CN104058794B - Microwave device delivery of energy window ceramics metallised paint and metalized coated method thereof - Google Patents

Microwave device delivery of energy window ceramics metallised paint and metalized coated method thereof Download PDF

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Publication number
CN104058794B
CN104058794B CN201410313436.6A CN201410313436A CN104058794B CN 104058794 B CN104058794 B CN 104058794B CN 201410313436 A CN201410313436 A CN 201410313436A CN 104058794 B CN104058794 B CN 104058794B
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parts
energy window
delivery
stainless steel
sintering
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CN104058794A (en
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杨磊
金宇
梁田
苏秘
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Nanjing Sanle Electronic Information Industry Group Co Ltd
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Nanjing Sanle Electronic Information Industry Group Co Ltd
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Abstract

The invention discloses a kind of microwave device delivery of energy window ceramics metallised paint and coating process, it is made up with binding agent 25 ~ 50 parts of metallization powder 100 parts; Is metallization powder by Mo? 65 ~ 75 parts, MnO? 9 ~ 11 parts, Al 2o 3?8 ~ 10 parts, CaO? 0.5 ~ 2 part, SiO 2?make for 7 ~ 9 parts: binding agent is made up of Terpineol 350 95 ~ 98 parts, ethyl cellulose 2 ~ 5 parts.Metallised paint of the present invention, each component proportion is scientific and reasonable, and bonding firmly, there will not be sinkings, is divided into, and bond the situation such as loosely, can obtain compact metal coating.Metalized coated method provided by the invention, the special tool of printed coating is filtered out by great many of experiments, best printing coating method, the processing step such as sintering processes and nickel plating process, densification can be formed on delivery of energy window ceramics, firmly, high metalized coated of cohesive strength, greatly can improve the serviceability of delivery of energy window.

Description

Microwave device delivery of energy window ceramics metallised paint and metalized coated method thereof
Technical field
The present invention designs a kind of microwave device delivery of energy window, is specifically related to a kind of microwave device delivery of energy window ceramics metallised paint and adopts this coating to carry out metalized coated method.
Background technology
In microwave device, delivery of energy window ceramics, when ensureing hermetic seal, mainly carries the transmission of high-frequency energy.In traditional delivery of energy window ceramics metallization processes, prior art adopts the mode of manual application to carry out metalized coated preparation, but it is larger that manual pen is coated with error, the homogeneity of component and thickness is all difficult to control, the ununiformity of this thickness can make stress of sealing concentrate, produce tiny crack, greatly reduce the performance of delivery of energy window.And metallised paint proportioning is scientific and reasonable not in prior art, the uneven meeting of component makes Mo and activator skewness, even occurs enrichment, thus causes the difference of each point activator viscosity, surface tension, linear expansivity etc., cause combination loosely, poor reliability; And delivery of energy window ceramics metalized shape is complicated, causes efficiency low.
In metallizing paste, the sedimentation under gravity of the powder particle in liquid medium, goes back the buoyancy of liquid body, drag effect simultaneously, through very short time, the power acted on particle reaches balance, and particle is with constant speed sedimentation, and the settling velocity equation for a spheroidal particle is:
v = ( ρ p - ρ ) g 18 η d p 2
As can be seen from the above equation, when the parameter such as granularity of powder is certain, the viscosity of liquid and the settling velocity of powder particle are inversely proportional to, so adopt the binding agent of large viscosity can reduce the demixing phenomenon of paste to a great extent, thus ensure the homogeneity of layer of paste component.The binding agent that manual pen of the prior art is coated with is made up of cotton solution, butylacetate and oxalic acid diethyl ester, and its viscosity is very little, must stir always, could reduce the layering of paste as much as possible in the process of paste coating.And in the process of manual application, the thickness of paste is by Artificial Control, the homogeneity impact on layer of paste thickness such as its skill level applied, the geomery of coating, the size of writing brush and nib etc. is larger, the tolerance of its thickness is 8 ~ 15 μm, therefore the microwave device delivery of energy window performance for preparing of art methods is lower, can not meet the need of work of the microwave device of high request.
