CN108250985A - A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof - Google Patents
A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof Download PDFInfo
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- CN108250985A CN108250985A CN201810087689.4A CN201810087689A CN108250985A CN 108250985 A CN108250985 A CN 108250985A CN 201810087689 A CN201810087689 A CN 201810087689A CN 108250985 A CN108250985 A CN 108250985A
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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
Abstract
The invention belongs to adhesive fields, and in particular to a kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof.A kind of room temperature fast-curing high-temperature Resistance Adhesives are 100 including mass ratio:150 first component and second component, wherein first component are oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；Second component is made of the raw material of following mass parts：50~90 parts of aluminium oxide, 0.1~25 part of aluminium nitride, 0.1~10 part of calcirm-fluoride, 0.2~15 part of high temperature resistant filler, 0.1~5 part of toughener.The low easy coating of adhesive viscosity that the present invention is prepared using modified phosphate aluminum dihydrogen, increases in terms of curing rate, water resistance, anti-thermal shock and adhesive strength；More mild curing accelerator is added in curing agent and adjusts its adding proportion, make entire solidification process more mild, solidfied material porosity is low, make solidfied material structure finer and close, so as to improve the mechanical property of adhesive solidfied material and water resistance, while solve the contradiction of room temperature fast-curing and working life.
Description
Technical field
The invention belongs to adhesive fields, and in particular to a kind of room temperature fast-curing high-temperature Resistance Adhesives and its preparation side
Method.
Background technology
According to the difference of chemical composition, adhesive can be divided into Organic adhesive and inorganic adhesive.With Organic adhesive phase
Than, inorganic adhesive have at low cost, easy to use, heat resistance is excellent, coefficient of thermal expansion is small, ambient temperature curable, ungauged regions,
The many merits such as oil resistant, radiation hardness and durability be good, play not in fields such as Aeronautics and Astronautics, machinery, electronics, chemical industry, buildings
Alternative effect, importance are increasingly prominent.
Phosphate adhesive is most important, is also the most promising inorganic adhesive of one kind.It is with aluminum phosphate or
Person's modified phosphate is curing matrix resin, adds in the high temperature resistant gluing that the reconciliations such as suitable curing agent and framework material form
Agent has the features such as environmentally friendly, resourceful, bonding force is strong, it is simple to prepare, heat-resisting, fire resisting and excellent in te pins of durability.It is inorganic in order to make
Phosphate adhesive realizes normal temperature cure, usually adds in alkaline metal oxide in adhesive curing agent, violent due to reacting,
Reunion is easily caused, increases solidfied material hole, is susceptible to the technical problems such as adhesive mechanical properties decrease, craftsmanship difference.
Invention content
To solve above-mentioned the deficiencies in the prior art, the present invention provides a kind of room temperature fast-curing high-temperature Resistance Adhesives and its
Preparation method.
Technical scheme of the present invention：
It is 100 that a kind of room temperature fast-curing high-temperature Resistance Adhesives, which include mass ratio,:150 first component and second component, wherein
First component is oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；Second component is made of the raw material of following mass parts：
Further, the phosphate dihydrogen aluminum solution of the modification be first by 100 parts of mass fractions be 85% phosphoric acid solution
Phosphate dihydrogen aluminum solution is obtained by the reaction, then by 0.1~10 part of magnesia and 0.1~10 part of iron oxide with 20~45 parts of aluminium hydroxides
Phosphate dihydrogen aluminum solution is modified obtained.
Further, high temperature resistant filler is made of the raw material of following mass parts in the second component：
0.1~10 part of titanium carbide
0.1~5 part of zirconium oxide or yttrium oxide.
Further, toughener is silicon carbide chopped strand or silicon carbide whisker in the second component.
Further, the solidification temperature of the adhesive is 21~25 DEG C, and hardening time is for 24 hours.
