CN108913039A - A method of preparing multicomponent modified inorganic phosphoric acid aluminium salt high-temperature Resistance Adhesives - Google Patents
A method of preparing multicomponent modified inorganic phosphoric acid aluminium salt high-temperature Resistance Adhesives Download PDFInfo
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- CN108913039A CN108913039A CN201810541309.XA CN201810541309A CN108913039A CN 108913039 A CN108913039 A CN 108913039A CN 201810541309 A CN201810541309 A CN 201810541309A CN 108913039 A CN108913039 A CN 108913039A
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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
A method of preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives comprising superfine metal silicon powder, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide and oxidation copper fine powder are mixed into mixture；By mixture ball milling；Aluminium hydroxide fine powder is added into phosphoric acid,diluted, mixed solution is made；It feeds the mixture into and forms sol solution in mixed solution；Continue to stir sol solution under vacuum conditions to exclude residual gas in sol solution.Advantage of the present invention：Adhesive is used for the connection and repairing, the thermal insulation protection of all kinds of high temperature resistant engineering material surfaces and anti-oxidation protection, the installation of thermal protection system and connection, the sealing at gap position etc. of all kinds of high temperature resistant engineering materials under hot environment.The special high temperature-resistant adhesive for being directed to high temperature resistant engineering structural material not of the same race can be modulated by the ingredient and ratio of additive not of the same race inside change adhesive.Effective connection suitable for ceramics, ceramic matric composite, high-temperature alloy in hot environment.
Description
Technical field
The invention belongs to the technical field of material of heat-insulated, sealing, repairing and interconnection technique, more particularly to a kind of system
The method of standby multicomponent modified inorganic phosphoric acid aluminium salt high-temperature Resistance Adhesives.
Background technique
High-temperature Resistance Adhesives are either in the preparation of high temperature resistant component, the installation of thermal protection sealing system, or resistance to
It is all had a decisive role in terms of the repairing of high temperature components.To meet high-temperature applications to the need of high-temperature Resistance Adhesives
Ask, quickly push the development in the fields such as China's aerospace cause and nuclear engineering, production preparation efficiently, it is green, general resistance to
The great strategic importance of high temperature adhesive.
Phosphalugel adhesive has that high temperature resistance is excellent, normal temperature cure, cure shrinkage are small, excellent durability, valence
The advantages that lattice are cheap, pollution-free, preparation process is simple, with short production cycle, easy to use is a kind of widely apply and with development
The adhesive of future.But traditional phosphalugel adhesive is mostly low-aluminium high phosphorous, and since additive types are few, such glue
Glutinous agent can generate volume contraction during the high temperature treatment process, cause adhesion strength relatively low.Simultaneously as this kind of adhesive is in high temperature
The heatproof phase type of lower generation is single, and bonding object applicatory is limited, i.e. the versatility of adhesive is lower.For example, industrial
Aluminium dihydrogen phosphate Al (the H that field is commonly used2PO4)3It is changed into AlPO at high temperature4Ceramic phase.Due to adding for no modified filler
Add, compactness is extremely low after heat treatment for the adhesive, adhesive layer product single (being only applicable to oxide ceramics), adhesion strength not
It is high.Therefore, it improves the high temperature cohesive strength of phosphalugel adhesive and expands its versatility and be still urgent problem.It is logical
Phosphorus aluminum ratio example is overregulated, adds poly modified additive, preparation is common to the novel resistance to of oxide and non-oxidized substance and alloy
High temperature inorganic phosphalugel adhesive is very significant.
Summary of the invention
To solve the above-mentioned problems, to prepare multicomponent modified inorganic phosphoric acid aluminium salt resistance to the purpose of the present invention is to provide a kind of
The method of high temperature adhesive.
