CN107639237A - Cu/SiO2The preparation method of composite, its preparation method and copper ceramic substrate - Google Patents
Cu/SiO2The preparation method of composite, its preparation method and copper ceramic substrate Download PDFInfo
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Abstract
The invention provides a kind of Cu/SiO2The preparation method of composite, comprises the following steps：Mantoquita, nano silicon, reducing agent and protective agent are subjected to hydro-thermal reaction, obtain Cu/SiO2Composite.Present invention also provides one kind to utilize Cu/SiO2The method that composite prepares copper ceramic substrate, comprises the following steps：By Cu/SiO2Composite mixes with organic solvent, obtains Nanometer Copper cream；The Nanometer Copper cream is printed in ceramic base plate surface, then is sintered, photoetching, development and plating is finally carried out successively, obtains copper ceramic substrate.During the application prepares copper ceramic substrate, due to Cu/SiO2The nanometer size effect of composite and Nano-meter SiO_2 therein2Can with the alundum (Al2O3) in ceramic substrate, nitridation reactive aluminum, so as to realize at a relatively low sintering temperature the high intensity between copper ceramics be bonded.
Description
Technical field
The present invention relates to technical field of electronic encapsulation, more particularly to Cu/SiO2Composite, its preparation method and copper-pottery
The preparation method of porcelain substrate.
Background technology
For power electronics encapsulation for, ceramic substrate due to high heat conductance, make heat from chip export, realize
Electrical interconnection and heat exchange with the external world, while also have the function of wiring (point interconnection) and mechanical support concurrently.Currently used radiating
Substrate mainly includes LTCC, HTCC, DBC and DPC ceramic substrate etc..LTCC and HTCC substrate interior metal circuit layers use silk
Net typography is made, be also easy to produce circuit it is coarse, contraposition not precisely, shrinkage rates problem, in high heat conduction, high power density, height
Application under pressure and high current environment is limited.
DBC substrate properties are good, high-power suitable for high withstand voltage.However, ceramic substrate nude film and metal material
Respond is low, wetability is poor, therefore stomata is also easy to produce between ceramic substrate and copper sheet finally so that bond strength reduces；In addition
Metallization process is complicated, and sintering temperature is of a relatively high (sintering temperature is about 1065 DEG C), and cost is difficult to effectively be controlled always
System, can be only applied to the field of specific demand at present.DPC substrates are the seeds that circuit and figure are completed using thin film technique
Layer, then circuit and figure are thickeied with the mode of electrochemical deposition, and then complete the metallization of whole substrate.But current DPC substrates
The problem of needing to overcome is that Seed Layer is low with ceramic substrate respond, is also easy to produce stomata so that bond strength reduces.
The method that the Chinese patent of application number 201110310121.2 discloses preparing metallized ceramic substrate by low-temperature sintering,
It is first to plate layer of metal layer in ceramic base plate surface, and then by silk-screen printing technique, nano metal cream is printed on into ceramics
Substrate surface forms metal layer of paste, is finally sintered at certain temperature and atmosphere.This method equally exists DPC substrate kinds
The problem of sublayer is with ceramic substrate bond strength deficiency.
The content of the invention
Present invention solves the technical problem that it is to provide a kind of Cu/SiO2Composite, its preparation method and copper-ceramic base
The preparation method of plate, the preparation method for copper-ceramic substrate that the application provides, it can realize at a lower temperature between copper-ceramics
High intensity bonding.
In view of this, this application provides a kind of Cu/SiO2The preparation method of composite, comprises the following steps：
Mantoquita, nano silicon, reducing agent and reducing agent are subjected to hydro-thermal reaction, obtain Cu/SiO2Composite.
Preferably, the mantoquita is copper chloride, copper sulphate or copper nitrate；The protective agent be selected from polyvinylpyrrolidone,
Cetyl trimethylammonium bromide, dodecyl sodium sulfate, neopelex, gelatin, polyvinyl alcohol, laurate and oil
One or more in acid；The reducing agent is hydrazine hydrate, hydrogen peroxide, ascorbic acid, formaldehyde, glucose, polyalcohol, hydroboration
Sodium, sodium hypophosphite or organic amine.
Preferably, the size of the nano silicon is 1~100nm.
Present invention also provides a kind of Cu/SiO2Composite, including nano silicon and it is attached to the nanometer two
The Nanometer Copper of silicon oxide surface.
Preferably, the Cu/SiO2The size of composite is 1~200nm.
Present invention also provides a kind of preparation method of copper-ceramic substrate, comprise the following steps：
By Cu/SiO2Composite mixes with organic solvent, obtains Nanometer Copper cream；The Cu/SiO2Composite is above-mentioned
Cu/SiO described in prepared by preparation method described in scheme or such scheme2Composite；
The Nanometer Copper cream is printed in ceramic base plate surface, then is sintered, finally carries out photoetching, development and electricity successively
Plating, obtains copper-ceramic substrate.
