CN102352190A - Microwave solidification type bonding agent and microwave solidification method thereof - Google Patents
Microwave solidification type bonding agent and microwave solidification method thereof Download PDFInfo
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Abstract
The invention discloses a microwave solidification type bonding agent and a microwave solidification method thereof. The bonding agent is prepared by adopting aluminum dihydrogen phosphate solution and phenolic resin as base materials, adopting compounds of two kinds of materials or several kinds of materials from magnesium oxide, zinc oxide, ferric oxide and zirconium oxide as solidification agents, adopting aluminum oxide as fillings and adopting boron carbide micro particles and ultra-fine silicon dioxide powder as modified fillings. All ingredients are mixed according to a certain proportion and are stirred at a high speed for obtaining the bonding agents. After the bonding agent is adopted for bonding devices, the convenient and fast solidification can be carried out under the microwave radiation effect. The bonding agent has excellent heat resistance performance, can be used for bonding ceramics, graphite, plastics, glass, epoxy resin, carbon/carbon composite materials and the like and has the characteristics that the temperature gradient of a solidified glue layer is small, the solidification is uniform, and the solidification time is short.
Description
Technical field
The present invention relates to a kind of caking agent, more particularly say, be meant a kind of microwave curing type caking agent and the microwave curing method thereof that can under microwave environment, carry out material adhesive.
Background technology
Phosphate-bonded dose with characteristics such as its excellent dielectric constant, resistance to elevated temperatures, low-expansion coefficient, low-temperature curing high temperature easy to process and middle uses and receive much concern; In reparation, the production and bonding of materials such as metal, glass, pottery, Resins, epoxy, many aspects such as preparation of high temperature resistant composite, coating and refractory materials play crucial effect.
Resol is widely used in the caking agent field with characteristics such as its good solvent resistance, anti-creep and bonding strength height.Yet as organic polymer material, its pyrolysis at high temperature is inevitable, and thermostability is limited, so use temperature is confined to 200～300 ℃ more.
At present, high temperature resistant adhesive adopts the mode of traditional heating to be cured under mesophilic condition more.But heat cured system exist the glue-line thermograde big, solidify inhomogeneous, solidify shortcomings such as required time is long, the raising of Joint strength is had certain restriction.Solidifying high temperature resistant adhesive under the room temperature is a kind of curing mode that proposes recently, but this method is long set time, needs about 10 days.
Summary of the invention
In order to shorten the curing reaction time, solve the glue-line thermograde that thermofixation exists big, solidify uneven problem, the present invention introduces microwave radiation in the solidify reaction process, and a kind of microwave curing type caking agent and microwave curing method are provided.
A kind of microwave curing type caking agent of the present invention is in the phosphate dihydrogen aluminum solution of 100ml, to add the solidifying agent of 5～20g and the aluminum oxide powder of 60～120g, and under 15～40 ℃ of temperature, mixes and make.
Another kind of microwave curing type caking agent of the present invention is in the phosphate dihydrogen aluminum solution of 100ml, to add the resol of 300～450ml and the modified filler of 200～250g, and under 15～40 ℃ of temperature, mixes and make.
Preparing method below the phosphate dihydrogen aluminum solution that uses adopts is: (A) phosphoric acid solution with 85wt% adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt%; (B) phosphoric acid solution with 60wt% is heated to 110～120 ℃, and in heat-processed, adds aluminium-hydroxide powder, is cooled to 15～40 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; The pH value of the phosphate dihydrogen aluminum solution that makes is 1～2, and density is 1.47～1.48g/cm
3Consumption: in the phosphoric acid solution of the 60wt% of 100ml, add 5～20g aluminium-hydroxide powder.
It is following that the microwave curing type caking agent that adopts the present invention to make carries out substrate solidified method:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 10～30 minutes afterwash; At storing temperature is in 50 ℃～70 ℃ the baking oven after dry 5～30 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 1～3 hour under 20 ℃～35 ℃ temperature; Place on the rotary-tray 7 of anti-microwave leakage metal inner cavity 3 of microwave reactor; Shut sliding door 5; Through control panel 1 applying frequency 2450MHz is set, output rating is 528W (middle-grade); Carrying out microwave curing under the microwave radiation of waveguide mouth 2 outgoing after 5～30 minutes; Take out, obtain solidifying substrate; During microwave curing, the operator can observe solidification process through looking screen window 4.