In order to achieve the above object, the method provided by the invention for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives include by
The following steps that sequence carries out：
(1) by as the superfine metal silicon powder of raw material, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide and
Copper fine powder is aoxidized according to 6~7.8:0~2.7:1~3.2:1~2.3:0~1 mass ratio is uniformly mixed and mixture is made；
(2) said mixture is poured into ball milling 2h~3h in ball mill；
(3) concentrated phosphoric acid that mass concentration is 85% is added in vinyon agitator tank, distilled water is then added will
Concentrated phosphoric acid is diluted to the phosphoric acid,diluted that mass concentration is 60%, and then phosphoric acid,diluted is put into water-bath and is heated to 80~85 DEG C and protects
Warm 10min；
(4) heating lateral dominance in side stirs at low speed the dilute hydrochloric acid in water-bath with mechanical agitator, while according to 1:1~
1:0.85 aluminium phosphorus molar ratio is slowly added to aluminium hydroxide fine powder into phosphoric acid,diluted, continues high low speed alternate agitation and mixing is made
Solution, until the viscosity of mixed solution reaches 1300-1500mPas；
It (5) is 1 according to the mass ratio of additive and mixed solution:5~1:3 is slow by manufactured mixture in step (2)
Ground, which is added in step (4), forms sol solution in manufactured mixed solution, continue moderate-speed mixer sol solution, make the viscosity of sol solution
Remain to 2300-2500mPas；
(6) pH value of manufactured sol solution in step (5) is adjusted to using superfine aluminium power>7；
(7) continue to stir sol solution under vacuum conditions finally to exclude the residual gas in sol solution, institute is thus made
The inorganic phosphate aluminium salt high-temperature Resistance Adhesives stated.
Superfine metal silicon powder, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide in the step (1)
Particle size be respectively less than 10 μm.
Oxidation copper fine powder in the step (1) is that Industrial Analysis is pure.
The revolving speed of ball mill is 4000~5000r/min in the step (2).
The aluminium hydroxide in concentrated phosphoric acid and step (4) in the step (3) is that Industrial Analysis is pure.
The method provided by the invention for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives has the following advantages that：Prepared glue
Glutinous agent is a kind of low-phosphorous type of high alumina, the novel fire resistant silicon inorganic phosphate aluminium salt gluing that additive types are more, high temperature resistant is mutually polynary
Agent has the outstanding feature of " room temperature curing in post-processing, room temperature to 1500 DEG C of temperature ranges without being all suitable for ", is common to air
And for the bonding of oxide and non-oxide ceramics, ceramic matric composite and part high-temperature alloy under oxygen-free environment.
Wherein the particle of Ultrafine Mullite powder and ultra fine silicon carbide has excellent high temperature resistant and high-strength characteristic.By adding metal
Silicon powder and boron carbide powder, the contraction hole that this adhesive generates in vivo after high-temperature process significantly reduce；By adding a variety of add
Add agent, this adhesive has a variety of high temperature resistant phase components, including mullite, aluminum phosphate, silicon carbide, high temperature boron after high-temperature process
Silicate glass and high temperature alloy etc.；This adhesive can bond various refractory ceramicses, ceramic matric composite and high temperature
Alloy, including carbon carbon composite, silicon carbide ceramics and silicon carbide fiber reinforced ceramic composite, aluminium oxide ceramics, Mo Lai
Feldspar, titanium alloy etc materials.Mechanical test shows that adhesion strength of the adhesive after high-temperature process significantly improves.This gluing
Agent be mainly used for the connection Yu repairing of all kinds of high temperature resistant engineering materials under hot environment, all kinds of high temperature resistant engineering material surfaces every
Thermal protection and anti-oxidation protection, the installation of thermal protection system and connection, the sealing at gap position etc..It can be by changing in adhesive
The ingredient and ratio of portion's additive not of the same race modulate the special high temperature-resistant glue for being directed to high temperature resistant engineering structural material not of the same race
Glutinous agent.This adhesive is applicable to effective connection of ceramics, ceramic matric composite, high-temperature alloy in hot environment.