Preferably, Cu/SiO in the Nanometer Copper cream2The content of composite is 70wt%~85wt%.
Preferably, the Nanometer Copper cream be printed in the thickness of the Nanometer Copper layer of paste of ceramic base plate surface formation for 0.05~
0.5mm。
Preferably, the organic solvent is toluene, dimethylbenzene, methanol, ethanol, isopropanol, propane diols, ether, acetone, first
One or more in base butanone, methyl acetate, ethyl acetate and ethyl acetate.
Preferably, the material of the ceramic substrate is aluminum oxide, aluminium nitride, beryllium oxide or carborundum.
This application provides a kind of preparation method of copper-ceramic substrate, and it is by Cu/SiO2Composite and organic solvent
Mixing, obtains Nanometer Copper cream；Nanometer Copper cream is printed in ceramic base plate surface again, is then sintered, finally carries out light successively
Carve, develop and electroplate, obtain copper-ceramic substrate.During copper-ceramic substrate is prepared, the application has by addition to be received
The Cu/SiO of the Nano grade of rice dimensional effect2Composite, simultaneously because Cu/SiO2Nano-meter SiO_2 in composite2Can be with
With the Al in ceramic substrate2O3Reacted with AlN, therefore can be between lower sintering temperature (200~450 DEG C) realize copper-ceramics
High intensity bonding.
Brief description of the drawings
Fig. 1 is the process chart that the present invention prepares copper-ceramic substrate.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are simply further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
At present, DPC substrates need to overcome Seed Layer low with ceramic substrate respond, are also easy to produce stomata and cause bond strength
The problem of reduction, thus this application provides a kind of Cu/SiO2The preparation method of composite, and provide and utilize the preparation
Cu/SiO2The method that composite prepares copper-ceramic substrate, this method can be high-strength between relatively low temperature realizes copper-ceramics
Degree bonding.Thus, this application provides the embodiment of the invention discloses a kind of Cu/SiO2The preparation method of composite, including
Following steps：
Mantoquita, nano silicon, reducing agent and protective agent are subjected to hydro-thermal reaction, obtain Cu/SiO2Composite.
Preparing Cu/SiO2During composite, the raw material of use includes protective agent, mantoquita, nano silicon
With reducing agent, source the application of above-mentioned raw materials has no particular limits.Specifically, the mantoquita is selected from copper chloride, copper sulphate
Or copper nitrate；The particle diameter of the nano silicon is 1~100nm, in a particular embodiment, the grain of the nano silicon
Footpath is 5~30nm.The protective agent can prevent the nano copper particle of generation from reuniting, and the protective agent is selected from polyvinylpyrrolidone
(PVP), cetyl trimethylammonium bromide (CTAB), dodecyl sodium sulfate (SDS), neopelex (SDBS),
One or more in gelatin, polyvinyl alcohol (PVA), laurate and oleic acid；In a particular embodiment, the protective agent is selected from ten
Six alkyl trimethyl ammonium bromides (CTAB).The reducing agent is selected from hydrazine hydrate, hydrogen peroxide, ascorbic acid, formaldehyde, glucose, more
First alcohol, sodium borohydride, sodium hypophosphite or organic amine；In a particular embodiment, the reducing agent is hydrazine hydrate.Above-mentioned raw materials mix
Laggard water-filling thermal response is closed, that is, obtains Cu/SiO2Composite, in the process, liquid phase reduction is prepared for Nanometer Copper first,
Adding nanometer silicon dioxide material makes the nanometer copper product of generation be attached to its surface, forms Cu/SiO2Composite.The water
The temperature of thermal response is 150~250 DEG C, and the time is 1~2h.
Present invention also provides a kind of Cu/SiO2Composite, the Cu/SiO2Composite includes nano silicon
With the Nanometer Copper for being attached to the nano-silica surface.
Heretofore described Cu/SiO2Composite is prepared according to such scheme, the Cu/SiO2Composite
Particle diameter is 1~200nm, in some specific embodiments, the Cu/SiO2The particle diameter of composite is 20~100nm.The application
The Cu/SiO2Composite has a nano-scale, therefore presents a nanometer chi when it is applied in the preparation of copper-ceramic substrate
Very little effect, it specifically refers to the small-size effect of nano material, when metallic particles is when being reduced in size to nano-scale, compound
The fusing point of grain will have obvious reduction, will realize the low-temperature sintering of Nanometer Copper cream well.Thus, this application provides one kind
The preparation method of copper-ceramic substrate, comprises the following steps：
By Cu/SiO2Composite mixes with organic solvent, obtains Nanometer Copper cream；
The Nanometer Copper cream is printed in ceramic base plate surface, then is sintered, finally carries out photoetching, development and electricity successively
Plating, obtains copper-ceramic substrate.