A kind of preparation method step of room temperature fast-curing high-temperature Resistance Adhesives is as follows：
Step 1：Each raw material is weighed by following mass parts：
100 parts of the phosphoric acid solution, 20~45 parts of aluminum hydroxide solid powder, magnesia 0.1~10 that mass fraction is 85%
Part, 0.1~10 part of iron oxide, 50~90 parts of aluminium oxide, 0.1~25 part of aluminium nitride, 0.1~10 part of calcirm-fluoride, titanium carbide 0.1~
0.1~5 part of 10 parts, zirconium oxide or yttrium oxide and 0.1~5 part of silicon carbide chopped strand or silicon carbide whisker；
Step 2：Prepare first component：
20~45 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%,
It is stirred under certain reaction temperature after a certain period of time, adds in 0.1~10 part of magnesia and 0.1~10 part of iron oxide, keep former reaction
Temperature continue stir certain time modified phosphate dihydro aluminum solutions are made；
Step 3：Prepare second component：
By 50~90 parts of aluminium oxide, 0.1~25 part of aluminium nitride, 0.1~10 part of calcirm-fluoride, 0.1~10 part of titanium carbide, 0.1
~5 parts of zirconium oxides or yttrium oxide and 0.1~5 part of silicon carbide chopped strand or silicon carbide whisker, which are added in blender, to be stirred and evenly mixed i.e.
It can；
Step 4：Prepare room temperature fast-curing high-temperature Resistance Adhesives：
By first component and second component according to 100:150 mass ratio is added in mortar, and uniform mixed grinding obtains room temperature
Rapid curing high-temperature Resistance Adhesives.
Further, the reaction temperature described in step 2 is 90~100 DEG C, and the speed of agitator is 80~100rmp.
Further, the reaction time of phosphoric acid solution described in step 2 and aluminum hydroxide solid powder is 1h, adds in oxidation
Reaction time after magnesium and iron oxide is 1.5h.
Beneficial effects of the present invention：
First, the present invention prepares resin using metal oxide modifieds aluminium dihydrogen phosphates such as magnesia, iron oxide first, relatively
In common aluminum phosphate resin, adhesive viscosity of the present invention is greatly lowered, and easily coats, and good manufacturability utilizes magnesium oxide modified phosphorus
Acid dihydride aluminium can improve curing rate, with curing accelerator aluminium nitride collective effect make adhesive provided by the invention can room temperature it is fast
Speed curing, the 50% of adhesive strength maximum value is can reach after curing 1h, is close to is fully cured for 24 hours under room temperature；Profit
The adhesive strength of adhesive can be improved with iron oxide modified aluminium dihydrogen phosphate；Meanwhile water resistance, the heat resistanceheat resistant of adhesive of the present invention
Shake and adhesive strength etc. also increase.
2nd, the present invention adds more mild curing accelerator aluminium nitride in curing agent aluminium oxide, adjusts curing and promotes
Agent adding proportion so that after resin is mixed with curing agent, adhesive viscosity is relatively low, and entire solidification process is more mild, solves
Room temperature fast-curing and the contradiction of working life.
3rd, the present invention adds calcirm-fluoride in adhesive system, and calcirm-fluoride can act synergistically with curing agent, more
In mild solidification process, by reducing the porosity of solidfied material, make solidfied material structure finer and close, so as to improve adhesive
The mechanical property and water resistance of solidfied material.
4th, titanium carbide, zirconium oxide or yttrium oxide be also added in adhesive system of the present invention as high temperature resistant filler, make glue
Glutinous agent remains to keep under 1600 DEG C of hot conditions certain adhesive strength；Toughening is also added in adhesive system of the present invention
Agent improves the toughness of adhesive system.
5th, room temperature fast-curing high-temperature Resistance Adhesives of the present invention and preparation method thereof are raw materials used at low cost, simple for process,
It is easily operated, non-environmental-pollution problem.
Specific embodiment
With reference to embodiment, the following further describes the technical solution of the present invention, and however, it is not limited to this, every right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of technical solution of the present invention, should all be contained
It covers in protection scope of the present invention.
