CN102222536A - Environment-friendly silver conductive paste for surface mounting of semiconductor chips and preparation method of environment-friendly silver conductive paste - Google Patents
Environment-friendly silver conductive paste for surface mounting of semiconductor chips and preparation method of environment-friendly silver conductive paste Download PDFInfo
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Abstract
The invention discloses an environment-friendly silver conductive paste for surface mounting of semiconductor chips and a preparation method of environment-friendly silver conductive paste. The paste comprises 65-80 percent of ultrafine silver powder, 10-30 percent of organic carriers, 2-8 percent of lead-free glass power and 3-12 percent of additives; the organic carriers comprise organic solvent and organic additives with mass percent of 4-7:3-6; and the additives comprise dispersing agents and surface active agents with mass ratio of 1-5:1. The preparation method of the environment-friendly silver conductive paste comprises the following steps: 1) the power is mixed for standby; 2) the organic carriers are prepared and cooled to room temperature for standby; and 3) the paste is mixed to obtain the environment-friendly silver conductive paste. The paste has good conductive performance, strong adhesive force, good stability, low expansion coefficient, difficulty in oxidization and good wettability and intermiscibility with a chip and a chip substrate.
Description
Technical field
The present invention relates to a kind of based semiconductor chip attachment environment-friendly silver conductor paste, be applicable to field of electronic components manufacturing such as semiconductor chip mounts, especially relate to a kind of based semiconductor chip attachment environment-friendly silver conductor paste and preparation method thereof.
Background technology
In hyundai electronics industry, people require more and more higher to electronic devices and components, produce and adopt procedures, standardization to carry out more to reduce cost, just mounting of semiconductor chip mounted by original welding, fluid welding technical development production line till now, conductor paste and mounting of semiconductor chip with regard to the new requirement of demand is complementary accordingly, and the research of carrying out new conductor paste is also just imperative.
In general, the main component of electric slurry includes function mutually as metal, noble metal powder etc., inorganic binder such as glass powder, oxide powder etc., organic binder bond, other solvent and additive.Usually, function in the electric slurry plays electric action mutually, have good electric conductivity, is generally served as by metal dust or noble metal powder, metal dust commonly used has copper powder, aluminium powder, zinc powder, nickel powder etc., and precious metal powder commonly used has bronze, silver powder, platinum powder, palladium powder etc.Inorganic binder plays fixedly that electric slurry is generally served as by oxide powder and glass powder to base material, but this composition is lower at the proportion of electric slurry, have in addition do not have; Organic binder bond mainly plays a part to make slurry to have certain shape, be easy to print or apply, mainly contain macromolecule resin, the micromolecule resin waits and serves as, along with this part effect in electric slurry of chemical industry development of technology is more and more outstanding, the composition that changes organic binder bond just can change drying, the sintering character of electric slurry.
In existing electric slurry field, silver-colored serial conductor paste has the conductance height, and stable performance with characteristics such as the substrate bond strength are big, is widely used in the production of electronic devices and components such as integrated circuit, chip attachment, thin film switch.But, the conductor paste of how making in the chip attachment field in the past with the flint glass powder, enforcement along with various environmental regulations, lead oxide becomes the material that national governments and environmental protection organization ban use of, electric slurry faces suchlike problem too to be needed to solve, the problem of environmental protection does not solve, and has just limited the development of conductor paste in product for civilian use market.
In view of the deficiency that above existing silver conductive paste exists, developing a kind of based semiconductor chip attachment just become the task of top priority with environment-friendly silver conductor paste and energy large-scale production.
Summary of the invention
One of purpose of the present invention provides a kind of based semiconductor chip attachment environment-friendly silver conductor paste, this slurry conducts electricity very well, strong adhesion, good stability, the coefficient of expansion are low, be difficult for oxidation, with chip, chip substrate excellent wetting capacity and compatibility is arranged.
Another object of the present invention provides a kind of preparation method of above-mentioned slurry; used in the process of preparation is the production equipment of existing slurry; so in the process of manufacture of slurry, do not need to carry out new investment in addition, help environmental protection simultaneously and contain the recovery and the recycling of the electronic product of this electrode slurry.
For achieving the above object, the following technical proposals of the present invention's employing:
A kind of based semiconductor chip attachment environment-friendly silver conductor paste, this slurry is formed by the feedstock production of following mass percent:
Super fine silver powder 65~80%, organic carrier 10~30%, leadless glass powder 2~8% and additive 3~12%;
Described super fine silver powder is that particle diameter is the super fine silver powder of 0.1~5 μ m;
Described organic carrier is organic solvent and organic additive, is 4~7: 3~6 compositions according to mass percent;
Described leadless glass powder is a boron manosil AS zinc glass frit;
Described additive is that dispersant, surfactant are 1~5: 1 ratio composition according to mass ratio.
