CN108675834A - A method of improving ceramic surface metallization adhesive force - Google Patents
A method of improving ceramic surface metallization adhesive force Download PDFInfo
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- CN108675834A CN108675834A CN201810536924.1A CN201810536924A CN108675834A CN 108675834 A CN108675834 A CN 108675834A CN 201810536924 A CN201810536924 A CN 201810536924A CN 108675834 A CN108675834 A CN 108675834A
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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Abstract
The invention discloses a kind of methods improving ceramic surface metallization adhesive force, include the following steps：（1）Ceramic matrix pre-treatment：Ceramic matrix is cleaned with small polarity to big polar solvent successively；Then toasted 1 to 3 hours in the case where temperature is 250 DEG C 680 DEG C of atmospheric pressure environment；（2）Deposited metal layer A：Using magnetron sputtering technique, it is evacuated to vacuum 5 × 10‑3After Pa, it is filled with argon gas, it is 1 × 10 that dynamic, which maintains air pressure,‑1Pa‑2×10‑1Within the scope of Pa, deposition thickness is the metal layer A of 50nm 500nm；（3）Deposit alloy layer AB：It is 5 × 10 to adjust argon flow amount dynamic and maintain air pressure‑1Pa 1Pa use the common magnetron sputtering deposition thickness of A, B target for the alloy-layer AB of 20nm 500nm；（4）Deposited metal layer B；Keep step（3）Air pressure conditions, again utilize magnetron sputtering technique deposition thickness be 200nm 2000nm metal layer B.The metallized ceramic prepared using the present invention has the characteristics that film layer big with Ceramic bond intensity, stable structure, production cost are low.
Description
Technical field
The present invention relates to a kind of methods improving ceramic surface metallization adhesive force, belong to ceramic metallization technology neck
Domain.
Background technology
Realize that ceramic metallization was obtaining quick development in recent years using magnetron sputtering technique.Patent
CN102503580A and CN104058796B discloses thermal sensitive ceramics and the magnetron sputtering method for metallising of PTC ceramics, relative to
For the technologies such as traditional chemical plating, plating, burning infiltration metal, evaporation coating, metallising, the ceramics of magnetron sputtering technique preparation
Metallized product has many advantages, such as that good product performance, consistency are high, environmentally friendly, at low cost.But in certain ceramic products as aoxidized
The adhesive force of metallized film prepared by the ceramic surfaces such as aluminium, aluminium nitride, magnesium titanate and zirconium oxide is relatively poor.In order to improve pottery
Porcelain surface metalation adhesive force, patent CN104072206B, which is disclosed, a kind of to carry out at dehumidifying substrate using vacuum bakeout
The method that reason improves aluminium nitride ceramic substrate thick film adhesive force, but it needs the special higher vacuum bakeout cavity of cost；Specially
Sharp 103360122B discloses a kind of using first corrosion roughening ceramic bases, recycling high-power impulse magnetron sputtering technology acquisition
High-energy particle bombardment ceramic bases surface obtain the preferable metallic film of adhesive force method, but this method need first with
Corrosive liquid handles ceramic matrix, does not allow for many ceramic products, and high power pulse magnetic control power supply price is high
It is expensive.Patent CN105777210A discloses a kind of method obtaining high adhesion force using laser pre-treatment aluminum nitride ceramic substrate,
The limitation of its laser treatment efficiency stimulated light device technology.
Compared to the metallization technology that conventional silk-screen silver paste re-sinters, above-mentioned its film layer of ceramic metallization technology and ceramics
Adhesive force has been increased to tens Ns in welding tensile test experiment from more than ten Ns, still, due to several layers of on ceramic surface
The reasons such as the intersolubility of layer of metallized film is poor, macroscopic property differs greatly, cause to exist between different metal film layer compared with
Big internal stress, this stress is while influencing the stability of metallization membrane system itself also by adverse effect conduction to ceramic base
On body and the contact surface of layer of metallized film.When ceramic component cycle operation under high/low temperature so that layer of metallized film and ceramics
Binding force significantly decline, seriously affect the reliability and stability of ceramic component.
