CN115353857A - Packaging medium for pressure sensor chip and preparation method thereof - Google Patents
Packaging medium for pressure sensor chip and preparation method thereof Download PDFInfo
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- CN115353857A CN115353857A CN202210812226.6A CN202210812226A CN115353857A CN 115353857 A CN115353857 A CN 115353857A CN 202210812226 A CN202210812226 A CN 202210812226A CN 115353857 A CN115353857 A CN 115353857A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
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- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention discloses a packaging medium for a pressure sensor chip and a preparation method thereof, and particularly relates to the technical field of chip packaging, wherein the packaging medium is prepared from the following raw materials: the packaging medium comprises organic silicon resin, an organic silicon cross-linking agent and a curing catalyst, wherein the mass ratio of the organic silicon resin to the organic silicon cross-linking agent is 4:1, and the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst are mixed to prepare the packaging medium; the prepared organic silicon resin, the organic silicon cross-linking agent and the curing catalyst are uniformly mixed according to the mixture ratio of 7.8-8.3. The organic silicon resin, the organic silicon cross-linking agent and the curing catalyst are mixed to prepare the packaging medium, and the ratio of the organic silicon resin to the cross-linking agent is 8:2, the organic silicon has thermodynamic and optical stability, so that the conditions of color change, deformation and cracking of the traditional packaging material under the influence of high temperature and high brightness are avoided, the packaging effect on the pressure sensor chip is improved, and the optical inspection work on the chip is facilitated.
Description
Technical Field
The invention relates to the technical field of chip packaging, in particular to a packaging medium for a pressure sensor chip and a preparation method thereof.
Background
The pressure sensor is a device or a device which can sense pressure signals and can convert the pressure signals into usable output electric signals according to a certain rule, generally comprises a pressure sensitive element and a signal processing unit, according to different test pressure types, the pressure sensor can be divided into a gauge pressure sensor, a differential pressure sensor and an absolute pressure sensor, the pressure sensor is the most common sensor in industrial practice, is widely applied to various industrial automatic control environments and relates to various industries such as water conservancy and hydropower, railway transportation, intelligent buildings, production automatic control, aerospace, war industry, petrochemical industry, oil wells, electric power, ships, machine tools, pipelines and the like.
In the manufacturing process of the pressure sensor, the pressure sensor chip is generally required to be packaged and processed, a packaging medium needs to be selected according to product requirements, at present, the packaging medium which is generally used, namely packaging adhesive, is mostly made of epoxy resin packaging materials, and because the epoxy resin packaging materials are exposed under ultraviolet rays or easily generate yellowing phenomena under high-temperature environments, stable light source output cannot be provided under high current, the optical inspection of the chip is not facilitated, meanwhile, the cracking phenomena easily occur under the high-temperature environments, and the heat resistance is poor, so that the problem is solved by the packaging medium for the pressure sensor chip with high stability and the preparation method thereof.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a packaging medium for a pressure sensor chip and a preparation method thereof, and the technical problems to be solved by the invention are as follows: the packaging medium that uses usually, the packaging adhesive, mostly adopt epoxy resin packaging material, because epoxy resin packaging material exposes under the ultraviolet ray or takes place the yellowing phenomenon easily under high temperature environment, can not provide stable light source output under the high current, be unfavorable for the optical inspection to the chip, the easy phenomenon that splits that appears under high temperature environment simultaneously, the relatively poor problem of heat resistance.
In order to achieve the purpose, the invention provides the following technical scheme: a packaging medium for a pressure sensor chip comprises the following raw materials:
the organic silicon packaging medium comprises organic silicon resin, an organic silicon cross-linking agent and a curing catalyst, wherein the mass ratio of the organic silicon resin to the organic silicon cross-linking agent is 3.5-4.
A preparation method of a packaging medium for a pressure sensor chip comprises the following steps:
s1, preparing organic silicon resin: mixing phenyl trichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, wherein the mass ratio of the phenyl trichlorosilane to the dimethyldichlorosilane to the methylvinyldichlorosilane is (9.5-11).