Detailed description of the invention
Fig. 1 is shearing of the bonded mullite ceramic bonding piece of adhesive of the preparation of embodiment 1 after treatment of different temperature
Intensity curve；
Fig. 2 be the bonded mullite ceramic bonding piece of adhesive for preparing of embodiment 1 at 1300 DEG C treated adhesive surface
Scanning electron microscope diagram piece；
Fig. 3 is shearing of the adhesive institute bonded silicon carbide bonding piece of the preparation of embodiment 2 after treatment of different temperature
Intensity curve；
Fig. 4 be the adhesive institute bonded silicon carbide bonding piece for preparing of embodiment 2 at 1300 DEG C treated adhesive surface
Scanning electron microscope diagram piece；
Fig. 5 is bonded carbon carbon composite bonding piece the cutting after treatment of different temperature of adhesive prepared by embodiment 3
Shearing stress curve；
Fig. 6 be embodiment 3 prepare the bonded carbon carbon composite bonding piece of adhesive at 1300 DEG C treated bond
Surface scan electron microscope picture；
Fig. 7 is shearing of the bonded titanium alloy material bonding piece of adhesive of the preparation of embodiment 4 after treatment of different temperature
Intensity curve；
Fig. 8 is that treated that adhesive surface is swept at 700 DEG C for the bonded titanium alloy material bonding piece of adhesive for preparing of embodiment 4
Retouch electron microscope picture.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1 (adhesive that preparation is suitable for mullite ceramic)
The method provided in this embodiment for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives include carry out in order it is following
Step：
(1) by as the superfine metal silicon powder of raw material, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide and
Copper fine powder is aoxidized according to 7.8:2.7:1.5:1:0 mass ratio is uniformly mixed and mixture is made；Superfine metal silicon powder, it is ultra-fine not
Come mountain flour, superfine boron carbide powder, ultra fine silicon carbide particle size be respectively less than 10 μm.
(2) said mixture is poured into ball mill, the ball milling 2h under the revolving speed of 4000r/min；
(3) concentrated phosphoric acid that mass concentration is 85% is added in vinyon agitator tank, distilled water is then added will
Concentrated phosphoric acid is diluted to the phosphoric acid,diluted that mass concentration is 60%, and then phosphoric acid,diluted is put into water-bath and is heated to 80 DEG C and keeps the temperature
10min；
(4) heating lateral dominance in side stirs at low speed the dilute hydrochloric acid in water-bath with mechanical agitator, while according to 1:1
Aluminium phosphorus molar ratio is slowly added to aluminium hydroxide fine powder into phosphoric acid,diluted, continues high low speed alternate agitation and mixed solution is made, directly
Viscosity to mixed solution reaches 1300mPas；
It (5) is 1 according to the mass ratio of additive and mixed solution:5 are slowly added into manufactured mixture in step (2)
Sol solution is formed in manufactured mixed solution in step (4), continues moderate-speed mixer sol solution, remains to the viscosity of sol solution
2300mPa·s；
(6) pH value of manufactured sol solution in step (5) is adjusted to using superfine aluminium power>7；
(7) continue to stir sol solution under vacuum conditions finally to exclude the residual gas in sol solution, institute is thus made
The inorganic phosphate aluminium salt high-temperature Resistance Adhesives stated.
Bonding experiment is carried out below with inorganic phosphate aluminium salt high-temperature Resistance Adhesives made of the present embodiment：First by testing
Mullite ceramic piece (40 × 10 × 5mm) after polishing grinding and cleaning-drying is laid in the smooth glass having no time by personnel
It on plate, bonds and places up, then medication spoon is by a certain amount of inorganic phosphate aluminium salt high temperature resistant gluing provided in this embodiment
Agent is laid in as far as possible on each adhesive surface, and bond area is 20 × 10mm, later with spreader by the adhesive of each adhesive surface
Thickness control is at 200 μm.Then the adhesive surface of two pieces of mullite ceramic pieces is bonded together and bonding piece is made.It will glue later
Part standing overnight at normal temperature is tied, adhesive solidification is waited, then handles bonding piece 1h at different temperatures, finally using omnipotent
Testing experiment machine tests the shear stress of bonding piece to assess the adhesive property of adhesive.
The adhesion strength of adhesive after treatment of different temperature is as shown in Figure 1.Through 1300 DEG C of treated mullite potteries
The scanning electron microscope diagram piece of the adhesive bonded part of porcelain bonding piece is as shown in Figure 2.
Embodiment 2 (adhesive that preparation is suitable for silicon carbide ceramics)
The method provided in this embodiment for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives include carry out in order it is following
Step：
(1) by as the superfine metal silicon powder of raw material, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide and
Copper fine powder is aoxidized according to 6:1:2.4:2.3:0 mass ratio is uniformly mixed and mixture is made；Superfine metal silicon powder, it is ultra-fine not come
Mountain flour, superfine boron carbide powder, ultra fine silicon carbide particle size be respectively less than 10 μm.