Invention content
The technical problem to be solved by the invention is to provide a kind of layer of metallized film and the strong adhesive force of ceramic matrix, life
Produce it is at low cost, can under the conditions of high/low temperature cycle operation steady operation ceramic metallization method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A method of ceramic surface metallization adhesive force is improved, is included the following steps：
（1）Ceramic matrix pre-treatment：Ceramic matrix is cleaned with small polarity to big polar solvent successively；It is in temperature then
It is toasted 1 to 3 hours under 250 DEG C -680 DEG C of atmospheric pressure environment；
（2）Deposited metal layer A：Using magnetron sputtering technique, it is evacuated to vacuum 5 × 10-3After Pa, it is filled with argon gas, dynamic maintains air pressure
It is 1 × 10-1Pa-2×10-1Within the scope of Pa, deposition thickness is the metal layer A of 50nm- 500nm；
（3）Deposit alloy layer AB：It is 5 × 10 to adjust argon flow amount dynamic and maintain air pressure-1Pa -1Pa, using the common magnetic of A, B target
Control the alloy-layer AB that sputtering sedimentation thickness is 20nm -500nm；
（4）Deposited metal layer B：Keep step（3）Air pressure conditions, again utilize magnetron sputtering technique deposition thickness be 200nm
The metal layer B of -2000nm.
Step（1）Middle selection polar reagent includes several in acetone, ethyl alcohol, deionized water or combinations thereof, using ultrasound
Wave cleans 5-30 minutes.
The one kind of the metal layer A in titanium, chromium, nickel, aluminium, molybdenum, tungsten or its alloy.
The metal layer B is selected from copper or silver.
Step（3）It is middle use the technique of the common magnetron sputtering deposition of A, B target for：The sputtering electricity of A, B target is controlled using computer
Source determines that the duration makes the sputtering power of A targets drop to 0%, while B from 100% within the duration according to thickness of deposited film
The sputtering power of target increases to 100% from 0%.
In step（4）According to the thickness requirement of metal layer B after completion, using plating or silk-screen printing technique to metal layer
B is thickeied, and thickness range is 2 μm -100 μm.
The ceramic matrix is selected from microwave ceramics, ferrite ceramics, aluminium nitride ceramics, aluminium oxide ceramics, dielectric ceramic, heat
Any one of quick ceramics, voltage-sensitive ceramic, piezoelectric ceramics, ferroelectric ceramics, magnetic ceramics, silicon oxide ceramics or zirconia ceramics.
The advantageous effect that the present invention is reached：Preparation process of the present invention is pollution-free, and the metallized ceramic of preparation has film layer
It is big with Ceramic bond intensity, the characteristics of stable structure, and relative to existing disclosed raising ceramic surface metallization film layer
The method of adhesive force, the present invention need not increase additional equipment investment, only need to control DC power supply by computer, have low
The advantage of cost.
Description of the drawings
Fig. 1 is metallized ceramic structural schematic diagram prepared by the present invention；Reference sign：1 is ceramic matrix, and 2 be gold
Belong to layer A, 3 be alloy-layer AB, and 4 be metal layer B.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings.Following embodiment is only used for clearly illustrating the present invention
Technical solution, and not intended to limit the protection scope of the present invention.
1 microwave ceramics of embodiment metallizes
The first step：The magnesium titanate microwave-medium ceramics that specification is 30mm × 30mm × 15mm are subjected to surface with 1000 mesh sand paper
After fine polishing, it is respectively put into acetone soln, ethanol solution, deionized water and is cleaned by ultrasonic each 15 minutes, in 350 DEG C of temperature
It is lower to be toasted 1 hour with air dry oven.
Second step：Microwave ceramics after pre-treatment is put into vacuum cavity at once, is evacuated to vacuum cavity in 10 minutes
Vacuum degree reaches 5 × 10-3Pa is filled with argon gas, and it is 1 × 10 that dynamic, which maintains air pressure,-1Pa - 2×10-1Within the scope of Pa, direct current is sputtered
Electric current 1A, DC voltage 500V, deposition thickness are closing chromium target shielding power supply after the metallic chromium layer of 50nm.
