CN114538932A - Preparation method of co-fired aluminum nitride ceramic substrate - Google Patents
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Abstract
The invention relates to the field of electronic ceramic substrates, and provides a method for co-firing an aluminum nitride ceramic substrate, which solves the defects of low thermal conductivity and high energy consumption caused by overhigh sintering temperature of the co-fired aluminum nitride ceramic in the prior art. The preparation method comprises the following preparation steps: (1) material mixing and ball milling: sending the aluminum nitride powder and the sintering aid into a ball mill for ball milling treatment; (2) defoaming: aging the ball-milled slurry for 2-3 h, and then sending the slurry into a defoaming machine for defoaming until the viscosity of the slurry reaches 20000-23000 mPa & s; (3) tape casting: feeding the slurry treated in the step (2) into a casting machine for tape casting, and standing for 6-8 hours; (4) punching; (5) laminating: decompressing the printed green sheet according to the thickness requirement; (6) rubber discharging: placing the green sheet treated in the step (5) into a nitrogen protection degumming furnace, and carrying out degumming under a nitrogen atmosphere until the carbon content is below 2000 ppm; (7) and (5) sintering.
Description
Technical Field
The invention relates to the field of electronic ceramic substrates, in particular to a preparation method of a co-fired aluminum nitride ceramic substrate.
Background
High temperature co-fired ceramics (HTCC) currently on the market are mainly classified into three categories: ceramics respectively using alumina, mullite and aluminum nitride as main components. The ceramic with alumina as main component is one kind of mature microelectronic package technology, and is formed with alumina in 92-96 wt% and sintering assistant in 4-8 wt% and through sintering at 1500-1700 deg.c, and the conducting wires are refractory metals, such as tungsten, molybdenum-manganese, etc. The substrate has mature technology, low medium cost, high thermal conductivity and high bending strength. However, the disadvantages of the alumina multilayer ceramic substrate are also significant as follows: the dielectric constant is high, and the improvement of the signal transmission speed is influenced; the electrical resistivity of the conductor is high, and the signal transmission loss is large; the coefficient of thermal expansion is very different from that of silicon, limiting its application to supercomputers.
The ceramic with mullite as the main component has dielectric constant lower than that of alumina (9.4), so that its transmission delay time is about 17% shorter than that of alumina, and the thermal expansion coefficient of mullite is very similar to that of silicon, so that it has been developed fast. However, the substrate can only adopt tungsten, nickel, molybdenum and the like, and has higher resistivity and lower thermal conductivity than an alumina substrate.
Ceramics using aluminum nitride as a main component have high thermal conductivity, thermal expansion coefficient matched with semiconductor materials such as Si, SiC and GaAs, dielectric constant and dielectric loss superior to those of aluminum oxide, and aluminum nitride is a harder ceramic and can still work well under severe environmental conditions, thus having been widely studied at home and abroad. However, there are many problems to be solved in the high temperature co-fired ceramic technology of aluminum nitride. For example: (1) after the aluminum nitride substrate is co-fired with conductors such as tungsten, molybdenum and the like, the thermal conductivity of the aluminum nitride substrate is reduced; (2) the common tungsten slurry as the outer conductor raw material is easy to oxidize; (3) the sintering temperature is high, and the energy consumption is large; (4) screen printed resistors and other passive components cannot be incorporated into a high temperature co-firing process.
Chinese patent application No. 201611115067.5 discloses a sintering method of high-temperature co-fired aluminum nitride ceramics, which comprises the following steps: (1) manufacturing an aluminum nitride green ceramic piece by using the aluminum nitride green ceramic and the metalized slurry according to a multilayer ceramic production process; (2) removing glue from the aluminum nitride green ceramic piece in a glue removing furnace; (3) placing the green porcelain piece after the glue is removed into a double-closed burning bearing device; (4) and (4) putting the sintering device filled with the aluminum nitride green porcelain product into a high-temperature atmosphere sintering furnace for sintering. The invention has the advantages that: 1) the high-temperature co-fired aluminum nitride ceramic can be prepared and applied to the fields of MCM substrates and packaging, substrates and shells of high-power devices, high-power LED packaging shells and the like; 2) the method can avoid the excessive volatilization of the second phase in the aluminum nitride ceramic by sintering, and the thermal conductivity, the breaking strength and the metallization strength of the obtained co-fired aluminum nitride ceramic meet the use requirements of electronic ceramics. And the sintering temperature is as high as 1900 ℃, and the energy consumption is large.
