Binding phase for tungsten-copper electronic paste and preparation method thereof

Abstract

The invention discloses a binding phase for tungsten-copper electronic paste and a preparation method thereof, and relates to the technical field of electronic paste preparation. The tungsten-copper electronic paste consists of 60-75wt% of aluminum oxide, 3-10wt% of magnesium oxide, 5-9wt% of calcium oxide, 8-15wt% of silicon dioxide and 3-10wt% of manganese oxide, and the binding force between the tungsten-copper electronic paste and an aluminum oxide substrate can be effectively improved. Aluminum oxide powder selected by the binding phase is subjected to long-time ball milling, so that the powder is fully ground and crushed, a large number of dislocations are filled in the powder, the superfine powder with the high specific surface area is fully mixed with other binding phase components, electronic paste with excellent performance can be obtained, the tungsten-copper electronic paste is printed on an aluminum oxide green tape through a screen printing machine, and the tungsten-copper electronic paste is obtained. After sintering at 1350 DEG C, the excellent bonding strength of the film layer and the aluminum oxide substrate can be maintained, and when an adhesive force test is carried out by adopting GB / T 9286-1998, the test result can stably maintain the ASTM grade to be 5B.

Description

Technical Field

[0001] The invention relates to the technical field of electronic paste preparation, and in particular to a binder phase for tungsten-copper electronic paste and a preparation method thereof. Background Art

[0002] Electronic paste is generally composed of three parts: conductive phase, adhesive phase and organic carrier. The adhesive phase can not only adjust the sintering shrinkage behavior of electronic paste, but also improve the interface bonding between the film layer and the substrate. The adhesive phase is usually composed of various metal oxides. Although it can improve the adhesion between the electronic paste and the ceramic substrate, it also seriously affects the conductive properties of the paste film layer. How to ensure the good adhesion of the electronic paste film layer while ensuring that the paste still maintains excellent conductive properties is an urgent problem to be solved.

[0003] In order to solve this problem, the present invention provides a high-performance adhesive phase of tungsten-copper electronic paste suitable for medium- and high-temperature co-fired ceramic substrates. The preparation method is simple, the raw materials are easily available, and it does not contain toxic heavy metal components such as lead and cadmium, and is pollution-free. While maintaining low square resistance performance, it also achieves the performance of firm adhesion and not easy to peel off. Summary of the invention

[0004] The purpose of the present invention is to provide a binder phase for tungsten copper electronic paste and a preparation method thereof, wherein the binder phase can effectively improve the bonding force between the tungsten copper electronic paste and the alumina substrate while also maintaining excellent conductive properties.

[0005] In order to achieve the above-mentioned purpose, the technical solution adopted by the present invention is:

[0006] A bonding phase for tungsten-copper electronic paste consists of 60-75wt% aluminum oxide, 3-10wt% magnesium oxide, 5-9wt% calcium oxide, 8-15wt% silicon dioxide and 3-10wt% manganese oxide.

[0007] The aluminum oxide is prepared by ball milling a powder raw material with a particle size of 1.78 to 3.36 μm for 25 to 40 hours to obtain a flaky structure.

[0008] The present invention also proposes a tungsten copper electronic paste, which is composed of a conductive phase, a bonding phase and an organic carrier, and the three account for 75-85wt%, 1-8wt% and 10-20wt% in the tungsten copper electronic paste. Among them, the conductive phase is a tungsten copper mixed powder, and the organic carrier is composed of 75wt% organic solvent, 20wt% thickener and 5wt% auxiliary agent.

[0009] Compared with the prior art, the beneficial effects of the present invention are mainly manifested in:

[0010] 1. The bonding phase does not have a complicated preparation process, can reduce process costs, will not affect the square resistance value of the tungsten copper slurry, and is easy to promote.

[0011] 2. The ingredients used in the bonding phase are all substances that are widely present in nature, safe and pollution-free to the environment, and meet the social development requirements of developing new environmentally friendly, high-performance, and low-cost slurries.

[0012] 3. The alumina powder used in the bonding phase is fully ground and crushed through long-term ball milling, and the powder is filled with a large number of dislocations. This ultra-fine powder with a high specific surface area is fully mixed with other bonding phase components to obtain an electronic paste with excellent performance. The tungsten-copper electronic paste is printed on an alumina green porcelain tape using a screen printer. After sintering at 1350°C, the film layer can maintain excellent bonding strength with the alumina substrate. When GB / T 9286-1998 is used for adhesion testing, the test results can stably maintain ASTM grade 5B. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 The metallographic image of the tungsten copper electronic paste prepared in Example 3 of the present invention after sintering and measured by the Baige method is shown. DETAILED DESCRIPTION

[0014] The present invention is further described in detail below in conjunction with embodiments and drawings.