S2, preparing an organic silicon cross-linking agent: mixing tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane, wherein the mass ratio of the tetramethyldisiloxane to the diphenyldimethoxysilane to the tetramethylcyclotetrasiloxane is 1.8-2.
S3, preparation of a curing catalyst: putting chloroplatinic acid and divinyltetramethyldisiloxane into a four-mouth bottle for mixing, wherein the mass ratio of the chloroplatinic acid to the divinyltetramethyldisiloxane is 0.8-1.2.
And S4, mixing the organic silicon resin prepared in the S1, the organic silicon cross-linking agent prepared in the S2 and the curing catalyst prepared in the S3 in proportion, and uniformly mixing the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst in the proportion of 7.8-8.3.
As a further scheme of the invention: the process of the organic silicon resin in the S1 specifically comprises the following steps:
s101, mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, pouring into a constant pressure dropping funnel, pouring water and toluene into a four-mouth bottle, and uniformly mixing.
S102, slowly dripping chlorosilane mixed liquid into a four-mouth bottle, controlling the dripping time to be 40-60min, and reacting for 5-6h at the temperature of 45-55 ℃.
S103, slowly heating the four-mouth bottle to 85 ℃, carrying out aging reaction for 1.5-2h, waiting for natural cooling to obtain a reaction product, pouring the reaction product into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of organic silicon resin, the middle layer is a floccule thin layer, and the lower layer is a water phase.
And S104, pouring the toluene solution of the upper organic silicon resin into a three-mouth bottle, washing with distilled water for multiple times to enable the toluene solution of the organic silicon resin to be organic phase neutral, filtering the neutral organic phase by using a sand type funnel to remove impurities, and carrying out reduced pressure distillation on the organic phase to obtain the organic silicon resin.
In the reduced pressure distillation of S104, toluene and oligomer are distilled under the condition that the vacuum degree is 0.1MPa, the initial distillation temperature is 35 ℃, the final distillation temperature is 145 ℃, the organic silicon resin is transparent, and the organic silicon resin is judged to contain methyl, phenyl and vinyl by forming an infrared spectrogram.
As a further scheme of the invention: the process of the organic silicon cross-linking agent in the S2 specifically comprises the following steps:
s201, pouring tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane into a three-necked bottle, mixing, and cooling by an ice water bath until the temperature is between 0 and 8 ℃ to form a mixed solution.
S202, mixing concentrated sulfuric acid with the mass of 2.7-3.5 and distilled water, pouring the mixture into a constant-pressure dropping funnel at the temperature of less than 10 ℃, dropping sulfuric acid into the mixed solution, keeping the temperature of the reaction system to be less than 10 ℃, continuing to react for 10-12 hours at the temperature of less than 10 ℃ after dropping, and reacting for 4-5 hours at room temperature.
S203, adding water and toluene in the reaction system, wherein the mass ratio of the water to the toluene is 20-28, stirring for 20-30min, pouring into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of the methylphenylhydrogenpolysiloxane, and the lower layer is a water phase.
And S204, adding the toluene solution of the upper-layer methylphenylhydrogenpolysiloxane into equal volume of distilled water, repeatedly extracting and dividing water until the organic phase is neutral, filtering the organic phase by using a sand funnel, removing impurities, and carrying out reduced pressure flash evaporation on the organic phase to obtain the organic silicon crosslinking agent.
In the reduced pressure flash evaporation of S204, under the condition that the vacuum degree is 0.1MPa, toluene and small molecular compounds are distilled out, the initial distillation temperature is 30 ℃, the final distillation temperature is 65 ℃, and the siloxane resin containing methyl, phenyl and hydrogen radicals in the organosilicon crosslinking agent is judged by forming an infrared spectrogram.
As a further scheme of the invention: the process of the curing catalyst in S3 specifically comprises the following steps:
s301, stirring a four-mouth bottle filled with chloroplatinic acid and divinyl tetramethyl disiloxane by nitrogen, heating to reflux temperature of 120 ℃, continuing to react at the temperature for 40-60min, naturally cooling to room temperature, filtering to remove black platinum black precipitate, adding equivalent divinyl tetramethyl disiloxane into light gray acidic filtrate, stirring uniformly, repeatedly washing to neutrality by distilled water, and removing chlorine-containing acidic byproducts.