Embodiment 1：A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof：
A kind of room temperature fast-curing high-temperature Resistance Adhesives are 100 including mass ratio:150 first component and second component, wherein
First component is oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；
Second component is made of the raw material of following mass parts：
In the first component modified phosphate dihydrogen aluminum solution be first by phosphoric acid solution that 100 parts of mass fractions are 85% with
Phosphate dihydrogen aluminum solution is obtained by the reaction in 20~45 parts of aluminium hydroxides, then by 0.1~10 part of magnesia and 0.1~10 part of iron oxide pair
Phosphate dihydrogen aluminum solution is modified obtained.
The solidification temperature of the room temperature fast-curing high-temperature Resistance Adhesives adhesive is 21~25 DEG C, hardening time for for 24 hours,
Working life is 40~60min.
A kind of preparation method step of room temperature fast-curing high-temperature Resistance Adhesives is as follows：
Step 1：Each raw material is weighed by following mass parts：
100 parts of the phosphoric acid solution, 20~45 parts of aluminum hydroxide solid powder, magnesia 0.1~10 that mass fraction is 85%
Part, 0.1~10 part of iron oxide, 50~90 parts of aluminium oxide, 0.1~25 part of aluminium nitride, 0.1~10 part of calcirm-fluoride, titanium carbide 0.1~
0.1~5 part of 10 parts, zirconium oxide or yttrium oxide and 0.1~5 part of silicon carbide chopped strand or silicon carbide whisker；
Step 2：Prepare first component：
20~45 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%,
It is stirred under certain reaction temperature after a certain period of time, adds in 0.1~10 part of magnesia and 0.1~10 part of iron oxide, keep former reaction
Temperature continue stir certain time modified phosphate dihydro aluminum solutions are made；
Step 3：Prepare second component：
By 50~90 parts of aluminium oxide, 0.1~25 part of aluminium nitride, 0.1~10 part of calcirm-fluoride, 0.1~10 part of titanium carbide, 0.1
~5 parts of zirconium oxides or yttrium oxide and 0.1~5 part of silicon carbide chopped strand or silicon carbide whisker, which are added in blender, to be stirred and evenly mixed i.e.
It can；
Step 4：Prepare room temperature fast-curing high-temperature Resistance Adhesives：
By first component and second component according to 100:150 mass ratio is added in mortar, and uniform mixed grinding obtains room temperature
Rapid curing high-temperature Resistance Adhesives.
Further, the reaction temperature described in step 2 be 90~100 DEG C, the speed of agitator be 80~100rmp, phosphorus
The reaction time of acid solution and aluminum hydroxide solid powder is 1h, and the reaction time added in after magnesia and iron oxide is 1.5h.
Embodiment 2：A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof：
A kind of room temperature fast-curing high-temperature Resistance Adhesives are 100 including mass ratio:150 first component and second component, wherein
First component is oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；Second component is made of the raw material of following mass parts：
In the first component modified phosphate dihydrogen aluminum solution be first by phosphoric acid solution that 100 parts of mass fractions are 85% with
25 parts of aluminium hydroxides are obtained by the reaction phosphate dihydrogen aluminum solution, then by 2 parts of magnesia and 2 parts of iron oxide to phosphate dihydrogen aluminum solution into
Made from row is modified.
The solidification temperature of the room temperature fast-curing high-temperature Resistance Adhesives adhesive is 21~25 DEG C, hardening time for for 24 hours,
Working life is 40~60min.
A kind of preparation method step of room temperature fast-curing high-temperature Resistance Adhesives is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 25 parts of aluminum hydroxide solid powder, 2 parts of magnesia, iron oxide 2
Part, 60 parts of aluminium oxide, 5 parts of aluminium nitride, 2 parts of calcirm-fluoride, 2 parts of titanium carbide, 1 part of zirconium oxide and 1 part of silicon carbide chopped strand；
Step 2：Prepare first component：
25 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, 92 DEG C are stirred
Under conditions of mix rotating speed is 80rmp after stirring 1h, 2 parts of magnesia and 2 parts of iron oxide are added in, are kept for 92 DEG C continue to stir 1.5h systems
Obtain modified phosphate dihydro aluminum solutions；
Step 3：Prepare second component：
60 parts of aluminium oxide, 5 parts of aluminium nitride, 2 parts of calcirm-fluoride, 2 parts of titanium carbides, 1 part of zirconium oxide and 1 part of silicon carbide are chopped fibre
Dimension is added in blender and is stirred, and stirring took out second component after 1 hour, manually pulverized some blocks, then pour into blender and stir
It mixes, so repeatedly for three times by raw material mixing each in second component；
Step 4：Prepare room temperature fast-curing high-temperature Resistance Adhesives：
By first component and second component according to 100:150 mass ratio is added in mortar, uniform mixed grinding, and placement 5~
10min, without solid particle in adhesive, no sharp interface obtains finished product room temperature fast-curing high-temperature Resistance Adhesives.
