CN112142376A - Thermosetting inorganic liquid electronic ceramic material and preparation method thereof - Google Patents
Thermosetting inorganic liquid electronic ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a thermosetting inorganic liquid electronic ceramic material and a preparation method thereof, wherein the thermosetting inorganic liquid electronic ceramic material comprises the following raw materials: inorganic solution, functional filler, curing agent, curing accelerator, inorganic pigment and solvent A; the preparation method comprises the following steps: s1, weighing the inorganic solution, the solvent A, the functional filler, the curing agent, the curing accelerator and the inorganic pigment according to parts by weight; s2, placing the inorganic solution weighed in the step S1 and the solvent A into a dispersion container for dispersion to obtain an inorganic solution mixture; s3, adding functional filler, curing agent, curing accelerator and inorganic pigment into the inorganic solution mixture obtained in the step S2, dispersing at a high speed, homogenizing, cooling and filtering to obtain the thermosetting inorganic liquid electronic ceramic material. The thermosetting inorganic liquid electronic ceramic material has excellent insulation reliability, electric breakdown resistance, medium-high temperature resistance and ultraviolet resistance.
Description
Technical Field
The invention relates to the technical field of inorganic liquid electronic ceramic materials, in particular to a thermosetting inorganic liquid electronic ceramic material.
Background
In recent years, with the rapid development of the electronic and aerospace industry in manufacturing electronic components, insulating materials and encapsulating materials for electronic parts have been rapidly developed. Electronic materials and packaging materials for electronic parts are required to have excellent insulation reliability, electric breakdown resistance, medium and high temperature resistance, and ultraviolet resistance. Existing electronic materials for electronic components are generally low cost non-conductive materials that tend to be electrically broken down at relatively low breakdown voltages and are not resistant to high temperatures and ultraviolet light. Therefore, there is a need to develop an insulating liquid electronic ceramic material and an encapsulating material for electronic parts, which can have both excellent dielectric breakdown voltage and insulation resistivity and can maintain good performance under high temperature and high ultraviolet environment.
Disclosure of Invention
The invention aims to overcome the defects and provides the thermosetting inorganic liquid electronic ceramic material which has excellent insulation reliability, electric breakdown resistance, medium-high temperature resistance and ultraviolet resistance; in addition, the invention also provides a preparation method of the thermosetting inorganic liquid electronic ceramic material.
In order to achieve the above object, a first aspect of the present invention provides a thermosetting inorganic liquid electronic ceramic material, comprising the following raw materials by weight: 100 parts of inorganic solution, 5-25 parts of functional filler, 0.2-2 parts of curing agent, 0.1-5 parts of curing accelerator, 15-35 parts of inorganic pigment and 20-70 parts of solvent A; wherein the inorganic solution comprises the following raw materials in parts by weight: 15-45 parts of methyltrimethoxysilane, 15-45 parts of tetraethoxysilane, 0-30 parts of methacryloxypropyltrimethoxysilane and 40-60 parts of colloidal silicon dioxide.
By adopting the technical scheme, the combination of two or more of methyltrimethoxysilane, tetraethoxysilane and methacryloxypropyltrimethoxysilane reacts with the colloidal silica, so that the insulation breakdown voltage of the liquid electronic ceramic material is more than or equal to 30 KV/MM; wherein, the content of the curing agent is 0.2-2 parts, if the content of the curing agent is more than 2 parts or less than 0.2 part, the hardening failure of the liquid electronic ceramic material is caused, and meanwhile, the moisture resistance and the heat resistance of the liquid electronic ceramic material are greatly reduced; wherein, the content of the curing accelerator is 0.1-5 parts, if the content of the curing accelerator is more than 5 parts, the coating performance of the liquid electronic ceramic material as a coating is deteriorated, and the storage stability is deteriorated, and if the content of the curing accelerator is less than 0.1 part, the liquid electronic ceramic material is poor in moisture resistance and heat resistance due to poor curing property and long curing time of the liquid electronic ceramic material; wherein the cumulative content of the functional filler and the inorganic pigment is 20-60 parts, when the cumulative content of the functional filler and the inorganic pigment is more than 55 parts, the impact resistance and the adhesiveness of the liquid electronic ceramic material are remarkably reduced, and when the cumulative content of the functional filler and the inorganic pigment is less than 25 parts, the impact resistance and the adhesiveness of the liquid electronic ceramic material are excellent, but the hiding power is reduced.