Disclosure of Invention
Therefore, aiming at the problems, the invention provides a method for co-firing an aluminum nitride ceramic substrate, which solves the defects of low thermal conductivity and high energy consumption caused by overhigh sintering temperature of the co-fired aluminum nitride ceramic in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a co-fired aluminum nitride ceramic substrate comprises the following preparation steps: (1) material mixing and ball milling: sending the aluminum nitride powder and the sintering aid into a ball mill for ball milling treatment;
(2) defoaming: aging the ball-milled slurry for 2-3 h, and then sending the slurry into a defoaming machine for defoaming until the viscosity of the slurry reaches 20000-23000 mPa & s;
(3) tape casting: feeding the slurry treated in the step (2) into a casting machine for tape casting, and standing for 6-8 hours;
(4) punching: slicing the cast green tape to obtain a green sheet with a required shape and size, and printing the green sheet by adopting tungsten slurry and then standing the green sheet or drying the tungsten slurry in an oven; the preparation method of the tungsten slurry comprises the following steps: selecting tungsten powder with the particle size of 0.8-1.1 mu m and tungsten powder with the particle size of 2-3 mu m, uniformly mixing the tungsten powder with ruthenium oxide, silicon oxide, aluminum oxide, calcium oxide and an organic medium in advance, and fully dispersing;
(5) laminating: decompressing the printed green sheet according to the thickness requirement;
(6) rubber discharging: placing the green sheet treated in the step (5) into a nitrogen protection degumming furnace, and carrying out degumming under a nitrogen atmosphere until the carbon content is below 2000 ppm;
(7) and (3) sintering: and sintering the green compact sheet after the binder removal is finished, and covering a layer of aluminum nitride ceramic green compact sheet without printing the tungsten slurry on the upper surface and the lower surface of the green compact sheet during sintering.
The further improvement is that: the concrete process for removing the glue in the step (6) comprises the following steps: the green sheet in the nitrogen protection binder removal furnace is firstly kept stand for 4-5 h at room temperature, then is heated to 130 ℃ and is kept warm for 17-18 h, then is heated to 190 ℃ and is kept warm for 10-11 h, then is heated to 240 ℃ and is kept warm for 12-13 h, and then is heated to 300 ℃ and is kept warm for 16-17 h.
The further improvement is that: the dosage ratio of the tungsten powder with the grain diameter of 0.8-1.1 mu m to the tungsten powder with the grain diameter of 2-3 mu m is 30-50 by weight: 50-70.
the further improvement is that: the tungsten slurry comprises the following components in parts by weight: ruthenium oxide: silicon oxide: alumina: calcium oxide: organic medium 10: 0.1-0.2: 0.5-0.8: 1-2: 0.3-0.5: 20-50.
the further improvement is that: the organic medium is a mixture of linseed oil, methyl cellulose, polyethylene glycol and polyacrylic resin.
The further improvement is that: the specific method for the dispersion treatment in the step (4) comprises the following steps: firstly, feeding tungsten powder and part of organic medium into a ball mill for dispersion treatment; ruthenium (II) oxide, silicon oxide, aluminum oxide and calcium oxide and other organic media are subjected to redispersion treatment.
The further improvement is that: the bonding assistant is yttrium oxide.
The further improvement is that: the tungsten slurry is also added with iron powder, and the dosage of the iron powder is 0.1-0.2 time of that of the tungsten powder.
The further improvement is that: and (7) during sintering, applying pressure of 20-50 MPa after the aluminum nitride ceramic green body which is not printed with the tungsten paste and covers the upper surface and the lower surface of the green body sheet during sintering.