And S302, adding anhydrous calcium chloride into chloric acid liquid in the S301, drying, and filtering calcium chloride to obtain the curing catalyst.
As a further scheme of the invention: the mixing rate in the S4 is 80-100r/min, the mixing time is controlled to be 40-50min, and 1000PPM coordination curing catalyst is added.
The invention has the beneficial effects that: the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst are mixed to prepare the packaging medium, and the ratio of the organic silicon resin to the cross-linking agent is 8:2, the organic silicon has thermodynamic and optical stability, so that the conditions of color change, deformation and cracking of the traditional packaging material under the influence of high temperature and high brightness are avoided, the packaging effect on the pressure sensor chip is improved, and the optical inspection work on the chip is facilitated.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1:
a packaging medium for a pressure sensor chip comprises the following raw materials:
the organic silicon packaging medium comprises organic silicon resin, an organic silicon cross-linking agent and a curing catalyst, wherein the mass ratio of the organic silicon resin to the organic silicon cross-linking agent is 8:2, and the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst are mixed to prepare the packaging medium.
The preparation method of the packaging medium for the pressure sensor chip comprises the following steps:
s1, preparing organic silicon resin: mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, wherein the mass ratio of the phenyltrichlorosilane to the dimethyldichlorosilane to the methylvinyldichlorosilane is (9.5-11).
S2, preparing an organic silicon cross-linking agent: mixing tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane, wherein the mass ratio of the tetramethyldisiloxane to the diphenyldimethoxysilane to the tetramethylcyclotetrasiloxane is 1.8-2.
S3, preparation of a curing catalyst: putting chloroplatinic acid and divinyltetramethyldisiloxane into a four-mouth bottle for mixing, wherein the mass ratio of the chloroplatinic acid to the divinyltetramethyldisiloxane is 0.8-1.2.
And S4, mixing the organic silicon resin prepared in the S1, the organic silicon cross-linking agent prepared in the S2 and the curing catalyst prepared in the S3 in proportion, and uniformly mixing the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst in the proportion of 7.8-8.3.
The process of the organic silicon resin in the S1 comprises the following specific steps:
s101, mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, pouring into a constant pressure dropping funnel, pouring water and toluene into a four-mouth bottle, and uniformly mixing.
S102, slowly dripping chlorosilane mixed liquid into a four-mouth bottle, controlling the dripping time to be 40-60min, and reacting for 5-6h at the temperature of 45-55 ℃.
S103, slowly heating the four-mouth bottle to 85 ℃, carrying out aging reaction for 1.5-2h, waiting for natural cooling to obtain a reaction product, pouring the reaction product into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of organic silicon resin, the middle layer is a floccule thin layer, and the lower layer is a water phase.
And S104, pouring the toluene solution of the upper organic silicon resin into a three-mouth bottle, washing with distilled water for multiple times to enable the toluene solution of the organic silicon resin to be organic phase neutral, filtering the neutral organic phase by using a sand type funnel to remove impurities, and carrying out reduced pressure distillation on the organic phase to obtain the organic silicon resin.
In the reduced pressure distillation of S104, toluene and oligomer are distilled under the condition that the vacuum degree is 0.1MPa, the initial distillation temperature is 35 ℃, the final distillation temperature is 145 ℃, the organic silicon resin is transparent, and the organic silicon resin is judged to contain methyl, phenyl and vinyl by forming an infrared spectrogram.
The process of the organic silicon cross-linking agent in S2 comprises the following specific steps:
s201, pouring tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane into a three-necked bottle, mixing, and cooling by an ice water bath until the temperature is between 0 and 8 ℃ to form a mixed solution.
S202, mixing concentrated sulfuric acid with the mass of 2.7-3.5 and distilled water, pouring the mixture into a constant-pressure dropping funnel at the temperature of less than 10 ℃, dropping sulfuric acid into the mixed solution, keeping the temperature of the reaction system to be less than 10 ℃, continuing to react for 10-12 hours at the temperature of less than 10 ℃ after dropping, and reacting for 4-5 hours at room temperature.
