of example 2 has high density, and the glass fibers with different lengths are reasonably and uniformly distributed, and the surface is smooth and fine.
The present embodiment is only for explanation of the present invention and is not to be construed as limiting the present invention, and modifications to the present embodiment, which may not creatively contribute to the present invention as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present invention.
Claims (10)
1. The zinc oxide varistor encapsulating material is characterized by comprising the following components in parts by mass:
15-25 parts of bisphenol F type epoxy resin;
10-15 parts of novolac epoxy resin;
10-15 parts of bisphenol A type epoxy resin;
6-8 parts of a composite curing agent;
20-30 parts of glass fiber;
2-4 parts of a laser marking agent;
5-10 parts of a flame retardant;
1-2 parts of a composite coupling agent;
2-4 parts of pigment and filler;
5-8 parts of titanium dioxide;
5-10 parts of fused quartz powder.
2. The zinc oxide varistor encapsulating material of claim 1, wherein the composite curing agent is a mixture of modified aromatic amine, dimethyl imidazole and trimellitic anhydride.
3. The zinc oxide varistor encapsulating material according to claim 2, wherein the mass ratio of the modified aromatic amine, the dimethyl imidazole and the trimellitic anhydride in the composite curing agent is as follows: 2-3:0.5-1:1-5.
4. The zinc oxide varistor encapsulant of claim 1, wherein the laser marking agent is a mixture of copper oxalate and calcium carbonate.
5. The zinc oxide varistor encapsulating material of claim 4, wherein the mass ratio of copper oxalate to calcium carbonate in the laser marking agent is 2-4:1-2.
6. The zinc oxide varistor encapsulating material according to claim 1, wherein the mixed glass fibers are a mixture of glass fibers with different lengths, and the mixed glass fibers with different lengths have the following mass ratio: 800 um-1000 um: 400-600 um, 100-200 um=3-5:2-3:1-3.
7. The zinc oxide varistor encapsulating material according to claim 1, wherein the flame retardant is a mixture of an organic phosphorus-nitrogen flame retardant and an electrodeless aluminum hydroxide flame retardant, and the mass ratio of the organic phosphorus-nitrogen flame retardant to the electrodeless aluminum hydroxide flame retardant is 2-3:1-2.
8. The zinc oxide varistor encapsulating material according to claim 1, wherein the composite coupling agent is a mixture of a silane coupling agent and a titanate coupling agent, and the mass ratio of the silane coupling agent to the titanate coupling agent is 1-2:1-2.
9. The method for preparing the zinc oxide varistor encapsulating material according to any one of claims 1 to 8, which is characterized by comprising the following specific steps:
s1: sequentially adding the weighed component materials into a mixing tank according to the proportion, firstly stirring and mixing for 5min at a low speed of 200-300rpm, and then stirring and mixing for 6min at a high speed of 1000-1200rpm to obtain a premix;
S2, adding the premix into an extruder for melt extrusion to obtain a semi-finished product, wherein the extrusion temperature is set in a partitioned manner;
S3, adding the extruded semi-finished product into a grinder for grinding and grading, and controlling the grain size distribution of the finished product to meet the D50 of 30-40um to obtain the target product.
10. The method for preparing a zinc oxide varistor encapsulating material according to claim 9, wherein in S2, a zone of extrusion temperature is set in sequence from the material conveying end to 60-70 ℃; the extrusion temperature of the second area is 70-80 ℃; the extrusion temperature of the three zones is 80-90 ℃.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311680294 | 2023-12-08 | ||
| CN2023116802942 | 2023-12-08 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118290899A true CN118290899A (en) | 2024-07-05 |
Family
ID=91682282
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410392357.2A Pending CN118290899A (en) | 2023-12-08 | 2024-04-02 | Zinc oxide piezoresistor encapsulation material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118290899A (en) |
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2024
- 2024-04-02 CN CN202410392357.2A patent/CN118290899A/en active Pending
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