Slurry of the present invention is further characterized in that:
Described organic solvent is one or more the mixture in terpinol, butyl carbitol, the turpentine oil.
Described organic additive is one or more the mixture in phenolic resins, ethyl cellulose, the methylcellulose.
The mixture of one or more in described dispersant selection o-phthalic acid dibutyl ester, lactic acid list glyceride, the propylene glycol butyl ether.
The mixture of one or more in described surfactant selection hexadecanol, lecithin, the castor oil.
The present invention gives the preparation method of this based semiconductor chip attachment with the environment-friendly silver conductor paste, and this method comprises the steps:
1) powder: be after the super fine silver powder of 0.1~5 μ m is 65~80% and 2~8% leadless glass powder mixings according to mass percent with particle diameter, stand-by;
2) preparation organic carrier: 10~30% weighing organic carriers by mass percentage, wherein, organic carrier is 4~7: 3~6 ratio preparation according to mass percent according to organic solvent terpinol, butyl carbitol or turpentine oil and organic additive phenolic resins, ethyl cellulose or methylcellulose, put into 70~100 ℃ water-bath heated at constant temperature, dissolve fully until organic additive, it is stand-by to be cooled to room temperature;
3) slurry mixes: with step 2) organic carrier and the mass percent of preparation be that 3~12% additive joins in the mixture of super fine silver powder that step 1) prepares and leadless glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
Additive is that dispersant and surfactant are 1~5: 1 ratio composition according to mass ratio;
4) slurry rolling: the preliminary slurry that step 3) is obtained carries out rolling 2~10 times with three-high mill, reach fineness to slurry less than 5 μ m till, obtain the slurry finished product through 400 purpose screen filtrations then.
From above preparation method as can be seen, the above-mentioned conductor paste and the major advantage of preparation process thereof are the following aspects:
1, above-mentioned conductor paste mainly with super fine silver powder as the function phase, be that large-scale production is easily accepted by people now because super fine silver powder is a kind of metal dust of technology comparative maturity on the one hand; Super fine silver powder has good performance on the other hand, and the conductor paste electric conductivity of making is good, relatively meets the requirement for high conductivity.
2, analyze in conjunction with the physical and chemical performance of in the past conductor paste and to it, the leadless glass powder that adds harmful substances such as not leaded, cadmium, the wetability of slurry, surface smoothing, intermiscibility, good with the bond strength of chip, chip substrate can substitute the suitability for industrialized production manufacturing field that leaded conductor paste is used for chip attachment fully.
3, the organic solvent carrier among the present invention is that solvent with different boiling and evaporation rate fits together according to a certain percentage, make silver conductive paste volatilization one by one in the patch block process, should not form defectives such as pore, crack, it is firm that conductor paste is connected with chip, chip substrate, improves bonding strength.
Zhi Bei conductor paste electric conductivity, contact performance, switching performance is good according to the method described above; The present invention can adapt with chip, chip substrate by adjusting the content of various inorganic constituentss and organic principle, reaches the effect that makes properties of product better, has guaranteed the steady quality of product.
Embodiment
Below by specific embodiment the present invention is described in further details.
Embodiment 1:
This based semiconductor chip attachment environment-friendly silver conductor paste, its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 65%, organic carrier 30%, leadless glass powder 2% and additive 3%;
Wherein super fine silver powder is that particle diameter is the super fine silver powder of 0.1~5 μ m; Organic solvent in the organic carrier is selected butyl carbitol, and organic additive is selected methylcellulose, and both ratios are 4.5: 5.5; Leadless glass powder is a boron manosil AS zinc glass frit; Described additive is dispersant and surfactant, and wherein dispersant is selected dioctyl phthalate; Surfactant is selected hexadecanol, and wherein dispersant and surfactant are formed according to 1: 1 ratio.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) powder: the weighing particle diameter is the super fine silver powder of 0.1~5 μ m at first by mass percentage, and then weighing super fine silver powder and leadless glass powder are mixed, and is stand-by behind the mixing;
2) preparation organic carrier: by aforementioned mass percent weighing organic solvent and organic additive, put into 70 ℃ water-bath heated at constant temperature, dissolve fully until organic additive, it is stand-by to be cooled to room temperature;
3) slurry mixes: according to aforementioned mass percent the organic carrier of weighing and other additive are joined in the mixture of above-mentioned super fine silver powder and leadless glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
4) slurry rolling: the above-mentioned preliminary slurry that obtains is carried out rolling 8 times with three-high mill, be checked through till the fineness less than 5 μ m, obtain the slurry finished product through 400 purpose screen filtrations then.
