Glass powder for electronic ceramic package and method for preparing the same

Abstract

The application discloses a kind of electronic ceramic packaging glass powder and preparation method thereof.The glass powder comprises the following components by weight percentage: bismuth oxide 20-40%, boron oxide 2-10%, diaphosphorus pentoxide 20-30%, zinc oxide 5-10%, aluminum oxide 1-8%, diavanadyl 20-30%, cobalt trioxide 1-10%, and the balance is titanium dioxide.The glass powder prepared by the application has the advantages of high bonding force, low softening temperature, high hardness, low thermal expansion coefficient, uniform particle size distribution, and no cracks at the packaging interface.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of glass powder, and particularly relates to a glass powder for electronic ceramic packaging and a preparation method thereof. BACKGROUND

[0002] With the progress of science and technology, electronic components are increasingly developing towards miniaturization and light weight. The development of electronic components cannot be separated from the role of electronic glass powder. Electronic glass powder has many applications in electronic products. Its most widely used application is for sealing of electronic products. From the sealing function, many other functions such as heat insulation, protection and bonding are derived.

[0003] Silver paste is an indispensable thing in the miniaturization development direction of electronic devices, and it plays a positive role in the miniaturization development direction. The silver paste is composed of a metal phase, a carrier adhesive phase and a glass phase. The metal phase is the core of the conductive core, the carrier adhesive phase is the manufacturer of the conductive metal line forming, and the glass phase is the core of the conductive line fixation and close adhesion.

[0004] Silver paste is composed of silver powder, glass powder, organic carrier and additives. The glass powder plays an important role in the performance of silver paste tension, conversion efficiency, aging tension, etc. In the existing PERC process, the glass powder destroys the passivation layer, causing efficiency reduction, and the glass powder affects the tension, aging tension and other factors affecting the reliability of the module. SUMMARY

[0005] In view of the above-mentioned deficiencies in the prior art, the application provides a glass powder for electronic ceramic packaging and a preparation method thereof, which can effectively solve the problems of poor air tightness, mismatched thermal expansion coefficient, cracks at the packaging interface, poor adhesion and the like of the existing glass powder in electronic ceramic packaging.

[0006] To achieve the above-mentioned purposes, the technical scheme adopted by the application to solve its technical problems is:

[0007] A glass powder for electronic ceramic packaging, comprising the following components by weight percentage:

[0008] 20%-40% of bismuth oxide, 2%-10% of boron oxide, 20%-30% of diaphosphorus pentoxide, 5%-10% of zinc oxide, 1%-8% of aluminum oxide, 20%-30% of divanadium pentoxide, 1-10% of cobalt trioxide, and the balance of titanium dioxide.

[0009] Further, the following components by weight percentage are included:

[0010] Bi2O3 25-35%, B2O3 2-8%, P2O5 20-25%, ZnO 5-10%, Al2O3 1-5%, V2O5 20-25%, Co3O4 1-5%, and the balance TiO2.

[0011] Further, the following components are included in the following weight percentages:

[0012] Bi2O3 30%, B2O3 3%, P2O5 20%, ZnO 5%, Al2O3 1%, V2O5 20%, Co3O4 1%, and the balance TiO2.

[0013] A method for preparing the above-mentioned glass powder for electronic ceramic packaging, comprising the following steps:

[0014] S1, pretreatment

[0015] Analytically pure Bi2O3, B2O3, P2O5, ZnO, Al2O3, V2O5, Co3O4, and TiO2 are selected;

[0016] S2, smelting modification

[0017] The above-mentioned raw materials are subjected to high-temperature smelting and solid-phase sintering reaction, so that the raw materials form a glass body;

[0018] S3, washing

[0019] The glass body is washed and cooled;

[0020] S4, drying

[0021] The washed glass body is dried, and the drying method is blow-drying;

[0022] S5, coarse grinding

[0023] The dried glass body is placed in a ball mill for ball milling;

[0024] S6, fine grinding

[0025] The coarsely ground material is finely ground;

[0026] S7, classification

[0027] The finely ground material is classified by a classifier, and the powder with a D50 of less than 5 μm is collected to obtain the final product.