Summary of the invention
Goal of the invention: the object of the invention is to solve the deficiencies in the prior art, there is provided a kind of component proportion scientific and reasonable, viscosity is large, can prevent from occurring demixing phenomenon in prior art, coating ingredients homogeneity can be ensured, can the microwave device delivery of energy window ceramics metallised paint of secure bond in metallic surface, another object of the present invention is to provide this coating and carries out metalized coated method.
Technical scheme: in order to realize above object, the technical scheme that the present invention takes is:
A kind of microwave device delivery of energy window ceramics metallised paint, it is made up of following raw materials according:
Metallization powder 100 parts, binding agent 25 ~ 50 parts;
Described metallization powder is made up of the raw material of following parts by weight: Mo65 ~ 75 part, MnO9 ~ 11 part, Al 2o 38 ~ 10 parts, CaO0.5 ~ 2 part, SiO 27 ~ 9 parts;
Described binding agent is made up of the raw material of following parts by weight: Terpineol 350 95 ~ 98 parts, ethyl cellulose 2 ~ 5 parts.
The method that microwave device delivery of energy window ceramics of the present invention is metalized coated, comprises the following steps:
A, ball-milling processing:
Get metallization powder by weight, employing dehydrated alcohol is dispersion medium, corundum ball is ball-milling medium, ball milling is carried out in corundum bottle, each powder is mixed, metallization powder: corundum ball: dehydrated alcohol=100g:120g:100ml, more than ball milling 72h, pours out oven dry, grind with mortar, and it is for subsequent use to cross 100 ~ 120 mesh sieves;
Get the binding agent of Terpineol 350 and ethyl cellulose composition by weight, in vial, more than mixing and ball milling 24h is for subsequent use;
Then by metallization powder good for above-mentioned ball milling and the good binding agent of ball milling, mix according to parts by weight 100:25 ~ 50 ratio, adopt planetary ball mill ball milling 48h;
B, assembling mould, printed metallization coating:
Graphic arts die comprises stainless steel locate moulds, be arranged on 120 ~ 300 order Stainless Steel Cloths on stainless steel locate moulds, the metallised paint scraper of printing, described stainless steel locate moulds top offers the groove placing delivery of energy window ceramics, described stainless steel locate moulds bottom offers the through hole be connected with groove, and through hole is connected with vacuum pump;
First delivery of energy window ceramics is placed in groove, then 120 ~ 180 order Stainless Steel Cloths are placed on above delivery of energy window ceramics, delivery of energy window ceramics and Stainless Steel Cloth are had good positioning, then the metallised paint that step a prepares is placed on Stainless Steel Wire online, then be coated with metallised paint scraper and scrape the metalized coated of print thickness 50 ~ 60 μm, open vacuum pump evacuation simultaneously, prevent delivery of energy window ceramics and Stainless Steel Cloth to be adhered;
Dry after printing, bake out temperature is 70 ~ 100 DEG C, and the time is 10 ~ 15min;
C, sintering processes:
The delivery of energy window ceramics getting metallic coating in step b printing carries out metallization sintering, and sintering process is: sintering temperature 1500 DEG C ~ 1600 DEG C, and sintering time is 50 ~ 60min;
D, Nickel Plating Treatment:
The delivery of energy window ceramics getting the good band metallic coating of step c sintering processes carries out Nickel Plating Treatment, and powering at metallic coating plates the metal nickel dam that thickness is 4 ~ 6 μm.
E, coating sintering processes:
Delivery of energy window ceramics after steps d Nickel Plating Treatment is carried out coating sintering, and sintering temperature is 1050 DEG C ~ 1100 DEG C, and sintering time is 15 ~ 20min.
Preferably, the method that above-described microwave device delivery of energy window ceramics is metalized coated, metallize in step a powder ball milling 72h, dries, grind rear mistake 120 mesh sieve.