In the thermosetting inorganic liquid electronic ceramic material, the functional filler is selected from any combination of a plurality of inorganic materials such as titanium dioxide, silica, mica, potassium titanate, alumina, aluminum nitride, boron nitride and the like.
In the thermosetting inorganic liquid electronic ceramic material, the curing agent is selected from one or a combination of two of inorganic acid and anhydride curing agent.
In the thermosetting inorganic liquid electronic ceramic material, the curing accelerator is selected from any one or a combination of more of amine compounds, imidazole compounds, organic metal salts and organic peroxides.
In the above thermosetting inorganic liquid electronic ceramic material, the solvent a is distilled water or a mixture with methanol.
By adopting the technical scheme, the solvent A is used for controlling the reaction speed of the methyltrimethoxysilane, the tetraethoxysilane and the methacryloxypropyltrimethoxysilane when reacting with the colloidal silicon dioxide.
The second aspect of the present invention provides a preparation method of the above thermosetting inorganic liquid electronic ceramic material, comprising the following steps:
s1, weighing the inorganic solution, the solvent A, the functional filler, the curing agent, the curing accelerator and the inorganic pigment according to parts by weight for later use;
s2, putting the inorganic solution and the solvent A weighed in the step S1 into a dispersing container, and dispersing for 20-30 minutes at the speed of 150-300 rpm to obtain an inorganic solution mixture;
and S3, adding a functional filler, a curing agent, a curing accelerator and an inorganic pigment into the inorganic solution mixture obtained in the step S2, dispersing at a high speed of 5000-6000 rpm by using a homogenizer, homogenizing for 4-6 hours, cooling and filtering to obtain the thermosetting inorganic liquid electronic ceramic material.
Compared with the prior art, the invention has the beneficial effects that:
1. the thermosetting inorganic liquid electronic ceramic material disclosed by the invention has excellent dielectric breakdown voltage, insulation resistivity, medium-high temperature resistance and ultraviolet resistance after being cured; wherein, the insulation breakdown voltage of the thermosetting inorganic liquid electronic ceramic material is more than or equal to 30 KV/mm.
2. The thermosetting inorganic liquid electronic ceramic material exists in a liquid state at room temperature, and a cured product of the thermosetting inorganic liquid electronic ceramic material has heat resistance with the heat resistance temperature of more than 700 ℃.
3. The thermosetting inorganic liquid electronic ceramic material is usually cured for 10-30 minutes at 100-200 ℃, and a cured coating film has excellent insulation reliability, electric breakdown resistance, medium-high temperature resistance and ultraviolet resistance.
4. When the thermosetting inorganic liquid electronic ceramic material is used for coating electronic components, electric and electronic devices, the thermosetting inorganic liquid electronic ceramic material can be used by any one of various construction processes such as spraying, canning, dripping and the like.
5. The thermosetting inorganic liquid electronic ceramic material disclosed by the invention is simple in preparation method and convenient for realizing industrial production, and the prepared liquid electronic ceramic material has excellent dielectric breakdown voltage and insulation resistivity.
Detailed Description
The present invention will be further described with reference to specific embodiments in order to make the technical means, inventive features, objectives and effects of the invention easy to understand.
Example 1
A thermosetting inorganic liquid electronic ceramic material comprises the following raw materials: 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 29g of inorganic pigment and 50g of solvent A; wherein the inorganic solution comprises the following raw materials: 15g of methyltrimethoxysilane, 15g of tetraethoxysilane, 15g of methacryloxypropyltrimethoxysilane and 55g of colloidal silicon dioxide, wherein the solvent A is a mixed solution of distilled water and methanol.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the functional filler includes silica with an average particle size of less than 5 μm, mica, potassium titanate whiskers, alumina, aluminum nitride, and boron nitride.
In the present embodiment, the curing agent in the thermosetting inorganic liquid electronic ceramic material is glacial acetic acid.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the curing accelerator is 2-methylimidazole.