By adopting the technical scheme, the invention has the beneficial effects that:
1. the traditional plane printing slurry is generally prepared by mixing tungsten powder, an inorganic phase and an organic phase according to a certain proportion, but because of the difference of the surface properties of the tungsten powder and the inorganic phase, if a single dispersant is adopted, the phenomenon of competitive adsorption is generated, so that stable and uniform slurry is difficult to obtain; the tungsten slurry is subjected to step dispersion treatment during preparation, namely, the tungsten powder is subjected to ball milling dispersion firstly, and then other inorganic media are subjected to dispersion treatment, and the tungsten powder and other inorganic media have adsorption requirements on the dispersing agent, so competitive adsorption on organic media can be generated if the tungsten powder and other inorganic media are added at the same time, the step dispersion treatment can effectively avoid the occurrence of competitive adsorption, and the stability of the tungsten slurry is improved.
2. The organic medium adopted by the invention contains linseed oil which is rich in unsaturated fatty acid and can be effectively adsorbed on the surface of tungsten powder to form stable steric hindrance, so that the viscosity of the prepared slurry is lower.
3. The iron powder is added into the tungsten slurry, so that the stability after brazing can be improved.
4. The upper surface and the lower surface of the green sheet are covered with a layer of aluminum nitride green sheet without tungsten slurry, so that other products can be prevented from being polluted in the sintering process.
5. The tungsten powder adopted by the invention has coarse and fine particle sizes, and the prepared tungsten slurry has stable performance by selecting two tungsten powders with specific particle sizes for matching.
Detailed Description
Example one
A preparation method of a co-fired aluminum nitride ceramic substrate comprises the following preparation steps: (1) material mixing and ball milling: feeding aluminum nitride powder and yttrium oxide into a ball mill for ball milling treatment, wherein the dosage of the yttrium oxide is 0.2 wt% of the aluminum nitride powder, and the particle size of the aluminum nitride powder is micron-sized, specifically, in the embodiment, the particle size of the aluminum nitride powder is 0.3 μm; absolute ethyl alcohol and alumina grinding balls are added into the ball mill during ball milling treatment;
(2) defoaming: aging the ball-milled slurry for 2 hours, and then sending the slurry into a defoaming machine for defoaming until the viscosity of the slurry reaches 20000mPa s;
(3) tape casting: feeding the slurry treated in the step (2) into a casting machine for tape casting, and standing for 6 hours;
(4) punching: slicing the cast green tape to obtain a green sheet with a required shape and size, and printing the green sheet by adopting tungsten slurry and then standing the green sheet or drying the tungsten slurry in an oven; the preparation method of the tungsten slurry comprises the following steps: firstly, feeding tungsten powder and part of organic medium into a ball mill for dispersion treatment: selecting tungsten powder with the particle size of 0.8 mu m and tungsten powder with the particle size of 2 mu m according to the weight ratio of 3: 7, and performing ball milling and dispersion treatment on the mixture and part of organic medium, wherein the organic medium is linseed oil, methylcellulose, polyethylene glycol and polyacrylic resin according to a weight ratio of 1: 1: 1: 2: 1, mixing the mixture; re-dispersing ruthenium oxide, silicon oxide, aluminum oxide, calcium oxide and other organic media; thirdly, mixing the materials subjected to the dispersion treatment in the first step and the second step together, and performing dispersion treatment again to obtain tungsten slurry; the tungsten slurry comprises the following components in parts by weight: ruthenium oxide: silicon oxide: alumina: calcium oxide: organic medium 10: 0.1: 0.5: 1: 0.3: 20; the dosage ratio of the organic medium in the step (I) to the organic medium in the step (II) is 6: 4;
(5) laminating: decompressing the printed green sheet according to the thickness requirement;
(6) rubber discharging: placing the green sheet treated in the step (5) into a nitrogen protection degumming furnace, and carrying out degumming under a nitrogen atmosphere until the carbon content is below 2000 ppm; the specific process comprises the following steps: the green sheet in the nitrogen protection binder removal furnace is firstly kept stand for 4h at room temperature, then is heated to 130 ℃ and is kept warm for 17h, then is heated to 190 ℃ and is kept warm for 10h, then is heated to 240 ℃ and is kept warm for 12h, and then is heated to 300 ℃ and is kept warm for 16 h.
