CN115505340B - Preparation method of nickel-aluminum modified silica sol inorganic adhesive - Google Patents
Preparation method of nickel-aluminum modified silica sol inorganic adhesive Download PDFInfo
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- CN115505340B CN115505340B CN202211226874.XA CN202211226874A CN115505340B CN 115505340 B CN115505340 B CN 115505340B CN 202211226874 A CN202211226874 A CN 202211226874A CN 115505340 B CN115505340 B CN 115505340B
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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
- C09J1/00—Adhesives based on inorganic constituents
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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Abstract
The invention relates to the field of adhesive preparation, in particular to a method for preparing nickel-aluminum modified silica sol inorganic high-temperature-resistant adhesive. The invention aims to solve the technical problem of low high-temperature bonding performance of inorganic adhesives. The method comprises the following steps: the method respectively adopts a nickel-containing substance and an aluminum-containing substance to modify silica sol to prepare modified silica sol resin; and preparing a curing agent by adopting phosphate, silicon carbide and metal oxide. The adhesive prepared by the invention can be cured at room temperature or by heating, and the cured product of the adhesive combines the high adhesiveness of the inorganic silicate adhesive and the high heat resistance of the inorganic phosphate adhesive, and reacts in the high-temperature use process to generate the high-heat-resistant intermetallic compound reinforced ceramic composite material, so that the ceramic composite material has excellent high-temperature stability and meets the high-temperature use requirement. The method is used for preparing the nickel-aluminum modified silica sol inorganic adhesive.
Description
Technical Field
The invention relates to the field of adhesive preparation, in particular to a method for preparing nickel-aluminum modified silica sol inorganic high-temperature-resistant adhesive.
Background
The silicate adhesive is an important inorganic adhesive, has the advantages of high adhesive strength and room temperature curing, is resistant to heat at the temperature of less than or equal to 1000 ℃, is resistant to oil, alkali and organic solvents, and can be used as a high-temperature-resistant adhesive and repair material in the aerospace field. However, with the development and progress of technology, higher requirements are put on the use temperature of the adhesive in some application places, and the traditional silicate adhesive is difficult to meet the heat-resistant requirement. Although the traditional phosphate adhesive has the advantage of good heat resistance, the high-temperature adhesive strength is low, so that the further application of the phosphate adhesive is limited. Therefore, development of novel inorganic adhesives to meet the increasing demand for high temperature resistance has been urgent.
Disclosure of Invention
The invention aims to solve the technical problem of low high-temperature bonding performance of an inorganic adhesive and provides a preparation method of a nickel-aluminum modified silica sol inorganic adhesive.
The preparation method of the nickel-aluminum modified silica sol inorganic adhesive comprises the steps of respectively modifying silica sol by using a nickel-containing substance and an aluminum-containing substance to prepare modified silica sol resin; and preparing a curing agent by adopting phosphate, silicon carbide and metal oxide.
The cured product of the invention reacts to generate intermetallic compound reinforced ceramic composite material in the high-temperature use process, so that the ceramic composite material has excellent high-temperature resistance and can meet the high-temperature use requirement of 1000-1600 ℃.
The preparation method for preparing the inorganic adhesive by using the nickel-aluminum modified silica sol comprises the following steps:
1. diluting silica sol to obtain diluted silica sol, and adding Ni (OH) 2 -ammonia water solution, heating and stirring for 20-40 min; then adding aluminum powder, aluminum metaphosphate and boron-containing auxiliary agent, heating and stirring for 2-4 hours to prepare modified silica sol resin;
2. fully mixing aluminum phosphate powder with the particle size of 50-100 mu m, silicon carbide powder with the particle size of 10-50 mu m, magnesium oxide powder with the particle size of 120-200 mu m, zirconium oxide powder with the particle size of 100-150 mu m and zinc oxide powder with the particle size of 150-200 mu m, and dispersing for 30-40 min to prepare a curing agent;
wherein the dispersion rotating speed is controlled to be 200-300 r/min;
3. adding the modified silica sol resin prepared in the first step and the curing agent prepared in the second step into a ball milling tank, controlling the rotating speed to be 200-300 r/min, and treating for 2-3 h, wherein the mass ratio of the ball materials is 1:1, so as to obtain the nickel-aluminum modified silica sol inorganic adhesive, and thus, the preparation is completed.