As shown in figure 1, Fig. 1 is the process chart that the present invention prepares copper-ceramic substrate；1 it is ceramic substrate in Fig. 1,2 is
Silk-screen printing orifice plate, 3 be Nanometer Copper layer of paste, 4 be a nanometer Cu metal line layer, 5 be photoresist, 6 be copper wire figure, 7 be gold
Belong to line pattern.Specifically, the application is during copper-ceramic substrate is prepared, first by Cu/SiO2Composite with it is organic
Solvent mixes, and obtains Nanometer Copper cream；The organic solvent is not special to this application to be well known to those skilled in the art
Limitation, example, the organic solvent is selected from toluene, dimethylbenzene, methanol, ethanol, isopropanol, propane diols, ether, acetone, first
One or more in base butanone, methyl acetate, ethyl acetate and ethyl acetate；In a particular embodiment, the organic solvent
Selected from ethyl acetate and isopropanol.In the Nanometer Copper cream, the Cu/SiO2The content of composite be 70wt%~
85wt%, in a particular embodiment, the Cu/SiO2The content of composite is 80wt%~85wt%；If organic solvent mistake
More, then it is in pulp-like to make mixed material, can not be in paste, and organic solvent evaporates in sintering, excessive organic solvent
The circuit after sintering a small amount of hole is occurred, influence electric conductivity.
After Nanometer Copper cream is obtained, in order to avoid introducing impurity, the ceramic substrate has carried out surface cleaning in advance, then will
Nanometer Copper cream is printed in ceramic base plate surface, and Nanometer Copper layer of paste is obtained after vacuum drying.In the process, the mode of the printing
It can carry out according to mode well known to those skilled in the art, in a particular embodiment, be carried out by the way of silk-screen printing；
The vacuum drying time is 10~20min, and the thickness of the Nanometer Copper layer of paste is 0.05~0.5mm, in specific embodiment
In, the thickness of the Nanometer Copper layer of paste is 100~350 μm.The material of the ceramic substrate can be aluminum oxide, can be nitridation
Aluminium, can also be beryllium oxide or carborundum.According to using needs, can in a surface printing Nanometer Copper cream of ceramic substrate,
Nanometer Copper cream can also be printed on two surfaces of ceramic substrate, this application is had no particular limits.
According to the present invention, then ceramic substrate is sintered, Nanometer Copper layer of paste is formed transition zone in interface, it is described
The temperature of sintering is 200~450 DEG C, and the time is 30~90min.Due to Cu/SiO2The presence of composite so that ceramic substrate
Sintering temperature reduce, and carry out ordinary sinter.
The application finally by copper-ceramic substrate of the layer of Cu metal line containing nanometer of preparation carry out successively photoetching, development and
Plating, obtains copper-ceramic substrate；The photoetching, development and plating are technological means well known to those skilled in the art, herein
Without special limitation.
In the preparation process for copper-ceramic substrate that the application provides, due to Cu/SiO2The nanometer size effect of composite
And Nano-meter SiO_22Can be with the Al in ceramic substrate2O3/ AlN reacts, and therefore, the application is preparing the mistake of copper-ceramic substrate
Cheng Zhongke realizes the high intensity bonding between copper-ceramics at relatively low temperatures and pressures.
For a further understanding of the present invention, with reference to embodiment to Cu/SiO provided by the invention2The system of composite
The preparation method of Preparation Method and copper-ceramic substrate is described in detail, and protection scope of the present invention is not limited by following examples
System.
Embodiment 1
The mantoquita of 40 mass parts, the nano silicon of 15 mass parts, the hexadecane of 30 mass parts are added in a kettle
Base trimethylammonium bromide (CTAB), the hydrazine hydrate of 15 mass parts is added after well mixed, 1~2h is reacted at a temperature of 200 DEG C,
It can obtain a nanometer Cu/SiO2Composite.Cu/SiO manufactured in the present embodiment2The particle diameter of composite is 20~100nm.
Nanometer Cu/SiO in following examples2Composite is prepared according to the method for embodiment 1.
