Alumina ceramic metalized tungsten slurry, preparation method and application

Abstract

The invention discloses aluminum oxide ceramic metalized tungsten slurry, a preparation method and application, and belongs to the technical field of metalized tungsten slurry, the metalized tungsten slurry is used for being matched and co-fired with aluminum oxide ceramic with 92%-96% of aluminum oxide, and the metalized tungsten slurry comprises, by mass, 65%-87% of conductive metal tungsten powder, 3%-15% of an inorganic bonding phase and 10%-30% of an organic carrier, the total mass ratio of the conductive metal tungsten powder, the inorganic bonding phase and the organic carrier is 100%, the inorganic bonding phase comprises 92%-96% of Al2O3 powder and 0.5%-7.5% of a sintering aid, the sintering aid comprises a rare earth oxide and an alkali metal oxide, and the organic carrier comprises 8%-38% of an organic bonding agent, 10%-50% of a plasticizer and 3%-75% of a solvent. The metalized tungsten slurry has the advantages of good fluidity, good thixotropy, high resolution and small sheet resistance, and the sheet resistance value is in the range of 9-28 m omega / square.

Description

Technical Field

[0001] The present invention relates to the technical field of metallized tungsten slurry, and in particular to an alumina ceramic metallized tungsten slurry, a preparation method and application thereof. Background Art

[0002] With the rapid development of electronic information industries such as microelectronics technology, computers, and communications technology, the requirements for high integration, high speed, high density, high reliability, and miniaturization of electronic components are becoming increasingly higher, leading to the rapid development of high-temperature co-fired ceramic (HTCC) technology and its corresponding materials. High-temperature co-fired alumina ceramic substrates have the advantages of high mechanical strength, good thermal conductivity, low material cost, corrosion resistance, high temperature resistance, long life, and high wiring density. They are widely used in the fields of high-reliability microelectronic integrated circuits, high-power micro-assembly circuits, and automotive high-power circuits. Summary of the invention

[0003] The technical problem to be solved by the present invention is to provide an alumina ceramic metallized tungsten slurry, a preparation method and an application thereof. The tungsten slurry has good fluidity, good thixotropy, high resolution and small square resistance, thereby solving the problem that the metallized tungsten slurry has poor versatility and it is difficult to balance material properties.

[0004] In order to solve the above technical problems, the technical solution of the present invention is:

[0005] The present invention discloses a metallized tungsten slurry of alumina ceramics, wherein the metallized tungsten slurry comprises, by mass ratio, 65% to 87% of conductive metal tungsten powder, 3% to 15% of an inorganic bonding phase, and 10% to 30% of an organic carrier, wherein the total mass ratio of the conductive metal tungsten powder, the inorganic bonding phase, and the organic carrier is 100%, and the inorganic bonding phase comprises 92% to 96% of Al 2 O 3 The powder and 0.5% to 7.5% of a sintering aid include rare earth oxides and alkali metal oxides; the organic carrier includes 8% to 38% of an organic binder, 10% to 50% of a plasticizer and 3% to 75% of a solvent.

[0006] Preferably, the particle size of the conductive metal tungsten powder is 0.3 μm to 2.5 μm.

[0007] Preferably, the organic adhesive is any one of methyl cellulose, polyvinyl alcohol, polyvinyl acid, phenolic resin, epoxy resin, or a mixture of two or more thereof.

[0008] Preferably, the plasticizer is any one of dibutyl phthalate, soybean lecithin, hydrogenated castor oil, or a mixture of two or more thereof.

[0009] Preferably, the solvent is any one of ethanol, toluene, acetone, xylene, and terpineol, or a mixture of two or more thereof.

[0010] Preferably, the rare earth oxide is Y 2 O 3 The alkali metal oxide is MgO, the sintering aid also includes talcum powder, and the content of each component of the sintering aid is 0.25% to 2.5% of Y 2 O 3 , 0.3%~5.5% MgO, 0.05%~1.5% talc.

