CN112512221B - Preparation method of metal conductor-coated ceramic circuit substrate - Google Patents
Preparation method of metal conductor-coated ceramic circuit substrate Download PDFInfo
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- CN112512221B CN112512221B CN202011352684.3A CN202011352684A CN112512221B CN 112512221 B CN112512221 B CN 112512221B CN 202011352684 A CN202011352684 A CN 202011352684A CN 112512221 B CN112512221 B CN 112512221B
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- metal
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- metal film
- ceramic substrate
- ceramic
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/0011—Working of insulating substrates or insulating layers
- H05K3/0017—Etching of the substrate by chemical or physical means
- H05K3/0026—Etching of the substrate by chemical or physical means by laser ablation
- H05K3/0029—Etching of the substrate by chemical or physical means by laser ablation of inorganic insulating material
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/24—Reinforcing the conductive pattern
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/11—Treatments characterised by their effect, e.g. heating, cooling, roughening
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention discloses a preparation method of a metal conductor-coated ceramic circuit substrate, which comprises the following steps: s1: etching a desired circuit pattern on the ceramic substrate using a laser beam; s2: carrying out multi-layer metal chemical coating; s3: and carrying out one-time hydrogen-passing sintering reaction. The metal conductor-coated ceramic circuit substrate prepared by the invention has the characteristics of high bonding strength, good conductivity, high substrate strength, excellent quality and the like.
Description
Technical Field
The invention relates to the technical field of electronic ceramic materials, in particular to a preparation method of a metal conductor-coated ceramic circuit substrate.
Background
The existing aluminum nitride-silicon nitride ceramic substrate coated with metal conductors (copper, gold, silver, nickel and the like) circuit mainly comprises two methods: active metal brazing ceramic substrate (AlN or Si) by (AMB indirect metal conductor copper, nickel and the like) method 3 N 4 ) The solder is prepared by using a small amount of active elements (usually, transition group elements such as: titanium, zirconium, etc.), and a small amount of glass phase in the ceramic substrate are sintered to react to obtain a transition intermediate layer, and then the transition intermediate layer is coated with conductor copper (or other large metals) to be sintered and adhered; a. a thin film method: the metal film is prepared by adopting PVD methods such as ion plating, vacuum evaporation, sputtering coating and the like. These methods are large in equipment investment and difficult to produce on a large scale. b. A thick film method: the thick film paste is prepared, and a conductor or a resistor is formed on a ceramic substrate by screen printing and then sintered to form a circuit. The method has insufficient bonding strength and is greatly affected by temperature control. c. Chemical coating method: the metal ions in the solution are reduced on the surface of the ceramic substrate with catalytic activity by utilizing a reducing agent to form a metal coating. This method has a drawback that the bonding strength is not high. The other method (DBC direct copper coating method) is to firstly prepare a ceramic substrate (AlN or Si) 3 N 4 Etc.) is subjected to thermal (oxidation) treatment, and then the oxide layer is bonded and sintered with the conductor copper oxide layer (or other metals) for adhesion. The main drawback is the low reliability.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a metal conductor-coated ceramic circuit substrate, which has the advantages of high bonding strength, good conductivity, high substrate strength and excellent quality.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the metal conductor-coated ceramic circuit substrate comprises the following steps:
s1: etching a desired circuit pattern on the ceramic substrate using a laser beam;
s2: carrying out multi-layer metal chemical coating;
s3: and carrying out one-time hydrogen peroxide sintering reaction.
Preferably, before the step S1, the laser beam engraving a circuit pattern, the method further includes the steps of: a. selecting an aluminum nitride and silicon nitride ceramic substrate; b. deoiling, ultrasonically cleaning and drying the selected ceramic substrate; c. a laser engraving machine with a selected thermal effect.
Preferably, the laser beam patterning comprises the following specific steps: a. adjusting the size of the laser beam port to achieve the width of the circuit path; b. adjusting power and speed by using a test piece; c. setting a reasonable program control program for engraving circuit patterns; d. the ceramic substrate of the device is automatically carved into a required circuit diagram board.