(7) And (3) sintering: and sintering the green compact sheet after the binder removal is finished, and covering a layer of aluminum nitride ceramic green compact sheet without printing the tungsten slurry on the upper surface and the lower surface of the green compact sheet during sintering.
Example two
A preparation method of a co-fired aluminum nitride ceramic substrate comprises the following preparation steps: (1) material mixing and ball milling: feeding aluminum nitride powder and yttrium oxide into a ball mill for ball milling treatment;
(2) defoaming: aging the ball-milled slurry for 2.5h, and then sending the slurry into a defoaming machine for defoaming until the viscosity of the slurry reaches 22000mPa & s;
(3) tape casting: feeding the slurry treated in the step (2) into a casting machine for tape casting, and standing for 7 hours;
(4) punching: slicing the cast green tape to obtain a green sheet with a required shape and size, and printing the green sheet by adopting tungsten slurry and then standing the green sheet or drying the tungsten slurry in an oven; the preparation method of the tungsten slurry comprises the following steps: firstly, feeding tungsten powder and part of organic medium into a ball mill for dispersion treatment: selecting tungsten powder with the particle size of 1.0 mu m and tungsten powder with the particle size of 2 mu m according to the weight ratio of 4: 6, and ball-milling and dispersing the mixture with a part of organic medium, wherein the organic medium is linseed oil, methylcellulose, polyethylene glycol and polyacrylic resin according to a weight ratio of 1: 1: 1: 2: 1, mixing the mixture; re-dispersing ruthenium oxide, silicon oxide, aluminum oxide, calcium oxide and other organic media; thirdly, mixing the materials subjected to the dispersion treatment in the first step and the second step together, and performing dispersion treatment again to obtain tungsten slurry; the tungsten slurry comprises the following components in parts by weight: ruthenium oxide: silicon oxide: alumina: calcium oxide: organic medium 10: 0.15: 0.6: 1.5: 0.4: 30, of a nitrogen-containing gas; the dosage ratio of the organic medium in the step (I) to the organic medium in the step (II) is 6: 4;
(5) laminating: decompressing the printed green sheet according to the thickness requirement;
(6) rubber discharging: placing the green sheet treated in the step (5) into a nitrogen protection degumming furnace, and carrying out degumming under a nitrogen atmosphere until the carbon content is below 2000 ppm; the specific process comprises the following steps: standing the green sheet in a nitrogen protection binder removal furnace at room temperature for 4.5h, heating to 130 ℃ and preserving heat for 17.5h, then heating to 190 ℃ and preserving heat for 10.5h, then heating to 240 ℃ and preserving heat for 12.5h, then heating to 300 ℃ and preserving heat for 16.5 h;
(7) and (3) sintering: and sintering the green compact sheet after the binder removal is finished, covering a layer of aluminum nitride ceramic green compact sheet without printing tungsten slurry on the upper surface and the lower surface of the green compact sheet during sintering, applying 25MPa of pressure after covering, and controlling the sintering temperature at 1650 ℃.