S203, adding water and toluene in the reaction system, wherein the mass ratio of water to toluene is 20-28, stirring for 20-30min, pouring into a separating funnel, standing for layering, wherein the upper layer is a toluene solution of methylphenylhydrogenpolysiloxane, and the lower layer is an aqueous phase.
And S204, adding the toluene solution of the upper-layer methylphenylhydrogenpolysiloxane into equal volume of distilled water, repeatedly extracting and dividing water until the organic phase is neutral, filtering the organic phase by using a sand funnel, removing impurities, and carrying out reduced pressure flash evaporation on the organic phase to obtain the organic silicon crosslinking agent.
In the reduced pressure flash evaporation of S204, under the condition that the vacuum degree is 0.1MPa, toluene and small molecular compounds are distilled out, the initial distillation temperature is 30 ℃, the final distillation temperature is 65 ℃, and the siloxane resin containing methyl, phenyl and hydrogen radicals in the organosilicon crosslinking agent is judged by forming an infrared spectrogram.
The process of the curing catalyst in S3 is specifically as follows:
s301, stirring a four-mouth bottle filled with chloroplatinic acid and divinyl tetramethyl disiloxane by nitrogen, heating to reflux temperature of 120 ℃, continuing to react at the temperature for 40-60min, naturally cooling to room temperature, filtering to remove black platinum black precipitate, adding an equal amount of divinyl tetramethyl disiloxane into light gray acidic filtrate, stirring uniformly, repeatedly washing to neutrality by distilled water, and removing chlorine-containing acidic byproducts.
And S302, adding anhydrous calcium chloride into chloric acid liquid in the S301, drying, and filtering calcium chloride to obtain the curing catalyst.
The mixing rate in S4 is 80-100r/min, the mixing time is controlled to be 40-50min, and 1000PPM coordination curing catalyst is added.
Example 2:
a packaging medium for a pressure sensor chip comprises the following raw materials:
the packaging medium comprises organic silicon resin, an organic silicon cross-linking agent and a curing catalyst, wherein the mass ratio of the organic silicon resin to the organic silicon cross-linking agent is 8.
The preparation method of the packaging medium for the pressure sensor chip comprises the following steps:
s1, preparing organic silicon resin: mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, wherein the mass ratio of phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane is (9.5-11).
S2, preparing an organic silicon cross-linking agent: mixing tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane, wherein the mass ratio of the tetramethyldisiloxane to the diphenyldimethoxysilane to the tetramethylcyclotetrasiloxane is 1.8-2.
S3, preparation of a curing catalyst: putting chloroplatinic acid and divinyltetramethyldisiloxane into a four-mouth bottle for mixing, wherein the mass ratio of the chloroplatinic acid to the divinyltetramethyldisiloxane is 0.8-1.2.
And S4, mixing the organic silicon resin prepared in the S1, the organic silicon cross-linking agent prepared in the S2 and the curing catalyst prepared in the S3 in proportion, and uniformly mixing the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst in proportion of 8.8.
The process of the organic silicon resin in the S1 specifically comprises the following steps:
s101, mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, pouring into a constant pressure dropping funnel, pouring water and toluene into a four-mouth bottle, and uniformly mixing.
S102, slowly dripping chlorosilane mixed liquid into a four-mouth bottle, controlling the dripping time to be 40-60min, and reacting for 5-6h at the temperature of 45-55 ℃.
S103, slowly heating the four-mouth bottle to 85 ℃, carrying out aging reaction for 1.5-2h, waiting for natural cooling to obtain a reaction product, pouring the reaction product into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of organic silicon resin, the middle layer is a floccule thin layer, and the lower layer is a water phase.
And S104, pouring the toluene solution of the upper layer of the organic silicon resin into a three-mouth bottle, washing the toluene solution of the upper layer of the organic silicon resin with distilled water for multiple times to enable the toluene solution of the organic silicon resin to be organic-phase neutral, filtering the neutral organic phase by using a sand type funnel to remove impurities, and carrying out reduced pressure distillation on the organic phase to obtain the organic silicon resin.