Embodiment 2:
This based semiconductor chip attachment environment-friendly silver conductor paste, its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 68%, organic carrier 18%, leadless glass powder 8% and additive 6%;
Wherein super fine silver powder is that particle diameter is the super fine silver powder of 0.1~5 μ m; Organic solvent in the organic carrier is selected turpentine oil, and organic additive is selected phenolic resins, and both ratios are 4: 6; Leadless glass powder is a boron manosil AS zinc glass frit; Described additive is dispersant and surfactant, and wherein dispersant is selected the propylene glycol butyl ether; Surfactant is selected castor oil, and wherein dispersant and surfactant are formed according to 3: 1 ratio.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) powder: the weighing particle diameter is the super fine silver powder of 0.1~5 μ m at first by mass percentage, and then weighing super fine silver powder and leadless glass powder are mixed, and is stand-by behind the mixing;
2) preparation organic carrier: by aforementioned mass percent weighing organic solvent and organic additive, put into 75 ℃ water-bath heated at constant temperature, dissolve fully until organic additive, it is stand-by to be cooled to room temperature;
3) will expect to mix: the organic carrier of weighing and other additive are joined in the mixture of above-mentioned super fine silver powder and leadless glass powder according to aforementioned mass percent, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
4) slurry rolling: the above-mentioned preliminary slurry that obtains is carried out rolling 6 times with three-high mill, be checked through till the fineness less than 5 μ m, obtain the slurry finished product through 400 purpose screen filtrations then.
Embodiment 3:
This based semiconductor chip attachment environment-friendly silver conductor paste, its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 66%, organic carrier 20%, leadless glass powder 2% and additive 12%;
Wherein super fine silver powder is that particle diameter is the super fine silver powder of 0.1~5 μ m; Organic solvent in the organic carrier is selected terpinol and butyl carbitol (mixing in 1: 2 by mass percentage), and organic additive is selected ethyl cellulose, and both ratios are 6.5: 3.5; Leadless glass powder is a boron manosil AS zinc glass frit; Described additive is dispersant and surfactant, and wherein dispersant is selected dioctyl phthalate; Surfactant is selected lecithin, and wherein dispersant and surfactant are formed according to 3.5: 1 ratio.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) powder: the weighing particle diameter is the super fine silver powder of 0.1~5 μ m at first by mass percentage, and then weighing super fine silver powder and leadless glass powder are mixed, and is stand-by behind the mixing;
2) preparation organic carrier: by aforementioned mass percent weighing organic solvent and organic additive, put into 85 ℃ water-bath heated at constant temperature, dissolve fully until organic additive, it is stand-by to be cooled to room temperature;
3) will expect to mix: the organic carrier of weighing and other additive are joined in the mixture of above-mentioned super fine silver powder and leadless glass powder according to aforementioned mass percent, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
4) slurry rolling: the above-mentioned preliminary slurry that obtains is carried out rolling 2 times with three-high mill, be checked through till the fineness less than 5 μ m, obtain the slurry finished product through 400 purpose screen filtrations then.
Embodiment 4:
This based semiconductor chip attachment environment-friendly silver conductor paste, its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 75%, organic carrier 15%, leadless glass powder 5% and additive 5%;
Wherein super fine silver powder is that particle diameter is the super fine silver powder of 0.1~5 μ m; Organic solvent in the organic carrier is selected terpinol, and organic additive is selected ethyl cellulose and methylcellulose (press mass ratio mixes at 4: 1), and both ratios are 7: 3; Leadless glass powder is a boron manosil AS zinc glass frit; Described additive is dispersant and surfactant, and wherein dispersant is selected dioctyl phthalate and propylene glycol butyl ether (press mass ratio mixes at 3: 1); Surfactant is selected hexadecanol, and wherein dispersant and surfactant are formed according to 5: 1 ratio.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) powder: the weighing particle diameter is the super fine silver powder of 0.1~5 μ m at first by mass percentage, and then weighing super fine silver powder and leadless glass powder are mixed, and is stand-by behind the mixing;
2) preparation organic carrier: by aforementioned mass percent weighing organic solvent and organic additive, put into 100 ℃ water-bath heated at constant temperature, dissolve fully until organic additive, it is stand-by to be cooled to room temperature;
3) will expect to mix: the organic carrier of weighing and other additive are joined in the mixture of above-mentioned super fine silver powder and leadless glass powder according to aforementioned mass percent, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
4) slurry rolling: the above-mentioned preliminary slurry that obtains is carried out rolling 10 times with three-high mill, be checked through till the fineness less than 5 μ m, obtain the slurry finished product through 400 purpose screen filtrations then.
