CN113121193A - High-temperature-resistant inorganic adhesive and preparation method thereof - Google Patents
High-temperature-resistant inorganic adhesive and preparation method thereof Download PDFInfo
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- CN113121193A CN113121193A CN202010040121.4A CN202010040121A CN113121193A CN 113121193 A CN113121193 A CN 113121193A CN 202010040121 A CN202010040121 A CN 202010040121A CN 113121193 A CN113121193 A CN 113121193A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/10—Mortars, concrete or artificial stone characterised by specific physical values for the viscosity
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-temperature-resistant inorganic adhesive and a preparation method thereof. The high-temperature-resistant inorganic adhesive provided by the invention has the advantages of low curing temperature, safety, environmental protection, long-time resistance at 300 ℃ and above, good bonding performance with ceramics at the temperature range of normal temperature to 300 ℃, good water resistance, acid and alkali resistance, compact structure of a cured body, and capability of isolating air and moisture permeation.
Description
Technical Field
The invention belongs to the field of electronic packaging, and particularly relates to high-temperature-resistant inorganic glue and a preparation method thereof.
Background
For electronic devices, a chip can only work stably and reliably for a long time after being packaged. Since many optoelectronic devices, such as VCSEL lasers, deep ultraviolet LEDs, accelerometers, gyroscopes, crystal oscillators, etc., have a very sensitive chip to air, moisture, etc., in order to improve the performance and reliability of these electronic devices, the chips must be packaged in vacuum or protective gas, isolated from the outside air, moisture, etc., to achieve hermetic packaging. However, for deep ultraviolet LED packaging, due to the large energy of deep ultraviolet photons, if organic material packaging is adopted, under the long-time high-energy ultraviolet irradiation condition, the organic material may undergo molecular dissociation damage, aging and yellowing, and the light-emitting efficiency and reliability of the device are greatly reduced. Meanwhile, since the organic material is non-airtight, harmful gases, particularly water vapor, easily enter the surface of the chip, thereby affecting the performance and the service life of the LED device. Meanwhile, because the temperature of the LED chip is lower than 260 ℃, in order to realize high-strength welding of a device and a substrate, some low-temperature bonding technologies such as low-temperature solder bonding, surface activation bonding and the like are developed in recent years, but the bonding strength is low, the heat resistance is poor, and the application range is limited. The high-temperature resistant inorganic adhesive is an inorganic cementing material which can be condensed and hardened through chemical reaction at normal temperature, and the material has the advantages of low-temperature curing, quick setting, early strength, good adhesion, good heat resistance, compact structure and the like.
Because the working temperature of the power device is higher (generally higher than 100 ℃); in photoelectric device packaging, the high-temperature resistant inorganic adhesive needs to have good bonding strength with heterogeneous materials (ceramics, glass and the like) at the temperature of between normal temperature and 300 ℃, which requires that the thermal expansion coefficient of the high-temperature resistant inorganic adhesive is adjustable at the temperature of between normal temperature and 300 ℃; the metal circuit layer attached to the upper part of the substrate is prepared by adopting a low-temperature process, and the difference between the thermal expansion coefficients of the metal layer and the substrate is large at high temperature (300 ℃), so that the high-temperature sintering process is not suitable for curing the inorganic adhesive.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides the high-temperature-resistant inorganic adhesive and the preparation method thereof, and the inorganic adhesive which is cured at low temperature, has high bonding strength with ceramics and the like, has compact structure of a cured body, resists high temperature and acid-base corrosion, has adjustable thermal expansion coefficient and can greatly promote the development of the packaging technology of the photoelectric device by adjusting the formula of the high-temperature-resistant inorganic adhesive.
In order to achieve the purpose, the invention adopts the technical scheme that:
the high-temperature-resistant inorganic adhesive is characterized in that: the high-temperature resistant inorganic glue contains sodium silicate, metakaolin, a curing agent, a cross-linking agent and an active filler.
The curing agent is silicon phosphate.
The cross-linking agent is styrene-acrylic emulsion and polyacrylic acid.
The active filler is magnesium oxide and spherical alumina.
Further, the weight percentages are as follows: 54-60% of sodium silicate; 29.5-38.5% of metakaolin; 4-5% of silicon phosphate; the styrene-acrylic emulsion accounts for 0.2-0.3%; 0.5-1% of magnesium oxide; polyacrylic acid accounts for 0.3-0.7%; the spherical alumina accounts for 2-4%.
Furthermore, the Baume degree of the sodium silicate solution is 39-45, and the modulus is 2.4-3.2.
Further, the metakaolin is a mixture of silicon oxide, aluminum oxide, titanium oxide, ferric oxide and calcium oxide.