In the reduced pressure distillation of S104, toluene and oligomer are distilled under the condition that the vacuum degree is 0.1MPa, the initial distillation temperature is 35 ℃, the final distillation temperature is 145 ℃, the organic silicon resin is transparent, and the organic silicon resin is judged to contain methyl, phenyl and vinyl by forming an infrared spectrogram.
The process of the organic silicon cross-linking agent in S2 comprises the following specific steps:
s201, pouring tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane into a three-necked bottle, mixing, and cooling by an ice water bath until the temperature is between 0 and 8 ℃ to form a mixed solution.
S202, mixing concentrated sulfuric acid with the mass of 2.7-3.5.
S203, adding water and toluene in the reaction system, wherein the mass ratio of the water to the toluene is 20-28, stirring for 20-30min, pouring into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of the methylphenylhydrogenpolysiloxane, and the lower layer is a water phase.
And S204, adding the toluene solution of the upper-layer methylphenylhydrogenpolysiloxane into equal volume of distilled water, repeatedly extracting and dividing water until the organic phase is neutral, filtering the organic phase by using a sand funnel, removing impurities, and carrying out reduced pressure flash evaporation on the organic phase to obtain the organic silicon crosslinking agent.
In the reduced pressure flash evaporation of S204, under the condition that the vacuum degree is 0.1MPa, toluene and small molecular compounds are distilled out, the initial distillation temperature is 30 ℃, the final distillation temperature is 65 ℃, and the siloxane resin containing methyl, phenyl and hydrogen in the organosilicon crosslinking agent is judged by forming an infrared spectrogram.
The process of the curing catalyst in S3 is specifically as follows:
s301, stirring a four-mouth bottle filled with chloroplatinic acid and divinyl tetramethyl disiloxane by nitrogen, heating to reflux temperature of 120 ℃, continuing to react at the temperature for 40-60min, naturally cooling to room temperature, filtering to remove black platinum black precipitate, adding equivalent divinyl tetramethyl disiloxane into light gray acidic filtrate, stirring uniformly, repeatedly washing to neutrality by distilled water, and removing chlorine-containing acidic byproducts.
And S302, adding anhydrous calcium chloride into chloric acid liquid in the S301, drying, and filtering calcium chloride to obtain the curing catalyst.
The mixing rate in S4 is 80-100r/min, the mixing time is controlled to be 40-50min, and 1000PPM coordination curing catalyst is added.
Example 3:
a packaging medium for a pressure sensor chip comprises the following raw materials:
the packaging medium comprises organic silicon resin, an organic silicon cross-linking agent and a curing catalyst, wherein the mass ratio of the organic silicon resin to the organic silicon cross-linking agent is 8.
The preparation method of the packaging medium for the pressure sensor chip comprises the following steps:
s1, preparing organic silicon resin: mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, wherein the mass ratio of the phenyltrichlorosilane to the dimethyldichlorosilane to the methylvinyldichlorosilane is (9.5-11).
S2, preparing an organic silicon cross-linking agent: mixing tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane, wherein the mass ratio of the tetramethyldisiloxane to the diphenyldimethoxysilane to the tetramethylcyclotetrasiloxane is 1.8-2.
S3, preparation of a curing catalyst: putting chloroplatinic acid and divinyltetramethyldisiloxane into a four-mouth bottle for mixing, wherein the mass ratio of the chloroplatinic acid to the divinyltetramethyldisiloxane is 0.8-1.2.
And S4, mixing the organic silicon resin prepared in the S1, the organic silicon cross-linking agent prepared in the S2 and the curing catalyst prepared in the S3 in proportion, and uniformly mixing the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst in the proportion of 8.5.
The process of the organic silicon resin in the S1 comprises the following specific steps:
s101, mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, pouring into a constant pressure dropping funnel, pouring water and toluene into a four-mouth bottle, and uniformly mixing.