[0011] Another aspect of the present invention discloses a method for preparing the above-mentioned alumina ceramic metallized tungsten slurry, and the method for preparing the metallized tungsten slurry comprises:

[0012] S1. Preparation of inorganic bonding phase:

[0013] Alumina powder, rare earth oxide, and alkali metal oxide are weighed in proportion and placed in a ball mill, and appropriate amounts of dispersant and anhydrous ethanol are added to the ball mill for 1 to 3 hours. After the ball milling is completed, the slurry is poured into a drying dish, dried, ground, and passed through a 200-mesh sieve for later use;

[0014] S2. Preparation of conductive metal tungsten powder mixture:

[0015] The inorganic binder phase and the conductive tungsten powder obtained in step S1 are weighed in proportion and placed in a ball mill, and then a dispersant and anhydrous ethanol are added to the ball mill, followed by ball milling for 1.5 to 2.5 hours. After the ball milling, the slurry is poured into a drying dish, dried, ground, and passed through a 200-mesh sieve for later use;

[0016] S3. Preparation of organic carrier:

[0017] Weigh the organic binder, plasticizer and solvent in proportion, first add the solvent and plasticizer into a stirring and dissolving container and stir evenly, heat the stirring and dissolving container at a temperature of 60 to 70° C. and a stirring speed of 99 to 999 r / min, add the organic binder while stirring until it is completely dissolved and evenly dispersed, and seal and store for later use;

[0018] S4. Preparation of tungsten slurry for multilayer alumina ceramics:

[0019] The conductive metal tungsten powder mixture obtained in step S2 and the organic carrier obtained in step S3 are weighed in a certain proportion and placed in a high-speed stirrer for rapid stirring to form a mixed slurry, wherein the stirring speed is 999-9999 r / min and the stirring time is 10-60 s. The rapidly stirred mixed slurry is then repeatedly rolled using a three-axis rolling machine until the required printing viscosity is met to obtain the required metallized tungsten slurry electronic slurry for multi-layer alumina ceramics.

[0020] Another aspect of the present invention also discloses an application of the metallized tungsten slurry of alumina ceramics. The metallized tungsten slurry is used for co-firing with alumina ceramics having an alumina content of 92% to 96%.

[0021] The above technical solution has the following beneficial effects:

[0022] The present invention selects metal tungsten powder with a particle size of 0.3μm to 2.5μm, an inorganic bonding phase composed of rare earth oxides and alkali metal oxides, and an organic carrier, and then uses a three-axis pulping machine to roll the metallized tungsten slurry electronic slurry for the required multilayer alumina ceramic. The metallized electronic slurry has good fluidity, good thixotropy, high resolution, and small square resistance. The square resistance value is in the range of 9 to 28mΩ / □;

[0023] The prepared metallized tungsten slurry can not only meet the high-temperature co-firing matching of multi-layer alumina ceramic wiring circuit boards, components and tube shells with different alumina contents, but also has high flatness and strong adhesion; it can be used to prepare high-precision functional printed graphics and prepare other multi-layer interconnected ceramic electronic circuits;

[0024] The metallized tungsten slurry electronic slurry of the present invention has a wide range of raw materials, a simple preparation process, can achieve large-scale industrialized and low-cost production, and is widely used in HTCC multi-layer alumina ceramic circuit boards, multi-layer components, integrated circuit substrates, integrated circuit packaging shells and other technical fields. DETAILED DESCRIPTION

[0025] The specific embodiments of the present invention are further described below. It should be noted that the description of these embodiments is used to help understand the present invention, but does not constitute a limitation of the present invention. In addition, the technical features involved in each embodiment of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0026] Example 1

[0027] An alumina ceramic metallized tungsten slurry, the metallized tungsten slurry comprises, by mass ratio:

[0028] 65% to 87% conductive metal tungsten powder, 3% to 15% inorganic bonding phase and 10% to 30% organic carrier, the total mass ratio of the conductive metal tungsten powder, the inorganic bonding phase and the organic carrier is 100%;