Preferably, the specific steps of performing the multilayer metal electroless plating comprise: a. soaking the ceramic substrate etched by the laser in a hydrochloric acid solution with the concentration of 20% for 3 minutes, taking out the ceramic substrate, washing the ceramic substrate in tap water, and then performing ultrasonic decontamination and cleaning in deionized water with the temperature of 50 ℃; b. immersing the cleaned ceramic substrate in an activating solution for 1-3 minutes; c. chemically plating a first metal film in the prepared bottom layer chemical plating solution; d. chemically plating a second metal film on the first metal film; e. chemically plating a third metal film on the second metal film; f. and after the chemical plating, carrying out ultrasonic cleaning and drying.
Preferably, the first metal film comprises Ti or Fe, and the thickness is 0.8-1.8 um.
Preferably, the second metal film comprises Ag or Ni and has a thickness of 0.5-1.5 um.
Preferably, the third metal film comprises Cu or Pt or Au, and the thickness is 2.5-8.5 um.
Preferably, the hydrogen peroxide sintering reaction comprises the following specific steps: a. selecting proper kiln furniture, and carrying out boat loading preparation on the ceramic substrate coated with the film; b. setting a temperature rise curve, rising the temperature at 5 degrees/minute before 300 degrees, then rising the temperature at 10 degrees/minute until 1150-1250 degrees, and preserving the temperature for 60 minutes; c. introducing dry hydrogen or nitrogen before 800 ℃, introducing wet hydrogen after 800 ℃ until high temperature heat preservation, then cooling to 800 ℃, ending introducing wet hydrogen, and turning to introduce nitrogen to blow out; d. cooling to below 80 ℃, opening the furnace and taking out the parts.
Preferably, the activating solution is PdCl 2-SnCl 2.
Compared with the prior art, the invention has the advantages that: the metal conductor-coated ceramic circuit substrate prepared by the invention has the characteristics of high bonding strength, good conductivity, high substrate strength, excellent quality and the like.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples, and it should be understood that the described examples are only a few examples of the present invention, rather than all examples, and that all other examples obtained by those skilled in the art based on the examples of the present invention without any inventive step are within the scope of the present invention.
The preparation method of the metal conductor-coated ceramic circuit substrate of the embodiment comprises the following steps:
s1: etching a desired circuit pattern on the ceramic substrate using a laser beam;
s2: carrying out multi-layer metal chemical coating;
s3: and carrying out one-time hydrogen-passing sintering reaction.
In this embodiment, the laser beam parameters are adjusted to obtain the required heat during the engraving process, so as to obtain a uniform oxide-oxide layer (which is a defect that the oxide layer is obtained only by a thermal [ oxidation ] treatment process in the DBC direct copper-coating method and is difficult to control) of the required ceramic substrate material at the engraving position, so that the subsequent sintering reaction with other metals to form compounds enhances the bonding force. Meanwhile, the circuit track of the needed rough surface can be obtained and adjusted after laser beam engraving, and preparation is made for omitting the process of roughening before subsequent chemical coating (in the chemical coating method, the chemical coating can be carried out after roughening is carried out on the position needing to be coated on the ceramic substrate so as to enhance the adhesive bonding force). Moreover, the ceramic substrate is not subjected to roughening treatment by a chemical method, so that the mechanical strength and the heat conducting property of the ceramic substrate are ensured.
In this embodiment, a plurality of metal electroless plating layers are formed to form one or more metal films of underlying metals (Ti, fe, mg, zn, cr, al, si, B, etc.), and the metal films are sintered to react with an oxide layer of a substrate to form a spinel-type compound. This forms a bonding transition layer and also greatly increases the bonding force. And one or more than two metal layers of complex conductive metals (Ag, pt, ni, cu, au and the like) are chemically plated on the metal of the bottom layer, so that the metal layers can be well fused with each other in a cooling manner and can well conduct electricity and heat.