S102, slowly dripping chlorosilane mixed liquid into a four-mouth bottle, controlling the dripping time to be 40-60min, and reacting for 5-6h at the temperature of 45-55 ℃.
And S103, slowly heating the four-mouth bottle to 85 ℃, carrying out aging reaction for 1.5-2h, namely waiting for natural cooling to obtain a reaction product, pouring the reaction product into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of organic silicon resin, the middle layer is a floccule thin layer, and the lower layer is a water phase.
And S104, pouring the toluene solution of the upper layer of the organic silicon resin into a three-mouth bottle, washing the toluene solution of the upper layer of the organic silicon resin with distilled water for multiple times to enable the toluene solution of the organic silicon resin to be organic-phase neutral, filtering the neutral organic phase by using a sand type funnel to remove impurities, and carrying out reduced pressure distillation on the organic phase to obtain the organic silicon resin.
In the reduced pressure distillation of S104, toluene and oligomer are distilled under the condition that the vacuum degree is 0.1MPa, the initial distillation temperature is 35 ℃, the final distillation temperature is 145 ℃, the organic silicon resin is transparent, and the organic silicon resin is judged to contain methyl, phenyl and vinyl by forming an infrared spectrogram.
The process of the organic silicon cross-linking agent in S2 comprises the following specific steps:
s201, pouring tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane into a three-necked bottle, mixing, and cooling by an ice water bath until the temperature is between 0 and 8 ℃ to form a mixed solution.
S202, mixing concentrated sulfuric acid with the mass of 2.7-3.5 and distilled water, pouring the mixture into a constant-pressure dropping funnel at the temperature of less than 10 ℃, dropping sulfuric acid into the mixed solution, keeping the temperature of the reaction system to be less than 10 ℃, continuing to react for 10-12 hours at the temperature of less than 10 ℃ after dropping, and reacting for 4-5 hours at room temperature.
S203, adding water and toluene in the reaction system, wherein the mass ratio of the water to the toluene is 20-28, stirring for 20-30min, pouring into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of the methylphenylhydrogenpolysiloxane, and the lower layer is a water phase.
And S204, adding the toluene solution of the upper-layer methylphenylhydrogenpolysiloxane into equal volume of distilled water, repeatedly extracting and dividing water until the organic phase is neutral, filtering the organic phase by using a sand funnel, removing impurities, and carrying out reduced pressure flash evaporation on the organic phase to obtain the organic silicon crosslinking agent.
In the reduced pressure flash evaporation of S204, under the condition that the vacuum degree is 0.1MPa, toluene and small molecular compounds are distilled out, the initial distillation temperature is 30 ℃, the final distillation temperature is 65 ℃, and the siloxane resin containing methyl, phenyl and hydrogen radicals in the organosilicon crosslinking agent is judged by forming an infrared spectrogram.
The process of the curing catalyst in S3 is specifically as follows:
s301, stirring a four-mouth bottle filled with chloroplatinic acid and divinyl tetramethyl disiloxane by nitrogen, heating to reflux temperature of 120 ℃, continuing to react at the temperature for 40-60min, naturally cooling to room temperature, filtering to remove black platinum black precipitate, adding equivalent divinyl tetramethyl disiloxane into light gray acidic filtrate, stirring uniformly, repeatedly washing to neutrality by distilled water, and removing chlorine-containing acidic byproducts.
And S302, adding anhydrous calcium chloride into the chloric acid liquid in the S301, drying, and filtering out the calcium chloride to finally obtain the curing catalyst.
The mixing rate in S4 is 80-100r/min, the mixing time is controlled to be 40-50min, and 1000PPM coordination curing catalyst is added.