Preferably, the method that above-described microwave device delivery of energy window ceramics is metalized coated, dry after printing in step b, bake out temperature is 90 ~ 100 DEG C, and the time is 15min.
Preferably, the method that above-described microwave device delivery of energy window ceramics is metalized coated, in step c, sintering process is: sintering temperature 1500 DEG C, and sintering time is 60min.
Preferably, the method that above-described microwave device delivery of energy window ceramics is metalized coated, in step e, sintering temperature is 1050 DEG C, and sintering time is 15min.
One, the screening experiment of metallization powder and binding agent
Because microwave device delivery of energy window is ceramic substrate, to form compact metal coating on delivery of energy window ceramics, suitable coating must be selected, in prior art, adopt the manual coating coated, cohesiveness not before, easy layering, and coat-thickness is uneven.The present invention screens best metallised paint by real in a large number, in test, adopts the ratio of optimum seeking method to the proportioning of powder component and powder and binding agent to carry out serial research.Glassy phase infiltration test is adopted to determine the composition (it is 1350 DEG C that glassy phase infiltrates test temperature) of activator in formula; When glassy phase composition is determined, adopt optimum seeking method to study to molybdenum powder (Mo) and the composition of glassy phase, final condition is 50 ~ 80%, through lot of experiments screening contrast, result shows, molybdenum content 65 ~ 75% time, and is added with 9 ~ 11%MnO, 8 ~ 10%Al 2o 3, 0.5 ~ 2%CaO and 7 ~ 9%SiO 2during composition metallised paint, coating can be the highest with delivery of energy window ceramics sealing strength, and resistance to air loss is best.
Then the present invention carries out great many of experiments screening to binding agent, and the settling velocity equation according to spheroidal particle is:
v = ( ρ p - ρ ) g 18 η d p 2
Screening binding agent, the comparing result of different binding agent shows, when adopting the binding agent of Terpineol 350 95 ~ 98 parts, ethyl cellulose 2 ~ 5 parts composition, can prevent coating layering, and bonding is very firm, and resistance to air loss is best.Therefore, the binding agent of the preferred Terpineol 350 of the present invention 95 ~ 98 parts, ethyl cellulose 2 ~ 5 parts composition.
After filtering out metallization powder and binding agent, the present invention is studied the consumption proportion of the two again, the present invention tests according to 100:15 ~ 60, show through test-results, when metallization powder and weight of binder portion rate are 100:25 ~ 50, each performance of printing the metallic coating obtained is best.
Two, preparation technology of coating screening
The mode all adopting artificial hand to be coated with in prior art carries out coating metal layer, there is a lot of deficiencies, and the present invention adopts the mode of printing to carry out metalized coated by great many of experiments.
The present invention realizes closing binding agent to metallised paint and carries out ball milling, and so mutual Special tool for assembling, carries out printed coating, then carry out carrying out sintering processes under selection process, can make the metalized coated metal level forming densification on delivery of energy window ceramics; And then under selection process, Nickel Plating Treatment is carried out on metallic coating top layer, and then nickel dam is carried out to the coating sintering processes of selection process, through multi step strategy, sealing strength can be prepared high on microwave device delivery of energy window ceramics, the metallic coating that compactness is good, can improve the working efficiency of microwave device delivery of energy window greatly.
Beneficial effect: the preparation method of microwave device delivery of energy window ceramics metallised paint provided by the invention and coating compared with prior art has the following advantages:
1, microwave device delivery of energy window ceramics metallised paint of the present invention, experimental study shows, each component proportion is scientific and reasonable, and bonding firmly, there will not be sinkings, is divided into, and the bonding situation such as loosely, can obtain the metalized coated of densification.
2, the method that microwave device delivery of energy window ceramics of the present invention is metalized coated, technological design is reasonable, workable, the special tool of printed coating is filtered out particularly by great many of experiments, best printing coating method, the processing step such as sintering processing method and nickel plating process, can form densification on delivery of energy window ceramics, firmly, high metalized coated of cohesive strength, greatly can improve the serviceability of delivery of energy window.
