CN103559940A - Copper electronic paste and preparation method and application thereof - Google Patents
Copper electronic paste and preparation method and application thereof Download PDFInfo
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- CN103559940A CN103559940A CN201310562651.5A CN201310562651A CN103559940A CN 103559940 A CN103559940 A CN 103559940A CN 201310562651 A CN201310562651 A CN 201310562651A CN 103559940 A CN103559940 A CN 103559940A
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Abstract
The invention belongs to the technical field of microelectronic packaging and relates to copper electronic paste and a preparation method and application thereof. Copper is adopted to serve as a raw material for preparing oil or water electronic paste which can be applied to the surface copper coating technology of ceramic, glass and high polymer material substrate. Compared with copper-containing electronic paste and forming process commonly used at present, the copper electronic paste and preparation method and application of the copper electronic paste have the advantages of that a raw material price is low, the finished product rate is high, a device is simple, process is simple and convenient, metal patterning is convenient, and the thickness of a copper layer is controllable, so that cost reduction and performance improvement are achieved. The copper electronic paste and preparation method and application of copper electronic paste can be applied to large power devices and large scale integrated circuits and will have good application prospects.
Description
Technical field
Appearance along with the various novel high-density packing forms of modern microelectronics, integrated circuit is just towards high integration, wiring granular, chip large scale development, the baseplate material adapting is with it except possessing low stress, low-thermal-expansion, also must possess efficient heat sinking function, and and the thermal coefficient of expansion that matches of semi-conducting material to reduce the thermal stress between components and parts and substrate.
Electrical insulating property and lower dielectric constant, to be applicable to high-frequency circuit, reduce time delay preferably.And the thermal conductivity of copper is 400W/mK, be one of the most frequently used baseplate material, can utilize the high thermal conductivity of copper metal that these microelectronics power devices or chip are loaded on to the heat derivation that the components and parts on substrate produce.
At present in the industrial method that realizes the combinations such as metal and pottery, macromolecular material, glass, mainly contain thick film and molybdenum manganese method etc.Wherein the particulate of precious metal being formed by being crimped on together, then adhered on base material by the glass of melting, is thick film.But the electric conductivity of thick film is poorer than metallic copper, and the temperature of sintering is more than 1000 ℃.Molybdenum manganese method is more ripe technical process; by realizing pottery and the good adhesive force of metal layer at basis material and the counterdiffusion of metal layer phase; but the temperature of sintering is often more than 1500 ℃; also need certain protective atmosphere; and the formed intermediate layer of this method is thicker; thermal resistance is still larger, is unfavorable for heat radiation rapidly in the fields such as high-power circuit, power model.Ceramic direct copper (DBC) substrate occurring in recent years combines copper and ceramic excellent properties, and is applied in high power device.DBC substrate is before applying termination process or in process, between copper and pottery, introduces appropriate oxygen element, within the scope of 1065 ℃～1083 ℃, and copper and oxygen formation Cu-O eutectic liquid, its eutectic liquid has been realized the combination of ceramic substrate and copper coin.But the content of accurately controlling micro amount of oxygen in its preparation process is difficult to accurately accomplish in industrial production.Therefore working out appropriate material system and easy process, to realize that metallic copper combines closely with pottery, macromolecular material, glass etc. be focus and the difficult point of studying always.
Summary of the invention
It is that the sintering temperature that exists in prior art is too high that the present invention will solve; the problem that needs reduction or protective atmosphere; provide and produce a kind of low-melting glass and reducing agent of utilizing in copper series electron slurry of air low temperature sintering and preparation method thereof and the application in bonded copper base; can be used in the application of pottery, glass, macromolecular material base material, can control copper layer thickness, facilitate metal patternization, reduce the production cost that applies copper ceramic substrate.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of copper series electron slurry of the present invention, comprises following component:
Copper powder, low-melting glass, reducing agent, alcohol, organic carrier.