The samples obtained in examples 1 to 3 were tested separately, and the results are shown in the following table:
| silicone resin: organosilicon crosslinking agent | Appearance of cured product | Hardness A | Room temperature cutting strength | |
| Example 1 | 8:2 | Hard elastomer | 90 | 8.1Mpa |
| Example 2 | 8:0.8 | Soft gels | 12 | 0.8Mpa |
| Example 3 | 8:3.5 | Elastomer, adhesive | 85 | 5.5Mpa |
From the comparison in the table above, it can be seen that: when the addition amount of the organic silicon cross-linking agent is not enough, the hardness of a cured product is small, and the strength is low; when the addition amount is too high, the excessive crosslinking agent is exuded, the surface of the cured product is sticky, and the hardness and the strength are reduced, which shows that the ratio of the organic silicon resin to the crosslinking agent is 8:2 is most suitable.
The organic silicon resin, the organic silicon cross-linking agent and the curing catalyst are mixed to prepare the packaging medium, and the ratio of the organic silicon resin to the cross-linking agent is 8:2, the organic silicon has thermodynamic and optical stability, so that the conditions of color change, deformation and cracking of the traditional packaging material under the influence of high temperature and high brightness are avoided, the packaging effect on the pressure sensor chip is improved, and the optical inspection work on the chip is facilitated.
The points to be finally explained are: although the present invention has been described in detail with reference to the general description and the specific embodiments, on the basis of the present invention, the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. The packaging medium for the pressure sensor chip is characterized by comprising the following raw materials:
the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst are mixed to prepare the packaging medium, wherein the mass ratio of the organic silicon resin to the organic silicon cross-linking agent is 3.5-4.
2. The method for preparing the packaging medium for the pressure sensor chip as claimed in claim 1, characterized by comprising the following steps:
s1, preparing organic silicon resin: mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, wherein the mass ratio of the phenyltrichlorosilane to the dimethyldichlorosilane to the methylvinyldichlorosilane is (9.5-11);
s2, preparing an organic silicon cross-linking agent: mixing tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane, wherein the mass ratio of the tetramethyldisiloxane to the diphenyldimethoxysilane to the tetramethylcyclotetrasiloxane is 1.8-2;
s3, preparation of a curing catalyst: putting chloroplatinic acid and divinyl tetramethyl disiloxane into a four-mouth bottle for mixing, wherein the mass ratio of the chloroplatinic acid to the divinyl tetramethyl disiloxane is 0.8-1.2;
and S4, mixing the organic silicon resin prepared in the S1, the organic silicon cross-linking agent prepared in the S2 and the curing catalyst prepared in the S3 in proportion, and uniformly mixing the organic silicon resin, the organic silicon cross-linking agent and the curing catalyst in the proportion of 7.8-8.3.
3. The method for preparing the packaging medium for the pressure sensor chip according to claim 2, wherein the method comprises the following steps: the process of the organic silicon resin in the S1 comprises the following specific steps:
s101, mixing phenyltrichlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane, pouring into a constant-pressure dropping funnel, pouring water and toluene into a four-mouth bottle, and uniformly mixing;
s102, slowly dripping chlorosilane mixed liquor into a four-mouth bottle, controlling the dripping time to be 40-60min, and reacting for 5-6h at the temperature of 45-55 ℃;
s103, slowly heating the four-mouth bottle to 85 ℃, carrying out aging reaction for 1.5-2h, namely waiting for natural cooling to obtain a reaction product, pouring the reaction product into a separating funnel, standing and layering, wherein the upper layer is a toluene solution of organic silicon resin, the middle layer is a floccule thin layer, and the lower layer is a water phase;
and S104, pouring the toluene solution of the upper organic silicon resin into a three-mouth bottle, washing with distilled water for multiple times to enable the toluene solution of the organic silicon resin to be organic phase neutral, filtering the neutral organic phase by using a sand type funnel to remove impurities, and carrying out reduced pressure distillation on the organic phase to obtain the organic silicon resin.