Also provides a preparation method of the high-temperature-resistant inorganic adhesive, which is characterized by comprising the following steps: stirring and mixing sodium silicate and silicon phosphate to obtain a suspension; and sequentially adding metakaolin, styrene-acrylic emulsion, magnesium oxide, polyacrylic acid and spherical alumina into the suspension, and stirring and mixing to obtain the high-temperature-resistant inorganic adhesive.
Further, the sodium silicate solution is subjected to suction filtration and purification treatment.
Furthermore, the particle size of a filter screen for suction filtration of the sodium silicate solution is 200 meshes, and the suction filtration time is 30 minutes.
Further, the stirring temperature is 20-30 ℃, the stirring speed is 200-300 r/min, and the stirring time is 2-3 min.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) the high-temperature-resistant inorganic adhesive provided by the invention has the characteristics of low curing temperature, short time, safety, energy conservation and environmental protection;
(2) the high-temperature-resistant inorganic adhesive solidified body provided by the invention has good high-temperature resistance and can resist high temperature of 300 ℃ and above for a long time;
(3) the thermal expansion coefficient of the high-temperature resistant inorganic adhesive solidified body provided by the invention is adjustable in a range of normal temperature to 300 ℃;
(4) the high-temperature-resistant inorganic adhesive solidified body provided by the invention has good bonding performance with a ceramic substrate at the temperature range of normal temperature to 300 ℃;
(5) the high-temperature-resistant inorganic adhesive solidified body provided by the invention has good acid and alkali resistance;
(6) the high-temperature-resistant inorganic adhesive solidified body provided by the invention has a compact structure and can isolate air and moisture permeation.
Drawings
FIG. 1 is a process flow diagram for preparing a high temperature resistant inorganic adhesive according to the present invention;
FIG. 2 is an SEM image of a cross-section of a refractory inorganic glue constructed in accordance with example 1 of the present invention;
FIG. 3 is an SEM image of a cross-section of a refractory inorganic glue constructed in accordance with example 2 of the present invention;
FIG. 4 is an SEM image of a cross-section of a refractory inorganic glue constructed in accordance with example 3 of the present invention;
FIG. 5 is an SEM image of a cross-section of a refractory inorganic glue constructed in accordance with example 4 of the present invention;
FIG. 6 is an SEM image of a cross-section of a refractory inorganic paste constructed in accordance with comparative example 1 of the present invention;
FIG. 7 is an SEM image of a cross-section of a refractory inorganic paste constructed in accordance with comparative example 2 of the present invention;
FIG. 8 is an SEM image of a cross-section of a refractory inorganic paste constructed in accordance with comparative example 3 of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments.
The sodium silicate is a sodium metasilicate aqueous solution, is a base material of the high-temperature-resistant inorganic adhesive, and has high heat resistance.
The metakaolin is a mixture of silicon oxide, aluminum oxide, titanium oxide, ferric oxide and calcium oxide, and the particle size of the metakaolin is 10-100 mu m.
The following detailed description is made in conjunction with fig. 1 and the specific examples:
example 1
Preparing a high-temperature-resistant inorganic adhesive, wherein the high-temperature-resistant inorganic adhesive is prepared from the following components in parts by weight: 60% of sodium silicate, 32% of metakaolin, 5% of silicon phosphate, 0.2% of styrene-acrylic emulsion, 0.5% of magnesium oxide, 0.3% of polyacrylic acid and 2% of spherical alumina;
the baume degree of the sodium water glass solution is 39, and the modulus is 3.2;
the average particle size of the metakaolin is 10 mu m;
the average grain diameter of the spherical alumina is 30 um;
the preparation method comprises the following steps: the following preparation methods were all carried out at room temperature.
Using a sand core movable filtering device to carry out suction filtration on the sodium silicate solution for 30 minutes by using a 200-mesh filter screen to obtain the sodium silicate after suction filtration; adding silicon phosphate in a weight ratio into the sodium silicate after suction filtration, stirring for 2min at a stirring speed of 200r/min, and mixing the two to obtain a suspension; adding metakaolin into the suspension, and continuously stirring at the stirring speed of 200r/min for 2min to obtain emulsion; adding the styrene-acrylic emulsion into the emulsion, and stirring for 2min at the same stirring speed of 200 r/min; adding magnesium oxide into the emulsion, and stirring at a stirring speed of 200r/min for 2 min; adding polyacrylic acid into the emulsion, and stirring at a stirring speed of 200r/min for 2 min; and finally adding spherical alumina into the emulsion, and stirring for 2min at the stirring speed of 200r/min to prepare the high-temperature-resistant inorganic adhesive.