In described copper series electron slurry, each ingredients weight parts is:
35～55 parts of copper powders
5～15 parts of low-melting glasses
10～20 parts of reducing agents
25～45 parts of alcohol
1～3 part of organic carrier.
Described reducing agent is one or more the combination in Mg powder, Zn powder, Ti powder, C powder.
Described organic carrier is one or more combination in castor oil, dibutyl phthalate, polyethylene glycol, ethyl cellulose, methylcellulose.
Described alcohol is one or more combination in methyl alcohol, ethanol, propyl alcohol, terpinol, polyvinyl alcohol.
The fusing point of described glass powder with low melting point is less than or equal to 700 ℃.
The particle diameter of described copper powder is less than 10 microns.
The preparation method of a kind of copper series electron slurry of the present invention, comprises the steps:
By copper powder, glass powder with low melting point, reducing agent, alcohol, organic carrier according to 35～55: 5～15: the weight ratio of 10～20:25～45:1～3 is mixed, after mixing, being ground to fineness and being 10 microns of following, viscosity is 0.1～100Pa.s.
A kind of copper series electron slurry of the present invention is prepared the method for bonded copper base, comprises the steps:
S1, by described copper series electron slurry coating at substrate surface, forming thickness is the coating of 20～150 μ m;
S2, the substrate that is coated with described copper series electron slurry making is placed in to 100～600 ℃ of environment heat-treats in step S1, obtain being coated with the substrate of copper layer;
S3, the copper layer in the substrate that is coated with copper layer making in step S2 is carried out to polishing, obtain described bonded copper base.
Substrate described in step S1 is a kind of in ceramic substrate, macromolecular material substrate or glass substrate; In step S2, the heat treated time is 8-24 hour.
Technique scheme of the present invention has the following advantages compared to existing technology:
1, a kind of copper series electron slurry provided by the present invention is with copper powder, and the reducing agent metal of glass powder with low melting point and anti-oxidation is main feature: raw material is easy to get, with low cost, and Stability of Slurry is high, and modest viscosity is not oxidizable under high temperature.
2, the preparation method of a kind of copper series electron slurry provided by the present invention, at air low temperature sintering, technique is simple.
3, the application of a kind of copper series electron slurry provided by the present invention in bonded copper base, metal patternization is convenient, copper layer is fine and close continuously, copper layer resistance and thermal resistance low, pattern precision is controlled.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of copper layer in bonded copper base described in example 1 of the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
Embodiment 1
The present embodiment provides a kind of copper series electron slurry and preparation method thereof and the application in bonded copper base.
The component of described copper series electron slurry and weight portion thereof are copper powder, low-melting glass, reducing agent, alcohol, organic carrier, and its ratio is 43:8:13:34:2; Wherein said reducing agent is zinc powder, described alcohol is 5wt% polyvinyl alcohol water solution, described organic carrier is rilanit special, polyethylene glycol and dibutyl phthalate, and the fusing point of described glass powder with low melting point is 600 ℃～700 ℃, and the particle diameter of described copper powder is below 10 μ m.
The preparation method of described copper series electron slurry is:
By copper powder body 43g, 5wt% polyvinyl alcohol water solution 34g, rilanit special 0.7g, polyethylene glycol 0.7g and dibutyl phthalate 0.6g, glass powder with low melting point 8g, reducing agent 13g mixes, and on planetary ball mill ball milling 2 hours, so just obtained water system copper electric slurry, by (instrument), recording fineness is 10 μ m, and viscosity is 10Pa.s.
The preparation method of described bonded copper base is:
S1: alumina ceramic plate is put into acetone or alcohol solution, and ultrasonic cleaning 15 minutes in ultrasonic cleaner, taking-up is dried; On coating machine, by rotary coating, described copper series electron slurry is evenly coated with on aluminium oxide ceramics surface subsequently, obtaining coating layer thickness is 20 μ m.
S2, the substrate that is coated with described copper series electron slurry prepared in step S1 is put into cabinet-type electric furnace, be heated to 400 ℃ under air, sintering 8 hours is also cooling with stove, and sample to be sintered takes out after being cooled to room temperature.