Step 3: the curing substrate that step 2 is made is warming up to 600～1200 ℃ with the temperature rise rate of 5～10 ℃/min and carries out high-temperature heat treatment after 2 hours, and cooling obtains microwave curing substrate 6.
In order to detect the tensile shear strength of bonding mera, survey the tensile shear strength under its room temperature according to GB (GB/T7124-2008/ISO 4587:2003) in the present invention.
The present invention utilizes microwave irradiation effect, has realized the fast setting of caking agent, has saved set time greatly, and easy enforcement simple to operate; In addition, reduced the glue-line thermograde, made curing more even.Can be used for microwave radiation curing caking agent among the present invention and be applicable to the bonding of pottery, graphite, plastics, glass, Resins, epoxy, carbon/carbon compound material etc.
Description of drawings
The synoptic diagram of the microwave reactor that Fig. 1 uses when being curing.
Embodiment
To combine embodiment and accompanying drawing that the present invention is done further explanation below.
A kind of microwave curing type caking agent of the present invention is in the phosphate dihydrogen aluminum solution of 100ml, to add the solidifying agent of 5～20g and the aluminum oxide powder of 60～120g, and under 15～40 ℃ of temperature, mixes and make.
In the present invention, the preparation method below the phosphate dihydrogen aluminum solution of use adopts is: (A) phosphoric acid solution with 85wt% (mass percent concentration) adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt% (mass percent concentration); (B) phosphoric acid solution with 60wt% (mass percent concentration) is heated to 110～120 ℃, and in heat-processed, adds aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm), is cooled to 15～40 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; The pH value of the phosphate dihydrogen aluminum solution that makes is 1～2, and density is 1.47～1.48g/cm
3Consumption: in the phosphoric acid solution of the 60wt% of 100ml (mass percent concentration), add 5～20g aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm).In the present invention, in the phosphoric acid solution of heating, add aluminium-hydroxide powder at leisure the pH value of adjustment phosphate dihydrogen aluminum solution and the effect of viscosity are arranged.
In the present invention, solidifying agent is a granularity less than the magnesia powder of 50 μ m, granularity less than the oxide powder and zinc of 50 μ m, granularity less than the brown iron oxide of 50 μ m and granularity less than one or more the compound in the zirconia powder of 50 μ m.Add the Natural manganese dioxide of 0～1.5g, the zinc oxide of 5.0～9g, the ferric oxide of 0～1.5g and the zirconium white of 0～8g in the phosphate dihydrogen aluminum solution of consumption: 100ml.
In the present invention, the granularity of said aluminum oxide powder is less than 50 μ m.
Another kind of microwave curing type caking agent of the present invention is in the phosphate dihydrogen aluminum solution of 100ml, to add the resol of 300～450ml and the modified filler of 200～250g, and under 15～40 ℃ of temperature, mixes and make.
In the present invention, the preparation method below the phosphate dihydrogen aluminum solution of use adopts is: (A) phosphoric acid solution with 85wt% (mass percent concentration) adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt% (mass percent concentration); (B) phosphoric acid solution with 60wt% (mass percent concentration) is heated to 110～120 ℃, and in heat-processed, adds aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm), is cooled to 15～40 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; The pH value of the phosphate dihydrogen aluminum solution that makes is 1～2, and density is 1.47～1.48g/cm
3Consumption: in the phosphoric acid solution of the 60wt% of 100ml (mass percent concentration), add 5～20g aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm).
In the present invention, resol is that solid content is 80 ± 3%, and free phenol is smaller or equal to 21%, and the carbon yield behind the high temperature carbonization is more than or equal to 45% resol.
In the present invention, one of modified filler is that granularity is the boron carbide particulate of 2.5～3.5 μ m, and norbide purity is more than or equal to 90%.
In the present invention, two of modified filler is powder mixs of boron carbide particulate and SiO 2 powder, and the mass ratio of boron carbide particulate and SiO 2 powder is 5: 1～1.5.The granularity of boron carbide particulate is that 2.5～3.5 μ m, purity are more than or equal to 90%; The granularity of SiO 2 powder is that 50 ± 5nm, purity are more than or equal to 95%.
Referring to shown in Figure 1, among the figure view that microwave reactor is opened.Label among the figure: 1 control panel, 2 waveguide mouths, 3 anti-microwave leakage metal inner cavities, 4 are looked screen window, 5 sliding doors, 6 microwave curing substrates, 7 rotary-trays.