[0028] Further, the particle size of the raw material selected in step S1 is 0.5-2 μm.

[0029] Further, the smelting temperature in step S2 is 1100-1400°C.

[0030] Furthermore, in step S5, the ball milling time is 3-5 hours and the rotation speed is 300-500 r / min.

[0031] The glass powders used in the preparation of electronic ceramic packaging can be applied in electronic ceramic packaging, including ZnO ceramics, AlN ceramics, alumina ceramics, NTC ceramics, PTC ceramics, and silicon wafers.

[0032] The beneficial effects of this invention are:

[0033] This invention employs a solid-state reaction, which involves sintering solid raw materials together to achieve high-temperature modification and enhance the performance of the glass. This results in a glass powder with better properties after melting. The glass powder prepared by this invention has the advantages of good airtightness, good transparency, low softening temperature, high hardness, low coefficient of thermal expansion, uniform particle size distribution, and no cracks at the encapsulation interface.

[0034] At high concentrations, V₂O₅ acts as a network former. Vanadium atoms tend to bridge with oxygen atoms produced during depolymerization, rather than with non-phosphorus atoms, thus forming their own network. The number of POP bonds in the phosphate chain decreases, while the number of POV bonds increases. Vanadium ions in V₂O₅ can depolymerize long phosphate chains, leading to wider channels, which is beneficial for Ag in silver paste. + Ion movement. The weak phosphate network connection and depolymerization structure can lower the glass transition temperature (Tg). The lower the Tg, the better the wetting, the smaller the wetting angle, and the better the adhesion between the ions, resulting in a denser bond.

[0035] Network-forming compounds B₂O₃, P₂O₅, and SiO₂ decrease the coefficient of thermal expansion. Intermediates ZnO, Co₂O₃, and Al₂O₃ provide sufficient free oxygen, similarly reducing the coefficient of thermal expansion. The network-forming compounds decrease the coefficient of thermal expansion, and the intermediates, under conditions of sufficient free oxygen, also contribute to this decrease. Furthermore, Al₂O₃ plays a special role in phosphate glass; aluminum can form aluminum-oxygen tetrahedra with double-bonded oxygen atoms in the phosphate glass, improving and strengthening the phosphate glass structure, thus enhancing a range of its properties. Intermediates ZnO and Al₂O₃ have high melting points (ZnO 1975℃, Al₂O₃ 2054℃) and are not easily decomposed, producing very little or no free oxygen. Co₂O₃ transforms into CoO during melting; during this transformation, Co₂O₃ generates a sufficiently large amount of free oxygen within the glass. Detailed Implementation

[0036] The specific embodiments of the present application are described below to enable those skilled in the art to understand the present application, but it should be clear that the present application is not limited to the scope of the specific embodiments, and for those skilled in the art, it is obvious that various changes are within the spirit and scope of the present application defined and determined by the appended claims, and all the inventions using the concept of the present application are within the scope of protection.

[0037] Embodiment 1

[0038] A glass powder for electronic ceramic packaging is prepared, comprising the following components by weight percentage:

[0039] 30% bismuth oxide, 3% boron oxide, 20% phosphorus pentoxide, 5% zinc oxide, 1% aluminum oxide, 20% vanadium pentoxide, 1% cobalt sesquioxide, and the balance is titanium dioxide.

[0040] The method for preparing the above-mentioned glass powder for electronic ceramic packaging comprises the following steps:

[0041] S1, pretreatment

[0042] Selecting analytical pure bismuth oxide, boron oxide, phosphorus pentoxide, zinc oxide, aluminum oxide, vanadium pentoxide, cobalt sesquioxide, and titanium dioxide;

[0043] S2, smelting modification

[0044] The above raw materials are subjected to high-temperature smelting and solid-phase sintering reaction to form a glass body;

[0045] S3, washing

[0046] The glass body is washed and cooled;

[0047] S4, drying

[0048] The washed glass body is dried by blowing type drying;

[0049] S5, rough grinding

[0050] The dried glass body is put into a ball mill for ball milling;

[0051] S6, fine grinding

[0052] The rough ground material is fine ground;

[0053] S7, classification

[0054] The fine ground material is classified by a classifier, and the powder with D50 below 5 μm is collected to obtain the final product.