In the preparation method, firstly, sodium silicate and metakaolin can generate alkali excitation reaction at normal temperature to obtain a high-temperature-resistant inorganic polymeric material;
firstly, mixing sodium silicate and silicon phosphate, and then reacting the suspension with metakaolin;
the heat-resistant temperature of the styrene-acrylic emulsion can reach 400 ℃, the compactness of the cured inorganic adhesive is improved, cracks and microcracks are reduced, and the surface glossiness of the cured inorganic adhesive is improved;
the magnesium oxide can play a role in adjusting the thermal expansion coefficient of the inorganic adhesive;
polyacrylic acid can remarkably adjust the rheological and thixotropic properties of the inorganic adhesive and can be well dissolved with solvents such as water and the like;
the spherical alumina can improve the compactness of the inorganic adhesive after curing.
Example 2
The high-temperature-resistant inorganic adhesive comprises the following raw materials in parts by weight: 60% sodium water glass, 29.5% metakaolin, 5% silicon phosphate, 0.2% styrene-acrylic emulsion, 1.0% magnesium oxide, 0.3% polyacrylic acid and 4% spherical alumina;
the baume degree of the sodium water glass solution is 42, and the modulus is 2.8;
the average particle size of the metakaolin is 30 mu m;
the average grain diameter of the spherical alumina is 20 um;
the preparation method comprises the following steps: the following preparation methods were all carried out at room temperature.
Using a sand core movable filtering device to carry out suction filtration on the sodium silicate solution for 30 minutes by using a 200-mesh filter screen to obtain the sodium silicate after suction filtration; adding silicon phosphate in a weight ratio into the sodium silicate after suction filtration, stirring for 2min at a stirring speed of 200r/min, and mixing the two to obtain a suspension; adding metakaolin into the suspension, and continuously stirring at the stirring speed of 200r/min for 2min to obtain emulsion; adding the styrene-acrylic emulsion into the emulsion, and stirring for 2min at the same stirring speed of 200 r/min; adding magnesium oxide into the emulsion, and stirring at a stirring speed of 200r/min for 2 min; adding polyacrylic acid into the emulsion, and stirring at a stirring speed of 200r/min for 2 min; and finally adding spherical alumina into the emulsion, and stirring for 2min at the stirring speed of 200r/min to prepare the high-temperature-resistant inorganic adhesive.
Example 3
The high-temperature-resistant inorganic adhesive comprises the following raw materials in parts by weight: 54% of sodium silicate, 38.5% of metakaolin, 4% of silicon phosphate, 0.3% of styrene-acrylic emulsion, 0.5% of magnesium oxide, 0.7% of polyacrylic acid and 2% of spherical alumina;
the baume degree of the sodium water glass solution is 43, and the modulus is 2.6;
the average particle size of the metakaolin is 50 μm;
the average grain diameter of the spherical alumina is 25 um;
the preparation method comprises the following steps: the following preparation methods were all carried out at room temperature.
Using a sand core movable filtering device to carry out suction filtration on the sodium silicate solution for 30 minutes by using a 200-mesh filter screen to obtain the sodium silicate after suction filtration; adding silicon phosphate in a weight ratio into the sodium silicate after suction filtration, stirring for 3min at a stirring speed of 300r/min, and mixing the two to obtain a suspension; adding metakaolin into the suspension, and continuously stirring at the stirring speed of 300r/min for 3min to obtain emulsion; adding the styrene-acrylic emulsion into the emulsion, and stirring for 3min at the same stirring speed of 300 r/min; adding magnesium oxide into the emulsion, and stirring at a stirring speed of 300r/min for 3 min; adding polyacrylic acid into the emulsion, and stirring at a stirring speed of 300r/min for 3 min; and finally adding spherical alumina into the emulsion, and stirring for 3min at the stirring speed of 300r/min to prepare the high-temperature-resistant inorganic adhesive.
Example 4
The high-temperature-resistant inorganic adhesive comprises the following raw materials in parts by weight: 54% of sodium silicate, 36% of metakaolin, 4% of silicon phosphate, 0.3% of styrene-acrylic emulsion, 1.0% of magnesium oxide, 0.7% of polyacrylic acid and 4% of spherical alumina;
the baume degree of the sodium silicate is 45, and the modulus is 2.4;
the particle size of the metakaolin is 100 mu m;
the preparation method comprises the following steps: the following preparation methods were all carried out at room temperature.
Using a sand core movable filtering device to carry out suction filtration on the sodium silicate solution for 30 minutes by using a 200-mesh filter screen to obtain the sodium silicate after suction filtration; adding silicon phosphate in a weight ratio into the sodium silicate after suction filtration, stirring for 2min at a stirring speed of 200r/min, and mixing the two to obtain a suspension; adding metakaolin into the suspension, and continuously stirring at the stirring speed of 200r/min for 2min to obtain emulsion; adding the styrene-acrylic emulsion into the emulsion, and stirring for 2min at the same stirring speed of 200 r/min; adding magnesium oxide into the emulsion, and stirring at a stirring speed of 200r/min for 2 min; adding polyacrylic acid into the emulsion, and stirring at a stirring speed of 200r/min for 2 min; and finally adding spherical alumina into the emulsion, and stirring for 2min at the stirring speed of 200r/min to prepare the high-temperature-resistant inorganic adhesive.
