CN102898027A - Ceramic powder for electronic component packaging material and production method for ceramic powder - Google Patents

Ceramic powder for electronic component packaging material and production method for ceramic powder Download PDF

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CN102898027A
CN102898027A CN2012103967188A CN201210396718A CN102898027A CN 102898027 A CN102898027 A CN 102898027A CN 2012103967188 A CN2012103967188 A CN 2012103967188A CN 201210396718 A CN201210396718 A CN 201210396718A CN 102898027 A CN102898027 A CN 102898027A
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CN102898027B (en
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李波
张树人
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University of Electronic Science and Technology of China
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Abstract

The invention belongs to ceramic powder for producing an electronic component packaging material and a production method for the ceramic powder. The ceramic powder comprises 35 to 85 weight percent of composite oxides containing part of BaO, B2O3, SiO2, Al2O3, MgO, CaO, SrO, ZnO, ZrO2, and TiO2, and 15 to 65 weight percent of quartz powder and colorant; and the production method comprises the following steps of preparing the composite oxides, preparing the raw materials of the ceramic powder, performing ball-milling, mixing and drying. According to the method, the composite oxides, quartz or composite oxides, quartz, and colorant are adopted, the composite oxides are sintered, and the sintered composite oxides and the quartz powder are mixed so as to obtain the ceramic powder for the packaging material, so that the method has the characteristics of simple process, high efficiency, low energy consumption and production cost and the like, and can be used for industrial large-scale production. The ceramic powder which is prepared by the method can be sintered at the temperature of between 800 and 1,000 DEG C by the conventional method to form the electronic component packaging material and a base plate for a chip, wherein the thermal expansion coefficient of the electronic component packaging material and the base plate is 10<-20> to 10<-6>/DEG C, and the electronic component packaging material and the base plate are high and reliable in comprehensive performance.

