CN101710509A - Preparation method of leadless nickel electrode slurry for thick-film resistor - Google Patents
Preparation method of leadless nickel electrode slurry for thick-film resistor Download PDFInfo
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- CN101710509A CN101710509A CN200910254519A CN200910254519A CN101710509A CN 101710509 A CN101710509 A CN 101710509A CN 200910254519 A CN200910254519 A CN 200910254519A CN 200910254519 A CN200910254519 A CN 200910254519A CN 101710509 A CN101710509 A CN 101710509A
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Abstract
The invention discloses a preparation method of leadless nickel electrode slurry for a thick-film resistor, which comprises the following steps: according to the mass percent, weighing 40-60% of superfine nickel powder, 2-10% of leadless glass powder, 20-50% of organic carrier and 5-12% of additive for standby use, wherein the average grain size of the superfine nickel powder is 0.05-5mu m, the average grain size of the leadless glass powder is 0.01-5mu m, and the total weight of the superfine nickel powder, the leadless glass powder, the organic carrier and the additive is 100%; uniformly mixing the superfine nickel powder and the leadless glass powder and then mixing the two materials in a ball mill or a ball grinder for 1-10 hours to obtain a primary mixture; and obtaining the leadless nickel electrode slurry after drying and roll milling. The nickel electrode slurry of the invention is free of harmful substances such as lead and the like, and no harmfulness exists in the process of production and processing of the slurry, thereby being beneficial to environmental protection; and the invention eliminates the factors of deformation caused before and after co-firing of a substrate of the traditional thick-film resistor, and the like which affects production, is conducive to reducing the production cost, and meets the general trend of social development nowadays.
Description
Technical field
The thick-film resistor that the invention belongs in the microelectronic component is made the field, relates to the preparation method of a kind of thick-film resistor with electrode slurry, especially a kind of preparation method of leadless nickel electrode slurry.
Background technology
Along with the develop rapidly of new material, new technology and new science and technology, the development of complete electronic set and surface installation technique is also very fast, and microelectronic component also more and more approaches daily life.As part indispensable in the microelectronic component, the thick-film technique technology forms integrated circuit or large scale integrated circuits with various assemblies (as little resistance, little electric capacity etc.) with different electrical properties with the form of thick film silk screen printing, thereby forms highly integrated, stable performance, cheap microelectronic product.Electric slurry is the material of preparation thick film circuit or microelectronic component functional electrode, it is by becoming slurry with functional powders decentralized system in organic binder bond, mix the back and printing various function components and parts such as forming conductivity, resistive element, insulator, capacitance body on the non-conductive substrate or on the semiconductor substrate, therefore being the basic material of development microelectronic component, also is the critical material of preparation thick film high accuracy hybrid integrated circuit and other large scale integrated circuit.
Since mid-term in 20th century, people have just carried out the research of electric slurry that electronic devices and components are used.Particularly after the World War II; along with electronics industry develops with exponential increasing; surface-mounted integrated circuit becomes multilayer wiring from individual layer; form hybrid integrated circuit module and multilayer sheet type electric capacity and plate resistor element; the significantly reduction of the manufacturing cost of electronics industry simultaneously; high-grade, precision and advanced electronic product also expands to civil electric appliance from simple military domain, various hybrid integrated circuits; electrode and segment electrode slurry in the new ceramics capacitor; the multilayer wiring conductor paste; the through hole slurry; the electromagnetic shielding film slurry; electric slurries such as thick-film resistor electrode slurry have also obtained large-scale development rapidly thereupon.
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, has good electric conductivity, generally serve as by metal dust or noble metal powder, metal dust commonly used has copper powder, aluminium powder, zinc powder, nickel powder etc., precious metal powder commonly used has silver powder, platinum powder, palladium powder etc., along with constantly skyrocketing of noble metal price, the base metal slurry comes into one's own day by day cheaply, substitutes noble metal slurry, particularly metallic nickel in some application, because nickel part has the favorable conductive characteristic, stable performance, good solderability, fusing point is higher, in electric field, be difficult for migration, be applied to electronics industry, mainly make ceramic capacitor and thermal sensitive ceramics electrode slurry.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, especially when being applied to silk screen printing, the composition that changes organic binder bond just can change printing, drying, the sintering character of electric slurry.Remove this outside, dispersant, the defoamer that also will add other in the electric slurry waits and changes slurry outward appearance, flowability, thixotropic composition.