(2) said mixture is poured into ball mill, the ball milling 2h under the revolving speed of 4500r/min；
(3) concentrated phosphoric acid that mass concentration is 85% is added in vinyon agitator tank, distilled water is then added will
Concentrated phosphoric acid is diluted to the phosphoric acid,diluted that mass concentration is 60%, and then phosphoric acid,diluted is put into water-bath and is heated to 80 DEG C and keeps the temperature
10min；
(4) heating lateral dominance in side stirs at low speed the dilute hydrochloric acid in water-bath with mechanical agitator, while according to 1:
0.95 aluminium phosphorus molar ratio is slowly added to aluminium hydroxide fine powder into phosphoric acid,diluted, continue high low speed alternate agitation and be made mixing it is molten
Liquid, until the viscosity of mixed solution reaches 1400mPas；
It (5) is 1 according to the mass ratio of additive and mixed solution:4 are slowly added into manufactured mixture in step (2)
Sol solution is formed in manufactured mixed solution in step (4), continues moderate-speed mixer sol solution, remains to the viscosity of sol solution
2400mPa·s；
(6) pH value of manufactured sol solution in step (5) is adjusted to using superfine aluminium power>7；
(7) continue to stir sol solution under vacuum conditions finally to exclude the residual gas in sol solution, institute is thus made
The inorganic phosphate aluminium salt high-temperature Resistance Adhesives stated.
Bonding experiment is carried out below with inorganic phosphate aluminium salt high-temperature Resistance Adhesives made of the present embodiment：First by testing
Silicon carbide ceramics piece after polishing grinding and cleaning-drying is laid on the smooth glass plate having no time by personnel, adhesive surface court
Upper placement, then a certain amount of inorganic phosphate aluminium salt high-temperature Resistance Adhesives provided in this embodiment are laid in respectively by medication spoon as far as possible
On a adhesive surface, bond area be 20 × 10mm, later with spreader by the adhesive thickness control of each adhesive surface in 200 μ
m.Then the adhesive surface of two pieces of silicon carbide ceramics pieces is bonded together and bonding piece is made.Later by bonding piece at normal temperature every
Night stands, and waits adhesive solidification, then handles bonding piece 1h at different temperatures, is finally tested using omnipotent testing experiment machine
The shear stress of bonding piece assesses the adhesive property of adhesive.
The adhesion strength of adhesive after treatment of different temperature is as shown in Figure 3.Through 1300 DEG C of treated silicon carbide potteries
The scanning electron microscope diagram piece of the adhesive bonded part of porcelain bonding piece is as shown in Figure 4.
Embodiment 3 (adhesive that preparation is suitable for carbon carbon composite)
The method provided in this embodiment for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives include carry out in order it is following
Step：
(1) by as the superfine metal silicon powder of raw material, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide and
Copper fine powder is aoxidized according to 7.8:1:3.2:1:0 mass ratio is uniformly mixed and mixture is made；Superfine metal silicon powder, it is ultra-fine not come
Mountain flour, superfine boron carbide powder, ultra fine silicon carbide particle size be respectively less than 10 μm.
(2) said mixture is poured into ball mill, the ball milling 2.5h under the revolving speed of 4700r/min；
(3) concentrated phosphoric acid that mass concentration is 85% is added in vinyon agitator tank, distilled water is then added will
Concentrated phosphoric acid is diluted to the phosphoric acid,diluted that mass concentration is 60%, and then phosphoric acid,diluted is put into water-bath and is heated to 80 DEG C and keeps the temperature
10min；
(4) heating lateral dominance in side stirs at low speed the dilute hydrochloric acid in water-bath with mechanical agitator, while according to 1:
0.85 aluminium phosphorus molar ratio is slowly added to aluminium hydroxide fine powder into phosphoric acid,diluted, continue high low speed alternate agitation and be made mixing it is molten
Liquid, until the viscosity of mixed solution reaches 1350mPas；
It (5) is 1 according to the mass ratio of additive and mixed solution:3 are slowly added into manufactured mixture in step (2)
Sol solution is formed in manufactured mixed solution in step (4), continues moderate-speed mixer sol solution, remains to the viscosity of sol solution
2500mPa·s；
(6) pH value of manufactured sol solution in step (5) is adjusted to using superfine aluminium power>7；
(7) continue to stir sol solution under vacuum conditions finally to exclude the residual gas in sol solution, institute is thus made
The inorganic phosphate aluminium salt high-temperature Resistance Adhesives stated.