S3, ethanol for the copper layer in the substrate that is coated with copper layer making in step S2 or acetone are cleaned, then carry out polishing, obtain described bonded copper base.
Embodiment 2
The present embodiment provides a kind of copper series electron slurry, comprises following component:
35 parts of copper powders
15 parts of low-melting glasses
10 parts of reducing agents
39 parts of alcohol
1 part of organic carrier.
Described reducing agent is Mg powder and the combination of Zn powder.
Described organic carrier is the combination of castor oil and dibutyl phthalate.
Described alcohol is methyl alcohol.
The fusing point of described glass powder with low melting point is 550～600 ℃.
The particle diameter of described copper powder is 5 microns.
The preparation method of described a kind of copper series electron slurry, comprises the steps:
Copper powder, glass powder with low melting point, reducing agent, alcohol, organic carrier are mixed according to aforementioned proportion, and after mixing, being ground to fineness and being 4 microns, viscosity is 25Pa.s.
Described a kind of copper series electron slurry is prepared the method for bonded copper base, comprises the steps:
S1, alumina ceramic plate is put into acetone or alcohol solution, and ultrasonic cleaning 15 minutes in ultrasonic cleaner, taking-up is dried; On coating machine, by rotary coating, described copper series electron slurry is evenly coated with on aluminium oxide ceramics surface subsequently, forming thickness is the coating of 20 μ m;
S2, the substrate that is coated with described copper series electron slurry prepared in step S1 is put into cabinet-type electric furnace, be heated to 100 ℃ under air, sintering 8 hours is also cooling with stove, and sample to be sintered takes out after being cooled to room temperature, obtains being coated with the substrate of copper layer;
S3, the copper layer in the substrate that is coated with copper layer making in step S2 is carried out to polishing, obtain described bonded copper base.
As other embodiment of the present invention; substrate described in step S1 can also be in ceramic substrate, macromolecular material substrate or glass substrate a kind of; in step S2, the heat treated time is 8-24 hour, all can realize object of the present invention, belongs to protection scope of the present invention.
Embodiment 3
The present embodiment provides a kind of copper series electron slurry, comprises following component:
55 parts of copper powders
5 parts of low-melting glasses
12 parts of reducing agents
25 parts of alcohol
3 parts of organic carriers.
Described reducing agent is C powder.
Described organic carrier is the combination of polyethylene glycol and ethyl cellulose.
Described alcohol is ethanol.
The fusing point of described glass powder with low melting point is less than or equal to 700 ℃.
The particle diameter of described copper powder is less than 10 microns.
The preparation method of described a kind of copper series electron slurry, comprises the steps:
Copper powder, glass powder with low melting point, reducing agent, alcohol, organic carrier are proportionally mixed, and after mixing, being ground to fineness is that 9 μ m, viscosity are 100Pa.s.
Described a kind of copper series electron slurry is prepared the method for bonded copper base, comprises the steps:
S1, alumina ceramic plate is put into acetone or alcohol solution, and ultrasonic cleaning 15 minutes in ultrasonic cleaner, taking-up is dried; On coating machine, by rotary coating, described copper series electron slurry is evenly coated with on aluminium oxide ceramics surface subsequently, forming thickness is the coating of 70 μ m;
S2, the substrate that is coated with described copper series electron slurry prepared in step S1 is put into cabinet-type electric furnace, be heated to 600 ℃ under air, sintering 15 hours is also cooling with stove, and sample to be sintered takes out after being cooled to room temperature, obtains being coated with the substrate of copper layer;
S3, the copper layer in the substrate that is coated with copper layer making in step S2 is carried out to polishing, obtain described bonded copper base.
Embodiment 4
The present embodiment provides a kind of copper series electron slurry, comprises following component:
35 parts of copper powders
9 parts of low-melting glasses
10 parts of reducing agents
45 parts of alcohol
1 part of organic carrier.
Described reducing agent is Ti powder.