[0029] Among them, the inorganic bonding phase includes 92% to 96% Al 2 O 3Powder and 0.5% to 7.5% of sintering aid, the sintering aid includes rare earth oxide and alkali metal oxide, the organic carrier includes 8% to 38% of organic binder, 10% to 50% of plasticizer and 3% to 75% of solvent;

[0030] The particle size of the conductive metal tungsten powder is 0.3 μm to 2.5 μm, which is selected according to the needs or actual conditions; the organic adhesive is any one of methyl cellulose, polyvinyl alcohol, polyvinyl acid, phenolic resin, epoxy resin, or a mixture of two or more thereof;

[0031] The plasticizer is any one of dibutyl phthalate, soybean lecithin, hydrogenated castor oil, or a mixture of two or more thereof;

[0032] The solvent is any one of ethanol, toluene, acetone, xylene, and terpineol, or a mixture of two or more thereof;

[0033] Rare earth oxide is Y 2 O 3 The alkali metal oxide is MgO, the sintering aid also includes talc, and the contents of the sintering aids are 0.25% to 2.5% of Y 2 O 3 , 0.3% to 5.5% MgO, 0.05% to 1.5% talc, Y 2 O 3 , MgO, and talc account for a total of 0.5% to 7.5%;

[0034] The present invention selects metal tungsten powder with a particle size of 0.3μm to 2.5μm, an inorganic bonding phase composed of rare earth oxides and alkali metal oxides, and an organic carrier, and then uses a three-axis pulping machine to roll the metallized tungsten slurry electronic slurry for the required multilayer alumina ceramic. The metallized electronic slurry has good fluidity, good thixotropy, high resolution, and small square resistance. The square resistance value is in the range of 9 to 28mΩ / □;

[0035] The prepared metallized tungsten paste can not only meet the high-temperature co-firing matching of multi-layer alumina ceramic wiring circuit boards, components and tube shells with different alumina contents (92% black porcelain and 96% white porcelain) but also has high flatness and strong adhesion; it can also prepare high-precision functional printed graphics and prepare other multi-layer interconnected ceramic electronic circuits;

[0036] The metallized tungsten slurry electronic slurry of the present invention has a wide range of raw materials, a simple preparation process, can achieve large-scale industrialized and low-cost production, and is widely used in HTCC multi-layer alumina ceramic circuit boards, multi-layer components, integrated circuit substrates, integrated circuit packaging shells and other technical fields.

[0037] Example 2

[0038] A metallized tungsten slurry for alumina ceramics, the metallized tungsten slurry comprises, by mass ratio, 65% conductive metal tungsten powder, 5% inorganic bonding phase and 30% organic carrier, wherein the inorganic bonding phase comprises 92.5% Al 2 O 3 powder and 7.5% sintering aid, Al 2 O 3 The total percentage of the powder and the sintering aid is 100%, the sintering aid includes rare earth oxide and alkali metal oxide, the organic carrier includes 8% of organic binder, 17% of plasticizer and 75% of solvent, and the total percentage of the organic binder, plasticizer and solvent is 100%;

[0039] The particle size of the conductive metal tungsten powder is 0.3 μm; the organic binder is any one of methyl cellulose, polyvinyl alcohol, polyvinyl acid, phenolic resin, and epoxy resin; the plasticizer is any one of dibutyl phthalate, soybean lecithin, and hydrogenated castor oil; the solvent is any one of ethanol, toluene, acetone, xylene, and pinene alcohol;

[0040] Rare earth oxide is Y 2 O 3 The alkali metal oxide is MgO, the sintering aid also includes talc, and the contents of the sintering aids are 0.25% to 2.5% of Y 2 O 3 , 0.3% to 5.5% MgO, 0.05% to 1.5% talc, Y 2 O 3 The total percentage of MgO and talc is 7.5%. The specific content of each component of the sintering aid can be 1% of Y 2 O 3 , 5% MgO, 1.5% talc;