Accompanying drawing explanation
Fig. 1 is mould assembling structure schematic diagram in the metalized coated process of microwave device delivery of energy window ceramics of the present invention.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Embodiment 1
1, a microwave device delivery of energy window ceramics metallised paint, it is made up of following raw materials according:
Metallization powder 100 parts, binding agent 50 parts;
Described metallization powder is made up of the raw material of following parts by weight: Mo75 part, MnO11 part, Al 2o 310 parts, CaO2 part, SiO 29 parts;
Described binding agent is made up of the raw material of following parts by weight: Terpineol 350 98 parts, ethyl cellulose 2 parts.
2, the method that microwave device delivery of energy window ceramics of the present invention is metalized coated, comprises the following steps:
A, ball-milling processing:
Get metallization powder Mo75 part, MnO11 part, Al by weight 2o 310 parts, CaO2 part, SiO 29 parts; Employing dehydrated alcohol is dispersion medium, corundum ball is ball-milling medium, in corundum bottle, carry out ball milling, and each powder is mixed, metallization powder: corundum ball: dehydrated alcohol=100g:120g:100ml, more than ball milling 72h, pours out oven dry, grind with mortar, and it is for subsequent use to cross 120 mesh sieves;
Get the binding agent of Terpineol 350 98 parts, ethyl cellulose 2 parts pine composition by weight, in vial, more than mixing and ball milling 24h is for subsequent use;
Then by metallization powder good for above-mentioned ball milling and the good binding agent of ball milling, mix according to parts by weight 100:50 ratio, adopt planetary ball mill ball milling 48h;
B, assembling mould, printed metallization coating:
Graphic arts die comprises stainless steel locate moulds (1), be arranged on 120 order Stainless Steel Cloths (2) on stainless steel locate moulds (1), the metallised paint scraper (3) of printing, described stainless steel locate moulds top (1) offers the groove (5) placing delivery of energy window ceramics (4), described stainless steel locate moulds bottom offers the through hole (6) be connected with groove (5), and through hole (6) is connected with vacuum pump (7);
First delivery of energy window ceramics (4) is placed in groove (5), then 180 order Stainless Steel Cloths (2) are placed on delivery of energy window ceramics (4) top, delivery of energy window ceramics (4) and Stainless Steel Cloth (2) are had good positioning, then the metallised paint that step a prepares is placed on Stainless Steel Cloth (2), then use metallised paint scraper (3) to be coated with and scrape the metalized coated of print thickness 60 μm, open vacuum pump (7) to vacuumize simultaneously, prevent delivery of energy window ceramics (4) and Stainless Steel Cloth (2) to be adhered;
Dry after printing, bake out temperature is 100 DEG C, and the time is 10min;
C, sintering processes:
The delivery of energy window ceramics (4) getting metallic coating in step b printing carries out metallization sintering, and sintering process is: sintering temperature 1500 DEG C, and sintering time is 50min;
D, Nickel Plating Treatment:
The delivery of energy window ceramics (4) getting the good band metallic coating of step c sintering processes carries out Nickel Plating Treatment, and powering at metallic coating plates the metal nickel dam that thickness is 4 ~ 6 μm.
E, coating sintering processes:
Delivery of energy window ceramics (4) after steps d Nickel Plating Treatment is carried out coating sintering, and sintering temperature is 1050 DEG C, and sintering time is 15min.
Embodiment 2
1, a microwave device delivery of energy window ceramics metallised paint, it is made up of following raw materials according:
Metallization powder 100 parts, binding agent 25 parts;
Described metallization powder is made up of the raw material of following parts by weight: Mo65 part, MnO9 part, Al 2o 38 parts, CaO0.5 part, SiO 27 parts;
Described binding agent is made up of the raw material of following parts by weight: Terpineol 350 95 parts, ethyl cellulose 5 parts.