Be applied to thick-film resistor silver-palladium slurry the most generally at present, but its cost costs an arm and a leg than higher, be difficult for a large amount of the employing.In addition, also contain the healthy elements of harm humans such as lead in silver-palladium slurry, along with the development of electronics industry, energy-conserving and environment-protective are more and more accepted by people, and the research of thick film nickel slurry more and more is subject to people's attention.
The nickel of development slurry is mainly used in the metal layer of electronic devices and components such as hybrid integrated circuit, display both at home and abroad at present, but seldom is useful on the nickel slurry of thick-film resistor.Representative nickel slurry patent is JP05-121204, proposes nickel powder as electric conducting material, but thermal endurance and non-oxidizability in order to improve nickel, has added noble metal platinum and the palladium of 2-15%, and its cost is increased.Proposed a kind of direct method of using chemical method to form silver-colored diaphragm on the nickel powder surface that adopts in Chinese patent 02145520.1, the protection nickel powder is at high temperature not oxidized, but the composition and the preparation method of not mentioned conductor paste.What propose in Chinese patent 200810047907.8 is a kind of method that adopts direct at submicron order nickel powder surface clad nano silver powder, obtain the nickel based metal powder, in slurry, added antioxidant boron, make the oxidation resistance temperature of its slurry can reach 900 ℃, be used for the electrode of ceramic capacitor etc.The nickel part that proposes usefulness in Chinese patent 200810047908.2 is the ball powder of 0.1-2.0 μ m, and antioxidant is one or more among B, Cr, the Y, and oxidation resistance temperature is adjustable at 800-900 ℃.But be not doped precious metal element in nickel in the above nickel slurry, make its cost than higher, the sintering temperature that is exactly slurry is higher, has wasted a large amount of energy, does not meet the energy-conservation requirement of modern people's growing interest.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art; adopt the special material proportioning; a kind of preparation of design is used for the method for leadless nickel electrode slurry for thick-film resistor; there is not harmfulness in its production and processing, that the preparation of the leadless nickel electrode slurry for thick-film resistor that obtains with this method has is cheap, can large-scale production, meet existing environmental regulation, can instead of part noble metal electrode slurry be used for microelectronic product and make the field.
The objective of the invention is to solve by the following technical programs: a kind of preparation method of leadless nickel electrode slurry for thick-film resistor:
(1) get the raw materials ready: according to mass percent, the extra-fine nickel powder, 2-10% leadless glass powder, 20-50% organic carrier and the 5-12% additive that take by weighing 40-60% are standby; Described extra-fine nickel powder average grain diameter is 0.05-5 μ m, and the leadless glass powder average grain diameter is 0.01-5 μ m; Described extra-fine nickel powder, leadless glass powder, organic carrier and additive gross mass are 100%; Described additive is made of curtain coating agent and thixotropic agent, and wherein the mass percent of curtain coating agent and thixotropic agent is 1: 1; Described curtain coating agent is a kind of or its mixture in dibutyl phthalate, polyvinylpyrrolidone, the laurate list glyceride; Described thixotropic agent is a kind of or its mixture in calcium carbonate, tricalcium phosphate, the sodium acid carbonate;
(2) mix: the extra-fine nickel powder and the leadless glass powder of gained in the step (1) are mixed, and make organic carrier, mix the back and obtained once mixture in 1-10 hour at ball mill or ball grinder mixing with absolute ethyl alcohol;
(3) drying: the mixture of gained in the step (2) was dried 0.5-2 hour under 40-80 ℃ of condition, and the room temperature cooling obtains secondary mixture then;
(4) add organic carrier: the additive of gained in the step (1) is joined in the secondary mixture of gained in the step (3) and mix, filter and obtain preliminary slurry;
(5) rolling: the preliminary slurry of gained in the step (4) is carried out 2-7 all over rolling with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
Described step (1) is got the raw materials ready: according to mass percent, it is standby to take by weighing 40%, 50% or 60% extra-fine nickel powder, 2%, 5%, 8% or 10% leadless glass powder, 20%, 30%, 40% or 50% organic carrier and 5%, 8% or 12% additive.