[0015] Example 1

[0016] The tungsten copper electronic paste prepared in this embodiment has a mass ratio of conductive phase, adhesive phase and organic carrier of 80:7:13. The preparation process is as follows:

[0017] Step 1: Prepare the bonding phase:

[0018] The binder phase components are 73wt%Al 2 O 3 , 7wt%MgO, 6wt%CaO, 10wt%SiO 2 、4wt%MnO 2 The proportions are determined, wherein alumina is prepared by ball milling for 25 hours using a powder raw material with a particle size of 1.78 to 3.36 μm to obtain a flaky structure (completely crushed).

[0019] Step 2: Mixing the conductive phase with the adhesive phase:

[0020] According to the preset ratio, the tungsten copper mixed powder and the components of the bonding phase are mixed into a material tank, and mixed for 15 hours using a three-dimensional powder mixer to obtain a premixed powder.

[0021] Step 3: Slurry grinding:

[0022] An organic carrier is added to the mixed conductive phase and the adhesive phase for preliminary grinding, wherein the organic carrier is composed of 75wt% organic solvent, 20wt% thickener and 5wt% auxiliary agent. The slurry after preliminary grinding is subjected to multi-step grinding using a three-roll grinder to obtain a tungsten copper electronic slurry.

[0023] Step 4: Slurry sintering:

[0024] The tungsten-copper electronic paste prepared in step 3 is printed onto an alumina green tape using a screen printer, and the temperature is raised to 1350° C. in a hydrogen-nitrogen mixed gas atmosphere for sintering (2 h) to finally obtain the product.

[0025] Example 2

[0026] The tungsten copper electronic paste prepared in this embodiment has a mass ratio of conductive phase, adhesive phase and organic carrier of 80:7:13. The preparation process is as follows:

[0027] Step 1: Prepare the bonding phase:

[0028] The binder phase components are 73wt%Al 2 O 3 , 5wt%MgO, 6wt%CaO, 10wt%SiO 2 、6wt%MnO 2 The proportions are determined, wherein alumina is prepared by ball milling for 25 hours using a powder raw material with a particle size of 1.78 to 3.36 μm to obtain a flaky structure (completely crushed).

[0029] Step 2: Mixing the conductive phase with the adhesive phase:

[0030] According to the preset ratio, the tungsten copper mixed powder and the components of the bonding phase are mixed into a material tank, and mixed for 15 hours using a three-dimensional powder mixer to obtain a premixed powder.

[0031] Step 3: Slurry grinding:

[0032] An organic carrier is added to the mixed conductive phase and the adhesive phase for preliminary grinding, wherein the organic carrier is composed of 75wt% organic solvent, 20wt% thickener and 5wt% auxiliary agent. The slurry after preliminary grinding is subjected to multi-step grinding using a three-roll grinder to obtain a tungsten copper electronic slurry.

[0033] Step 4: Slurry sintering:

[0034] The tungsten-copper electronic paste prepared in step 3 is printed onto an alumina green tape using a screen printer, and the temperature is raised to 1350° C. in a hydrogen-nitrogen mixed gas atmosphere for sintering (2 h) to finally obtain the product.

[0035] Example 3

[0036] The tungsten copper electronic paste prepared in this embodiment has a mass ratio of conductive phase, adhesive phase and organic carrier of 80:7:13. The preparation process is as follows:

[0037] Step 1: Prepare the bonding phase:

[0038] The binder phase components are 73wt%Al 2 O 3 , 5wt%MgO, 8wt%CaO, 10wt%SiO 2 、4wt%MnO 2 The proportions are determined, wherein alumina is prepared by ball milling for 25 hours using a powder raw material with a particle size of 1.78 to 3.36 μm to obtain a flaky structure (completely crushed).

[0039] Step 2: Mixing the conductive phase with the adhesive phase:

[0040] According to the preset ratio, the tungsten copper mixed powder and the components of the bonding phase are mixed into a material tank, and mixed for 15 hours using a three-dimensional powder mixer to obtain a premixed powder.

[0041] Step 3: Slurry grinding:

[0042] An organic carrier is added to the mixed conductive phase and the adhesive phase for preliminary grinding, wherein the organic carrier is composed of 75wt% organic solvent, 20wt% thickener and 5wt% auxiliary agent. The slurry after preliminary grinding is subjected to multi-step grinding using a three-roll grinder to obtain a tungsten copper electronic slurry.