Described organic carrier is polyvinyl alcohol.
Described alcohol is propyl alcohol.
The fusing point of described glass powder with low melting point is 600 ℃～700 ℃.
The particle diameter of described copper powder is 2 μ m.
The preparation method of described a kind of copper series electron slurry, comprises the steps:
Copper powder, glass powder with low melting point, reducing agent, alcohol, organic carrier are mixed according to aforementioned proportion, and after mixing, being ground to fineness is that 1.5 μ m, viscosity are 150pa.s.
Described a kind of copper series electron slurry is prepared the method for bonded copper base, comprises the steps:
S1, alumina ceramic plate is put into acetone or alcohol solution, and ultrasonic cleaning 15 minutes in ultrasonic cleaner, taking-up is dried; On coating machine, by rotary coating, described copper series electron slurry is evenly coated with on aluminium oxide ceramics surface subsequently, forming thickness is the coating of 100 μ m;
S2, the substrate that is coated with described copper series electron slurry prepared in step S1 is put into cabinet-type electric furnace, be heated to 300 ℃ under air, sintering 12 hours is also cooling with stove, and sample to be sintered takes out after being cooled to room temperature, obtains being coated with the substrate of copper layer;
S3, the copper layer in the substrate that is coated with copper layer making in step S2 is carried out to polishing, obtain described bonded copper base.
Embodiment 5
The present embodiment provides a kind of copper series electron slurry, comprises following component:
40 parts of copper powders
10 parts of low-melting glasses
20 parts of reducing agents
28 parts of alcohol
2 parts of organic carriers.
Described reducing agent is Mg powder.
Described organic carrier is dibutyl phthalate.
Described alcohol is the combination of propyl alcohol and terpinol.
The fusing point of described glass powder with low melting point is 500 ℃～700 ℃.
The particle diameter of described copper powder is 0.5 μ m～10 μ m.
The preparation method of described a kind of copper series electron slurry, comprises the steps:
Copper powder, glass powder with low melting point, reducing agent, alcohol, organic carrier are mixed according to aforementioned proportion, and after mixing, being ground to fineness is that 0.4 μ m～9 μ m, viscosity are 50pa.s～500Pa.s.
Described a kind of copper series electron slurry is prepared the method for bonded copper base, comprises the steps:
S1, alumina ceramic plate is put into acetone or alcohol solution, and ultrasonic cleaning 15 minutes in ultrasonic cleaner, taking-up is dried; On coating machine, by rotary coating, described copper series electron slurry is evenly coated with on aluminium oxide ceramics surface subsequently, forming thickness is the coating of 80 μ m;
S2, the substrate that is coated with described copper series electron slurry prepared in step S1 is put into cabinet-type electric furnace, be heated to 500 ℃ under air, sintering 24 hours is also cooling with stove, and sample to be sintered takes out after being cooled to room temperature, obtains being coated with the substrate of copper layer;
S3, the copper layer in the substrate that is coated with copper layer making in step S2 is carried out to polishing, obtain described bonded copper base.
Embodiment 6:
The present embodiment provides a kind of copper series electron slurry, and component and preparation method are with embodiment 1.The method that described a kind of copper series electron slurry is prepared bonded copper base is also with embodiment 1, unique different be by silk screen printing, at glass surface, to form circuitous pattern in step S1.
Above-mentioned embodiment of the present invention all can only think explanation of the present invention can not limit the present invention, and claims have been pointed out scope of the present invention.Therefore, in the situation that not violating basic thought of the present invention, at metal, apply and connect in the production process of basis material, as long as having adopted copper powder is raw material, metal powder or the C powder of low-melting glass and reducing agent have been adopted, and similar to additive of the present invention, maybe can carry out multiple modification and replacement.Therefore, this modification and replacement are also interpreted as falling into scope of the present invention.Concrete protection range of the present invention limits by claims.
Claims (10)
1. a copper series electron slurry, is characterized in that, comprises following component:
Copper powder, low-melting glass, reducing agent, alcohol, organic carrier.