Third walks：Argon flow amount is adjusted, maintains dynamic air pressure 5 × 10-1Pa is again turned on chromium target shielding power supply, simultaneously
Copper target shielding power supply is opened, is controlled using computer, chromium target DC current is made to drop to 0 from 1A, and copper target shielding power supply rises from 0
To 1A, whole process continues 2 minutes, and film thickness is about 100nm.
4th step closes chromium target power supply after the completion of third step, keeps copper target power supply direct current 1A, deposition film thickness is to about 1 μm.
The microwave ceramic devices that 4th step is prepared are put into electroplating device by the 5th step, and plating thickeies copper film to 20 μ
m。
The sample being prepared is up to 344N in welding tensile test（At this point, ceramics have been stripped）.
The sample of preparation is heated to 150 DEG C in an oven, is immediately placed in after taking out in 20 °C of cold water, is then carried out again
Tensile test, adhesive force, which declines, is not more than 3%.
Film layer crackle is not found on -55 DEG C -125 DEG C surfaces high/low temperature cycle 1000h.
2 ferrite ceramics of embodiment metallizes
The first step：The ferrite ceramics for the clean surface that specification is 78mm × 70mm × 50mm is respectively put into acetone soln, is gone
It is cleaned by ultrasonic in ionized water each 15 minutes, is toasted 1.5 hours at a temperature of 250 DEG C.
Second step：Vacuum cavity is put into after ferrite ceramics after pre-treatment is shelved at once, by vacuum chamber in 15 minutes
The vacuum degree that body is evacuated to reaches 5 × 10-3Pa is filled with argon gas, and it is 1 × 10 that dynamic, which maintains air pressure,-1Pa - 2×10-1Within the scope of Pa,
DC current 1A, DC voltage 500V are sputtered, nickel target shielding power supply is closed after the metal nickel layer that deposition thickness is 500nm.
Third walks：Argon flow amount is adjusted, maintains dynamic air pressure 5 × 10-1Pa is again turned on nickel target shielding power supply, simultaneously
Silver target sputtering power supply is opened, is controlled using computer, nickel target DC current is made to drop to 0 from 1A, and silver target sputtering power supply rises from 0
To 1A, whole process continues 5 minutes, and film thickness is about 400nm.
4th step closes nickel target power supply after the completion of third step, keeps silver-colored target power supply direct current 1A, deposition film thickness is to about 1 μm.
Up to 150N in the sample welding tensile test being prepared.
3 aluminium nitride ceramics of embodiment metallizes
The first step：Aluminium nitride ceramic substrate acetone, ethyl alcohol volume ratio 1 by specification for 10mm × 10mm × 0.3mm:1 mixing
Solution is cleaned by ultrasonic 15min；Deionized water is cleaned by ultrasonic 15min；Then in the case where temperature is 550 DEG C of atmospheric pressure environment, baking 1 is small
When.
Second step：Aluminium nitride ceramics thin slice after pre-treatment is put into vacuum cavity at once, by vacuum cavity in 15 minutes
The vacuum degree being evacuated to reaches 5 × 10-3Pa is filled with argon gas, and it is 1 × 10 that dynamic, which maintains air pressure,-1Pa - 2×10-1Within the scope of Pa, splash
DC current 1A, DC voltage 500V are penetrated, chromium target shielding power supply is closed after the metallic chromium layer that deposition thickness is 50nm.
Third walks：Argon flow amount is adjusted, maintains dynamic air pressure 5 × 10-1Pa is again turned on chromium target shielding power supply, simultaneously
Copper target shielding power supply is opened, is controlled using computer, chromium target DC current is made to drop to 0 from 1A, and copper target shielding power supply rises from 0
To 1A, whole process continues 1 minute, and film thickness is about 50nm.
4th step closes chromium target power supply after the completion of third step, keeps copper target power supply direct current 1A, deposition film thickness is to about 2 μm.
The microwave ceramic devices that 4th step is prepared are put into electroplating device by the 5th step, and plating is thickeied to 50 μm.
Up to 170N in the sample welding tensile test being prepared.
4 aluminium oxide ceramics of embodiment metallizes
The first step：95 alumina ceramic plate acetone, ethyl alcohol volume ratio 1 by specification for 100mm × 100mm × 0.3mm:1 is mixed
It closes solution and is cleaned by ultrasonic 5min；Deionized water is cleaned by ultrasonic 5min；Then in the case where temperature is 350 DEG C of atmospheric pressure environment, baking 1 is small
When.