Embodiment 3：A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof：
A kind of room temperature fast-curing high-temperature Resistance Adhesives are 100 including mass ratio:150 first component and second component, wherein
First component is oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；Second component is made of the raw material of following mass parts：
In the first component modified phosphate dihydrogen aluminum solution be first by phosphoric acid solution that 100 parts of mass fractions are 85% with
30 parts of aluminium hydroxides are obtained by the reaction phosphate dihydrogen aluminum solution, then by 4 parts of magnesia and 4 parts of iron oxide to phosphate dihydrogen aluminum solution into
Made from row is modified.
The solidification temperature of the room temperature fast-curing high-temperature Resistance Adhesives adhesive is 21~25 DEG C, hardening time for for 24 hours,
Working life is 40~60min.
A kind of preparation method step of room temperature fast-curing high-temperature Resistance Adhesives is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 4 parts of magnesia, iron oxide 4
Part, 70 parts of aluminium oxide, 10 parts of aluminium nitride, 4 parts of calcirm-fluoride, 4 parts of titanium carbide, 2 parts of zirconium oxide and 2 parts of silicon carbide chopped strand；
Step 2：Prepare first component：
30 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, 94 DEG C are stirred
Under conditions of mix rotating speed is 90rmp after stirring 1h, 4 parts of magnesia and 4 parts of iron oxide are added in, are kept for 94 DEG C continue to stir 1.5h systems
Obtain modified phosphate dihydro aluminum solutions；
Step 3：Prepare second component：
70 parts of aluminium oxide, 10 parts of aluminium nitride, 4 parts of calcirm-fluoride, 4 parts of titanium carbides, 2 parts of zirconium oxides and 2 parts of silicon carbide are chopped
Fiber is added in blender and is stirred, and stirring took out second component after 1 hour, manually pulverized some blocks, then pour into blender
Stirring, so repeatedly for three times by raw material mixing each in second component；
Step 4：Prepare room temperature fast-curing high-temperature Resistance Adhesives：
By first component and second component according to 100:150 mass ratio is added in mortar, uniform mixed grinding, and placement 5~
10min, without solid particle in adhesive, no sharp interface obtains finished product room temperature fast-curing high-temperature Resistance Adhesives.
Embodiment 4：A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof：
A kind of room temperature fast-curing high-temperature Resistance Adhesives are 100 including mass ratio:150 first component and second component, wherein
First component is oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；Second component is made of the raw material of following mass parts：
In the first component modified phosphate dihydrogen aluminum solution be first by phosphoric acid solution that 100 parts of mass fractions are 85% with
35 parts of aluminium hydroxides are obtained by the reaction phosphate dihydrogen aluminum solution, then by 6 parts of magnesia and 6 parts of iron oxide to phosphate dihydrogen aluminum solution into
Made from row is modified.
The solidification temperature of the room temperature fast-curing high-temperature Resistance Adhesives adhesive is 21~25 DEG C, hardening time for for 24 hours,
Working life is 40~60min.