[0041] The present invention selects metal tungsten powder with a particle size of 0.3 μm, an inorganic bonding phase composed of rare earth oxides and alkali metal oxides, and an organic carrier, and then uses a three-axis pulping machine to roll the metallized tungsten slurry electronic slurry for the required multilayer alumina ceramic. The metallized electronic slurry has good fluidity, good thixotropy, high resolution, and small square resistance. The square resistance value is in the range of 9 to 28 mΩ / □;

[0042] The prepared metallized tungsten paste can not only meet the high-temperature co-firing matching of multi-layer alumina ceramic wiring circuit boards, components and tube shells with different alumina contents (92% black porcelain and 96% white porcelain) but also has high flatness and strong adhesion; it can also prepare high-precision functional printed graphics and prepare other multi-layer interconnected ceramic electronic circuits;

[0043] The metallized tungsten slurry electronic slurry of the present invention has a wide range of raw materials, a simple preparation process, can achieve large-scale industrialized and low-cost production, and is widely used in HTCC multi-layer alumina ceramic circuit boards, multi-layer components, integrated circuit substrates, integrated circuit packaging shells and other technical fields.

[0044] Example 3

[0045] A metallized tungsten slurry for alumina ceramics, the metallized tungsten slurry comprises, by mass ratio, 87% conductive metal tungsten powder, 3% inorganic bonding phase and 10% organic carrier, wherein the inorganic bonding phase comprises 96% Al 2 O 3 powder and 4% sintering aid, the sintering aid includes rare earth oxide and alkali metal oxide, and the organic carrier includes 20% organic binder, 30% plasticizer and 50% solvent;

[0046] The particle size of the conductive metal tungsten powder is 2.5 μm; the organic adhesive is any two of methyl cellulose, polyvinyl alcohol, polyvinyl acid, phenolic resin, epoxy resin, or a mixture of two or more thereof;

[0047] The plasticizer is any two of dibutyl phthalate, soybean lecithin, hydrogenated castor oil, or a mixture of two or more thereof;

[0048] The solvent is any two of ethanol, toluene, acetone, xylene, terpineol, or a mixture of two or more thereof;

[0049] Rare earth oxide is Y 2 O 3 The alkali metal oxide is MgO, the sintering aid also includes talc, and the contents of the sintering aids are 1.5% Y 2 O 3 , 2% MgO, 0.5% talc;

[0050] The present invention selects metal tungsten powder with a particle size of 2.5 μm, an inorganic bonding phase composed of rare earth oxides and alkali metal oxides, and an organic carrier, and then uses a three-axis pulping machine to roll the metallized tungsten slurry electronic slurry for the required multilayer alumina ceramic. The metallized electronic slurry has good fluidity, good thixotropy, high resolution, and small square resistance. The square resistance value is in the range of 9 to 28 mΩ / □;

[0051] The prepared metallized tungsten paste can not only meet the high-temperature co-firing matching of multi-layer alumina ceramic wiring circuit boards, components and tube shells with different alumina contents (92% black porcelain and 96% white porcelain) but also has high flatness and strong adhesion; it can also prepare high-precision functional printed graphics and prepare other multi-layer interconnected ceramic electronic circuits;

[0052] The metallized tungsten slurry electronic slurry of the present invention has a wide range of raw materials, a simple preparation process, can achieve large-scale industrialized and low-cost production, and is widely used in HTCC multi-layer alumina ceramic circuit boards, multi-layer components, integrated circuit substrates, integrated circuit packaging shells and other technical fields.