It is following that the microwave curing type caking agent that adopts the present invention to make carries out substrate solidified method:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 10～30 minutes afterwash; At storing temperature is in 50 ℃～70 ℃ the baking oven after dry 5～30 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 1～3 hour under 20 ℃～35 ℃ temperature; Place on the rotary-tray 7 of anti-microwave leakage metal inner cavity 3 of microwave reactor; Shut sliding door 5; Through control panel 1 applying frequency 2450MHz is set, output rating is 528W (middle-grade); Carrying out microwave curing under the microwave radiation of waveguide mouth 2 outgoing after 5～30 minutes; Take out, obtain solidifying substrate; During microwave curing, the operator can observe solidification process through looking screen window 4.
Step 3: the curing substrate that step 2 is made is warming up to 600～1200 ℃ with the temperature rise rate of 5～10 ℃/min and carries out high-temperature heat treatment after 2 hours, and cooling obtains bonding mera (being microwave curing substrate 6).
In order to detect the tensile shear strength of bonding mera, survey the tensile shear strength under its room temperature according to GB (GB/T7124-2008/ISO 4587:2003) in the present invention.
The microwave curing type caking agent of system embodiment 1; Be magnesium oxide powder (granularity is less than 50 μ m), the Zinc oxide powder (granularity is less than 50 μ m) of 6g and the aluminum oxide powder (granularity is less than 50 μ m) of 120g that in the phosphate dihydrogen aluminum solution of 100ml, adds 1.5g, and under 30 ℃ of temperature, mix and make.
Being prepared as of phosphate dihydrogen aluminum solution: (A) phosphoric acid solution with 85wt% (mass percent concentration) adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt% (mass percent concentration); (B) phosphoric acid solution with 60wt% (mass percent concentration) is heated to 120 ℃, and in heat-processed, adds aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm), is cooled to 20 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; In the phosphoric acid solution of the 60wt% of 100ml (mass percent concentration), add the 12g aluminium-hydroxide powder.The pH value of the phosphate dihydrogen aluminum solution that makes is 1.5, and density is 1.48g/cm
3
It is bonding with embodiment 1 caking agent two alumina ceramic substrates (A substrate and B substrate) to be carried out gluing:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 10 minutes afterwash; At storing temperature is in 60 ℃ the baking oven after dry 10 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 1.5 hours under 35 ℃ of temperature; Place in the microwave reactor, applying frequency 2450MHz is set, output rating is 528W (middle-grade), under microwave radiation, carries out microwave curing after 20 minutes, take out, obtain solidifying substrate;
Step 3: the curing substrate that step 2 is made is warming up to 600 ℃, 800 ℃, 1000 ℃, 1200 ℃ respectively with the temperature rise rate of 8 ℃/min and carries out high-temperature heat treatment after 2 hours; Cooling; Take out; And surveying the tensile shear strength under its room temperature according to GB (GB/T7124-2008/ISO 4587:2003), the result sees table 1.
The microwave curing type caking agent of system embodiment 2; Be Zirconium oxide powder (granularity is less than 50 μ m), the Zinc oxide powder (granularity is less than 50 μ m) of 7.5g and the aluminum oxide powder (granularity is less than 50 μ m) of 60g that in the phosphate dihydrogen aluminum solution of 100ml, adds 7.5g, and under 40 ℃ of temperature, mix and make.
Being prepared as of phosphate dihydrogen aluminum solution: (A) phosphoric acid solution with 85wt% (mass percent concentration) adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt% (mass percent concentration); (B) phosphoric acid solution with 60wt% (mass percent concentration) is heated to 110 ℃, and in heat-processed, adds aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm), is cooled to 30 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; The pH value of the phosphate dihydrogen aluminum solution that makes is 2, and density is 1.47g/cm
3Consumption: in the phosphoric acid solution of the 60wt% of 100ml (mass percent concentration), add the 20g aluminium-hydroxide powder.