Wherein the aluminum powder in the first step is 500 meshes.
The curing process of the nickel-aluminum modified silica sol inorganic adhesive comprises the following steps: applying pressure of 0.01MPa-0.003MPa or contact pressure, curing at room temperature for 24h or curing at 80 ℃ for 2h.
The beneficial effects of the invention are as follows:
the invention respectively adopts substances containing nickel and aluminum to modify silica sol to prepare modified silica sol resin, and in an alkaline solution system, aluminum and the silica sol form aluminum silicate, ni (OH) 2 Complexing to promote Ni 2+ Grafted into an aluminum silicate framework; aluminum phosphate is used as a curing accelerator, and silicon carbide and metal oxide are used as aggregate to prepare the curing agent. Then, mixing resin and curing agent, aluminum phosphate changing pH value of silica sol to promote crosslinking, the prepared adhesive can be cured at room temperature or by heating, high heat-resistant intermetallic compound reinforced ceramic composite material is generated in the high temperature use process of 1000 ℃, phosphorus pentoxide in aluminum phosphate overflows in the high temperature use process of 1400 ℃ and is converted into more heat-resistant aluminum oxide ceramic, so that the aluminum oxide ceramic has excellent high temperature stability and bonding performance in a high temperature area, and the cured product combines the high bonding property of silicate adhesive and the high heat resistance of inorganic phosphate adhesive, thereby meeting the high temperature use requirement of 1000-1600 ℃.
The method is used for preparing the nickel-aluminum modified silica sol inorganic adhesive.
Drawings
FIG. 1 is a scanning electron microscope image of a commercially available silica sol adhesive after 500 ℃ treatment;
FIG. 2 is a scanning electron microscope image of the nickel aluminum modified silica sol inorganic adhesive prepared in the first embodiment after 500 ℃ treatment;
FIG. 3 is a scanning electron microscope image of a commercially available silica sol adhesive after 1000 ℃ treatment;
FIG. 4 is a scanning electron microscope image of the nickel aluminum modified silica sol inorganic adhesive prepared in the first embodiment after 1000 ℃ treatment;
FIG. 5 is a scanning electron microscope image of a commercially available silica sol adhesive after 1600 ℃ treatment;
FIG. 6 is a scanning electron microscope image of the nickel aluminum modified silica sol inorganic adhesive prepared in the first embodiment after 1600 ℃.
Detailed Description
The present invention is not limited to the above embodiments, and the object of the invention can be achieved by one or a combination of several embodiments.
The first embodiment is as follows: according to the preparation method of the nickel-aluminum modified silica sol inorganic adhesive, a nickel-containing substance and an aluminum-containing substance are respectively adopted to modify silica sol, so that modified silica sol resin is prepared; and preparing a curing agent by adopting phosphate, silicon carbide and metal oxide.
According to the preparation method, the modified silica sol resin is prepared by adopting phosphates, silicon carbide, metal oxides and the like to prepare the curing agent, the prepared adhesive can be cured at room temperature or under heating, the high adhesiveness of the inorganic silicate adhesive and the high heat resistance of the inorganic phosphate adhesive are both considered, and the high heat-resistant intermetallic compound reinforced ceramic composite material is generated by reaction in the high-temperature use process, so that the high-temperature stability of the high-temperature ceramic composite material is excellent, and the high-temperature use requirement of 1000-1600 ℃ can be met. The method for preparing the novel inorganic adhesive by using the nickel-aluminum modified silica sol has the advantages of simple preparation steps, short period, low cost and the like, and has wide application prospect.