Bonding experiment is carried out below with inorganic phosphate aluminium salt high-temperature Resistance Adhesives made of the present embodiment：First by testing
Carbon carbon composite piece after polishing grinding and cleaning-drying is laid on the smooth glass plate having no time by personnel, adhesive surface
It places upward, then a certain amount of inorganic phosphate aluminium salt high-temperature Resistance Adhesives provided in this embodiment are laid in by medication spoon as far as possible
On each adhesive surface, bond area be 20 × 10mm, later with spreader by the adhesive thickness control of each adhesive surface 200
μm.Then the adhesive surface of two pieces of carbon carbon composite pieces is bonded together and bonding piece is made.Later by bonding piece in room temperature
Under standing overnight, wait adhesive solidification, then at different temperatures handle bonding piece 1h, finally utilize omnipotent testing experiment machine
The shear stress of bonding piece is tested to assess the adhesive property of adhesive.
The adhesion strength of adhesive after treatment of different temperature is as shown in Figure 5.Through 1300 DEG C, treated that carbon carbon is compound
The scanning electron microscope diagram piece of the adhesive bonded part of material bonding piece is as shown in Figure 6.
Embodiment 4 (adhesive that preparation is suitable for titanium alloy material)
The method provided in this embodiment for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives include carry out in order it is following
Step：
(1) by as the superfine metal silicon powder of raw material, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide and
Copper fine powder is aoxidized according to 7.8:0:2.4:1.5:1 mass ratio is uniformly mixed and mixture is made；Superfine metal silicon powder, it is ultra-fine not
Come mountain flour, superfine boron carbide powder, ultra fine silicon carbide particle size be respectively less than 10 μm.
(2) said mixture is poured into ball mill, the ball milling 3h under the revolving speed of 5000r/min；
(3) concentrated phosphoric acid that mass concentration is 85% is added in vinyon agitator tank, distilled water is then added will
Concentrated phosphoric acid is diluted to the phosphoric acid,diluted that mass concentration is 60%, and then phosphoric acid,diluted is put into water-bath and is heated to 80 DEG C and keeps the temperature
10min；
(4) heating lateral dominance in side stirs at low speed the dilute hydrochloric acid in water-bath with mechanical agitator, while according to 1:0.9
Aluminium phosphorus molar ratio aluminium hydroxide fine powder is slowly added into phosphoric acid,diluted, continue high low speed alternate agitation and mixed solution be made,
Until the viscosity of mixed solution reaches 1450mPas；
It (5) is 1 according to the mass ratio of additive and mixed solution:3 are slowly added into manufactured mixture in step (2)
Sol solution is formed in manufactured mixed solution in step (4), continues moderate-speed mixer sol solution, remains to the viscosity of sol solution
2500mPa·s；
(6) pH value of manufactured sol solution in step (5) is adjusted to using superfine aluminium power>7；
(7) continue to stir sol solution under vacuum conditions finally to exclude the residual gas in sol solution, institute is thus made
The inorganic phosphate aluminium salt high-temperature Resistance Adhesives stated.
Bonding experiment is carried out below with inorganic phosphate aluminium salt high-temperature Resistance Adhesives made of the present embodiment：First by testing
Titanium alloy piece after polishing grinding and cleaning-drying is laid on the smooth glass plate having no time by personnel, and bonding is put up
It sets, then a certain amount of inorganic phosphate aluminium salt high-temperature Resistance Adhesives provided in this embodiment are laid in each viscous by medication spoon as far as possible
In junction, bond area be 20 × 10mm, later with spreader by the adhesive thickness control of each adhesive surface at 200 μm.So
The adhesive surface of two pieces of titanium alloy pieces is bonded together afterwards and bonding piece is made.Later by bonding piece standing overnight at normal temperature,
Adhesive solidification is waited, then handles bonding piece 1h at different temperatures, finally tests bonding piece using omnipotent testing experiment machine
Shear stress assess the adhesive property of adhesive.
