CN-121553985-B - Hollow spherical electronic packaging material and preparation method thereof

Abstract

The invention discloses a hollow spherical electronic packaging material and a preparation method thereof, and relates to the field of electronic packaging material preparation, wherein the preparation method of the hollow spherical Cu 2 V 2 O 7 material comprises the steps of preparing a copper ion solution A and a vanadium ion solution B by taking deionized water as a solvent, and mixing the solution A and the solution B to obtain a precursor solution; adding a precursor solution into an atomization generating device, atomizing the precursor solution into liquid drops, introducing inert gas into an air inlet pipe of the atomization generating device, delivering the liquid drops into a preheated tubular furnace for calcination, wherein the calcination temperature is 630-700 ℃, the calcination time is 4-10 h, and collecting hollow spherical Cu 2 V 2 O 7 products in a quartz tube. The invention solves the technical problems of complex preparation flow, insufficient mechanical property, high cost and poor environmental protection of the inorganic filler in the existing electronic packaging technology and lower structural reliability caused by mismatch of thermal expansion coefficients of packaging materials and epoxy resin after compounding.

Inventors

• HU LEI
• LV YIPING
• QIN FEIYU
• BAI XIAOYA

Assignees

• 西安交通大学

Dates

Publication Date

20260508

Application Date

20260123

Claims (4)

1. 1. The preparation method of the hollow spherical Cu 2 V 2 O 7 material is characterized by comprising the following steps of: step 1, preparing a copper ion solution A by taking deionized water as a solvent, wherein the solution concentration of the copper ion solution A is 0.15-0.20 mol/L; Step 2, preparing a vanadium ion solution B by taking deionized water as a solvent, wherein the solution concentration of the vanadium ion solution B is 0.15-0.20 mol/L; Step 3, mixing the solution A prepared in the step 1 and the solution B prepared in the step 2, wherein the ratio of the solution A to the solution B is 1:1 according to the mole ratio to obtain a suspension, regulating the pH of the suspension to 2-3 by adopting a nitric acid solution until the solution is clear to obtain a precursor solution, and the mole ratio of a solute HNO 3 in the nitric acid solution to vanadium ions in the solution B is 1:2; Step 4, adding the precursor solution obtained in the step 3 into an atomization generating device, and atomizing the precursor solution into liquid drops, wherein the total mist making rate of the atomization generating device is 1800-2400 mL/h, and the ultrasonic frequency of each mist making device is 1.75 MHz; And 5, introducing inert gas into an air inlet pipe of the atomization generating device, wherein the flow rate of the inert gas is 6L/min, delivering the liquid drops in the step 4 into a preheated tubular furnace for calcination, wherein the calcination temperature is 630-700 ℃, the calcination time is 4-10 h, and collecting hollow spherical Cu 2 V 2 O 7 products in a quartz tube.
2. 2. The method for preparing a hollow spherical Cu 2 V 2 O 7 material according to claim 1, wherein in the step 1, the copper ion solution a is prepared from Cu (NO 3 )·3H 2 O、Cu(CH 3 COO) 2 ·H 2 O or CuSO 4 ·5H 2 O), and in the step 2, the vanadium ion solution B is prepared from NH 4 VO 3 .
3. 3. A hollow sphere-shaped Cu 2 V 2 O 7 material obtained by the preparation method according to any one of claims 1 to 2.
4. 4. The hollow sphere-shaped Cu 2 V 2 O 7 material as claimed in claim 3, wherein the hollow sphere-shaped Cu 2 V 2 O 7 material has a particle size of 0.73 0.21 μm。

Description

Hollow spherical electronic packaging material and preparation method thereof Technical Field The invention relates to the field of electronic packaging material preparation, in particular to a hollow spherical electronic packaging material and a preparation method thereof. Background As microelectronic packaging technology advances toward higher density, miniaturization, and higher reliability, flip-chip packaging has become one of the dominant technologies. In this structure, the underfill plays a key role in effectively relieving stress concentrations due to Coefficient of Thermal Expansion (CTE) mismatch by filling the gap between the die and the substrate, improving solder joint reliability and device lifetime. The currently widely used underfill mainly uses epoxy resin as a matrix, however, the epoxy resin has a higher thermal expansion coefficient (generally greater than 60×10 -6/°c), which easily causes interface delamination of the package structure in thermal cycle, and causes problems such as signal transmission loss and device leakage. To reduce the thermal expansion coefficient, a large amount of silica (SiO 2) filler (the filling amount is often higher than 60% wt%) is usually required, but the high silica filling amount can lead to a sharp increase in the viscosity of the composite material, a decrease in the flow filling performance, a decrease in fracture toughness, and weakening of interface bonding, which adversely affects the overall reliability of the package. In recent years, negative thermal expansion materials provide a new way for precise thermal expansion regulation. Cu 2V2O7, as a typical negative thermal expansion compound, exhibits a pronounced volume shrinkage behavior in a specific temperature region and is ideally well suited for use in tuning the thermal expansion properties of epoxy resins. In order to further realize the multi-element optimization of the negative thermal expansion performance of Cu 2V2O7, an attempt is made to modify the material by ion doping, for example, zn 2+ is introduced to partially replace Cu 2+, so that the negative thermal expansion coefficient can be regulated and controlled, and the compatibility of the material with a polymer matrix is expected to be improved. In addition, the filler morphology has a particularly significant impact on the composite properties. Compared with the existing Cu 2V2O7 filler which is in an irregular shape or solid particle form, the hollow spherical structure has the potential advantages in the aspects of enhancing the interaction between the filler and the matrix, promoting the stress dispersion and improving the thermal and mechanical properties due to the high specific surface area, the low density and the adjustable pore structure. Meanwhile, zn 2+ doping is combined with the hollow sphere structure, so that the multielement optimization of the negative thermal expansion performance of Cu 2V2O7 can be realized in a coordinated manner theoretically. By changing the Zn 2+ content, the negative thermal expansion coefficient and stronger interface binding force are regulated and controlled. The negative thermal expansion coefficient is milder and helps to be compatible with the matrix. Meanwhile, the filler with different NTE coefficients can realize more accurate thermal expansion compensation. Although hollow sphere Cu 2V2O7 has the advantages of synergistically achieving low thermal expansion, light weight and good mechanical properties in theory, no published report on its controllable preparation and application in polymer-based composites is currently seen. In summary, the underfill materials in the existing microelectronic packaging technology have the following problems: 1. The problems of inorganic filler synthesis cost and environmental protection are that in the existing epoxy resin molding compound (EMC) for electronic packaging, the main stream inorganic filler is amorphous silicon dioxide, and the synthesis of the amorphous silicon dioxide requires a high temperature of more than 2500 ℃, which directly leads to high equipment cost, large energy consumption and remarkable carbon emission. While other common fillers (such as AlN, graphene, BN and the like) have excellent performance, the raw material cost is high or the processing technology is complex, so that the economic burden of industrial application is further increased. 2. Structural reliability problems caused by thermal expansion mismatch are that epoxy has a Coefficient of Thermal Expansion (CTE) as high as hundreds of 10 -6/°c, while silicon chips (2.5 x 10 -6/°c), copper microbumps (17 x 10 -6/°c), organic substrates (24 x 10 -6/°c) have significant CTE differences. While the existing filler (such as silicon dioxide CTE-0.5X10 -6/° C) can reduce the CTE of the composite material, the CTE is difficult to accurately match the thermal expansion requirements of various components, so that mechanical deformation such as lamination, cracking, warp