[0053] Example 4

[0054] A method for preparing alumina ceramic metallized tungsten slurry. The ratio of each substance added during the preparation process can refer to Example 1. The specific preparation method includes the following steps:

[0055] S1. Preparation of inorganic bonding phase:

[0056] Alumina powder, rare earth oxide, and alkali metal oxide are weighed in proportion and placed in a ball mill. In other embodiments of this embodiment, the sintering aid is a mixture of rare earth oxide, alkali metal oxide, and talcum powder. A proper amount of dispersant and anhydrous ethanol are added and ball milled for 1 to 3 hours. In other embodiments of this embodiment, a proper amount of dispersant and anhydrous ethanol are added and ball milled for 2 hours. The proportion of alumina powder, rare earth oxide, and alkali metal oxide can be added according to the proportion in Example 2 or Example 3, wherein the rare earth oxide is Y 2 O 3 , the alkali metal oxide is MgO, after the ball milling, the slurry is poured into a drying dish for drying, grinding, and passing through a 200-mesh sieve for later use;

[0057] S2. Preparation of conductive metal tungsten powder mixture:

[0058] The inorganic binder phase and the conductive tungsten powder obtained in the above step S1 are weighed in proportion and placed in a ball mill, and then a dispersant and anhydrous ethanol are added to the ball mill and ball milled for 1.5 to 2.5 hours. In other implementations of this embodiment, the ball milling time can also be 2 hours. After the ball milling is completed, the slurry is poured into a drying dish, dried, ground, and passed through a 200-mesh sieve for later use;

[0059] S3. Preparation of organic carrier:

[0060] Weigh the organic binder, plasticizer and solvent in proportion, first add the solvent and plasticizer into the stirring and dissolving container and stir evenly, the specific proportion can refer to Examples 2 and 3, the stirring and dissolving container is heated, the heating temperature is 60-70°C, the stirring speed is 99-999r / min, the organic binder is added while stirring until it is completely dissolved and evenly dispersed, and the mixture is sealed and stored for later use. In other implementations of this embodiment, the heating temperature of the stirring and dissolving is 65°C, and the stirring speed is 599r / min;

[0061] The organic adhesive is any one of methyl cellulose, polyvinyl alcohol, polyvinyl acid, phenolic resin, epoxy resin, or a mixture of two or more thereof;

[0062] The plasticizer is any one of dibutyl phthalate, soybean lecithin, hydrogenated castor oil, or a mixture of two or more thereof;

[0063] The solvent is any one of ethanol, toluene, acetone, xylene, and terpineol, or a mixture of two or more thereof;

[0064] S4. Preparation of tungsten slurry for multilayer alumina ceramics:

[0065] The conductive metal tungsten powder mixture obtained in step S2 and the organic carrier obtained in step S3 are weighed in a certain proportion and then placed in a high-speed stirrer for rapid stirring to form a mixed slurry, wherein the stirring speed is 999-9999 r / min and the stirring time is 10-60 s. In other implementations of this embodiment, the stirring speed may be 5999 r / min and the stirring time may be 50 s. The rapidly stirred mixed slurry is repeatedly rolled multiple times using a three-axis rolling machine until the required printing viscosity is met to obtain the required metallized tungsten slurry electronic slurry for multi-layer alumina ceramics;

[0066] The metallized tungsten slurry electronic slurry of the present invention has a wide range of raw materials, a simple preparation process, can achieve large-scale industrialized and low-cost production, and is widely used in HTCC multi-layer alumina ceramic circuit boards, multi-layer components, integrated circuit substrates, integrated circuit packaging shells and other technical fields.

[0067] Example 5

[0068] An application of the above-mentioned metallized tungsten slurry of alumina ceramics, the above-mentioned metallized tungsten slurry is used for co-firing with alumina ceramics with an alumina content of 92% to 96%; the metallized tungsten slurry prepared by the present invention can simultaneously meet the high-temperature co-firing matching of multi-layer alumina ceramic wiring circuit boards, components and tube shells with different alumina contents (92% black porcelain and 96% white porcelain), and has high flatness and strong adhesion; it can be used to prepare high-precision functional printed graphics and prepare other multi-layer interconnected ceramic electronic circuits.

[0069] The embodiments of the present invention are described in detail above, but the present invention is not limited to the described embodiments. For those skilled in the art, various changes, modifications, substitutions and variations of these embodiments are made without departing from the principles and spirit of the present invention, and still fall within the protection scope of the present invention.