Embodiment 2
Material：Nanometer Cu/SiO2The size of composite is 20~50nm, and organic solvent is ethyl acetate, isopropanol；
Manufacture craft：
1) nanometer Cu/SiO2Composite and organic solvent in mass ratio 80:20 are mixed evenly, and Nanometer Copper is made
Cream；
2) surface cleaning：Dried after aluminium oxide ceramic substrate is cleaned by ultrasonic 10 minutes；
3) printing is coated and dried：Nanometer Copper cream is coated in aluminium oxide ceramic substrate surface using silk-screen printing device,
After vacuum drying 20 minutes, the Nanometer Copper layer of paste that thickness is 200 microns is obtained；
4) sinter：Aluminium oxide ceramic substrate with Nanometer Copper layer of paste is put into sintering furnace, 350 under the protection of nitrogen
DEG C sintering 60 minutes after cool down, obtain copper-ceramic substrate of the layer of Cu metal line containing nanometer；
5) metallic copper circuit is made：Photoresist is coated on ceramic substrate, according still further to circuit carry out development treatment, it is laggard
Row graphic plating, finally the photoresist outside circuit is removed, obtain the ceramic substrate for having metallic copper circuit；
6) clean：Ceramic substrate is put into plasma cleaner and cleaned, circuit surface is cleaned.
Embodiment 3
Material：Nanometer Cu/SiO2The size of composite is 50~80nm, and organic solvent is ethyl acetate, isopropanol；
Manufacture craft：
1) nanometer Cu/SiO2Composite and organic solvent in mass ratio 85:15 are mixed evenly, and Nanometer Copper is made
Cream；
2) surface cleaning：Dried after aluminum nitride ceramic substrate is cleaned by ultrasonic 10 minutes；
3) printing is coated and dried：Nanometer Copper cream is coated in aluminium oxide ceramic substrate surface using silk-screen printing device,
Vacuum drying obtains the Nanometer Copper layer of paste that thickness is 300 microns after 20 minutes；
4) sinter：Aluminum nitride ceramic substrate with Nanometer Copper layer of paste is put into sintering furnace, 400 under the protection of nitrogen
DEG C sintering 60 minutes after cool down, obtain copper-ceramic substrate of the layer of Cu metal line containing nanometer；
5) circuit is made：Photoresist is coated on ceramic substrate, development treatment is carried out according still further to circuit, carries out figure afterwards
Plating, finally the photoresist outside circuit is removed, it is possible to which obtaining has the ceramic substrate of metallic copper circuit；
6) clean：Ceramic substrate is put into plasma cleaner and cleaned, circuit surface is cleaned.
The explanation of above example is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that pair
For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
- A kind of 1. Cu/SiO2The preparation method of composite, comprises the following steps：Mantoquita, nano silicon, reducing agent and reducing agent are subjected to hydro-thermal reaction, obtain Cu/SiO2Composite.
- 2. preparation method according to claim 1, it is characterised in that the mantoquita is copper chloride, copper sulphate or copper nitrate； The protective agent is selected from polyvinylpyrrolidone, cetyl trimethylammonium bromide, dodecyl sodium sulfate, detergent alkylate sulphur One or more in sour sodium, gelatin, polyvinyl alcohol, laurate and oleic acid；The reducing agent is hydrazine hydrate, hydrogen peroxide, anti-bad Hematic acid, formaldehyde, glucose, polyalcohol, sodium borohydride, sodium hypophosphite or organic amine.
- 3. preparation method according to claim 1, it is characterised in that the size of the nano silicon be 1~ 100nm。
- A kind of 4. Cu/SiO2Composite, it is characterised in that including nano silicon and be attached to the nano silicon The Nanometer Copper on surface.
- 5. composite according to claim 4, it is characterised in that the Cu/SiO2The size of composite be 1~ 200nm。
- 6. a kind of preparation method of copper-ceramic substrate, comprises the following steps：By Cu/SiO2Composite mixes with organic solvent, obtains Nanometer Copper cream；The Cu/SiO2Composite is claim Cu/SiO described in prepared by preparation method described in 1~3 any one or any one of claim 4~52Composite；The Nanometer Copper cream is printed in ceramic base plate surface, then is sintered, finally carries out photoetching, development and plating successively, Obtain copper-ceramic substrate.
- 7. preparation method according to claim 6, it is characterised in that Cu/SiO in the Nanometer Copper cream2Composite contains Measure as 70wt%~85wt%.
- 8. preparation method according to claim 6, it is characterised in that the Nanometer Copper cream is printed in ceramic base plate surface shape Into the thickness of Nanometer Copper layer of paste be 0.05~0.5mm.
- 9. preparation method according to claim 6, it is characterised in that the organic solvent be toluene, dimethylbenzene, methanol, One kind or more in ethanol, isopropanol, propane diols, ether, acetone, espeleton, methyl acetate, ethyl acetate and ethyl acetate Kind.
- 10. preparation method according to claim 6, it is characterised in that the material of the ceramic substrate is aluminum oxide, nitridation Aluminium, beryllium oxide or carborundum.
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