A kind of preparation method step of room temperature fast-curing high-temperature Resistance Adhesives is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 35 parts of aluminum hydroxide solid powder, 6 parts of magnesia, iron oxide 6
Part, 80 parts of aluminium oxide, 15 parts of aluminium nitride, 6 parts of calcirm-fluoride, 6 parts of titanium carbide, 3 parts of yttrium oxide and 3 parts of silicon carbide whisker；
Step 2：Prepare first component：
35 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, 95 DEG C are stirred
Under conditions of mix rotating speed is 100rmp after stirring 1h, 6 parts of magnesia and 6 parts of iron oxide are added in, are kept for 95 DEG C continue to stir 1.5h
Modified phosphate dihydro aluminum solutions are made；
Step 3：Prepare second component：
By 80 parts of aluminium oxide, 15 parts of aluminium nitride, 6 parts of calcirm-fluoride, 6 parts of titanium carbides, 3 parts of yttrium oxides and 3 parts of silicon carbide whiskers
It adding in blender and stirs, stirring took out second component after 1 hour, manually pulverized some blocks, then poured into blender stirring,
So repeatedly for three times by raw material mixing each in second component；
Step 4：Prepare room temperature fast-curing high-temperature Resistance Adhesives：
By first component and second component according to 100:150 mass ratio is added in mortar, uniform mixed grinding, and placement 5~
10min, without solid particle in adhesive, no sharp interface obtains finished product room temperature fast-curing high-temperature Resistance Adhesives.
Embodiment 5：A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof：
A kind of room temperature fast-curing high-temperature Resistance Adhesives are 100 including mass ratio:150 first component and second component, wherein
First component is oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；Second component is made of the raw material of following mass parts：
In the first component modified phosphate dihydrogen aluminum solution be first by phosphoric acid solution that 100 parts of mass fractions are 85% with
40 parts of aluminium hydroxides are obtained by the reaction phosphate dihydrogen aluminum solution, then by 8 parts of magnesia and 8 parts of iron oxide to phosphate dihydrogen aluminum solution into
Made from row is modified.
The solidification temperature of the room temperature fast-curing high-temperature Resistance Adhesives adhesive is 21~25 DEG C, hardening time for for 24 hours,
Working life is 40~60min.
A kind of preparation method step of room temperature fast-curing high-temperature Resistance Adhesives is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 40 parts of aluminum hydroxide solid powder, 8 parts of magnesia, iron oxide 8
Part, 85 parts of aluminium oxide, 20 parts of aluminium nitride, 8 parts of calcirm-fluoride, 8 parts of titanium carbide, 4 parts of yttrium oxide and 4 parts of silicon carbide whisker；
Step 2：Prepare first component：
40 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, 98 DEG C are stirred
Under conditions of mix rotating speed is 80rmp after stirring 1h, 8 parts of magnesia and 8 parts of iron oxide are added in, are kept for 98 DEG C continue to stir 1.5h systems
Obtain modified phosphate dihydro aluminum solutions；
Step 3：Prepare second component：
By 85 parts of aluminium oxide, 20 parts of aluminium nitride, 8 parts of calcirm-fluoride, 8 parts of titanium carbides, 4 parts of yttrium oxides and 4 parts of silicon carbide whiskers
It adding in blender and stirs, stirring took out second component after 1 hour, manually pulverized some blocks, then poured into blender stirring,
So repeatedly for three times by raw material mixing each in second component；
Step 4：Prepare room temperature fast-curing high-temperature Resistance Adhesives：
By first component and second component according to 100:150 mass ratio is added in mortar, uniform mixed grinding, and placement 5~
10min, without solid particle in adhesive, no sharp interface obtains finished product room temperature fast-curing high-temperature Resistance Adhesives.
Room temperature fast-curing high-temperature Resistance Adhesives performance test：
(1) heat resistance test is carried out to each adhesive that embodiment 2-5 is provided, it is as a result as follows：
Room temperature curing for 24 hours, is warming up to 1300 DEG C, thermal weight loss is 7~8% under air environment with 10 DEG C/min.
(2) curing rate is tested：
Comparative example 1：Adhesive I and preparation method thereof：
Adhesive I is 100 including mass ratio:150 first component and second component, wherein first component are molten for aluminium dihydrogen phosphate
Liquid；Second component is made of the raw material of following mass parts：
Phosphate dihydrogen aluminum solution is by phosphoric acid solution and 30 part hydrogen-oxygens of 100 parts of mass fractions for 85% in the first component
Change reactive aluminum and obtain phosphate dihydrogen aluminum solution.