The preparation method of the thermosetting inorganic liquid electronic ceramic material in the embodiment comprises the following steps:
s1, weighing 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 29g of inorganic pigment and 50g of solvent A for later use;
s2, placing the inorganic solution and the solvent A weighed in the step S1 into a closed dispersing container, controlling the environmental temperature to be below 35 ℃, controlling the liquid surface temperature to be below 50 ℃, and dispersing for 20-30 minutes at the speed of 150-300 rpm to obtain an inorganic solution mixture;
and S3, adding a functional filler, a curing agent, a curing accelerator and an inorganic pigment into the inorganic solution mixture, sealing, controlling the temperature of the reaction solution to be 40-50 ℃, dispersing and homogenizing at a high speed of 5000-6000 rpm for 4-6 hours by a homogenizer, and finishing the reaction when the viscosity of the mixture reaches 14-16 seconds (detected by a Ford cup). And cooling and filtering to obtain the thermosetting inorganic liquid electronic ceramic material.
Example 2
A thermosetting inorganic liquid electronic ceramic material comprises the following raw materials: 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 29g of inorganic pigment and 50g of solvent A; wherein the inorganic solution comprises the following raw materials: 30g of methyltrimethoxysilane, 15g of tetraethoxysilane and 55g of colloidal silicon dioxide; wherein the solvent A is a mixed solution of distilled water and methanol.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the functional filler includes silica with an average particle size of less than 5 μm, mica, potassium titanate whiskers, alumina, aluminum nitride, and boron nitride.
In the present embodiment, the curing agent in the thermosetting inorganic liquid electronic ceramic material is glacial acetic acid.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the curing accelerator is 2-methylimidazole.
The preparation method of the thermosetting inorganic liquid electronic ceramic material in the embodiment comprises the following steps:
s1, weighing 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 50g of inorganic pigment and solvent A for later use;
s2, placing the inorganic solution and the solvent A weighed in the step S1 into a closed dispersing container, controlling the environmental temperature to be below 35 ℃, controlling the liquid surface temperature to be below 50 ℃, and dispersing for 20-30 minutes at the speed of 150-300 rpm to obtain an inorganic solution mixture;
and S3, adding a functional filler, a curing agent, a curing accelerator and an inorganic pigment into the inorganic solution mixture, sealing, controlling the temperature of the reaction solution to be 40-50 ℃, dispersing and homogenizing at a high speed of 5000-6000 rpm for 4-6 hours by a homogenizer, and finishing the reaction when the viscosity of the mixture reaches 14-15 seconds (detected by a Ford cup). And cooling and filtering to obtain the thermosetting inorganic liquid electronic ceramic material.
Comparative example 1
A thermosetting inorganic liquid electronic ceramic material comprises the following raw materials: 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 29g of inorganic pigment and 50g of solvent A; wherein the inorganic solution comprises the following raw materials: 45g of methyltrimethoxysilane and 55g of colloidal silicon dioxide; wherein the solvent A is a mixed solution of distilled water and methanol.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the functional filler includes silica with an average particle size of less than 5 μm, mica, potassium titanate whiskers, alumina, aluminum nitride, and boron nitride.
In the present embodiment, the curing agent in the thermosetting inorganic liquid electronic ceramic material is glacial acetic acid.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the curing accelerator is 2-methylimidazole.
The preparation method of the thermosetting inorganic liquid electronic ceramic material in the embodiment comprises the following steps:
s1, weighing 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 29g of inorganic pigment and 50g of solvent A for later use;
s2, placing the inorganic solution and the solvent A weighed in the step S1 into a closed dispersing container, controlling the environmental temperature to be below 35 ℃, controlling the liquid surface temperature to be below 50 ℃, and dispersing for 20-30 minutes at the speed of 150-300 rpm to obtain an inorganic solution mixture;
and S3, adding a functional filler, a curing agent, a curing accelerator and an inorganic pigment into the inorganic solution mixture, sealing, controlling the temperature of the reaction solution to be 40-50 ℃, dispersing and homogenizing at a high speed of 5000-6000 rpm for 4-6 hours by a homogenizer, and finishing the reaction when the viscosity of the mixture reaches 14-15 seconds (detected by a Ford cup). And cooling and filtering to obtain the thermosetting inorganic liquid electronic ceramic material in the embodiment.