The second embodiment is as follows: the preparation method of the nickel-aluminum modified silica sol inorganic adhesive comprises the following steps of:
1. diluting silica sol to obtain diluted silica sol, and adding Ni (OH) 2 -ammonia water solution, heating and stirring for 20-40 min; then adding aluminum powder, aluminum metaphosphate and boron-containing auxiliary agent, heating and stirring for 2-4 hours to prepare modified silica sol resin;
2. fully mixing aluminum phosphate powder with the particle size of 50-100 mu m, silicon carbide powder with the particle size of 10-50 mu m, magnesium oxide powder with the particle size of 120-200 mu m, zirconium oxide powder with the particle size of 100-150 mu m and zinc oxide powder with the particle size of 150-200 mu m, and dispersing for 30-40 min to prepare a curing agent;
wherein the dispersion rotating speed is controlled to be 200-300 r/min;
3. adding the modified silica sol resin prepared in the first step and the curing agent prepared in the second step into a ball milling tank, controlling the rotating speed to be 200-300 r/min, and treating for 2-3 h, wherein the mass ratio of the ball materials is 1:1, so as to obtain the nickel-aluminum modified silica sol inorganic adhesive, and thus, the preparation is completed.
And a third specific embodiment: the present embodiment and the second embodiment are not: the mass percentage of the diluted silica sol is 10-15%. The other is the same as in the second embodiment.
The specific embodiment IV is as follows: the second or third embodiment is different from the first embodiment in that: step one the Ni (OH) 2 Ni (OH) in aqueous ammonia solution 2 The molar ratio of the catalyst to the ammonia water is 1: (4-6). The other is the same as the second or third embodiment.
Fifth embodiment: the second to fourth embodiments of the present embodiment are not: in the first step, the silica sol is diluted to 100 parts by weight of Ni (OH) 2 100 to 120 parts of ammonia water solution, 150 to 200 parts of aluminum powder, 40 to 60 parts of aluminum metaphosphate and 1 part of boron-containing auxiliary agent. The others are the same as in the second to fourth embodiments.
Specific embodiment six: the present embodiment is not limited to the second to fifth embodiments: step one Ni (OH) is added 2 -ammonia water solution, heating and stirring for 20-40 min at 60 ℃. The others are the same as in one of the second to fifth embodiments.
Seventh embodiment: the present embodiment and one of the second to sixth embodiments are not: adding aluminum powder, aluminum metaphosphate and boron-containing auxiliary agent, heating and stirring for 2-4 h at the temperature of 60 ℃. The others are the same as in the second to sixth embodiments.
Eighth embodiment: the present embodiment and one of the second to seventh embodiments are not: the boron-containing auxiliary agent is one or a mixture of two of boric anhydride and alkali boron glass micropowder. The others are the same as in one of the second to seventh embodiments.
Detailed description nine: the present embodiment and one of the second to eighth embodiments are not: step two, according to the weight portions of 40 to 60 portions of aluminum phosphate powder with the grain diameter of 50 to 100 mu m, 60 to 100 portions of silicon carbide powder with the grain diameter of 10 to 50 mu m, 50 to 100 portions of magnesia powder with the grain diameter of 120 to 200 mu m, 10 to 30 portions of zirconia powder with the grain diameter of 100 to 150 mu m and 5 to 20 portions of zinc oxide powder with the grain diameter of 150 to 200 mu m. The others are the same as in one of the second to eighth embodiments.
Detailed description ten: the present embodiment and one of the second to ninth embodiments are not: and step three, 100 parts of modified silica sol resin and 10-20 parts of curing agent. The others are the same as in one of the second to ninth embodiments.
The following examples and comparative experiments were used to verify the beneficial effects of the present invention:
embodiment one:
the preparation method for preparing the inorganic adhesive by using the nickel-aluminum modified silica sol is specifically carried out according to the following steps:
1. diluting the silica sol to obtain diluted silica sol with the mass percent of 12%, and adding 100 parts of Ni (OH) into 100 parts of diluted silica sol according to the mass parts 2 -ammonia water solution, heating and stirring for 25min at 60 ℃; then adding 200 parts of aluminum powder, 40 parts of aluminum metaphosphate and 1 part of boron-containing auxiliary agent boric anhydride, heating and stirring for 2 hours at the temperature of 60 ℃ to prepare modified silica sol resin;
the Ni (OH) 2 Ni (OH) in aqueous ammonia solution 2 The molar ratio of the catalyst to the ammonia water is 1:4, a step of;
2. according to the parts by mass, fully mixing 40 parts of aluminum phosphate powder with the particle size of 50-100 mu m, 60 parts of silicon carbide powder with the particle size of 10-50 mu m, 80 parts of magnesium oxide powder with the particle size of 120-200 mu m, 20 parts of zirconium oxide powder with the particle size of 100-150 mu m and 10 parts of zinc oxide powder with the particle size of 150-200 mu m, and dispersing for 30min to prepare a curing agent;
wherein the dispersion rotating speed is controlled to be 200r/min;
3. according to the parts by weight, adding 100 parts of the modified silica sol resin prepared in the first step and 10 parts of the curing agent prepared in the second step into a ball milling tank, controlling the rotating speed to be 200r/min, and treating the mixture for 3 hours, wherein the mass ratio of the ball materials is 1:1, so that the nickel-aluminum modified silica sol inorganic adhesive is prepared.