It is bonding with embodiment 2 caking agents two graphite substrates (A substrate and B substrate) to be carried out gluing:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 30 minutes afterwash; At storing temperature is in 50 ℃ the baking oven after dry 30 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 3 hours under 25 ℃ of temperature; Place in the microwave reactor, applying frequency 2450MHz is set, output rating is 528W (middle-grade), under microwave radiation, carries out microwave curing after 12 minutes, take out, obtain solidifying substrate;
Step 3: the curing substrate that step 2 is made is elevated to the temperature rise rate of 10 ℃/min in 600 ℃, 800 ℃, 1000 ℃, 1200 ℃ the hot environment of differing temps; Kept 2 hours, cooling is taken out; And surveying the tensile shear strength under its room temperature, the result sees table 1.
The microwave curing type caking agent of system embodiment 3; Be the aluminum oxide powder (granularity is less than 50 μ m) of Zinc oxide powder (granularity is less than 50 μ m), 1.5g croci (granularity is less than 50 μ m) and the 60g of the Zirconium oxide powder (granularity is less than 50 μ m) that in the phosphate dihydrogen aluminum solution of 100ml, adds 0.5g, 6.1g, and under 25 ℃ of temperature, mix and make.
Being prepared as of phosphate dihydrogen aluminum solution: (A) phosphoric acid solution with 85wt% (mass percent concentration) adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt% (mass percent concentration); (B) phosphoric acid solution with 60wt% (mass percent concentration) is heated to 115 ℃, and in heat-processed, adds aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm), is cooled to 15 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; The pH value of the phosphate dihydrogen aluminum solution that makes is 1, and density is 1.47g/cm
3Consumption: in the phosphoric acid solution of the 60wt% of 100ml (mass percent concentration), add 16g aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm).
It is bonding with embodiment 3 caking agents two alumina ceramic substrates (A substrate and B substrate) to be carried out gluing:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 15 minutes afterwash; At storing temperature is in 50 ℃ the baking oven after dry 10 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 2 hours under 25 ℃ of temperature; Place in the microwave reactor, applying frequency 2450MHz is set, output rating is 528W (middle-grade), under microwave radiation, carries out microwave curing after 10 minutes, take out, obtain solidifying substrate;
Step 3: the curing substrate that step 2 is made is elevated to the temperature rise rate of 5 ℃/min in 600 ℃, 800 ℃, 1000 ℃, 1200 ℃ the hot environment of differing temps; Kept 2 hours, cooling is taken out; And surveying the tensile shear strength under its room temperature, the result sees table 1.
System embodiment 4 microwave curing type caking agents are in the phosphate dihydrogen aluminum solution of 100ml, to add the resol of 400ml and the norbide (granularity is 3.5 μ m) of 210g, and under 30 ℃ of temperature, mix and make.
Being prepared as of phosphate dihydrogen aluminum solution: (A) phosphoric acid solution with 85wt% (mass percent concentration) adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt% (mass percent concentration); (B) phosphoric acid solution with 60wt% (mass percent concentration) is heated to 110 ℃, and in heat-processed, adds aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm), is cooled to 22 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; The pH value of the phosphate dihydrogen aluminum solution that makes is 2, and density is 1.48g/cm
3Consumption: in the phosphoric acid solution of the 60wt% of 100ml (mass percent concentration), add 12g aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm).
It is bonding with embodiment 4 caking agents two alumina ceramic substrates (A substrate and B substrate) to be carried out gluing:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 30 minutes afterwash; At storing temperature is in 50 ℃ the baking oven after dry 30 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 1.5 hours under 30 ℃ of temperature; Place in the microwave reactor, applying frequency 2450MHz is set, output rating is 528W (middle-grade), under microwave radiation, carries out microwave curing after 18 minutes, take out, obtain solidifying substrate;
Step 3: the curing substrate that step 2 is made is elevated to the temperature rise rate of 10 ℃/min in 600 ℃, 800 ℃, 1000 ℃, 1200 ℃ the hot environment of differing temps; Kept 2 hours, cooling is taken out; And surveying the tensile shear strength under its room temperature, the result sees table 1.
Being prepared as of phosphate dihydrogen aluminum solution: (A) phosphoric acid solution with 85wt% (mass percent concentration) adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt% (mass percent concentration); (B) phosphoric acid solution with 60wt% (mass percent concentration) is heated to 120 ℃, and in heat-processed, adds aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm), is cooled to 30 ℃, gets the phosphate dihydrogen aluminum solution of transparent homogeneous; The pH value of the phosphate dihydrogen aluminum solution that makes is 1.5, and density is 1.48g/cm
3Consumption: in the phosphoric acid solution of the 60wt% of 100ml (mass percent concentration), add 7g aluminium-hydroxide powder (granularity of aluminium-hydroxide powder is less than 50nm).