The adhesion strength of adhesive after treatment of different temperature is as shown in Figure 7.Through 700 DEG C of treated titanium alloy materials
The scanning electron microscope diagram piece of the adhesive bonded part of bonding piece is as shown in Figure 8.
The present invention is not limited to above example, can obtain difference by adjusting additive types, additive level etc.
The high-temperature Resistance Adhesives material of performance, those skilled in the art's announcement according to the present invention, for the improvement made of the present invention and
Modification all should be within protection scope of the present invention.
Each raw material cited by the present invention can realize the present invention, not be illustrated one by one herein.
Claims (5)
1. a kind of method for preparing multicomponent modified inorganic phosphoric acid aluminium salt high-temperature Resistance Adhesives, it is characterised in that：The method
Including the following steps carried out in order：
It (1) will be as the superfine metal silicon powder of raw material, Ultrafine Mullite powder, superfine boron carbide powder, ultra fine silicon carbide and oxidation
Copper fine powder is according to 6~7.8:0~2.7:1~3.2:1~2.3:0~1 mass ratio is uniformly mixed and mixture is made；
(2) said mixture is poured into ball milling 2h~3h in ball mill；
(3) concentrated phosphoric acid that mass concentration is 85% is added in vinyon agitator tank, distilled water is then added by dense phosphorus
Acid is diluted to the phosphoric acid,diluted that mass concentration is 60%, and then phosphoric acid,diluted is put into water-bath and is heated to 80~85 DEG C and keeps the temperature
10min；
(4) heating lateral dominance in side stirs at low speed the dilute hydrochloric acid in water-bath with mechanical agitator, while according to 1:1~1:
0.85 aluminium phosphorus molar ratio is slowly added to aluminium hydroxide fine powder into phosphoric acid,diluted, continue high low speed alternate agitation and be made mixing it is molten
Liquid, until the viscosity of mixed solution reaches 1300-1500mPas；
It (5) is 1 according to the mass ratio of additive and mixed solution:5~1:3 slowly add manufactured mixture in step (2)
Enter and form sol solution in manufactured mixed solution in step (4), continues moderate-speed mixer sol solution, keep the viscosity of sol solution
To 2300-2500mPas；
(6) pH value of manufactured sol solution in step (5) is adjusted to using superfine aluminium power>7；
(7) continue to stir sol solution under vacuum conditions finally to exclude the residual gas in sol solution, be thus made described
Inorganic phosphate aluminium salt high-temperature Resistance Adhesives.
2. the method according to claim 1 for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives, it is characterised in that：Described
Superfine metal silicon powder, Ultrafine Mullite powder in step (1), superfine boron carbide powder, the particle size of ultra fine silicon carbide are small
In 10 μm.
3. the method according to claim 1 for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives, it is characterised in that：Described
Oxidation copper fine powder in step (1) is that Industrial Analysis is pure.
4. the method according to claim 1 for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives, it is characterised in that：Described
The revolving speed of ball mill is 4000~5000r/min in step (2).
5. the method according to claim 1 for preparing inorganic phosphate aluminium salt high-temperature Resistance Adhesives, it is characterised in that：Described
The aluminium hydroxide in concentrated phosphoric acid and step (4) in step (3) is that Industrial Analysis is pure.
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| CN115724645A (en) * | 2022-11-23 | 2023-03-03 | 天津大学 | High-temperature sealing adhesive and preparation method thereof |
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| CN113402988A (en) * | 2021-08-11 | 2021-09-17 | 清华大学 | Sub-nanowire adhesive and preparation method and application thereof |
| CN115010463A (en) * | 2022-07-12 | 2022-09-06 | 中国民航大学 | Preparation method of flaky kyanite in-situ growth locking self-strengthening phosphate-based high-temperature adhesive |
| CN115724645A (en) * | 2022-11-23 | 2023-03-03 | 天津大学 | High-temperature sealing adhesive and preparation method thereof |
| CN115724645B (en) * | 2022-11-23 | 2023-09-26 | 天津大学 | High-temperature sealing adhesive and preparation method thereof |
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Application publication date: 20181130 |