Claims

1. An alumina ceramic metallized tungsten slurry, characterized in that: The metallized tungsten slurry comprises, by mass ratio, 65% to 87% of conductive metal tungsten powder, 3% to 15% of inorganic bonding phase and 10% to 30% of organic carrier, the total mass ratio of the conductive metal tungsten powder, the inorganic bonding phase and the organic carrier is 100%, the inorganic bonding phase comprises 92% to 96% of Al2O3 powder and 0.5% to 7.5% of sintering aid, the sintering aid comprises rare earth oxide and alkali metal oxide, the organic carrier comprises 8% to 38% of organic binder, 10% to 50% of plasticizer and 3% to 75% of solvent.

2. The alumina ceramic metallized tungsten slurry according to claim 1, characterized in that: The particle size of the conductive metal tungsten powder is 0.3 μm to 2.5 μm.

3. The alumina ceramic metallized tungsten slurry according to claim 1, characterized in that: The organic adhesive is any one of methyl cellulose, polyvinyl alcohol, polyvinyl acid, phenolic resin, epoxy resin, or a mixture of two or more thereof.

4. The alumina ceramic metallized tungsten slurry according to claim 1, characterized in that: The plasticizer is any one of dibutyl phthalate, soybean lecithin, and hydrogenated castor oil, or a mixture of two or more of the two.

5. The alumina ceramic metallized tungsten slurry according to claim 1, characterized in that: The solvent is any one of ethanol, toluene, acetone, xylene and terpineol, or a mixture of two or more thereof.

6. The alumina ceramic metallized tungsten slurry according to claim 1, characterized in that: The rare earth oxide is Y2O3, the alkali metal oxide is MgO, and the sintering aid further comprises talc powder. The contents of the components of the sintering aid are 0.25% to 2.5% of Y2O3, 0.3% to 5.5% of MgO, and 0.05% to 1.5% of talc powder respectively.

7. A method for preparing alumina ceramic metallized tungsten slurry as claimed in any one of claims 1 to 6, characterized in that: The preparation method of the metallized tungsten slurry comprises: S1. Preparation of inorganic bonding phase: Alumina powder, rare earth oxide, and alkali metal oxide are weighed in proportion and placed in a ball mill, and appropriate amounts of dispersant and anhydrous ethanol are added to the ball mill for 1 to 3 hours. After the ball milling is completed, the slurry is poured into a drying dish, dried, ground, and passed through a 200-mesh sieve for later use; S2. Preparation of conductive metal tungsten powder mixture: The inorganic binder phase and the conductive tungsten powder obtained in step S1 are weighed in proportion and placed in a ball mill, and then a dispersant and anhydrous ethanol are added to the ball mill, followed by ball milling for 1.5 to 2.5 hours. After the ball milling, the slurry is poured into a drying dish, dried, ground, and passed through a 200-mesh sieve for later use; S3. Preparation of organic carrier: Weigh the organic binder, plasticizer and solvent in proportion, first add the solvent and plasticizer into a stirring and dissolving container and stir evenly, heat the stirring and dissolving container at a temperature of 60 to 70° C. and a stirring speed of 99 to 999 r / min, add the organic binder while stirring until it is completely dissolved and evenly dispersed, and seal and store for later use; S4. Preparation of tungsten slurry for multilayer alumina ceramics: The conductive metal tungsten powder mixture obtained in step S2 and the organic carrier obtained in step S3 are weighed in a certain proportion and placed in a high-speed stirrer for rapid stirring to form a mixed slurry, wherein the stirring speed is 999-9999 r / min and the stirring time is 10-60 s. The rapidly stirred mixed slurry is then repeatedly rolled using a three-axis rolling machine until the required printing viscosity is met to obtain the required metallized tungsten slurry electronic slurry for multi-layer alumina ceramics.

8. An application of the alumina ceramic metallized tungsten slurry as claimed in any one of claims 1 to 6, characterized in that: The metallized tungsten slurry is used for co-firing with alumina ceramics having an alumina content of 92% to 96%.