4. The method for preparing the packaging medium for the pressure sensor chip according to claim 2, wherein the method comprises the following steps: the process of the organic silicon cross-linking agent in S2 comprises the following specific steps:
s201, pouring tetramethyldisiloxane, diphenyldimethoxysilane and tetramethylcyclotetrasiloxane into a three-necked bottle, mixing, and cooling by an ice water bath until the temperature is between 0 and 8 ℃ to form a mixed solution;
s202, mixing concentrated sulfuric acid with the mass of 2.7-3.5 and distilled water, pouring the mixture into a constant-pressure dropping funnel at the temperature of less than 10 ℃, dropping sulfuric acid into the mixed solution, keeping the temperature of the reaction system to be less than 10 ℃, continuing to react for 10-12 hours at the temperature of less than 10 ℃ after dropping, and reacting for 4-5 hours at room temperature;
s203, adding water and toluene in the reaction system, wherein the mass ratio of the water to the toluene is 20-28;
and S204, adding the toluene solution of the upper-layer methylphenylhydrogenpolysiloxane into equal volume of distilled water, repeatedly extracting and dividing water until the organic phase is neutral, filtering the organic phase by using a sand funnel, removing impurities, and carrying out reduced pressure flash evaporation on the organic phase to obtain the organic silicon crosslinking agent.
5. The method for preparing the packaging medium for the pressure sensor chip according to claim 2, wherein the method comprises the following steps: the process of the curing catalyst in S3 specifically comprises the following steps:
s301, stirring a four-mouth bottle filled with chloroplatinic acid and divinyl tetramethyl disiloxane by nitrogen, heating to reflux temperature of 120 ℃, continuing to react at the temperature for 40-60min, naturally cooling to room temperature, filtering to remove black platinum black precipitate, adding equivalent divinyl tetramethyl disiloxane into light gray acidic filtrate, stirring uniformly, repeatedly washing to neutrality by distilled water, and removing chlorine-containing acidic byproducts;
and S302, adding anhydrous calcium chloride into chloric acid liquid in the S301, drying, and filtering calcium chloride to obtain the curing catalyst.
6. The method for preparing the packaging medium for the pressure sensor chip according to claim 2, wherein the method comprises the following steps: the mixing rate in the S4 is 80-100r/min, the mixing time is controlled to be 40-50min, and 1000PPM coordination curing catalyst is added.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2390378A (en) * | 1942-08-21 | 1945-12-04 | Gen Electric | Method of making silicone resins |
| US20070244214A1 (en) * | 2003-12-19 | 2007-10-18 | Makoto Yoshitake | Addition-Curable Organopolysiloxane Resin Composition |
| CN101343365A (en) * | 2008-08-28 | 2009-01-14 | 杭州师范大学 | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED |
| CN101619170A (en) * | 2008-07-04 | 2010-01-06 | 中国科学院成都有机化学有限公司 | Preparation and application of silica gel for LED packaging |
| JP2012012563A (en) * | 2010-06-02 | 2012-01-19 | Nitto Denko Corp | Composition for thermosetting silicone resin |
| CN102660027A (en) * | 2012-05-04 | 2012-09-12 | 浙江润禾有机硅新材料有限公司 | Polysiloxane curing agent |
| CN104151555A (en) * | 2014-08-11 | 2014-11-19 | 黑龙江省科学院石油化学研究院 | Preparation method of methyl phenyl vinyl silicone resin |
-
2022
- 2022-07-11 CN CN202210812226.6A patent/CN115353857B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2390378A (en) * | 1942-08-21 | 1945-12-04 | Gen Electric | Method of making silicone resins |
| US20070244214A1 (en) * | 2003-12-19 | 2007-10-18 | Makoto Yoshitake | Addition-Curable Organopolysiloxane Resin Composition |
| CN101619170A (en) * | 2008-07-04 | 2010-01-06 | 中国科学院成都有机化学有限公司 | Preparation and application of silica gel for LED packaging |
| CN101343365A (en) * | 2008-08-28 | 2009-01-14 | 杭州师范大学 | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED |
| JP2012012563A (en) * | 2010-06-02 | 2012-01-19 | Nitto Denko Corp | Composition for thermosetting silicone resin |
| CN102660027A (en) * | 2012-05-04 | 2012-09-12 | 浙江润禾有机硅新材料有限公司 | Polysiloxane curing agent |
| CN104151555A (en) * | 2014-08-11 | 2014-11-19 | 黑龙江省科学院石油化学研究院 | Preparation method of methyl phenyl vinyl silicone resin |
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