Comparative example 1
The components and the content of the high-temperature resistant inorganic adhesive are the same as those in example 1, but the components do not contain silicon phosphate;
the preparation method of the high-temperature resistant inorganic adhesive comprises the steps of repeating the step process of the embodiment 1, but silicon phosphate is not added in the preparation process.
Comparative example 2
The components and the content of the high-temperature resistant inorganic adhesive are the same as those in example 2, but the components do not contain spherical alumina;
the preparation method of the high-temperature resistant inorganic adhesive comprises the step process of repeating the step process of the example 1, but spherical alumina is not added in the preparation process.
Comparative example 3
The components and the content of the high-temperature resistant inorganic adhesive are the same as those in the embodiment 2, but the components do not contain styrene-acrylic emulsion and magnesium oxide;
the preparation method of the high-temperature resistant inorganic adhesive comprises the steps of repeating the step process of the embodiment 1, but the styrene-acrylic emulsion and the magnesium oxide are not added in the preparation process.
TABLE 1 determination results of high temperature resistant inorganic adhesive properties
As can be seen from Table 1, in comparative example 1 in which no silicon phosphate was added, the high temperature resistant inorganic paste was very much decreased in shear strength after the water resistance test, and the curing time was increased because Na in the high temperature resistant inorganic paste+The ions are soluble in water, and there is no hydrophobic collection in comparative example 1The cluster replaces Na+So that the bonding strength of the inorganic adhesive and the ceramic is rapidly reduced after the water resistance test; as can be seen from fig. 7 and the SEM pictures of comparative example 2, the cross section of the refractory inorganic glue is rough, loose, and uneven, and has more pores, compared to fig. 2 and the SEM picture of example 1; from fig. 8, the SEM pictures of comparative example 3 show that the high temperature resistant inorganic glue cross section is rough, loose, and uneven compared to the SEM pictures of fig. 2 and example 1, and the thermal expansion coefficient is reduced compared to example 1.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The high-temperature-resistant inorganic adhesive is characterized in that: the high-temperature resistant inorganic glue contains sodium silicate, metakaolin, a curing agent, a cross-linking agent and an active filler; the curing agent is silicon phosphate, the cross-linking agent is styrene-acrylic emulsion and polyacrylic acid, and the active filler is magnesium oxide and spherical alumina.
2. The high temperature resistant inorganic adhesive of claim 1, wherein: according to the weight percentage: 54-60% of sodium silicate; 29.5-38.5% of metakaolin; 4-5% of silicon phosphate; the styrene-acrylic emulsion accounts for 0.2-0.3%; 0.5-1% of magnesium oxide; polyacrylic acid accounts for 0.3-0.7%; the spherical alumina accounts for 2-4%.
3. The high temperature resistant inorganic glue of claim 1 or 2, characterized in that: the baume degree of the sodium water glass solution is 39-45, and the modulus is 2.4-3.2.
4. The high temperature resistant inorganic glue of claim 1 or 2, characterized in that: the metakaolin is a mixture of silicon oxide, aluminum oxide, titanium oxide, ferric oxide and calcium oxide.
5. The high temperature resistant inorganic glue of claim 1 or 2, characterized in that: the average particle size of the metakaolin is 10-100 mu m.
6. A method for preparing the high-temperature resistant inorganic adhesive as defined in claim 1 or 2, characterized in that: firstly, stirring and mixing sodium silicate and silicon phosphate to obtain a suspension; and secondly, adding metakaolin into the suspension to obtain emulsion, and finally sequentially adding styrene-acrylic emulsion, magnesium oxide, polyacrylic acid and spherical alumina, stirring and mixing to obtain the high-temperature-resistant inorganic adhesive.
7. The method for preparing the high-temperature-resistant inorganic adhesive according to claim 6, wherein the method comprises the following steps: and carrying out suction filtration and purification treatment on the sodium water glass solution.
8. The method for preparing the high-temperature-resistant inorganic adhesive according to claim 7, wherein the method comprises the following steps: the particle size of the filter screen for suction filtration of the sodium silicate solution is 200 meshes, and the suction filtration time is 30 minutes.
9. The method for preparing the high-temperature-resistant inorganic adhesive according to claim 6, wherein the method comprises the following steps: the stirring temperature is room temperature, the stirring speed is 200-300 r/min, and the stirring time is 2-3 min.
10. The method for preparing the high-temperature-resistant inorganic adhesive according to claim 8, wherein the method comprises the following steps: the stirring temperature is room temperature, the stirring speed is 200-300 r/min, and the stirring time is 2-3 min.
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2020
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