In this embodiment, electroless plating is melted between a plurality of metal films on a desired circuit pattern, and the melted body and an oxide layer on a ceramic substrate are reacted with each other to form a compound at an interface. The high-strength metal film-coated ceramic circuit substrate is obtained, and has good electric and thermal conductivity.
Wherein, before the laser beam engraving circuit pattern in the step S1, the method further comprises the following steps: a. selecting an aluminum nitride ceramic substrate and a silicon nitride ceramic substrate; b. deoiling the selected ceramic substrate for 3 minutes, ultrasonically cleaning for 15 minutes, and drying in an oven at 60 ℃; c. selecting a laser engraving machine with thermal effect.
The laser beam engraving circuit pattern comprises the following specific steps: a. adjusting the size of the laser beam port to achieve the width of the circuit path; b. adjusting power and speed by using a test piece to obtain the optimal thickness of an oxide layer within the range of 3-8 um, and simultaneously obtaining the roughness of the surface of a circuit path between 0.8 and 1.2um; c. setting a reasonable program control program for engraving circuit patterns; d. the ceramic substrate of the device is automatically carved into a required circuit diagram board.
The specific steps of carrying out the multilayer metal chemical plating comprise: a. soaking the ceramic substrate etched by the laser in a hydrochloric acid solution with the concentration of 20% for 3 minutes, taking out the ceramic substrate, washing the ceramic substrate in tap water, and then performing ultrasonic decontamination and cleaning in deionized water with the temperature of 50 ℃; b. immersing the cleaned ceramic substrate in an activating solution for 1-3 minutes; c. chemically plating a first metal film in the prepared bottom layer chemical plating solution; d. chemically plating a second metal film on the first metal film; e. chemically plating a third metal film on the second metal film; f. and after the chemical plating, carrying out ultrasonic cleaning and drying.
Wherein, the first layer of metal film comprises Ti or Fe, and the thickness is 0.8-1.8 um.
Wherein, the second layer of metal film comprises Ag or Ni, and the thickness is 0.5-1.5 um.
In this embodiment, the lower melting points of Ag and Ni play a role in fluxing and cooling.
Wherein the third layer of metal film comprises Cu or Pt or Au, and the thickness is 2.5-8.5 um.
In this example, cu, pt, and Au are metals having good conductivity and not easily oxidized.
Wherein, the hydrogen-passing sintering reaction comprises the following specific steps: a. selecting proper kiln furniture, and carrying out boat loading preparation on the ceramic substrate coated with the film; b. setting a temperature rise curve, rising the temperature at 5 degrees/minute before 300 degrees, then rising the temperature at 10 degrees/minute until 1150-1250 degrees, and preserving the temperature for 60 minutes; c. introducing dry hydrogen or nitrogen before 800 ℃, introducing wet hydrogen after 800 ℃ until high temperature is kept, cooling to 800 ℃, introducing wet hydrogen, and turning to introduce nitrogen to blow out; d. cooling to below 80 ℃, opening the furnace and taking out the parts.
Wherein the activating solution is PdCl 2-SnCl 2.
The above is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above-described examples. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.
Claims (9)
1. A preparation method of a metal conductor-coated ceramic circuit substrate is characterized by comprising the following steps:
s1: etching a desired circuit pattern on the ceramic substrate using a laser beam;
s2: performing multi-layer metal chemical plating to obtain one or more than two metal films of the bottom layer metal, sintering the metal films to react with the substrate oxide layer to form a spinel-type compound, and chemically plating one or more than two metal layers of complex conductive metals on the bottom layer metal;
s3: and carrying out one-time hydrogen-passing sintering reaction.
2. The method for producing a metal conductor-clad ceramic circuit substrate as set forth in claim 1, wherein: before the step S1, the laser beam engraving a circuit pattern further comprises the steps of: a. selecting an aluminum nitride and silicon nitride ceramic substrate; b. degreasing the selected ceramic substrate, ultrasonically cleaning and drying; c. a laser engraving machine with a selected thermal effect.