EXAMPLE III
A preparation method of a co-fired aluminum nitride ceramic substrate comprises the following preparation steps: (1) material mixing and ball milling: feeding aluminum nitride powder and yttrium oxide into a ball mill for ball milling treatment;
(2) defoaming: aging the ball-milled slurry for 3 hours, and then sending the slurry into a defoaming machine for defoaming until the viscosity of the slurry reaches 23000mPa & s;
(3) tape casting: feeding the slurry treated in the step (2) into a casting machine for tape casting, and standing for 8 hours;
(4) punching: slicing the cast green tape to obtain a green sheet with a required shape and size, and printing the green sheet by adopting tungsten slurry and then standing the green sheet or drying the tungsten slurry in an oven; the preparation method of the tungsten slurry comprises the following steps: firstly, feeding tungsten powder and part of organic medium into a ball mill for dispersion treatment: selecting tungsten powder with the particle size of 1.1 mu m and tungsten powder with the particle size of 3 mu m according to the proportion of 5: 5, and ball-milling and dispersing the mixture with a part of organic medium, wherein the organic medium is linseed oil, methylcellulose, polyethylene glycol and polyacrylic resin according to a weight ratio of 1: 1: 1: 2: 1, mixing the mixture; re-dispersing ruthenium oxide, silicon oxide, aluminum oxide, calcium oxide and other organic media; thirdly, mixing the materials subjected to the dispersion treatment in the first step and the second step together, and performing dispersion treatment again to obtain tungsten slurry; the tungsten slurry comprises the following components in parts by weight: ruthenium oxide: silicon oxide: alumina: calcium oxide: organic medium 10: 0.2: 0.8: 2: 0.5: 50; the dosage ratio of the organic medium in the step (I) to the organic medium in the step (II) is 5: 5;
(5) laminating: decompressing the printed green sheet according to the thickness requirement;
(6) rubber discharging: placing the green sheet treated in the step (5) into a nitrogen protection degumming furnace, and carrying out degumming under a nitrogen atmosphere until the carbon content is below 2000 ppm; the specific process comprises the following steps: standing the green sheet in a nitrogen protection binder removal furnace at room temperature for 5 hours, heating to 130 ℃ and preserving heat for 18 hours, then heating to 190 ℃ and preserving heat for 11 hours, then heating to 240 ℃ and preserving heat for 13 hours, then heating to 300 ℃ and preserving heat for 17 hours;
(7) and (3) sintering: and sintering the green sheet after the glue discharging is finished, covering a layer of aluminum nitride ceramic green sheet without printing the tungsten slurry on the upper surface and the lower surface of the green sheet during sintering, and applying a pressure of 50 MPa.
Example four
Referring to the first embodiment, iron powder is further added into the tungsten slurry, the amount of the iron powder is 0.1 times of that of the tungsten powder, the iron powder and the tungsten powder are mixed in advance in the preparation process of the tungsten slurry in the step (4), and other technical schemes are the same as those in the first embodiment.
Comparative example 1
A preparation method of a co-fired aluminum nitride ceramic substrate comprises the following preparation steps: (1) material preparation and ball milling: feeding aluminum nitride powder and yttrium oxide into a ball mill for ball milling treatment, wherein the dosage of the yttrium oxide is 0.2 wt% of the aluminum nitride powder, and the particle size of the aluminum nitride powder is micron-sized, specifically, in the embodiment, the particle size of the aluminum nitride powder is 0.3 μm; the ball mill is added with absolute ethyl alcohol and alumina grinding balls during ball milling treatment;
(2) defoaming: aging the ball-milled slurry for 2 hours, and then sending the slurry into a defoaming machine for defoaming until the viscosity of the slurry reaches 20000mPa s;
(3) tape casting: feeding the slurry treated in the step (2) into a casting machine for tape casting, and standing for 6 hours;
(4) punching: slicing the cast green tape to obtain a green sheet with a required shape and size, and printing the green sheet by adopting tungsten slurry and then standing the green sheet or drying the tungsten slurry in an oven; the preparation method of the tungsten slurry comprises the following steps: selecting tungsten powder with the particle size of 1.1 mu m and tungsten powder with the particle size of 3 mu m according to the proportion of 5: 5, and ball-milling and dispersing the mixture with ruthenium oxide, silicon oxide, aluminum oxide, calcium oxide and an organic medium, wherein the organic medium is linseed oil, methyl cellulose, polyethylene glycol and polyacrylic resin according to a weight ratio of 1: 1: 1: 2: 1, mixing the mixture; the tungsten slurry comprises the following components in parts by weight: ruthenium oxide: silicon oxide: alumina: calcium oxide: organic medium 10: 0.2: 0.8: 2: 0.5: 50; (5) laminating: decompressing the printed green sheet according to the thickness requirement;
(6) rubber discharging: placing the green sheet treated in the step (5) into a nitrogen protection degumming furnace, and carrying out degumming under a nitrogen atmosphere until the carbon content is below 2000 ppm; the specific process comprises the following steps: the green sheet in the nitrogen protection binder removal furnace is firstly kept stand for 4h at room temperature, then is heated to 130 ℃ and is kept warm for 17h, then is heated to 190 ℃ and is kept warm for 10h, then is heated to 240 ℃ and is kept warm for 12h, and then is heated to 300 ℃ and is kept warm for 16 h.
