CN112430118A - Magnesium fluoride infrared hood bonding process method - Google Patents
Magnesium fluoride infrared hood bonding process method Download PDFInfo
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- CN112430118A CN112430118A CN202011408477.5A CN202011408477A CN112430118A CN 112430118 A CN112430118 A CN 112430118A CN 202011408477 A CN202011408477 A CN 202011408477A CN 112430118 A CN112430118 A CN 112430118A
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- magnesium fluoride
- bonding
- process method
- bonding process
- adhesive
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
- C04B2237/525—Pre-treatment of the joining surfaces, e.g. cleaning, machining by heating
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/55—Pre-treatments of a coated or not coated substrate other than oxidation treatment in order to form an active joining layer
Abstract
The invention discloses a bonding process method of a magnesium fluoride infrared hood, which adopts a phosphate compound adhesive to realize the bonding of magnesium fluoride and a quartz ceramic material, has the advantages of high bonding strength and high temperature resistance, can be cured at a lower temperature, and has high efficiency, stability and low cost. The method is not only suitable for bonding the magnesium fluoride material with quartz ceramic, but also suitable for bonding the magnesium fluoride material with metal such as aluminum alloy and the like.
Description
Technical Field
The invention belongs to the technical field of wave-transparent ceramics for spaceflight, and particularly relates to a bonding process method of a magnesium fluoride infrared hood.
Background
The radar has the advantages of long acting distance, all-weather fighting capacity, poor interference resistance and low target resolution. The infrared target seeking has the advantage of high resolution and can complement the radar target seeking. Therefore, the radar/infrared dual-mode guidance technology is vigorously researched in all countries in the world. The radar head cover is made of high-temperature-resistant wave-transmitting quartz ceramic or quartz composite ceramic materials mostly, the infrared head cover is made of magnesium fluoride, spinel and the like mostly, and the radar/infrared dual-mode common-aperture composite head cover is formed by forming the quartz ceramic or the quartz composite ceramic and the magnesium fluoride materials in parts and then is assembled into a whole by adopting technological methods such as crimping, embedding, bonding and the like to form the head cover with radar/infrared dual-mode wave-transmitting function. The quartz ceramic and the magnesium fluoride material are both brittle materials, are easy to be brittle in press fit and mosaic assembly, and cannot be assembled in a press fit and mosaic mode due to the limiting factors such as structural size and the like. And the bonding mode is adopted, so that the connecting structure is simple, the process is easy to implement, and the method is an ideal assembling method.
The magnesium fluoride infrared wave-transmitting material is a fluorine-containing material, the fluorine-containing material is typically the most difficult to adhere, the surface energy of the fluorine-containing material is low, the wettability of the fluorine-containing material is poor, and a general adhesive cannot fully wet the fluorine-containing material, so that the fluorine-containing material cannot be well adhered to the fluorine-containing material, and the adhesion strength is seriously influenced. In particular, the magnesium fluoride material is bonded with the brittle quartz ceramic material, and the performance difficulty of bonding expansion matching, high temperature resistance and the like is higher.
Disclosure of Invention
Aiming at the problems in the background art, the invention aims to provide a magnesium fluoride infrared hood bonding process method which can realize the bonding of magnesium fluoride and quartz ceramic materials, has the advantages of high bonding strength and high temperature resistance, and has an efficient and controllable process method.
In order to achieve the purpose, the invention designs a magnesium fluoride infrared hood bonding process method which is characterized by comprising the following steps:
s1, preparing an adhesive: mixing aluminum dihydrogen phosphate and aluminum oxide in a weight ratio of 1: mixing and stirring uniformly according to the mass ratio of 0.85-0.95, then ultrasonically vibrating, vacuumizing and maintaining the pressure for a period of time to form phosphate; then, sequentially adding 0.5-1% of white carbon black, 1-1.6% of carboxyl POSS and 4-5% of alkoxy silane by mass percent into phosphate, mixing and stirring, then ultrasonically vibrating, vacuumizing and maintaining pressure for a period of time to form an adhesive;
s2, processing the magnesium fluoride hood bonding surface: firstly, roughening the bonding surface of the magnesium fluoride head cover by laser; then, coating the phosphate prepared in S1 on the bonding surface, standing for 10-20 min, washing with absolute ethyl alcohol, and drying in the air; finally, coating a layer of alkoxy silane on the surface, and airing for later use;
s3, processing the bonding surface of the quartz ceramic head cover: polishing the surface of the quartz ceramic head cover roughly by using abrasive paper, and then firing the bonding surface by using oxyhydrogen flame for 3-5 s;
s4, uniformly blade-coating an adhesive on the bonding surface of the quartz ceramic hood and the magnesium fluoride hood, adjusting and aligning on a tool, then carrying out counterweight bonding, then placing the tool into a blast drying oven, curing for 4-5 hours at the temperature of 60-80 ℃, and cooling to room temperature along with a furnace;
s5, post-processing: and (4) cleaning the overflowed glue, and performing secondary coating and curing on the gap pits by using an adhesive.