Embodiment 5:
This based semiconductor chip attachment environment-friendly silver conductor paste, its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 80%, organic carrier 10%, leadless glass powder 6% and additive 4%;
Wherein super fine silver powder is that particle diameter is the super fine silver powder of 0.1~5 μ m; Organic solvent in the organic carrier is selected butyl carbitol, and organic additive is selected phenolic resins, and both ratios are 6: 4; Leadless glass powder is a boron manosil AS zinc glass frit; Described additive is dispersant and surfactant, and wherein dispersant is selected the lactic acid monoglyceride; Surfactant is selected hexadecanol and lecithin (press mass ratio mixes at 4: 1), and wherein dispersant and surfactant are formed according to 2.5: 1 ratio.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) powder: the weighing particle diameter is the super fine silver powder of 0.1~5 μ m at first by mass percentage, and then weighing super fine silver powder and leadless glass powder are mixed, and is stand-by behind the mixing;
2) preparation organic carrier: by aforementioned mass percent weighing organic solvent and organic additive, put into 90 ℃ water-bath heated at constant temperature, dissolve fully until organic additive, it is stand-by to be cooled to room temperature;
3) will expect to mix: the organic carrier of weighing and other additive are joined in the mixture of above-mentioned super fine silver powder and leadless glass powder according to aforementioned mass percent, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
4) slurry rolling: the above-mentioned preliminary slurry that obtains is carried out rolling 9 times with three-high mill, be checked through till the fineness less than 5 μ m, obtain the slurry finished product through 400 purpose screen filtrations then.
Claims (6)
1. based semiconductor chip attachment environment-friendly silver conductor paste is characterized in that this slurry is formed by the feedstock production of following mass percent:
Super fine silver powder 65~80%, organic carrier 10~30%, leadless glass powder 2~8% and additive 3~12%;
Described super fine silver powder is that particle diameter is the super fine silver powder of 0.1~5 μ m;
Described organic carrier is organic solvent and organic additive, is 4~7: 3~6 compositions according to mass ratio;
Described leadless glass powder is a boron manosil AS zinc glass frit;
Described additive is that dispersant, surfactant are 1~5: 1 ratio composition according to mass ratio.
2. a kind of based semiconductor chip attachment environment-friendly silver conductor paste according to claim 1 is characterized in that, described organic solvent is one or more the mixture in terpinol, butyl carbitol, the turpentine oil.
3. a kind of based semiconductor chip attachment environment-friendly silver conductor paste according to claim 1 is characterized in that, described organic additive is one or more the mixture in phenolic resins, ethyl cellulose, the methylcellulose.
4. a kind of based semiconductor chip attachment environment-friendly silver conductor paste according to claim 1 is characterized in that, the mixture of one or more in described dispersant selection o-phthalic acid dibutyl ester, lactic acid list glyceride, the propylene glycol butyl ether.
5. a kind of based semiconductor chip attachment environment-friendly silver conductor paste according to claim 1 is characterized in that, the mixture of one or more in described surfactant selection hexadecanol, lecithin, the castor oil.
6. the preparation method of a based semiconductor chip attachment usefulness environment-friendly silver conductor paste is characterized in that this method comprises the steps:
1) powder: be after the super fine silver powder of 0.1~5 μ m is 65~80% and 2~8% leadless glass powder mixings according to mass percent with particle diameter, stand-by;
2) preparation organic carrier: 10~30% weighing organic carriers by mass percentage, wherein, organic carrier is 4~7: 3~6 ratio preparation according to mass percent according to organic solvent terpinol, butyl carbitol or turpentine oil and organic additive phenolic resins, ethyl cellulose or methylcellulose, put into 70~100 ℃ water-bath heated at constant temperature, dissolve fully until organic additive, it is stand-by to be cooled to room temperature;
3) slurry mixes: with step 2) organic carrier and the mass percent of preparation be that 3~12% additive joins in the mixture of super fine silver powder that step 1) prepares and leadless glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
Additive is that dispersant and surfactant are 1~5: 1 ratio composition according to mass ratio;
4) slurry rolling: the preliminary slurry that step 3) is obtained carries out rolling 2~10 times with three-high mill, reach fineness to slurry less than 5 μ m till, obtain the slurry finished product through 400 purpose screen filtrations then.
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CN103559957B (en) * | 2013-09-22 | 2016-11-23 | 江苏瑞德新能源科技有限公司 | A kind of preparation method of positive silver paste |
CN105934799A (en) * | 2014-01-17 | 2016-09-07 | 纳美仕有限公司 | Conductive paste and method for producing a semiconductor device using the same |
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CN104036842A (en) * | 2014-05-12 | 2014-09-10 | 铜陵市超远精密电子科技有限公司 | Lead-free environmental-friendly circuit board conductive silver paste and preparation method thereof |
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CN104078098A (en) * | 2014-06-04 | 2014-10-01 | 乐凯特科技铜陵有限公司 | Low-silver-bearing printed circuit board silver paste and preparation method thereof |
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