The nickel aluminum modified silica sol inorganic adhesive prepared in the embodiment has good fluidity and viscosity of 73000 mPa.s.
The nickel-aluminum modified silica sol inorganic adhesive prepared by the embodiment is used for bonding the SiC/SiC test piece; the curing process comprises the following steps: the pressure is applied to 0.008MPa, and the mixture is cured for 24 hours at room temperature.
Carrying out mechanical and high temperature resistance test on the SiC/SiC test piece after bonding and curing, wherein the tensile shear strength at room temperature is 6.6MPa, the tensile shear strength at 500 ℃ is 8.8MPa, and the treatment is carried out for 30min; treating at 1000 ℃ for 30min, wherein the tensile shear strength is 7.7MPa; treating at 1200 ℃ for 30min, wherein the tensile shear strength is 7.2MPa; the tensile shear strength is 4.3MPa after 30min of treatment at 1600 ℃.
Mixing commercially available silica sol (i.e. the silica sol in the first step of the embodiment) with an aluminum powder curing agent, and bonding SiC/SiC test pieces; the test piece is treated for 30min at 500 ℃ and the tensile shear strength is 8.5MPa; treating at 1000 ℃ for 30min, wherein the tensile shear strength is 6.7MPa; treating at 1200 ℃ for 30min, wherein the tensile shear strength is 3.2MPa; the tensile shear strength cannot be measured after 30 minutes of treatment at 1600 ℃.
Therefore, the nickel-aluminum modified silica sol inorganic adhesive has excellent high-temperature resistance stability and bonding performance in a high-temperature area.
The commercially available silica sol (i.e., the silica sol of example one step one) was subjected to different temperature treatments (500 ℃, 1000 ℃, 1600 ℃) in combination with the curing agent of example one and the nickel aluminum modified silica sol inorganic adhesive prepared in example one.
FIG. 1 is a scanning electron microscope image of a commercially available silica sol adhesive after 500 ℃ treatment;
FIG. 2 is a scanning electron microscope image of the nickel aluminum modified silica sol inorganic adhesive prepared in the first embodiment after 500 ℃ treatment;
FIG. 3 is a scanning electron microscope image of a commercially available silica sol adhesive after 1000 ℃ treatment;
FIG. 4 is a scanning electron microscope image of the nickel aluminum modified silica sol inorganic adhesive prepared in the first embodiment after 1000 ℃ treatment;
FIG. 5 is a scanning electron microscope image of a commercially available silica sol adhesive after 1600 ℃ treatment;
FIG. 6 is a scanning electron microscope image of the nickel aluminum modified silica sol inorganic adhesive prepared in the first embodiment after 1600 ℃.
Comparing fig. 1 to 6, the unmodified silica sol has a more porous loose network structure at 500 ℃ temperature treatment; when the temperature reached 1000 ℃, the network backbone began to break (fig. 3); when the temperature is further raised to 1600 ℃, the Si-O-Al skeleton is almost destroyed and collapse occurs; this is accompanied by the formation of a large number of cracks (fig. 5). According to the invention, the gap of the Si-O-Al network is filled by introducing the intermetallic compound, and the gap is used as compensation for improving the strength of the network skeleton, as shown in figures 2, 4 and 6, the density and the porosity of the modified adhesive are obviously reduced at 500 ℃; when the temperature is raised to 1000 ℃, the silicate framework and intermetallic compound show an agglomerated state (fig. 4), which improves the continuity, mechanical properties and heat resistance of the system; at 1600 ℃, all the components sinter almost completely together, forming a dense homogeneous structure (fig. 6); this compensates for the volumetric loss of the heated released silica sol. If the intermetallic compound starts to oxidize, the system can still provide sufficient adhesion properties.