Described step (2) obtained once mixture in 1 hour, 3 hours, 5 hours, 8 hours or 10 hours at ball mill or ball grinder mixing.
Described step (3) drying: with the oven dry 0.5 hour, 1 hour, 1.5 hours or 2 hours under 40 ℃, 50 ℃, 60 ℃, 70 ℃ or 80 ℃ of conditions of the mixture of gained in the step (2).
Described step (5) rolling: the preliminary slurry of gained in the step (4) is carried out rolling 2,3,4,5,6 or 7 times with three-high mill.
In the present invention, extra-fine nickel powder has constituted the conducting function phase of this electrode slurry, and the adding proportion that changes extra-fine nickel powder can be regulated the electrode performance of the nickel electrode slurry of finally making.Organic carrier has been selected ethyl cellulose terpinol, hydroxyl alcohol system, changes the processing performance that the composition of organic carrier can be regulated the nickel electrode slurry of finally making, as viscosity etc.Leadless glass powder is selected boron manosil AS zinc system, can be according to the physical property of selected thick-film resistor substrate such as the composition of selection leadless glass powders such as the coefficient of expansion, transition temperature, make both physical property such as the coefficient of expansion, transition temperature etc. basic identical or approaching, so just can obtain stronger adhesive force.The adding proportion that changes dispersant, defoamer and surfactant can be regulated apparent and printing performances such as the trickling of the silver electrode paste of finally making, thixotropy.Use the nickel electrode slurry printing that this method obtains or be coated on the corresponding thick-film resistor substrate, smooth and level at normal temperatures 10-30 minute, dry under 100-150 ℃ of temperature conditions, under 500-700 ℃ of temperature conditions, carry out common burning, the nickel electrode smooth surface, the electrical property that obtain are good, are applicable to the production of thick-film resistor.
Because there is not harmfulness in harmful material such as not leaded grade in the nickel electrode slurry of the present invention in the process of manufacture of slurry, helps environmental protection simultaneously; Glass powder in the nickel electrode slurry of the present invention in addition is basic identical or approaching with physical property such as the coefficient of expansion, the transition temperature etc. of corresponding thick-film resistor substrate, having solved in the past the thick-film resistor substrate produces distortion before and after burning altogether and waits and influence factor of production, help reducing production costs, meet the main trend of current social development.
Embodiment
The preparation method of a kind of leadless nickel electrode slurry for thick-film resistor of the present invention is as follows:
The first, the mixing of inorganic powder: at first take by weighing the extra-fine nickel powder that mass percent is 40-60%, its average grain diameter is 0.05-5 μ m, taking by weighing mass percent then is the 2-10% leadless glass powder, its average grain diameter is 0.01-5 μ m, then extra-fine nickel powder and leadless glass powder are mixed, make organic carrier with absolute ethyl alcohol, with ball mill or ball grinder mixing 1-10 hour;
The second, inorganic mixture drying: extra-fine nickel powder that mixes and leadless glass powder were dried 0.5-2 hour room temperature cooling then under 40-80 ℃ of condition;
Three, the adding of organic carrier: the organic carrier of weighing and other additive are joined in the mixture of above-mentioned ultra-fine nickel part and leadless glass powder according to aforementioned mass percent, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
Four, the rolling of slurry: the above-mentioned preliminary slurry that obtains is carried out 2-7 all over rolling with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
Further specify preparation process of the present invention below in conjunction with specific embodiment:
Embodiment 1:
The average grain diameter that at first takes by weighing 55 grams is the extra-fine nickel powder of 0.05-5 μ m, taking by weighing 7 gram average grain diameters then is the leadless glass powder of 0.01-5 μ m, then extra-fine nickel powder and leadless glass powder are mixed, make organic carrier, mixed 7 hours with ball mill or ball grinder with absolute ethyl alcohol;
Then nickel powder that mixes and leadless glass powder were dried 2 hours room temperature cooling then under 55 ℃ of conditions;