2. a kind of copper series electron slurry according to claim 1, is characterized in that, each ingredients weight parts is:
35～55 parts of copper powders
5～15 parts of low-melting glasses
10～20 parts of reducing agents
25～45 parts of alcohol
1～3 part of organic carrier.
3. a kind of copper series electron slurry according to claim 1 and 2, is characterized in that, described reducing agent is one or more the combination in Mg powder, Zn powder, Ti powder, C powder.
4. according to the arbitrary described a kind of copper series electron slurry of claim 1-3, it is characterized in that, described organic carrier is one or more combination in castor oil, dibutyl phthalate, polyethylene glycol, ethyl cellulose, methylcellulose.
5. according to the arbitrary described a kind of copper series electron slurry of claim 1-4, it is characterized in that, described alcohol is one or more combination in methyl alcohol, ethanol, propyl alcohol, terpinol, polyvinyl alcohol.
6. according to the arbitrary described a kind of copper series electron slurry of claim 1-5, it is characterized in that, the fusing point of described glass powder with low melting point is less than or equal to 700 ℃.
7. according to the arbitrary described a kind of copper series electron slurry of claim 1-6, it is characterized in that, the particle diameter of described copper powder is less than 10 microns.
8. a preparation method for the arbitrary described copper series electron slurry of claim 1-7, is characterized in that, comprises the steps:
Copper powder, glass powder with low melting point, reducing agent, alcohol, organic carrier are mixed according to the weight ratio of 35～55:5～15:10～20:25～45:1～3, and after mixing, being ground to fineness and being 10 microns of following, viscosity is 0.1～100Pa.s.
9. the arbitrary described copper series electron slurry of claim 1-7 is prepared a method for bonded copper base, it is characterized in that, comprises the steps:
S1, by the arbitrary described copper series electron slurry coating of claim 1-7 at substrate surface, forming thickness is the coating of 20～150 μ m;
S2, the substrate that is coated with described copper series electron slurry making is placed in to 100～600 ℃ of environment heat-treats in step S1, obtain being coated with the substrate of copper layer;
S3, the copper layer in the substrate that is coated with copper layer making in step S2 is carried out to polishing, obtain described bonded copper base.
10. copper series electron slurry according to claim 9 is prepared the method for bonded copper base, it is characterized in that, substrate described in step S1 is a kind of in ceramic substrate, macromolecular material substrate or glass substrate; In step S2, the heat treated time is 8-24 hour.
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| CN105439643A (en) * | 2015-11-16 | 2016-03-30 | 徐州中韵新材料科技有限公司 | Method for preparing copper/ceramic composite substrate on basis of low-melting-point glass powder |
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| CN105957642A (en) * | 2016-06-08 | 2016-09-21 | 天津大学 | Preparation method for silicon-dioxide-coated copper electronic paste used for LTCC substrate |
| CN106887268A (en) * | 2017-01-07 | 2017-06-23 | 东莞易力禾电子有限公司 | Silk-screen printing circuit electrode and preparation method thereof |
| CN108624271A (en) * | 2018-05-30 | 2018-10-09 | 盐城工学院 | A kind of cupric conductive adhesive and preparation method thereof |
| CN109411113A (en) * | 2017-08-18 | 2019-03-01 | 西安宏星电子浆料科技有限责任公司 | Groove Self-leveling conductor paste and its application method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105439643A (en) * | 2015-11-16 | 2016-03-30 | 徐州中韵新材料科技有限公司 | Method for preparing copper/ceramic composite substrate on basis of low-melting-point glass powder |
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| CN106887268A (en) * | 2017-01-07 | 2017-06-23 | 东莞易力禾电子有限公司 | Silk-screen printing circuit electrode and preparation method thereof |
| CN109411113A (en) * | 2017-08-18 | 2019-03-01 | 西安宏星电子浆料科技有限责任公司 | Groove Self-leveling conductor paste and its application method |
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Application publication date: 20140205 |