Embodiment two:
the preparation method for preparing the inorganic adhesive by using the nickel-aluminum modified silica sol is specifically carried out according to the following steps:
1. diluting the silica sol to obtain diluted silica sol with the mass percent of 13%, and adding 110 parts of Ni (OH) into 100 parts of diluted silica sol according to the mass parts 2 -ammonia water solution, heating and stirring for 30min at 60 ℃; then 180 parts of aluminum powder, 50 parts of aluminum metaphosphate and 1 part of boron-containing auxiliary agent alkali boron glass micro powder are added, and the temperature is controlled to be 60 ℃ and the mixture is heated and stirred for 3 hours to prepare modified silica sol resin;
the Ni (OH) 2 Ni (OH) in aqueous ammonia solution 2 The molar ratio of the catalyst to the ammonia water is 1:5；
2. according to the parts by mass, fully mixing 50 parts of aluminum phosphate powder with the particle size of 50-100 mu m, 70 parts of silicon carbide powder with the particle size of 10-50 mu m, 70 parts of magnesium oxide powder with the particle size of 120-200 mu m, 20 parts of zirconium oxide powder with the particle size of 100-150 mu m and 10 parts of zinc oxide powder with the particle size of 150-200 mu m, and dispersing for 35min to prepare a curing agent;
wherein the dispersion rotating speed is controlled to be 250r/min;
3. according to the parts by weight, adding 100 parts of the modified silica sol resin prepared in the first step and 12 parts of the curing agent prepared in the second step into a ball milling tank, controlling the rotating speed to be 260r/min, and treating for 3 hours, wherein the mass ratio of the ball materials is 1:1, so that the nickel-aluminum modified silica sol inorganic adhesive is obtained, and the preparation is completed.
The nickel aluminum modified silica sol inorganic adhesive prepared in the embodiment has good fluidity and viscosity of 71000 mPa.s.
The nickel-aluminum modified silica sol inorganic adhesive prepared by the embodiment is used for bonding the SiC/SiC test piece; the curing process comprises the following steps: the mixture was cured at 80℃under a pressure of 0.006MPa for 2 hours.
Carrying out mechanical and high temperature resistance test on the SiC/SiC test piece after bonding and curing, wherein the tensile shear strength at room temperature is 9.8MPa, the tensile shear strength at 500 ℃ is 10.4MPa, and the treatment is carried out for 30min; treating at 1000 ℃ for 30min, wherein the tensile shear strength is 7.4MPa; treating at 1200 deg.c for 30min with tensile shear strength of 6.8MPa; the treatment is carried out for 30min at 1600 ℃, and the tensile shear strength is 5.4MPa.
Embodiment III:
the preparation method for preparing the inorganic adhesive by using the nickel-aluminum modified silica sol is specifically carried out according to the following steps:
1. diluting the silica sol to obtain diluted silica sol with the mass percent of 14%, and adding 120 parts of Ni (OH) into 100 parts of diluted silica sol according to the mass parts 2 -ammonia water solution, heating and stirring for 40min at 60 ℃; then 200 parts of aluminum powder, 40 parts of aluminum metaphosphate and 1 part of boron-containing auxiliary agent are added, the boron-containing auxiliary agent is prepared by mixing boric anhydride with alkali boron glass micro powder in equal mass, heating and stirring for 4 hours at the temperature of 60 ℃ to prepare modified silica sol resin;
the Ni (OH) 2 -ammonia waterNi (OH) in solution 2 The molar ratio of the catalyst to the ammonia water is 1:4, a step of;
2. according to the parts by weight, fully mixing 60 parts of aluminum phosphate powder with the particle size of 50-100 mu m, 60 parts of silicon carbide powder with the particle size of 10-50 mu m, 80 parts of magnesium oxide powder with the particle size of 120-200 mu m, 15 parts of zirconium oxide powder with the particle size of 100-150 mu m and 15 parts of zinc oxide powder with the particle size of 150-200 mu m, and dispersing for 40min to prepare a curing agent;
wherein the dispersion rotating speed is controlled to be 220r/min;
3. according to the parts by weight, adding 100 parts of the modified silica sol resin prepared in the first step and 14 parts of the curing agent prepared in the second step into a ball milling tank, controlling the rotating speed to be 260r/min, and treating the mixture for 2.5 hours according to the mass ratio of the ball materials to 1:1 to obtain the nickel-aluminum modified silica sol inorganic adhesive, thereby completing the preparation.