[0055] Embodiment 2

[0056] An electronic ceramic packaging glass powder, comprising the following components by weight percentage:

[0057] Bismuth oxide 25%, boron oxide 5%, phosphorus pentoxide 25%, zinc oxide 5%, aluminum oxide 5%, vanadium pentoxide 25%, cobalt sesquioxide 5%, and the balance being titanium dioxide.

[0058] A method for preparing the above electronic ceramic packaging glass powder, comprising the following steps:

[0059] S1, pretreatment

[0060] Selecting analytical pure bismuth oxide, boron oxide, phosphorus pentoxide, zinc oxide, aluminum oxide, vanadium pentoxide, cobalt sesquioxide, and titanium dioxide;

[0061] S2, smelting modification

[0062] The above raw materials are subjected to high-temperature smelting and solid-phase sintering reaction to form a glass body;

[0063] S3, washing

[0064] The glass body is washed and cooled;

[0065] S4, drying

[0066] The washed glass body is dried by blowing drying;

[0067] S5, rough grinding

[0068] The dried glass body is put into a ball mill for ball milling;

[0069] S6, fine grinding

[0070] The rough ground material is fine ground;

[0071] S7, classification

[0072] The fine ground material is classified by a classifier, and the powder with D50 below 5 μm is collected to obtain the final product.

[0073] Example 3

[0074] An electronic ceramic packaging glass powder, comprising the following components by weight percentage:

[0075] Bismuth oxide 35%, boron oxide 5%, phosphorus pentoxide 20%, zinc oxide 5%, aluminum oxide 5%, vanadium pentoxide 20%, cobalt sesquioxide 5%, and the balance being titanium dioxide.

[0076] A method for preparing the above electronic ceramic packaging glass powder, comprising the following steps:

[0077] S1, pretreatment

[0078] Analyzed pure bismuth oxide, boron oxide, diaphosphorus pentoxide, zinc oxide, aluminum oxide, diavanadyl oxide, cobaltous oxide, titanium dioxide are selected;

[0079] S2, smelting modification

[0080] The above raw materials are subjected to high-temperature smelting and solid-phase sintering reaction to form a glass body;

[0081] S3, washing

[0082] The glass body is washed and cooled;

[0083] S4, drying

[0084] The washed glass body is dried by blowing drying;

[0085] S5, rough grinding

[0086] The dried glass body is put into a ball mill for ball milling;

[0087] S6, fine grinding

[0088] The rough ground material is fine ground;

[0089] S7, classification

[0090] The fine ground material is classified by a classifier, and the powder with D50 below 5 μm is collected to obtain the final product.

[0091] Example 4

[0092] Compared with Example 1, tellurium oxide is used to replace boron oxide, and the rest of the process is the same as Example 1.

[0093] Example 5

[0094] Compared with Example 1, zirconium oxide is used to replace vanadium oxide, and the rest of the process is the same as Example 1.

[0095] Example 6

[0096] Compared with Example 1, titanium oxide is used to replace diaphosphorus pentoxide, and zirconium oxide is used to replace boron oxide, and the rest of the process is the same as Example 1.

[0097] Experimental example

[0098] 1. The thermal expansion coefficient of the glass powder prepared in Examples 1-6 is detected by a thermal expansion coefficient detector (PCY-G-1200), and the test temperature is 20-120℃, and the specific results are shown in Table 1.

[0099] Table 1 thermal expansion coefficient of glass powder

[0100]

[0101] From the data in Table 1, it can be seen that the thermal expansion coefficient of the powder processed by the technical scheme of the application is significantly reduced.

[0102] 2, the powder prepared in Example 1 and Examples 4-6 were respectively mixed with silver powder with an average particle size of 2 μm to prepare silver paste, and the silver paste was printed on the front and back surfaces of a silicon wafer in a predetermined pattern by screen printing, dried, and then rapidly sintered at 400-600°C, and then cooled to room temperature, and then the conductivity, adhesion, and conversion efficiency of the product were detected, and the results are shown in Table 2.