Join in the mixture of above-mentioned extra-fine nickel powder and leadless glass powder as thixotropic agent etc. as the tricalcium phosphates of curtain coating agent and 4 grams according to the dibutyl phthalate of aforementioned mass percent weighing 31 gram organic carriers and 3 again, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
At last the above-mentioned preliminary slurry that obtains is carried out rolling 6 times with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
Embodiment 2:
The average grain diameter that at first takes by weighing 40 grams is the extra-fine nickel powder of 0.05-5 μ m, taking by weighing 8.5 gram average grain diameters then is the leadless glass powder of 0.01-5 μ m, then extra-fine nickel powder and leadless glass powder are mixed, make organic carrier, mixed 7 hours with ball mill or ball grinder with absolute ethyl alcohol;
Then nickel powder that mixes and leadless glass powder were dried 2 hours room temperature cooling then under 50 ℃ of conditions;
Join in the mixture of above-mentioned extra-fine nickel powder and leadless glass powder as thixotropic agent etc. as the sodium acid carbonates of curtain coating agent and 1.5 grams according to the polyvinylpyrrolidones of aforementioned mass percent weighing 42 gram organic carriers and 7 grams again, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
At last the above-mentioned preliminary slurry that obtains is carried out rolling 7 times with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
Embodiment 3:
The average grain diameter that at first takes by weighing 60 grams is the extra-fine nickel powder of 0.05-5 μ m, taking by weighing 4.5 gram average grain diameters then is the leadless glass powder of 0.01-5 μ m, then extra-fine nickel powder and leadless glass powder are mixed, make organic carrier, mixed 7 hours with ball mill or ball grinder with absolute ethyl alcohol;
Then nickel powder that mixes and leadless glass powder were dried 1 hour room temperature cooling then under 60 ℃ of conditions;
Join in the mixture of above-mentioned extra-fine nickel powder and leadless glass powder as thixotropic agent etc. as the tricalcium phosphates of curtain coating agent and 2 grams according to the laurate list glyceride of aforementioned mass percent weighing 30 gram organic carriers and 3.5 grams again, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
At last the above-mentioned preliminary slurry that obtains is carried out rolling 4 times with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
Embodiment 4:
The average grain diameter that at first takes by weighing 45.5 grams is the extra-fine nickel powder of 0.05-5 μ m, taking by weighing 6.5 gram average grain diameters then is the leadless glass powder of 0.01-5 μ m, then extra-fine nickel powder and leadless glass powder are mixed, make organic carrier with absolute ethyl alcohol, mixed 5 hours with ball mill or ball grinder;
Then nickel powder that mixes and leadless glass powder were dried 1.5 hours room temperature cooling then under 70 ℃ of conditions;
Join in the mixture of above-mentioned extra-fine nickel powder and leadless glass powder as thixotropic agent etc. as the calcium carbonate of curtain coating agent and 3.5 grams according to the polyvinylpyrrolidones of aforementioned mass percent weighing 39.5 gram organic carriers and 5 grams again, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
At last the above-mentioned preliminary slurry that obtains is carried out rolling 7 times with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
Embodiment 5:
The average grain diameter that at first takes by weighing 56.5 grams is the extra-fine nickel powder of 0.05-5 μ m, taking by weighing 5.5 gram average grain diameters then is the leadless glass powder of 0.01-5 μ m, then extra-fine nickel powder and leadless glass powder are mixed, make organic carrier with absolute ethyl alcohol, mixed 5 hours with ball mill or ball grinder;
Then nickel powder that mixes and leadless glass powder were dried 2 hours room temperature cooling then under 45 ℃ of conditions;
Join in the mixture of above-mentioned extra-fine nickel powder and leadless glass powder as thixotropic agent etc. as the tricalcium phosphates of curtain coating agent and 1.25 grams according to the dibutyl phthalates of the organic carrier of aforementioned mass percent weighing 32 grams and 4.75 grams again, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
At last the above-mentioned preliminary slurry that obtains is carried out rolling 5 times with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
Above content is to further describing that the present invention did in conjunction with concrete preferred implementation; can not assert that the specific embodiment of the present invention only limits to this; for the general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by claims of being submitted to.