Second step：Alumina ceramic plate after pre-treatment is put into vacuum cavity at once, takes out vacuum cavity in 15 minutes
Vacuum degree extremely reaches 5 × 10-3Pa is filled with argon gas, and it is 1 × 10 that dynamic, which maintains air pressure,-1Pa - 2×10-1Within the scope of Pa, sputtering
DC current 1A, DC voltage 500V, deposition thickness are closing chromium target shielding power supply after the metallic chromium layer of 50nm.
Third walks：Argon flow amount is adjusted, maintains dynamic air pressure 5 × 10-1Pa is again turned on chromium target shielding power supply, simultaneously
Copper target shielding power supply is opened, is controlled using computer, chromium target DC current is made to drop to 0 from 1A, and copper target shielding power supply rises from 0
To 1A, whole process continues 1 minute, and film thickness is about 50nm.
4th step closes chromium target power supply after the completion of third step, keeps copper target power supply direct current 1A, deposition film thickness is to about 2 μm.
The microwave ceramic devices that 4th step is prepared are put into electroplating device by the 5th step, and electro-coppering is thickeied to 50 μm.
Up to 200N in the sample welding tensile test being prepared.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations
Also it should be regarded as protection scope of the present invention.
Claims (7)
1. a kind of method improving ceramic surface metallization adhesive force, characterized in that include the following steps：
（1）Ceramic matrix pre-treatment：Ceramic matrix is cleaned with small polarity to big polar solvent successively；It is in temperature then
It is toasted 1 to 3 hours under 250 DEG C -680 DEG C of atmospheric pressure environment；
（2）Deposited metal layer A：Using magnetron sputtering technique, it is evacuated to vacuum 5 × 10-3After Pa, it is filled with argon gas, dynamic maintains air pressure
It is 1 × 10-1Pa-2×10-1Within the scope of Pa, deposition thickness is the metal layer A of 50nm-500nm；
（3）Deposit alloy layer AB：It is 5 × 10 to adjust argon flow amount dynamic and maintain air pressure-1Pa-1Pa, using the common magnetic control of A, B target
Sputtering sedimentation thickness is the alloy-layer AB of 20nm -500nm；
（4）Deposited metal layer B：Keep step（3）Air pressure conditions, again utilize magnetron sputtering technique deposition thickness be 200nm
The metal layer B of -2000nm.
2. a kind of method improving ceramic surface metallization adhesive force according to claim 1, characterized in that step
（1）Middle selection polar reagent includes several in acetone, ethyl alcohol, deionized water or combinations thereof, using ultrasonic cleaning 5-30 points
Clock.
3. a kind of method improving ceramic surface metallization adhesive force according to claim 1, characterized in that described
The one kind of metal layer A in titanium, chromium, nickel, aluminium, molybdenum, tungsten or its alloy.
4. a kind of method improving ceramic surface metallization adhesive force according to claim 1, characterized in that described
Metal layer B is selected from copper or silver.
5. a kind of method improving ceramic surface metallization adhesive force according to claim 1, characterized in that step
（3）It is middle use the technique of the common magnetron sputtering deposition of A, B target for：The shielding power supply that A, B target are controlled using computer, according to deposition film
The duration that thickness determines makes the sputtering power of A targets drop to 0%, while the sputtering power of B targets from 100% within the duration
100% is increased to from 0%.
6. a kind of method improving ceramic surface metallization adhesive force according to claim 1, characterized in that in step
Suddenly（4）According to the thickness requirement of metal layer B after completion, metal layer B is thickeied using plating or silk-screen printing technique, it is thick
Ranging from 2 μm -100 μm of degree.