Preferably, in S1, the time for two ultrasonic vibrations is 8-10 min.
Preferably, in S1, the requirement of two times of vacuum pumping is: the vacuum pressure is less than or equal to-90 kPa, and the pressure maintaining time is 10min to 15 min.
Preferably, in S1, the particle size of the aluminum dihydrogen phosphate and the aluminum oxide is 0.2-0.5 micron.
Preferably, in S1, the carboxy POSS is an octacarboxysilsesquioxane.
Preferably, in S1, the alkoxysilane is alkyltriethoxysilane or phenyltrimethoxysilane or dimethyldimethoxysilane.
Preferably, in S2, the laser texturing roughness of the bonding surface of the magnesium fluoride hood is 2-3 microns.
Preferably, in S2, the alkoxysilane is alkyltriethoxysilane or phenyltrimethoxysilane or dimethyldimethoxysilane.
Preferably, in S3, the polishing is performed using 120-mesh sandpaper.
Preferably, in the step S4, the bonding surface is an S-shaped curved surface, the S-shaped bonding surface effectively increases the bonding area and improves the bonding strength, the ceramic material is prevented from brittle fracture through smooth transition, the upper and lower contact surfaces at the S-shaped position can be in contact positioning, the bonding gap is ensured, and the gap between the bonding surfaces is controlled to be 0.10-0.18 mm.
Preferably, in S4, after the adhesive is scraped, a piece of quartz fiber cloth is taken, and the adhesive is uniformly scraped on the surface of the quartz fiber cloth; and then uniformly paving the cloth on the bonding surface of the quartz ceramic head cover, scraping the cloth firmly by using a scraper, pressing the magnesium fluoride head cover on the quartz fiber cloth, and bonding by using a tool after adjusting and aligning.
More preferably, the quartz fiber cloth adopts a satin-structured quartz fiber cloth, and the thickness of the quartz fiber cloth is less than 0.05 mm.
Preferably, the quartz fiber cloth is dried for more than 1 hour at 120-150 ℃ before being scraped.
Preferably, in S4, the weight pressure against the adhesive surface region is 0.1 to 0.15 MPa.
The invention has the beneficial effects that: compared with the prior art, the invention has the following advantages:
firstly, the invention can be solidified at lower temperature and can be suitable for bonding magnesium fluoride materials with low surface energy.
Compared with assembly modes such as compression joint and embedding, the invention has the advantages of simple bonding connection structure, easy process implementation and low cost, is not only suitable for bonding magnesium fluoride and quartz ceramic, but also suitable for bonding magnesium fluoride head covers and metal materials such as aluminum alloy and the like, and can be expanded to be applied.
Thirdly, the S-shaped bonding surface is adopted, the bonding area is effectively increased, the bonding strength is improved, smooth transition is realized, the ceramic material is prevented from being brittle, the upper contact surface and the lower contact surface at the S-shaped position can be in contact positioning, the bonding gap is ensured, and the high-temperature-resistant ceramic material has high bonding strength (more than or equal to 1.5MPa) and high temperature resistance.
Drawings
FIG. 1 is a schematic view of the bonding structure of the tool and the hood
In the figure: 1. the device comprises a quartz ceramic hood, 2, a magnesium fluoride hood, 3, a bonding tool base, 4, a bonding tool fixing plate and 5, a bonding tool pressing plate.
Detailed Description
The invention will now be described in further detail, including the preferred embodiments, by means of figure 1 and by way of a list of some alternative embodiments of the invention. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
As shown in FIG. 1, the bonding process method of the magnesium fluoride infrared hood designed by the invention comprises the following steps:
s1, adhesive preparation: mixing aluminum dihydrogen phosphate and aluminum oxide in a weight ratio of 1: mixing and stirring uniformly at a mass ratio of 0.9, ultrasonically vibrating for 10min, vacuumizing at a vacuum pressure of less than or equal to-90 kPa, and maintaining the pressure for 10min to 15min to form phosphate; then, 0.8 mass percent of white carbon black, 1.3 mass percent of carboxyl POSS and 4-5 mass percent of alkoxy silane are sequentially added into phosphate, mixed and stirred, ultrasonically vibrated for 8-10 min, the vacuum pressure is less than or equal to-90 kPa, and the pressure is maintained for 10-15 min to form the adhesive. The particle sizes of the aluminum dihydrogen phosphate and the aluminum oxide are 0.2-0.5 micron, the phosphate is used as an adhesive, the temperature resistance is high, and the phosphate has certain corrosivity on fluorine-containing materials and can be better adhered with magnesium fluoride materials; the white carbon black can not be replaced by silicon micropowder or nano-silica, has a large amount of surface hydroxyl groups, has reaction activity, is easy to form strong hydrogen bond effect in the adhesive, and improves the bonding strength with the fluorine-containing material; the carboxyl POSS is octacarboxyl silsesquioxane, carboxyl has reactivity with adhesive components and bonded materials, and the POSS is in a cage structure and is in the adhesive; the alkoxy silane can be alkyl triethoxysilane, phenyl trimethoxysilane, dimethyl dimethoxysilane and the like, is a wetting agent, has low surface energy, and can enhance the penetrability and wettability of the adhesive on a bonded material.