3. The method of manufacturing a metal conductor-clad ceramic circuit substrate as set forth in claim 2, wherein: the laser beam circuit pattern engraving method specifically comprises the following steps: a. adjusting the size of the laser beam port to achieve the width of the circuit path; b. adjusting power and speed by using a test piece; c. setting a reasonable program control program for engraving circuit patterns; d. the ceramic substrate of the device is automatically carved into a required circuit diagram board.
4. The method of manufacturing a metal conductor-clad ceramic circuit substrate as set forth in claim 3, wherein: the specific steps for carrying out the multilayer metal electroless plating comprise: a. soaking the ceramic substrate etched by the laser in a hydrochloric acid solution with the concentration of 20% for 3 minutes, taking out the ceramic substrate, washing the ceramic substrate in tap water, and then performing ultrasonic decontamination and cleaning in deionized water with the temperature of 50 ℃; b. immersing the cleaned ceramic substrate in an activating solution for 1-3 minutes; c. chemically plating a first metal film in the prepared bottom layer chemical plating solution; d. chemically plating a second metal film on the first metal film; e. chemically plating a third metal film on the second metal film; f. and after the chemical plating, carrying out ultrasonic cleaning and drying.
5. The method of manufacturing a metal conductor-clad ceramic circuit substrate as claimed in claim 4, wherein: the first layer of metal film comprises Ti or Fe, and the thickness of the first layer of metal film is 0.8-1.8 um.
6. The method of manufacturing a metal conductor-clad ceramic circuit substrate as claimed in claim 4, wherein: the second layer of metal film comprises Ag or Ni, and the thickness of the second layer of metal film is 0.5-1.5 um.
7. The method of manufacturing a metal conductor-clad ceramic circuit substrate as claimed in claim 4, wherein: the third layer of metal film comprises Cu or Pt or Au, and the thickness is 2.5-8.5 um.
8. The method of manufacturing a metal conductor-clad ceramic circuit substrate as claimed in claim 4, wherein: the hydrogen-passing sintering reaction comprises the following specific steps: a. selecting proper kiln furniture, and carrying out boat loading preparation on the ceramic substrate coated with the film; b. setting a temperature rise curve, rising the temperature at 5 degrees/minute before 300 degrees, then rising the temperature at 10 degrees/minute until 1150-1250 degrees, and preserving the temperature for 60 minutes; c. introducing dry hydrogen or nitrogen before 800 ℃, introducing wet hydrogen after 800 ℃ until high temperature is kept, cooling to 800 ℃, introducing wet hydrogen, and turning to introduce nitrogen to blow out; d. cooling to below 80 ℃, opening the furnace and taking out the parts.
9. The method of manufacturing a metal conductor-clad ceramic circuit substrate as claimed in claim 4, wherein: the activating solution is PdCl 2-SnCl 2.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011352684.3A CN112512221B (en) | 2020-11-26 | 2020-11-26 | Preparation method of metal conductor-coated ceramic circuit substrate |
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| CN202011352684.3A CN112512221B (en) | 2020-11-26 | 2020-11-26 | Preparation method of metal conductor-coated ceramic circuit substrate |
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| CN112512221A CN112512221A (en) | 2021-03-16 |
| CN112512221B true CN112512221B (en) | 2023-03-21 |
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| US6800211B2 (en) * | 2002-08-26 | 2004-10-05 | Tong Hsing Electric Industries Ltd. | Method for removing voids in a ceramic substrate |
| CN104392935A (en) * | 2014-11-10 | 2015-03-04 | 北京大学东莞光电研究院 | Metallization method of power device module encapsulation-used ceramic substrate |
| CN108054106B (en) * | 2018-01-11 | 2020-03-27 | 北京大学东莞光电研究院 | Method for preparing high-heat-dissipation ceramic packaging substrate |
| CN108658627B (en) * | 2018-06-01 | 2020-06-02 | 中国工程物理研究院流体物理研究所 | Metallization method of aluminum nitride ceramic |
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