2, the method that microwave device delivery of energy window ceramics is metalized coated, comprises the following steps:
A, ball-milling processing:
Get metallization powder Mo65 part, MnO9 part, Al 2o 38 parts, CaO0.5 part, SiO 27 parts; Employing dehydrated alcohol is dispersion medium, corundum ball is ball-milling medium, in corundum bottle, carry out ball milling, and each powder is mixed, metallization powder: corundum ball: dehydrated alcohol=100g:120g:100ml, more than ball milling 72h, pours out oven dry, grind with mortar, and it is for subsequent use to cross 100 mesh sieves;
Get the binding agent of Terpineol 350 described in claim 1 and ethyl cellulose composition, in vial, mixing and ball milling 24h is for subsequent use;
Then by metallization powder good for above-mentioned ball milling and the good binding agent of ball milling, mix according to parts by weight 100:25 ratio, adopt planetary ball mill ball milling 48h;
B, assembling mould, printed metallization coating:
Graphic arts die comprises stainless steel locate moulds (1), be arranged on 300 order Stainless Steel Cloths (2) on stainless steel locate moulds (1), the metallised paint scraper (3) of printing, described stainless steel locate moulds top (1) offers the groove (5) placing delivery of energy window ceramics (4), described stainless steel locate moulds bottom offers the through hole (6) be connected with groove (5), and through hole (6) is connected with vacuum pump (7);
First delivery of energy window ceramics (4) is placed in groove (5), then 120 order Stainless Steel Cloths (2) are placed on delivery of energy window ceramics (4) top, delivery of energy window ceramics (4) and Stainless Steel Cloth (2) are had good positioning, then the metallised paint that step a prepares is placed on Stainless Steel Cloth (2), then use metallised paint scraper (3) to be coated with and scrape the metalized coated of print thickness 50 μm, open vacuum pump (7) to vacuumize simultaneously, prevent delivery of energy window ceramics (4) and Stainless Steel Cloth (2) to be adhered;
Dry after printing, bake out temperature is 70 DEG C, and the time is 15min;
C, sintering processes:
The delivery of energy window ceramics (4) getting metallic coating in step b printing carries out metallization sintering, and sintering process is: sintering temperature 1600 DEG C, and sintering time is 50min;
D, Nickel Plating Treatment:
The delivery of energy window ceramics (4) getting the good band metallic coating of step c sintering processes carries out Nickel Plating Treatment, and powering at metallic coating plates the metal nickel dam that thickness is 4 ~ 6 μm.
E, coating sintering processes:
Delivery of energy window ceramics (4) after steps d Nickel Plating Treatment is carried out coating sintering, and sintering temperature is 1100 DEG C, and sintering time is 15min.
Embodiment 3
1, get the invention process 1 and implement the 2 microwave device delivery of energy window ceramics with metallic coating prepared, detected result shows, metallic coating and ceramics sealing strength are 150MPa, leak rate≤10 -11pam 3/ s.
2 and by enforcement 1 with implement the 2 microwave device delivery of energy window ceramics with metallic coating that prepare in hydrogen atmosphere, repeat 6 times from 650 DEG C to room temperature; The lower 550 DEG C of baking 48h of low vacuum environment, leak rate all≤10 -11pam 3/ s.