It is bonding with embodiment 5 caking agents two alumina ceramic substrates (A substrate and B substrate) to be carried out gluing:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 10 minutes afterwash; At storing temperature is in 60 ℃ the baking oven after dry 10 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 1.5 hours under 35 ℃ of temperature; Place in the microwave reactor, applying frequency 2450MHz is set, output rating is 528W (middle-grade), under microwave radiation, carries out microwave curing after 15 minutes, take out, obtain solidifying substrate;
Step 3: the curing substrate that step 2 is made is elevated to the temperature rise rate of 5 ℃/min in 600 ℃, 800 ℃, 1000 ℃, 1200 ℃ the hot environment of differing temps; Kept 2 hours, cooling is taken out; And surveying the tensile shear strength under its room temperature, the result sees table 1.
The room temperature shearing resistance of the bonding sample of table 1 after heat treatments at different
From table 1, can find out; It is bonding that the microwave curing type caking agent of the present invention of employing heterogeneity carries out substrate; Substrate after bonding still has higher tensile shear strength behind 5～20 minutes microwave curings and under different heat treatment temperature (600 ℃, 800 ℃, 1000 ℃, 1200 ℃).
Claims (10)
1. microwave curing type caking agent, it is characterized in that: said microwave curing type caking agent is in the phosphate dihydrogen aluminum solution of 100ml, to add the solidifying agent of 5～20g and the aluminum oxide powder of 60～120g, under 15～40 ℃ of temperature, mixes then to make.
2. microwave curing type caking agent according to claim 1; It is characterized in that: said microwave curing type caking agent is in the phosphate dihydrogen aluminum solution of 100ml, to add the resol of 300～450ml and the modified filler of 200～250g, under 15～40 ℃ of temperature, mixes then to make.
3. microwave curing type caking agent according to claim 1 and 2 is characterized in that being prepared as of phosphate dihydrogen aluminum solution: (A) phosphoric acid solution with 85wt% adds the phosphoric acid solution that the proper amount of deionized water adjustment obtains 60wt%; (B) in the phosphoric acid solution of 60wt%, add the aluminium-hydroxide powder of granularity, mix post-heating to 110～120 ℃, be cooled to 15～40 ℃ then less than 50nm, the pH value of transparent homogeneous is 1～2, density is 1.47～1.48g/cm
3Phosphate dihydrogen aluminum solution;
Consumption: in the mass percent concentration of 100ml is the phosphoric acid solution of 60wt%, add 5～20g aluminium-hydroxide powder.
4. microwave curing type caking agent according to claim 1 is characterized in that: said solidifying agent is a granularity less than the magnesia powder of 50 μ m, granularity less than the oxide powder and zinc of 50 μ m, granularity less than the brown iron oxide of 50 μ m and granularity less than one or more the compound in the zirconia powder of 50 μ m.Add the Natural manganese dioxide of 0～1.5g, the zinc oxide of 5.0～9g, the ferric oxide of 0～1.5g and the zirconium white of 0～8g in the phosphate dihydrogen aluminum solution of consumption: 100ml.
5. microwave curing type caking agent according to claim 1 is characterized in that: the granularity of said aluminum oxide powder is less than 50 μ m.
6. microwave curing type caking agent according to claim 2 is characterized in that: said resol is that solid content is 80 ± 3%, and free phenol is smaller or equal to 21%, and the carbon yield behind the high temperature carbonization is more than or equal to 45% resol.
7. microwave curing type caking agent according to claim 2 is characterized in that: said modified filler is that granularity is the boron carbide particulate of 2.5～3.5 μ m, and norbide purity is more than or equal to 90%.
8. microwave curing type caking agent according to claim 2 is characterized in that: said modified filler is the powder mix of boron carbide particulate and SiO 2 powder, and the mass ratio of boron carbide particulate and SiO 2 powder is 5: 1～1.5.The granularity of boron carbide particulate is that 2.5～3.5 μ m, purity are more than or equal to 90%; The granularity of SiO 2 powder is that 50 ± 5nm, purity are more than or equal to 95%.