7. a kind of method improving ceramic surface metallization adhesive force according to claim 1, characterized in that described
Ceramic matrix is selected from microwave ceramics, ferrite ceramics, aluminium nitride ceramics, aluminium oxide ceramics, dielectric ceramic, thermal sensitive ceramics, pressure-sensitive
Any one of ceramics, piezoelectric ceramics, ferroelectric ceramics, magnetic ceramics, silicon oxide ceramics or zirconia ceramics.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109461556A (en) * | 2018-11-15 | 2019-03-12 | 中国科学院新疆理化技术研究所 | A kind of preparation method of the Ohm contact electrode of p-type negative temperature coefficient ceramics material |
| CN109574713A (en) * | 2019-01-14 | 2019-04-05 | 广东致卓环保科技有限公司 | Method for surface metallation and its package substrate for aluminium nitride ceramics package substrate |
| CN110272721A (en) * | 2019-07-26 | 2019-09-24 | 中国电子科技集团公司第三十三研究所 | A kind of thermally conductive wave-absorbing powder of nitride/carbonyl iron and preparation method of core-shell structure |
| CN113174575A (en) * | 2021-03-31 | 2021-07-27 | 西安交通大学 | Method for preparing AlN ceramic substrate by metallization and heat sink integration |
| CN113403651A (en) * | 2021-06-21 | 2021-09-17 | 集美大学 | Method for improving coating uniformity of release agent by using nano coating |
| CN113981383A (en) * | 2020-10-30 | 2022-01-28 | 东莞市烽元科技有限公司 | Method for plating titanium film on surface of AlN ceramic matrix by multi-arc ions |
| CN114315427A (en) * | 2022-01-19 | 2022-04-12 | 四川科尔威光电科技有限公司 | Preparation process of metal system film for increasing adhesion between aluminum nitride ceramic and metal layer |
| CN115313012A (en) * | 2022-08-04 | 2022-11-08 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | Method for improving adhesive force of metal circuit on surface of ceramic nested ferrite substrate |
| CN116813388A (en) * | 2023-07-07 | 2023-09-29 | 四川富乐华半导体科技有限公司 | Sintering jig manufactured by ceramic metallization method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109461556A (en) * | 2018-11-15 | 2019-03-12 | 中国科学院新疆理化技术研究所 | A kind of preparation method of the Ohm contact electrode of p-type negative temperature coefficient ceramics material |
| CN109574713A (en) * | 2019-01-14 | 2019-04-05 | 广东致卓环保科技有限公司 | Method for surface metallation and its package substrate for aluminium nitride ceramics package substrate |
| CN110272721A (en) * | 2019-07-26 | 2019-09-24 | 中国电子科技集团公司第三十三研究所 | A kind of thermally conductive wave-absorbing powder of nitride/carbonyl iron and preparation method of core-shell structure |
| CN110272721B (en) * | 2019-07-26 | 2022-04-19 | 中国电子科技集团公司第三十三研究所 | Nitride/carbonyl iron heat-conducting wave-absorbing powder with core-shell structure and preparation method thereof |
| CN113981383B (en) * | 2020-10-30 | 2024-04-05 | 东莞市烽元科技有限公司 | Method for plating titanium film on AlN ceramic substrate surface by multi-arc ions |
| CN113981383A (en) * | 2020-10-30 | 2022-01-28 | 东莞市烽元科技有限公司 | Method for plating titanium film on surface of AlN ceramic matrix by multi-arc ions |
| CN113174575A (en) * | 2021-03-31 | 2021-07-27 | 西安交通大学 | Method for preparing AlN ceramic substrate by metallization and heat sink integration |
| CN113403651A (en) * | 2021-06-21 | 2021-09-17 | 集美大学 | Method for improving coating uniformity of release agent by using nano coating |
| CN114315427A (en) * | 2022-01-19 | 2022-04-12 | 四川科尔威光电科技有限公司 | Preparation process of metal system film for increasing adhesion between aluminum nitride ceramic and metal layer |
| CN115313012B (en) * | 2022-08-04 | 2023-11-03 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | Method for improving adhesion of metal circuit on surface of ceramic nested ferrite substrate |
| CN115313012A (en) * | 2022-08-04 | 2022-11-08 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | Method for improving adhesive force of metal circuit on surface of ceramic nested ferrite substrate |
| CN116813388A (en) * | 2023-07-07 | 2023-09-29 | 四川富乐华半导体科技有限公司 | Sintering jig manufactured by ceramic metallization method |
| CN116813388B (en) * | 2023-07-07 | 2023-12-26 | 四川富乐华半导体科技有限公司 | Sintering jig manufactured by ceramic metallization method |
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