[0103] Table 2 performance detection of different glass powders

[0104] Example 1 Example 4 Example 5 Example 6 Conductivity (mΩ / D) 5 8 7 9 Bonding force (N / mm 2 )]]> 18 13 11 7 Conversion efficiency (Fff) 23.22 21.04 20.16 20.01

[0105] According to the detection results in Table 2, it can be seen that the glass powder prepared by the technical scheme of the application has excellent conductivity, tight adhesion, and high conversion efficiency. As for Examples 4-6, compared with Example 1, the commonly used zirconium oxide, tellurium oxide, titanium oxide, etc. are used to replace one or more components in the scheme, and after the replacement, the conductivity, adhesion, or conversion efficiency of the formed scheme is significantly reduced. This shows that the components in the scheme of the application are not randomly selected, and each component does not simply play its own role, but only when each component is combined together, can the glass powder with good conductivity, strong adhesion, and high conversion efficiency be prepared.

[0106] Finally, it should be pointed out that the above specific embodiments are only used to illustrate the technical scheme of the application and not to limit it, and although the application has been described in detail with reference to the examples, those skilled in the art should understand that the technical scheme of the application can be modified or replaced by equivalents without departing from the spirit and scope of the technical scheme of the application, and all of them should be covered in the scope of the claims of the application.

Claims

1. A glass powder for electronic ceramic packaging, characterized in that, It consists of the following components by weight percentage: Bismuth oxide 20%-40%, boron oxide 2%-10%, phosphorus pentoxide 20%-30%, zinc oxide 5%-10%, aluminum oxide 1%-8%, vanadium pentoxide 20%-30%, cobalt trioxide 1-10%, with the balance being titanium dioxide.

2. The glass powder for electronic ceramic packaging according to claim 1, characterized in that, It consists of the following components by weight percentage: Bismuth oxide 25%-35%, boron oxide 2%-8%, phosphorus pentoxide 20%-25%, zinc oxide 5%-10%, aluminum oxide 1%-5%, vanadium pentoxide 20%-25%, cobalt trioxide 1-5%, with the balance being titanium dioxide.

3. The glass powder for electronic ceramic packaging according to claim 1 or 2, characterized in that, It consists of the following components by weight percentage: Bismuth oxide 30%, boron oxide 3%, phosphorus pentoxide 20%, zinc oxide 5%, aluminum oxide 1%, vanadium pentoxide 20%, cobalt trioxide 1%, and the balance is titanium dioxide.

4. A method for preparing the glass powder for electronic ceramic packaging according to any one of claims 1 to 3, characterized in that, Includes the following steps: S1, Preprocessing Analytical grade bismuth oxide, boron oxide, phosphorus pentoxide, zinc oxide, aluminum oxide, vanadium pentoxide, cobalt trioxide, and titanium dioxide were selected. S2, Smelting Modification The above raw materials are smelted at high temperature and subjected to solid-state sintering reaction to form a glassy substance. S3, Washing The vitreous body is washed and cooled; S4, Drying The washed glass body is dried by air drying. S5, Coarse Grinding The dried glass body is placed in a ball mill for ball milling; S6, Fine Grinding The coarsely ground material is then finely ground; S7, Classification The finely ground material is classified by a classifier, and powder with D50 below 5μm is collected to obtain the final product.

5. The preparation method according to claim 4, characterized in that, The raw material particle size selected in step S1 is 0.5-2μm.

6. The preparation method according to claim 4, characterized in that, The melting temperature in step S2 is 1200-1400℃.

7. The preparation method according to claim 4, characterized in that, In step S5, the ball milling time is 3-5 hours and the rotation speed is 300-500 r / min.

8. The application of the glass powder for electronic ceramic packaging according to any one of claims 1 to 3 in the preparation of electronic ceramic packaging products.

9. The application according to claim 8, characterized in that, The electronic ceramic packaging products include ZnO ceramics, AlN ceramics, alumina ceramics, NTC ceramics, PTC ceramics, and silicon wafers.

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