The metalized coated method of the present invention, by producing checking for a long time, good article rate >=99.8%, the manual application of production efficiency and prior art can improve more than 5 times.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (1)

1. the method that microwave device delivery of energy window ceramics is metalized coated, is characterized in that, comprise the following steps:
A, ball-milling processing:
Get metallization powder, employing dehydrated alcohol is dispersion medium, corundum ball is ball-milling medium, ball milling is carried out in corundum bottle, each powder is mixed, metallization powder: corundum ball: dehydrated alcohol=100g:120g:100ml, more than ball milling 72h, pours out oven dry, grind with mortar, and it is for subsequent use to cross 120 mesh sieves;
Get binding agent, in vial, more than mixing and ball milling 24h is for subsequent use;
Then by metallization powder good for above-mentioned ball milling and the good binding agent of ball milling, mix according to parts by weight 100:25 ~ 50 ratio, adopt planetary ball mill ball milling 48h;
B, assembling mould, printed metallization coating:
Graphic arts die comprises stainless steel locate moulds (1), be arranged on 120 ~ 300 order Stainless Steel Cloths (2) on stainless steel locate moulds (1), the metallised paint scraper (3) of printing, described stainless steel locate moulds (1) top offers the groove (5) placing delivery of energy window ceramics (4), described stainless steel locate moulds bottom offers the through hole (6) be connected with groove (5), and through hole (6) is connected with vacuum pump (7);
First delivery of energy window ceramics (4) is placed in groove (5), then 120 ~ 300 order Stainless Steel Cloths (2) are placed on delivery of energy window ceramics (4) top, delivery of energy window ceramics (4) and Stainless Steel Cloth (2) are had good positioning, then the metallised paint that step a prepares is placed on Stainless Steel Cloth (2), then use metallised paint scraper (3) to be coated with and scrape the metalized coated of print thickness 50 ~ 60 μm, open vacuum pump (7) to vacuumize simultaneously, prevent delivery of energy window ceramics (4) and Stainless Steel Cloth (2) to be adhered;
Dry after printing, bake out temperature is 90 ~ 100 DEG C, and the time is 15min;
C, sintering processes:
The delivery of energy window ceramics (4) getting metallic coating in step b printing carries out metallization sintering, and sintering process is: sintering temperature 1500 DEG C, and sintering time is 60min;
D, Nickel Plating Treatment:
The delivery of energy window ceramics (4) getting the good band metallic coating of step c sintering processes carries out Nickel Plating Treatment, and powering at metallic coating plates the metal nickel dam that thickness is 4 ~ 6 μm;
E, coating sintering processes:
Delivery of energy window ceramics (4) after steps d Nickel Plating Treatment is carried out coating sintering, and sintering temperature is 1050 DEG C, and sintering time is 15min;
Described metallization powder is 100 parts, binding agent is 25 ~ 50 parts;
Described metallization powder is made up of the raw material of following parts by weight: Mo65 ~ 75 part, MnO9 ~ 11 part, Al 2o 38 ~ 10 parts, CaO0.5 ~ 2 part, SiO 27 ~ 9 parts;
Described binding agent is made up of the raw material of following parts by weight: Terpineol 350 95 ~ 98 parts, ethyl cellulose 2 ~ 5 parts.
CN201410313436.6A 2014-07-02 2014-07-02 Microwave device delivery of energy window ceramics metallised paint and metalized coated method thereof Expired - Fee Related CN104058794B (en)

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CN113117976B (en) * 2021-04-13 2022-05-24 浙江蔚蓝航盾精密陶瓷科技有限公司 Manufacturing method of metallized ceramic substrate
CN114835512B (en) * 2022-03-28 2023-05-02 南京三乐集团有限公司 High-reliability small-size sapphire Mo-Mn metallization method
CN115057727A (en) * 2022-07-28 2022-09-16 安徽建筑大学 High-purity alumina ceramic gradient coating metallization method

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CN102049514A (en) * 2009-11-11 2011-05-11 福建泉州万顺捷集团有限公司 Powder for aluminum oxide ceramics nano metallized paste and preparation method thereof
CN103102180A (en) * 2013-02-22 2013-05-15 浙江亚通金属陶瓷有限公司 Metallized surface of zirconia ceramic and preparation method

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102049514A (en) * 2009-11-11 2011-05-11 福建泉州万顺捷集团有限公司 Powder for aluminum oxide ceramics nano metallized paste and preparation method thereof
CN103102180A (en) * 2013-02-22 2013-05-15 浙江亚通金属陶瓷有限公司 Metallized surface of zirconia ceramic and preparation method

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