S2, magnesium fluoride hood bonding surface treatment: firstly, roughening the bonding surface of a magnesium fluoride hood by adopting a laser roughening mode, wherein the roughening roughness is 2-3 microns; then, coating the adhesive prepared in S1 on an adhesive surface, standing for 10-20 min, washing with absolute ethyl alcohol, and airing; finally, coating a layer of alkoxy silane on the surface; and (5) airing for standby. The laser texturing roughness of the bonding surface of the magnesium fluoride hood reaches 2-3 microns, the surface area can be increased through the laser texturing, the surface energy is improved, and the bonding adhesive force is enhanced; the phosphate has stronger corrosivity, changes the surface lattice form and weakens the fluorine characteristic; the alkoxy silane is a wetting agent, has low surface energy, can enhance the penetrability and wettability of the adhesive on a bonded material, and can be alkyl triethoxysilane, phenyl trimethoxysilane, dimethyl dimethoxysilane and the like.
S3, processing the bonding surface of the quartz ceramic head cover: and (3) polishing the surface of the quartz ceramic head cover roughly by using 120-mesh abrasive paper, then burning the bonding surface by using oxyhydrogen flame for 3-5 s, removing surface moisture, activating the surface and improving the content of hydroxyl.
4) Head cover bonding: firstly, preparing and processing a bonding surface of a quartz ceramic head cover 1 and a magnesium fluoride head cover 2, wherein the bonding surface is required to be an S-shaped curved surface, and the gap between the two bonding surfaces is controlled to be 0.10-0.18 mm; fixing the quartz ceramic head cover 1 on the bonding tool base 3, adjusting and aligning, and fixing by using a bonding tool fixing plate 4; then uniformly coating the adhesive prepared in the step 1) on the bonding surface of the quartz ceramic head cover 1 and the magnesium fluoride head cover 2 by scraping; then taking a piece of quartz fiber cloth with the thickness of 0.05mm, and uniformly coating the adhesive prepared in the step 1) on the surface of the quartz fiber cloth in a scraping way; then, uniformly paving the cloth on the bonding surface of the quartz ceramic head cover 1, scraping the cloth firmly by using a scraper, pressing the magnesium fluoride head cover 2 on the bonding surface of the quartz ceramic head cover 1, and adjusting and aligning; then pressing the magnesium fluoride hood 2 by using a bonding tool pressing plate 5; and (3) placing the mixture into a blast drying oven, curing for 4-5 hours at the temperature of 60-80 ℃, and cooling to room temperature along with the oven. When the bonding surface of the hood is scraped, a rubber scraper is adopted for scraping, no bubble exists, and no casting exists; the thickness of the quartz fiber cloth is 0.05mm, the quartz fiber cloth is in a satin structure and easy to spread, and the quartz fiber cloth needs to be dried for more than 1h at 120-150 ℃ before glue scraping to remove water; the magnesium fluoride hood 2 is pressurized through the bonding tool pressing plate 5, the pressure of a bonding surface is 0.1-0.15 MPa through a counterweight mode, and the pressurizing contact position is a bonding surface area so as to avoid damaging the magnesium fluoride hood 2; blowing is needed during heating and curing, so that uneven heating is guaranteed.
5) And (3) post-treatment: cleaning up the excessive glue of the bonding seam of the hood, cleaning the excessive glue, and secondarily coating and curing the adhesive at the gap pit of the bonding position.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and any modification, combination, replacement, or improvement made within the spirit and principle of the present invention is included in the scope of the present invention.