Claims (5)
1. the preparation method of a leadless nickel electrode slurry for thick-film resistor is characterized in that:
(1) get the raw materials ready: according to mass percent, the extra-fine nickel powder, 2-10% leadless glass powder, 20-50% organic carrier and the 5-12% additive that take by weighing 40-60% are standby; Described extra-fine nickel powder average grain diameter is 0.05-5 μ m, and the leadless glass powder average grain diameter is 0.01-5 μ m; Described extra-fine nickel powder, leadless glass powder, organic carrier and additive gross mass are 100%; Described additive is made of curtain coating agent and thixotropic agent, and wherein the mass percent of curtain coating agent and thixotropic agent is 1: 1; Described curtain coating agent is a kind of or its mixture in dibutyl phthalate, polyvinylpyrrolidone, the laurate list glyceride; Described thixotropic agent is a kind of or its mixture in calcium carbonate, tricalcium phosphate, the sodium acid carbonate;
(2) mix: the extra-fine nickel powder and the leadless glass powder of gained in the step (1) are mixed, and make organic carrier, mix the back and obtained once mixture in 1-10 hour at ball mill or ball grinder mixing with absolute ethyl alcohol;
(3) drying: the mixture of gained in the step (2) was dried 0.5-2 hour under 40-80 ℃ of condition, and the room temperature cooling obtains secondary mixture then;
(4) add organic carrier: the additive of gained in the step (1) is joined in the secondary mixture of gained in the step (3) and mix, filter and obtain preliminary slurry;
(5) rolling: the preliminary slurry of gained in the step (4) is carried out 2-7 all over rolling with three-high mill, be checked through till the fineness of 0-5 μ m, obtain leadless nickel electrode slurry through 400 purpose screen filtrations then.
2. a kind of preparation method of leadless nickel electrode slurry for thick-film resistor according to claim 1, it is characterized in that: described step (1) is got the raw materials ready: according to mass percent, it is standby to take by weighing 40%, 50% or 60% extra-fine nickel powder, 2%, 5%, 8% or 10% leadless glass powder, 20%, 30%, 40% or 50% organic carrier and 5%, 8% or 12% additive.
3. a kind of preparation method of leadless nickel electrode slurry for thick-film resistor according to claim 1 is characterized in that: described step (2) is mixed at ball mill or ball grinder and was obtained once mixture in 1 hour, 3 hours, 5 hours, 8 hours or 10 hours.
4. a kind of preparation method of leadless nickel electrode slurry for thick-film resistor according to claim 1 is characterized in that: described step (3) drying: with the oven dry 0.5 hour, 1 hour, 1.5 hours or 2 hours under 40 ℃, 50 ℃, 60 ℃, 70 ℃ or 80 ℃ of conditions of the mixture of gained in the step (2).
5. a kind of preparation method of leadless nickel electrode slurry for thick-film resistor according to claim 1 is characterized in that: described step (5) rolling: the preliminary slurry of gained in the step (4) is carried out rolling 2,3,4,5,6 or 7 times with three-high mill.
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| CN102610752A (en) * | 2012-03-23 | 2012-07-25 | 清华大学深圳研究生院 | Method for manufacturing memory resistor through three-dimensional maskless slurry direct writing forming and memory resistor |
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| CN106205875A (en) * | 2016-08-31 | 2016-12-07 | 安徽斯迈尔电子科技有限公司 | A kind of preparation method of thick-film resistor resistance slurry |
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