9. method that adopts microwave curing type caking agent as claimed in claim 1 or 2 to carry out microwave curing is characterized in that including the following step:
Step 1: the bonding plane of treating of A substrate and B substrate is cleaned; And in 10% sodium hydroxide solution, soak several 10～30 minutes afterwash; At storing temperature is in 50 ℃～70 ℃ the baking oven after dry 5～30 minutes; Take out; At the coating microwave curing type caking agent on the bonding plane of treating of A substrate, obtain the A intermediate then; The coating microwave curing type caking agent on the bonding plane of treating at the B substrate obtains the B intermediate; At last the A intermediate is docked with the bonding plane of treating of B intermediate, obtain docking substrate;
Step 2: after the butt joint substrate that step 1 is made places and hangs 1～3 hour under 20 ℃～35 ℃ temperature; Place on the rotary-tray 7 of anti-microwave leakage metal inner cavity 3 of microwave reactor; Shut sliding door 5; Through control panel 1 applying frequency 2450MHz is set, output rating is 528W (middle-grade); Carrying out microwave curing under the microwave radiation of waveguide mouth 2 outgoing after 5～30 minutes; Take out, obtain solidifying substrate; During microwave curing, the operator can observe solidification process through looking screen window 4;
Step 3: the curing substrate that step 2 is made is warming up to 600～1200 ℃ with the temperature rise rate of 5～10 ℃/min and carries out high-temperature heat treatment after 2 hours, and cooling obtains microwave curing substrate 6;
In order to detect the tensile shear strength of bonding mera, survey the tensile shear strength under its room temperature according to GB (GB/T7124-2008/ISO 4587:2003) in the present invention.
10. microwave curing type caking agent according to claim 1 and 2 is characterized in that: microwave radiation curing caking agent is applicable to the bonding of pottery, graphite, plastics, glass, Resins, epoxy, carbon/carbon compound material etc.
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| CN110217770A (en) * | 2019-06-18 | 2019-09-10 | 佛山市德方纳米科技有限公司 | The preparation method of aluminium dihydrogen phosphate |
| CN110484158A (en) * | 2019-08-12 | 2019-11-22 | 江南大学 | A kind of bonding layer based on epoxy adhesive |
| CN111892045A (en) * | 2019-05-05 | 2020-11-06 | 深圳光启岗达创新科技有限公司 | Composite material, preparation method and application thereof |
| CN114654607A (en) * | 2022-03-28 | 2022-06-24 | 广东高景太阳能科技有限公司 | Method for quickly sticking silicon rod to crystal |
| CN115416376A (en) * | 2022-09-29 | 2022-12-02 | 上海昌海船舶技术有限公司 | High-temperature-resistant high-strength heat-insulating cushion block and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805489A (en) * | 2010-04-27 | 2010-08-18 | 黑龙江省科学院石油化学研究院 | Low volatile and thermostable phenolic resin and fabrication method thereof |
-
2011
- 2011-06-16 CN CN 201110162302 patent/CN102352190B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805489A (en) * | 2010-04-27 | 2010-08-18 | 黑龙江省科学院石油化学研究院 | Low volatile and thermostable phenolic resin and fabrication method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库 工程科技I辑》 20080515 刘继江 "磷酸盐胶黏剂的制备及性能研究" B016-104 1,3,4,5,10 第2008卷, 第5期 * |
| 刘继江: ""磷酸盐胶黏剂的制备及性能研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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| CN110217770A (en) * | 2019-06-18 | 2019-09-10 | 佛山市德方纳米科技有限公司 | The preparation method of aluminium dihydrogen phosphate |
| CN110217770B (en) * | 2019-06-18 | 2021-08-13 | 佛山市德方纳米科技有限公司 | Preparation method of aluminum dihydrogen phosphate |
| CN110484158A (en) * | 2019-08-12 | 2019-11-22 | 江南大学 | A kind of bonding layer based on epoxy adhesive |
| CN110484158B (en) * | 2019-08-12 | 2021-09-07 | 江南大学 | Adhesive layer based on epoxy adhesive |
| CN114654607A (en) * | 2022-03-28 | 2022-06-24 | 广东高景太阳能科技有限公司 | Method for quickly sticking silicon rod to crystal |
| CN115416376A (en) * | 2022-09-29 | 2022-12-02 | 上海昌海船舶技术有限公司 | High-temperature-resistant high-strength heat-insulating cushion block and preparation method thereof |
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