The preparation method step of adhesive I is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 70 parts of aluminium oxide, calcirm-fluoride 4
Part, 4 parts of titanium carbide, 2 parts of zirconium oxide and 2 parts of silicon carbide chopped strand；
Step 2：Prepare first component：
30 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, 94 DEG C are stirred
Phosphate dihydrogen aluminum solution is made after stirring 1h under conditions of mix rotating speed is 90rmp；
Step 3：Prepare second component：
70 parts of aluminium oxide, 4 parts of calcirm-fluoride, 4 parts of titanium carbides, 2 parts of zirconium oxides and 2 parts of silicon carbide chopped strands are added in into stirring
It is stirred in machine, stirring took out second component after 1 hour, manually pulverized some blocks, then poured into blender stirring, so repeatedly
Three times by raw material mixing each in second component；
Step 4：Prepare adhesive I：
By first component and second component according to 100:150 mass ratio is added in mortar, uniform mixed grinding, and placement 5~
10min obtains adhesive I in adhesive without solid particle, no sharp interface.
The room temperature fast-curing high-temperature Resistance Adhesives made from embodiment 3 and adhesive I are bonded C/SiC, SiC, C/C and resistance to
High-temperature alloy material tests the shear strength of adhesive under different hardening times, and the results are shown in Table 1：
Table 1：
The present invention prepares room temperature fast-curing high temperature resistant gluing it can be seen from adhesive shear strength comparison in table 1
During agent, curing rate is improved using magnesia and iron oxide modified aluminium dihydrogen phosphate, with curing accelerator aluminium nitride
Collective effect makes adhesive provided by the invention rapid curing at ambient temperature, and shear strength maximum is can reach after curing 1h
The 50% of value is close to is fully cured under room temperature for 24 hours；And the adhesive I that comparative example 1 provides cures due to not having to add in
Accelerating agent aluminium nitride, so curing rate is relatively slow, generally curing needs 5 to 7 days could arrive shear strength under room temperature
Maximum value, after curing 48h, shear strength maximum value is much smaller than the shear strength maximum value of embodiment 3, illustrates that embodiment 3 is made
The adhesive obtained can improve the curing rate of Phosphate adhesive.
(3) heat-resisting ability is tested：
Comparative example 2：Adhesive II and preparation method thereof：
It is 100 that adhesive II, which includes mass ratio,:150 first component and second component, wherein first component are oxidized magnesium and oxygen
Change the phosphate dihydrogen aluminum solution that iron is modified；Second component is made of the raw material of following mass parts：
In the first component modified phosphate dihydrogen aluminum solution be first by phosphoric acid solution that 100 parts of mass fractions are 85% with
30 parts of aluminium hydroxides are obtained by the reaction phosphate dihydrogen aluminum solution, then by 4 parts of magnesia and 4 parts of iron oxide to phosphate dihydrogen aluminum solution into
Made from row is modified.
II preparation method step of adhesive is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 4 parts of magnesia, iron oxide 4
Part, 70 parts of aluminium oxide, 10 parts of aluminium nitride, 4 parts of calcirm-fluoride and 2 parts of silicon carbide chopped strand；
Step 2：Prepare first component：
30 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, 94 DEG C are stirred
Under conditions of mix rotating speed is 90rmp after stirring 1h, 4 parts of magnesia and 4 parts of iron oxide are added in, are kept for 94 DEG C continue to stir 1.5h systems
Obtain modified phosphate dihydro aluminum solutions；
Step 3：Prepare second component：
70 parts of aluminium oxide, 10 parts of aluminium nitride, 4 parts of calcirm-fluoride and 2 parts of silicon carbide chopped strands are added in blender and stirred,
Stirring took out second component after 1 hour, manually pulverized some blocks, then poured into blender stirring, so repeatedly for three times by second
Each raw material mixing in component；
Step 4：Prepare adhesive II：
By first component and second component according to 100:150 mass ratio is added in mortar, uniform mixed grinding, and placement 5~
10min obtains adhesive II in adhesive without solid particle, no sharp interface.