Comparative example 2
A thermosetting inorganic liquid electronic ceramic material comprises the following raw materials: 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 29g of inorganic pigment and 50g of solvent A; wherein the inorganic solution comprises the following raw materials: 45g of tetraethoxysilane and 55g of colloidal silicon dioxide; wherein the solvent A is a mixed solution of distilled water and methanol.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the functional filler includes silica with an average particle size of less than 5 μm, mica, potassium titanate whiskers, alumina, aluminum nitride, and boron nitride.
In the present embodiment, the curing agent in the thermosetting inorganic liquid electronic ceramic material is glacial acetic acid.
In the thermosetting inorganic liquid electronic ceramic material of the present embodiment, the curing accelerator is 2-methylimidazole.
The preparation method of the thermosetting inorganic liquid electronic ceramic material in the embodiment comprises the following steps:
s1, weighing 100g of inorganic solution, 20g of functional filler, 0.5g of curing agent, 0.5g of curing accelerator, 35g of inorganic pigment and 50g of solvent A for later use;
s2, placing the inorganic solution and the solvent A weighed in the step S1 into a closed dispersing container, controlling the environmental temperature to be below 35 ℃, controlling the liquid surface temperature to be below 50 ℃, and dispersing for 20-30 minutes at the speed of 150-300 rpm to obtain an inorganic solution mixture;
and S3, adding a functional filler, a curing agent, a curing accelerator and an inorganic pigment into the inorganic solution mixture, sealing, controlling the temperature of the reaction solution to be 40-50 ℃, dispersing and homogenizing at a high speed of 5000-6000 rpm for 4-6 hours by a homogenizer, and finishing the reaction when the viscosity of the mixture reaches 14-15 seconds (detected by a Ford cup). And cooling and filtering to obtain the thermosetting inorganic liquid electronic ceramic material in the embodiment.
Test example 1
One of the thermosetting inorganic liquid electronic ceramic materials prepared in example 1 was labeled as sample 1, one of the thermosetting inorganic liquid electronic ceramic materials prepared in example 2 was labeled as sample 2, one of the thermosetting inorganic liquid electronic ceramic materials prepared in comparative example 1 was labeled as comparative sample 1, and one of the thermosetting inorganic liquid electronic ceramic materials prepared in comparative example 2 was labeled as comparative sample 2.
The compositions of the functional fillers in samples 1 and 2, and comparative samples 1 and 2 are the same, and the compositions of the inorganic pigments are the same.
Physical properties including open time, surface hardness (pencil hardness), breakdown voltage, and insulation resistivity of sample 1, sample 2, comparative sample 1, and comparative sample 2 were measured, respectively.
The detection method of the surface drying time comprises the following steps: preparing four glass plates, respectively coating the sample 1, the sample 2, the comparative sample 1 and the comparative sample 2 on the four glass plates through a distributor, wherein the thicknesses of the sample 1, the sample 2, the comparative sample 1 and the comparative sample 2 after being dried on the glass plates are all 40 mu m, whether a coating film on the glass plates has viscosity is touched every 30 seconds in the drying process, and the time for the coating film on the glass plates to lose the viscosity for the first time is the surface drying time. The open time is an indicator of the physical properties of the fast drying liquid electronic ceramic material.
The detection method of the breakdown voltage comprises the following steps: after sample 1, sample 2, comparative sample 1, and comparative sample 2 were coated on four test boards of 95mm × 95mm × 1t, respectively, curing was performed in a hot air drying oven at 150 ℃ with a cured film thickness of 1mm, and then the dielectric breakdown voltage was measured in KV/mm units.
The detection method of the insulation resistivity comprises the following steps: 45. + -.0.05 g of sample 1, 45. + -.0.05 g of sample 2, 45. + -.0.05 g of comparative sample 1, 45. + -.0.05 g of comparative sample 2 were molded into disks having a diameter of 10mm and a thickness of 3mm, respectively, and then baked in a hot air drying oven at 150 ℃ for 30 minutes, and then the insulation resistivity was measured in units of. omega. cm.