The nickel-aluminum modified silica sol inorganic adhesive prepared in the embodiment has good fluidity and viscosity of 70000 mPa.s.
The nickel-aluminum modified silica sol inorganic adhesive prepared by the embodiment is used for bonding the SiC/SiC test piece; the curing process comprises the following steps: contact pressure, curing at 80 ℃ for 2h.
Carrying out mechanical and high temperature resistance test on the SiC/SiC test piece after bonding and curing, wherein the tensile shear strength at room temperature is 11.8MPa, the tensile shear strength at 500 ℃ is 13.5MPa, and the treatment is carried out for 30min; treating at 1000 ℃ for 30min, wherein the tensile shear strength is 11.3MPa; treating at 1200 ℃ for 30min, wherein the tensile shear strength is 11.0MPa; the treatment is carried out for 30min at 1600 ℃, and the tensile shear strength is 6.7MPa.
Embodiment four:
the preparation method for preparing the inorganic adhesive by using the nickel-aluminum modified silica sol is specifically carried out according to the following steps:
1. diluting the silica sol to obtain diluted silica sol with the mass percent of 11%, and adding 115 parts of Ni (OH) into 100 parts of diluted silica sol according to the mass parts 2 -ammonia water solution, heating and stirring for 35min at 60 ℃; then 180 parts of aluminum powder, 50 parts of aluminum metaphosphate and 1 part of boron-containing auxiliary agent are added, the boron-containing auxiliary agent is prepared by mixing boric anhydride with alkali boron glass micro powder in equal mass, heating and stirring for 3 hours at the temperature of 60 ℃ to prepare modified silica sol resin;
the Ni (OH) 2 Ni (OH) in aqueous ammonia solution 2 The molar ratio of the catalyst to the ammonia water is 1:4, a step of;
2. according to the parts by mass, fully mixing 40 parts of aluminum phosphate powder with the particle size of 50-100 mu m, 60 parts of silicon carbide powder with the particle size of 10-50 mu m, 80 parts of magnesium oxide powder with the particle size of 120-200 mu m, 20 parts of zirconium oxide powder with the particle size of 100-150 mu m and 10 parts of zinc oxide powder with the particle size of 150-200 mu m, and dispersing for 40min to prepare a curing agent;
wherein the dispersion rotating speed is controlled to be 300r/min;
3. according to the parts by weight, adding 100 parts of the modified silica sol resin prepared in the first step and 11 parts of the curing agent prepared in the second step into a ball milling tank, controlling the rotating speed to be 240r/min, and treating the mixture for 2 hours, wherein the mass ratio of the ball materials is 1:1, so that the nickel-aluminum modified silica sol inorganic adhesive is prepared.
The nickel aluminum modified silica sol inorganic adhesive prepared in the embodiment has good fluidity and the viscosity is 72000 mPa.s.
The nickel-aluminum modified silica sol inorganic adhesive prepared by the embodiment is used for bonding the SiC/SiC test piece; the curing process comprises the following steps: and applying the pressure of 0.006MPa, and curing for 24 hours at room temperature.
Carrying out mechanical and high temperature resistance test on the SiC/SiC test piece after bonding and curing, wherein the tensile shear strength at room temperature is 8.6MPa, the tensile shear strength at 500 ℃ is 7.5MPa, and the treatment is carried out for 30min; treating at 1000 ℃ for 30min, wherein the tensile shear strength is 6.3MPa; treating at 1200 deg.c for 30min with tensile shear strength of 5.7MPa; the treatment is carried out for 30min at 1600 ℃, and the tensile shear strength is 4.9MPa.