The room temperature fast-curing high-temperature Resistance Adhesives made from embodiment 3 and adhesive II be bonded C/SiC, SiC, C/C and
High-temperature resistant alloy material tests the adhesive property of adhesive under different temperatures, and 1000 DEG C or more of test result is at this temperature
After keeping the temperature 30min, room temperature test result, remaining is on-line testing as a result, the results are shown in Table 2：
Table 2：
Adhesive of the present invention can be seen that because being added to titanium carbide, zirconium oxide or yttrium oxide by the data comparison in table 2
As high temperature resistant filler, these fillers play the role of skeletal support under the high temperature conditions, and in addition to this, their addition can be with
So that the structure of solidfied material is finer and close, adhesive is made to remain to keep certain adhesive strength under 1600 DEG C of hot conditions；And
For adhesive II because not containing high temperature resistant filler, solidfied material structure is not fine and close enough, lacks support construction under high temperature, thus 1000 DEG C with
Upper bonding force declines more violent.
(4) water resistance is tested：
Comparative example 3：Adhesive III and preparation method thereof
It is 100 that adhesive III, which includes mass ratio,:150 first component and second component, wherein first component are oxidized magnesium and oxygen
Change the phosphate dihydrogen aluminum solution that iron is modified；Second component is made of the raw material of following mass parts：
In the first component modified phosphate dihydrogen aluminum solution be first by phosphoric acid solution that 100 parts of mass fractions are 85% with
30 parts of aluminium hydroxides are obtained by the reaction phosphate dihydrogen aluminum solution, then by 4 parts of magnesia and 4 parts of iron oxide to phosphate dihydrogen aluminum solution into
Made from row is modified.
A kind of preparation method step of room temperature fast-curing high-temperature Resistance Adhesives is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 4 parts of magnesia, iron oxide 4
Part, 70 parts of aluminium oxide, 10 parts of aluminium nitride, 4 parts of titanium carbide, 2 parts of zirconium oxide and 2 parts of silicon carbide chopped strand；
Step 2：Prepare first component：
30 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, 94 DEG C are stirred
Under conditions of mix rotating speed is 90rmp after stirring 1h, 4 parts of magnesia and 4 parts of iron oxide are added in, are kept for 94 DEG C continue to stir 1.5h systems
Obtain modified phosphate dihydro aluminum solutions；
Step 3：Prepare second component：
70 parts of aluminium oxide, 10 parts of aluminium nitride, 4 parts of titanium carbides, 2 parts of zirconium oxides and 2 parts of silicon carbide chopped strand additions are stirred
It mixes in machine and stirs, stirring took out second component after 1 hour, manually pulverized some blocks, then poured into blender stirring, so anti-
Again three times by raw material mixing each in second component；
Step 4：Prepare adhesive III：
By first component and second component according to 100:150 mass ratio is added in mortar, uniform mixed grinding, and placement 5~
10min obtains adhesive III in adhesive without solid particle, no sharp interface.
The room temperature fast-curing high-temperature Resistance Adhesives made from embodiment 3 and adhesive II be bonded C/SiC, SiC, C/C and
Bonding test piece is soaked in tap water by High-temperature resistant alloy material at room temperature, tests the shearing of adhesive under soaking time
Intensity, the results are shown in Table 3：
Table 3：
Adhesive of the present invention can be seen that by the data comparison in table 3,30 days its shear strengths are impregnated in tap water
8~10% are only had dropped, and adhesive III impregnates 30 days its shear strengths in tap water and has dropped more than 60%, this illustrates this
Invention adds calcirm-fluoride in adhesive system, and calcirm-fluoride can act synergistically with curing agent, by the hole for reducing solidfied material
Gap rate makes solidfied material structure finer and close, so as to improve the mechanical property of adhesive solidfied material and water resistance.