[0043] Step 4: Slurry sintering:

[0044] The tungsten-copper electronic paste prepared in step 3 is printed onto an alumina green tape using a screen printer, and the temperature is raised to 1350° C. in a hydrogen-nitrogen mixed gas atmosphere for sintering (2 h) to finally obtain the product.

[0045] Example 4

[0046] The tungsten copper electronic paste prepared in this embodiment has a mass ratio of conductive phase, adhesive phase and organic carrier of 80:7:13. The preparation process is as follows:

[0047] Step 1: Prepare the bonding phase:

[0048] The binder phase components were 70wt% Al 2 O 3 , 10wt%MgO, 5wt%CaO, 10wt%SiO 2 、5wt%MnO 2 The proportions are determined, wherein alumina is prepared by ball milling for 25 hours using a powder raw material with a particle size of 1.78 to 3.36 μm to obtain a flaky structure (completely crushed).

[0049] Step 2: Mixing the conductive phase with the adhesive phase:

[0050] According to the preset ratio, the tungsten copper mixed powder and the components of the bonding phase are mixed into a material tank, and mixed for 15 hours using a three-dimensional powder mixer to obtain a premixed powder.

[0051] Step 3: Slurry grinding:

[0052] An organic carrier is added to the mixed conductive phase and the adhesive phase for preliminary grinding, wherein the organic carrier is composed of 75wt% organic solvent, 20wt% thickener and 5wt% auxiliary agent. The slurry after preliminary grinding is subjected to multi-step grinding using a three-roll grinder to obtain a tungsten copper electronic slurry.

[0053] Step 4: Slurry sintering:

[0054] The tungsten-copper electronic paste prepared in step 3 is printed onto an alumina green tape using a screen printer, and the temperature is raised to 1350° C. in a hydrogen-nitrogen mixed gas atmosphere for sintering (2 h) to finally obtain the product.

[0055] Example 5

[0056] The tungsten copper electronic paste prepared in this embodiment has a mass ratio of conductive phase, adhesive phase and organic carrier of 80:7:13. The preparation process is as follows:

[0057] Step 1: Prepare the bonding phase:

[0058] The binder phase components were 70wt% Al 2 O 3 , 10wt%MgO, 8wt%CaO, 8wt%SiO 2 、4wt%MnO 2 The proportions are determined, wherein alumina is prepared by ball milling for 25 hours using a powder raw material with a particle size of 1.78 to 3.36 μm to obtain a flaky structure (completely crushed).

[0059] Step 2: Mixing the conductive phase with the adhesive phase:

[0060] According to the preset ratio, the tungsten copper mixed powder and the components of the bonding phase are mixed into a material tank, and mixed for 15 hours using a three-dimensional powder mixer to obtain a premixed powder.

[0061] Step 3: Slurry grinding:

[0062] An organic carrier is added to the mixed conductive phase and the adhesive phase for preliminary grinding, wherein the organic carrier is composed of 75wt% organic solvent, 20wt% thickener and 5wt% auxiliary agent. The slurry after preliminary grinding is subjected to multi-step grinding using a three-roll grinder to obtain a tungsten copper electronic slurry.

[0063] Step 4: Slurry sintering:

[0064] The tungsten-copper electronic paste prepared in step 3 is printed onto an alumina green tape using a screen printer, and the temperature is raised to 1350° C. in a hydrogen-nitrogen mixed gas atmosphere for sintering (2 h) to finally obtain the product.

[0065] Performance table of products obtained from Examples 1 to 5

[0066]

[0067] Combination Figure 1 As can be seen from Table 1, the adhesive phase proposed by the present invention can effectively improve the bonding strength between the tungsten copper electronic paste and the alumina substrate, while also maintaining excellent conductivity. After sintering at 1350°C, the film layer can maintain excellent bonding strength with the alumina substrate. When the adhesion test is performed using GB / T 9286-1998, the test results can stably maintain ASTM grade 5B.

[0068] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A binder phase for tungsten copper electronic paste, characterized in that: The invention is composed of 60-75wt% of aluminum oxide, 3-10wt% of magnesium oxide, 5-9wt% of calcium oxide, 8-15wt% of silicon dioxide and 3-10wt% of manganese oxide.

2. The adhesive phase according to claim 1, characterized in that The aluminum oxide is prepared by ball milling a powder raw material with a particle size of 1.78 to 3.36 μm for 25 to 40 hours to obtain a flaky structure.

3. A tungsten copper electronic paste containing the binder phase as claimed in claim 1, characterized in that: The binder phase accounts for 1-8 wt % in the tungsten copper electronic paste.

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