Claims (5)
1. A preparation method of a nickel-aluminum modified silica sol inorganic adhesive is characterized by comprising the following steps of: the method respectively adopts a nickel-containing substance and an aluminum-containing substance to modify silica sol to prepare modified silica sol resin; preparing a curing agent by adopting phosphate, silicon carbide and metal oxide;
the preparation method of the nickel-aluminum modified silica sol inorganic adhesive comprises the following steps of:
1. diluting silica sol to obtain diluted silica sol, and adding Ni (OH) 2 -ammoniaHeating and stirring the aqueous solution for 20-40 min; then adding aluminum powder, aluminum metaphosphate and a boron-containing auxiliary agent, heating and stirring for 2-4 hours to prepare modified silica sol resin;
2. fully mixing aluminum phosphate powder with the particle size of 50-100 mu m, silicon carbide powder with the particle size of 10-50 mu m, magnesium oxide powder with the particle size of 120-200 mu m, zirconium oxide powder with the particle size of 100-150 mu m and zinc oxide powder with the particle size of 150-200 mu m, and dispersing for 30-40 min to prepare a curing agent;
wherein the dispersion rotating speed is controlled to be 200-300 r/min;
3. adding the modified silica sol resin prepared in the first step and the curing agent prepared in the second step into a ball milling tank, controlling the rotating speed to be 200-300 r/min, and treating for 2-3 hours, wherein the mass ratio of the ball materials is 1:1, so as to obtain the nickel-aluminum modified silica sol inorganic adhesive, and finishing the preparation;
the mass percentage of the diluted silica sol is 10-15%;
step one the Ni (OH) 2 Ni (OH) in aqueous ammonia solution 2 The molar ratio of the catalyst to the ammonia water is 1: (4-6);
in the first step, the silica sol is diluted to 100 parts by weight of Ni (OH) 2 100-120 parts of ammonia water solution, 150-200 parts of aluminum powder, 40-60 parts of aluminum metaphosphate and 1 part of boron-containing auxiliary agent;
and secondly, 40-60 parts of aluminum phosphate powder with the particle size of 50-100 mu m, 60-100 parts of silicon carbide powder with the particle size of 10-50 mu m, 50-100 parts of magnesium oxide powder with the particle size of 120-200 mu m, 10-30 parts of zirconium oxide powder with the particle size of 100-150 mu m and 5-20 parts of zinc oxide powder with the particle size of 150-200 mu m.
2. The method for preparing the nickel-aluminum modified silica sol inorganic adhesive according to claim 1, which is characterized in that: step one Ni (OH) is added 2 And (3) heating and stirring the ammonia water solution for 20-40 min at the temperature of 60 ℃.
3. The method for preparing the nickel-aluminum modified silica sol inorganic adhesive according to claim 1, which is characterized in that: and firstly, adding aluminum powder, aluminum metaphosphate and a boron-containing auxiliary agent, and heating and stirring for 2-4 hours at the temperature of 60 ℃.
4. The method for preparing the nickel-aluminum modified silica sol inorganic adhesive according to claim 1, which is characterized in that: the boron-containing auxiliary agent is one or a mixture of two of boric anhydride and alkali boron glass micropowder.
5. The method for preparing the nickel-aluminum modified silica sol inorganic adhesive according to claim 1, which is characterized in that: and thirdly, 100 parts of modified silica sol resin and 10-20 parts of curing agent.
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| EP1539842A1 (en) * | 2002-08-23 | 2005-06-15 | Celanese Ventures GmbH | Novel polyvinyl esters |
| CN104804665A (en) * | 2015-04-20 | 2015-07-29 | 许金兰 | Anti-mildew dextrin adhesive and preparation method thereof |
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| CN114149276A (en) * | 2020-12-31 | 2022-03-08 | 郑州轻工业大学 | Micro-nano hole heat insulation refractory material containing zirconium oxide and preparation method thereof |
| CN113185921A (en) * | 2021-06-03 | 2021-07-30 | 哈尔滨工程大学 | Preparation method of ceramic precursor modified phosphate adhesive |
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