Claims (8)
1. a kind of room temperature fast-curing high-temperature Resistance Adhesives, it is characterised in that it is 100 that the adhesive, which includes mass ratio,:150
First component and second component, wherein first component are oxidized magnesium and the phosphate dihydrogen aluminum solution of iron oxide modified；Second component is by as follows
The raw material composition of mass parts：
A kind of 2. room temperature fast-curing high-temperature Resistance Adhesives according to claim 1, it is characterised in that the phosphoric acid of the modification
Dihydro aluminum solutions are that di(2-ethylhexyl)phosphate first is obtained by the reaction by phosphoric acid solution and 20~45 parts of aluminium hydroxides that 100 parts of mass fractions are 85%
Hydrogen aluminum solutions, then by 0.1~10 part of magnesia and 0.1~10 part of iron oxide phosphate dihydrogen aluminum solution is modified obtained.
3. a kind of room temperature fast-curing high-temperature Resistance Adhesives according to claim 2, it is characterised in that resistance in the second component
High temperature filler is made of the raw material of following mass parts：
0.1~10 part of titanium carbide
0.1~5 part of zirconium oxide or yttrium oxide.
4. a kind of room temperature fast-curing high-temperature Resistance Adhesives according to claim 3, it is characterised in that increase in the second component
Tough dose is silicon carbide chopped strand or silicon carbide whisker.
5. according to a kind of any room temperature fast-curing high-temperature Resistance Adhesives of claim 1-4, it is characterised in that the gluing
The solidification temperature of agent is 21~25 DEG C, and hardening time is for 24 hours.
6. a kind of preparation method of room temperature fast-curing high-temperature Resistance Adhesives, it is characterised in that the preparation method step is as follows：
Step 1：Each raw material is weighed by following mass parts：
Mass fraction is 85% 100 parts of phosphoric acid solution, 20~45 parts of aluminum hydroxide solid powder, 0.1~10 part of magnesia, oxygen
Change 0.1~10 part of iron, 50~90 parts of aluminium oxide, 0.1~25 part of aluminium nitride, 0.1~10 part of calcirm-fluoride, 0.1~10 part of titanium carbide,
Zirconium oxide or 0.1~5 part of yttrium oxide and 0.1~5 part of silicon carbide chopped strand or silicon carbide whisker；
Step 2：Prepare first component：
20~45 parts of aluminum hydroxide solid powder are slowly added into the phosphoric acid solution that 100 parts of mass fractions are 85%, certain
It is stirred under reaction temperature after a certain period of time, adds in 0.1~10 part of magnesia and 0.1~10 part of iron oxide, keep former reaction temperature
Continue stir certain time modified phosphate dihydro aluminum solutions are made；
Step 3：Prepare second component：
By 50~90 parts of aluminium oxide, 0.1~25 part of aluminium nitride, 0.1~10 part of calcirm-fluoride, 0.1~10 part of titanium carbide, 0.1~5 part
Zirconium oxide or yttrium oxide and 0.1~5 part of silicon carbide chopped strand or silicon carbide whisker, which are added in blender, to be stirred and evenly mixed；
Step 4：Prepare room temperature fast-curing high-temperature Resistance Adhesives：
By first component and second component according to 100:150 mass ratio is added in mortar, and it is quick that uniform mixed grinding obtains room temperature
Cure high-temperature Resistance Adhesives.
A kind of 7. preparation method of room temperature fast-curing high-temperature Resistance Adhesives according to claim 6, it is characterised in that step
Reaction temperature described in two is 90~100 DEG C, and the speed of agitator is 80~100rmp.
A kind of 8. preparation method of room temperature fast-curing high-temperature Resistance Adhesives described according to claim 6 or 7, it is characterised in that step
The reaction time of rapid two phosphoric acid solution and aluminum hydroxide solid powder is 1h, when adding in the reaction after magnesia and iron oxide
Between be 1.5h.
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| CN114751772A (en) * | 2022-05-13 | 2022-07-15 | 无锡海飞凌半导体材料有限公司 | Ceramic repairing method for high-temperature thermal field and application thereof |
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