Claims (10)
1. A magnesium fluoride infrared hood bonding process method is characterized by comprising the following steps:
s1, preparing an adhesive: mixing aluminum dihydrogen phosphate and aluminum oxide in a weight ratio of 1: mixing and stirring uniformly according to the mass ratio of 0.85-0.95, then ultrasonically vibrating, vacuumizing and maintaining the pressure for a period of time to form phosphate; then, sequentially adding 0.5-1% of white carbon black, 1-1.6% of carboxyl POSS and 4-5% of alkoxy silane by mass percent into phosphate, mixing and stirring, then ultrasonically vibrating, vacuumizing and maintaining pressure for a period of time to form an adhesive;
s2, processing the magnesium fluoride hood bonding surface: firstly, roughening the bonding surface of the magnesium fluoride head cover by laser; then, coating the phosphate prepared in S1 on the bonding surface, standing for 10-20 min, washing with absolute ethyl alcohol, and drying in the air; finally, coating a layer of alkoxy silane on the surface, and airing for later use;
s3, processing the bonding surface of the quartz ceramic head cover: polishing the surface of the quartz ceramic head cover roughly by using abrasive paper, and then firing the bonding surface by using oxyhydrogen flame for 3-5 s;
s4, uniformly blade-coating an adhesive on the bonding surface of the quartz ceramic hood and the magnesium fluoride hood, adjusting and aligning on a tool, then carrying out counterweight bonding, then placing the tool into a blast drying oven, curing for 4-5 hours at the temperature of 60-80 ℃, and cooling to room temperature along with a furnace;
s5, post-processing: and (4) cleaning the overflowed glue, and performing secondary coating and curing on the gap pits by using an adhesive.
2. The bonding process method of the magnesium fluoride infrared hood according to claim 1, characterized in that: in S1, the time of the two ultrasonic vibrations is 8-10 min; the vacuum pressure is less than or equal to-90 kPa, and the pressure maintaining time is 10min to 15 min.
3. The bonding process method of the magnesium fluoride infrared hood according to claim 1 or 2, characterized in that: in S1, the particle size of the aluminum dihydrogen phosphate and the aluminum oxide is 0.2-0.5 micron.
4. The bonding process method of the magnesium fluoride infrared hood according to claim 1 or 2, characterized in that: in S1, the carboxyl POSS is octacarboxyl silsesquioxane; the alkoxy silane is alkyl triethoxy silane or phenyl trimethoxy silane or dimethyl dimethoxy silane.
5. The bonding process method of the magnesium fluoride infrared hood according to claim 1, characterized in that: in S2, the laser texturing roughness of the bonding surface of the magnesium fluoride hood is 2-3 microns; the alkoxy silane is alkyl triethoxy silane or phenyl trimethoxy silane or dimethyl dimethoxy silane.
6. The bonding process method of the magnesium fluoride infrared hood according to claim 1, characterized in that: in S4, the cross section of the bonding surface is an "S" shaped curved surface.
7. The bonding process method of the magnesium fluoride infrared hood according to claim 1, characterized in that: in S4, after the adhesive is scraped, a piece of quartz fiber cloth is taken, and the adhesive is uniformly scraped on the surface of the quartz fiber cloth; and then uniformly paving the cloth on the bonding surface of the quartz ceramic head cover, scraping the cloth firmly by using a scraper, pressing the magnesium fluoride head cover on the quartz fiber cloth, and bonding by using a tool after adjusting and aligning.
8. The bonding process method of the magnesium fluoride infrared hood according to claim 7, characterized in that: the quartz fiber cloth is of a satin structure, and the thickness of the quartz fiber cloth is less than 0.05 mm.
9. The bonding process method of the magnesium fluoride infrared hood according to claim 7 or 8, characterized in that: the quartz fiber cloth is dried for more than 1h at the temperature of 120-150 ℃ before being scraped.
10. The bonding process method of the magnesium fluoride infrared hood according to claim 9, characterized in that: in S4, the counter weight pressure to the bonding surface area is 0.1-0.15 MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011408477.5A CN112430118B (en) | 2020-12-04 | 2020-12-04 | Magnesium fluoride infrared hood bonding process method |
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| CN202011408477.5A CN112430118B (en) | 2020-12-04 | 2020-12-04 | Magnesium fluoride infrared hood bonding process method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744046A (en) * | 2013-12-27 | 2015-07-01 | 日本碍子株式会社 | Bonding material composition, aluminum nitride bonded body, and method for producing the same |
| CN105565841A (en) * | 2015-12-30 | 2016-05-11 | 潮州三环（集团）股份有限公司 | Shading ceramic and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744046A (en) * | 2013-12-27 | 2015-07-01 | 日本碍子株式会社 | Bonding material composition, aluminum nitride bonded body, and method for producing the same |
| CN105565841A (en) * | 2015-12-30 | 2016-05-11 | 潮州三环（集团）股份有限公司 | Shading ceramic and preparation method thereof |
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