(7) And (3) sintering: sintering the green compact sheet after the binder removal, and covering a layer of aluminum nitride ceramic green compact sheet without printing tungsten slurry on the upper and lower surfaces of the green compact sheet during sintering
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method of a co-fired aluminum nitride ceramic substrate is characterized by comprising the following preparation steps:
(1) material mixing and ball milling: sending the aluminum nitride powder and the sintering aid into a ball mill for ball milling treatment;
(2) defoaming: aging the ball-milled slurry for 2-3 h, and then sending the slurry into a defoaming machine for defoaming until the viscosity of the slurry reaches 20000-23000 mPa & s;
(3) tape casting: feeding the slurry treated in the step (2) into a casting machine for tape casting, and standing for 6-8 hours;
(4) punching: slicing the cast green tape to obtain a green sheet with a required shape and size, and printing the green sheet by adopting tungsten slurry and then standing the green sheet or drying the tungsten slurry in an oven; the preparation method of the tungsten slurry comprises the following steps: selecting tungsten powder with the particle size of 0.8-1.1 mu m and tungsten powder with the particle size of 2-3 mu m, uniformly mixing the tungsten powder with ruthenium oxide, silicon oxide, aluminum oxide, calcium oxide and an organic medium in advance, and fully dispersing;
(5) laminating: decompressing the printed green sheet according to the thickness requirement;
(6) rubber discharging: placing the green sheet treated in the step (5) into a nitrogen protection degumming furnace, and carrying out degumming under a nitrogen atmosphere until the carbon content is below 2000 ppm;
(7) and (3) sintering: and sintering the green compact sheet after the binder removal is finished, and covering a layer of aluminum nitride ceramic green compact sheet without printing the tungsten slurry on the upper surface and the lower surface of the green compact sheet during sintering.
2. The method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein: the concrete process for removing the glue in the step (6) comprises the following steps: the green sheet in the nitrogen protection binder removal furnace is firstly kept stand for 4-5 h at room temperature, then is heated to 130 ℃ and is kept warm for 17-18 h, then is heated to 190 ℃ and is kept warm for 10-11 h, then is heated to 240 ℃ and is kept warm for 12-13 h, and then is heated to 300 ℃ and is kept warm for 16-17 h.
3. The method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein: the dosage ratio of the tungsten powder with the grain diameter of 0.8-1.1 mu m to the tungsten powder with the grain diameter of 2-3 mu m is 30-50 by weight: 50-70.
4. the method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein: the tungsten slurry comprises the following components in parts by weight: ruthenium oxide: silicon oxide: alumina: calcium oxide: organic medium 10: 0.1-0.2: 0.5-0.8: 1-2: 0.3-0.5: 20-50.
5. the method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein: the organic medium is a mixture of linseed oil, methyl cellulose, polyethylene glycol and polyacrylic resin.
6. The method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein: the specific method for the dispersion treatment in the step (4) comprises the following steps: firstly, feeding tungsten powder and part of organic medium into a ball mill for dispersion treatment; ruthenium (II) oxide, silicon oxide, aluminum oxide and calcium oxide and other organic media are subjected to redispersion treatment.
7. The method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein the method comprises the following steps: the bonding assistant is yttrium oxide.
8. The method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein the method comprises the following steps: the tungsten slurry is also added with iron powder, and the dosage of the iron powder is 0.1-0.2 time of that of the tungsten powder.
9. The method for preparing a co-fired aluminum nitride ceramic substrate according to claim 1, wherein: and (7) during sintering, applying pressure of 20-50 MPa after the aluminum nitride ceramic green body which is not printed with the tungsten paste and covers the upper surface and the lower surface of the green body sheet during sintering.
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