Wherein the pencil hardness is carried out according to GB/T6739-2006 standard.
The results of measuring physical properties of sample 1, sample 2, comparative sample 1, and comparative sample 2 are shown in table 1.
TABLE 1 results of measuring physical Properties of sample 1, sample 2, comparative sample 1, and comparative sample 2
| Physical Properties | Sample 1 | Sample 2 | Comparative sample 1 | Comparative sample 2 |
| Surface drying time/minute | 124 | 120 | 112 | 110 |
| Surface hardness (Pencil hardness) | 7-9H | 6-8H | 7-9H | 6-8H |
| Breakdown voltage (KV/mm) | 35 | 30 | 24 | 20 |
| Insulation resistivity/(omega. cm) | 2.6×1014 | 1.4×1016 | 3.7×1015 | 4.3×1014 |
As shown in table 1, the open time, breakdown voltage, and insulation resistivity of samples 1 and 2 are significantly better than those of comparative samples 1 and 2.
In conclusion, the thermosetting inorganic liquid electronic ceramic material has excellent dielectric breakdown voltage, insulation resistivity, medium-high temperature resistance and ultraviolet ray resistance when being used for coating electronic parts, electric and electronic devices.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The thermosetting inorganic liquid electronic ceramic material is characterized by comprising the following raw materials in parts by weight: 100 parts of inorganic solution, 5-25 parts of functional filler, 0.2-2 parts of curing agent, 0.1-5 parts of curing accelerator, 15-35 parts of inorganic pigment and 20-70 parts of solvent A; wherein the inorganic solution comprises the following raw materials in parts by weight: 15-45 parts of methyltrimethoxysilane, 15-45 parts of tetraethoxysilane, 0-30 parts of methacryloxypropyltrimethoxysilane and 40-60 parts of colloidal silicon dioxide.
2. A thermosetting inorganic liquid electronic ceramic material according to claim 1, wherein the functional filler is selected from any combination of a plurality of inorganic materials such as titanium dioxide, mica, potassium titanate, alumina, aluminum nitride, boron nitride, etc.
3. A thermosetting inorganic liquid electronic ceramic material according to claim 1, wherein the curing agent is selected from any one or a combination of two of inorganic acid and anhydride curing agents.
4. A thermosetting inorganic liquid electronic ceramic material according to claim 1, wherein the curing accelerator is selected from any one or more of amine compounds, imidazole compounds, organic metal salts, and organic peroxides.
5. A thermosetting inorganic liquid electronic ceramic material according to claim 1, wherein the solvent a is distilled water or a mixture with methanol.
6. A process for the preparation of a thermosetting inorganic liquid electronic ceramic material according to any of claims 1 to 5, comprising the steps of:
s1, weighing the inorganic solution, the solvent A, the functional filler, the curing agent, the curing accelerator and the inorganic pigment according to parts by weight for later use;
s2, putting the inorganic solution and the solvent A weighed in the step S1 into a dispersing container, and dispersing for 20-30 minutes at the speed of 150-300 rpm to obtain an inorganic solution mixture;
and S3, adding a functional filler, a curing agent, a curing accelerator and an inorganic pigment into the inorganic solution mixture obtained in the step S2, dispersing at a high speed of 5000-6000 rpm by using a homogenizer, homogenizing for 4-6 hours, cooling and filtering to obtain the thermosetting inorganic liquid electronic ceramic material.
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2019
- 2019-06-28 CN CN201910576779.4A patent/CN112142376B/en active Active
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| CN105038335A (en) * | 2015-07-08 | 2015-11-11 | 刘晓东 | Room-temperature curable inorganic coating and manufacturing method thereof |
| US20170009079A1 (en) * | 2015-07-08 | 2017-01-12 | Xiaodong Liu | Inorganic coating composition which can be cured at low temperature and a preparation method thereof |
| CN107201168A (en) * | 2017-07-19 | 2017-09-26 | 合肥铭佑高温技术有限公司 | A kind of high Wear-resistant, high-temperature resistant coating of adhesive force |
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