Description

Electronic devices and components used for packing material ceramics powder and production method thereof
Technical field
The invention belongs in the electron ceramic material technical field production method for the production of ceramics powder and this ceramics powder of electronic devices and components packaged material; Particularly a kind ofly can be used for producing thermal expansivity (TCE) for 10-20 * 10 -6/ ℃ ceramics powder and the production method of electronic package material.This ceramics powder not only can be produced the packaged material for electronic devices and components such as integrated circuit (IC) chip, particularly ball grid array (BGA), also can be used for making chip substrate.
Background technology
Along with the continuous frivolous miniaturization of electronics, multifunction, high-performance and low-cost, the unicircuit of its core (IC) improves constantly at aspects such as chip size, integrated scale, packaging density, signal frequencies, and this key link of microelectronic packaging technology is had higher requirement.The develop rapidly of large-scale integrated circuit (LSI) impels the Chip Packaging form of array to occur and becomes gradually main flow, and its typical case is such as ball grid array (BGA), grid array (LGA).Packaged material provides the effects such as electrical connection, protection, support, heat radiation, assembling as being the important composition of encapsulation technology for chip.Ceramic packaging material wherein satisfies the single-chip package of high frequency, numeral, radio frequency and microwave device or the technical requirements of multi-chip assembling with its good electricity, machinery, calorifics and operational characteristic, is widely applied in each class of electronic devices.
There is the high 1500-1900 of sintering temperature ℃ in traditional alumina ceramic material, and Mo, W metal line resistance are large, shortcoming, especially thermal expansivity (TCE) 6-8 * 10 such as specific inductivity is bigger than normal -6/ ℃ with the 11-18 of printed circuit board (pcb) * 10 -6/ ℃ existence is not seriously mated, and in use easy fracture lost efficacy, thereby there are the disadvantages such as reliability in chip bga.In recent years, the LTCC that develops rapidly (LTCC) has low-k, and can burn altogether with low resistivity metal Au, Ag, Cu etc. about 900 ℃, has solved the problems such as high-frequency high-speed, wiring miniaturization.But still there is the general lower drawback of thermal expansivity in existing low-temperature co-burning ceramic material product, such as the A6 of Ferro company type TCE ≈ 7.0 * 10- 6/ ℃, the 951 type TCE ≈ 5.8 * 10 of DuPont company -6/ ℃, the CT700 of Heraeus company type TCE ≈ 6.7 * 10 -6/ ℃.
The general lower drawback of thermal expansivity that exists for overcoming LTCC (LTCC), the patent No. be CN03130760.4, denomination of invention for disclosing a kind of magnesia borosilicate glass of alkali metal containing in the patent document of " high thermal expansion glass and band composition ", this magnesia borosilicate glass comprises 10-25% SiO 2, 10-25% B 2O 3, 5-10% BaO, 40-65% MgO, 0.5-3% ZrO 2, 0.3-3% P 2O 5With 0.2-5% M 2O, wherein M is selected from basic metal Li, Na and K and composition thereof (in molar percentage); Ceramic packing is Al 2O 3, ZrO 2, TiO 2, BaTiO 3And composition thereof; Tinting material is selected from Cu 2O, Fe 2O 3And composition thereof; But the curtain coating dielectric combination comprises that 50-90% glass, 10-50% ceramic packing and 0.2-3% tinting material (by weight percentage) are dispersed in the solution of organic polymer binder and volatile organic solvent composition.Above-mentioned glass is prepared by traditional glass technique, the elder generation weigh batching, be mixed in proportion, in smelting furnace, be heated to 1400-1600 ℃, in platinum crucible, form melt and become uniform liquid fully, then the glass melt quenching is rolled into sheet glass, obtains the glass powder of 1-5 μ m through grinding again.The TCE of this glass>9 * 10 -6/ ℃ (25-300 ℃).Above-mentioned curtain coating band composition can be used to make the multilayer circuit of BGA purposes; Similarly patent also has the US 6835682 of the U.S..Although this type of magnesia borosilicate glass has higher thermal expansivity (TCE), exist and adopt expensive Li in the component 2O has not only improved cost and Li belongs to rare material, and the electricity that the existence of alkalimetal oxide makes microelectronic device use the monovalent base metal ion can produce electromigration, increase encapsulation medium under life-time service, especially hot environment is led, and reduces the reliability of product; And adopt traditional glass technique under 1400-1600 ℃ of temperature, to reach 5 hours melting, not only energy consumption is high and also high to the requirement of capabilities of refractory materials, the loss of volatile substances in the composition in melting process also is difficult to control, adopt in addition the glass melt quenching to be rolled into sheet glass, the hardness of glass is high, the grinding difficulty is large.Thereby, there is glass melting temperature and high to performance requriements height, the energy consumption of melting equipment in above-mentioned magnesia borosilicate glass, complex manufacturing, production cost is high, and the poor stability of resulting product performance, its thermal expansivity (TCE) 11-18 of difficult and printed circuit board (pcb) * 10 still -6/ ℃ coupling, and be not suitable for the disadvantages such as industrialized mass.
Be that CN101421199B, denomination of invention comprise 30-55% SiO for disclosing a kind of its component in the patent document of " high thermal expansion cyclosilicate glass-ceramics " at notification number 2, 5-40% CaO, 0-50% BaO, 0.1-10% Al 2O 3With 0-40% SrO(CaO+BaO+SrO=35-65%),〉0-15% MgO and at least a among the 0-10% ZnO, the silicate glass-pottery of at least a transition metal of 0-10% or the oxide compound (by weight percentage) of rare earth metal.This glass-ceramic also is to adopt the preparation of traditional glass technique, adopts platinum crucible to found 2-5 hour under 1450-1650 ℃ of temperature, and its principal crystalline phase has the cyclosilicate structure, TCE=8.5-11.5 * 10 -6/ ℃, this high thermal expansion cyclosilicate glass-ceramics only is used as the sealing agent of metal to metal, metal pair pottery and ceramic-on-ceramic, and the high-performance coating of metal and pottery, and should not be as encapsulation and the baseplate material of electronic devices and components; And this silicate glass-pottery adopts traditional glass technique, glass melting temperature up to 1450-1650 ℃, and with the higher original ore powder of foreign matter content and rare-earth oxide as a part of raw material, thereby have still that energy consumption is high, production cost is high, product properties is poor, and is not suitable for the disadvantages such as industrialized mass.
Summary of the invention
The objective of the invention is the disadvantage for the background technology existence, study a kind of electronic devices and components used for packing material ceramics powder and production method thereof, on the basis of simplifying production technique, reduce sintering temperature, energy consumption and production cost, improve the performance of ceramics powder and the homogeneity of morphology microstructure; Production technique is simple, efficient is high to reach, and energy consumption and production cost are low, can carry out industrialized mass, and is that the Electronic Packaging of subsequent production high comprehensive performance and substrate are 10-20 * 10 with thermal expansivity (TCE) -6/ ℃ the purposes such as ceramics powder raw material.
Solution of the present invention is the defective that exists for background technology, adopts to contain BaO, B 2O 3, SiO 2, Al 2O 3Or BaO, B 2O 3, SiO 2, Al 2O 3And MgO, CaO, SrO, ZnO, ZrO 2, TiO 2Composite oxides are made in middle part or all in proportion wet-milling mixing of composition, sintering, grinding, and then with these composite oxides and silica powder in proportion wet-milling mixes, dry and sieve processing, namely get used for packing material ceramics powder (white); When need production band look ceramics powder, being as the criterion with the gross weight of combined oxidation raw material adds the composite oxides of making again respective color behind the tinting material through wet-milling mixing, sintering, grinding in proportion again, or with composite oxides and the gross weight of silica powder be as the criterion add in proportion tinting material after, again through wet-milling mix, dry and sieve and process the ceramics powder of directly making respective color; The present invention adopts the composite oxides composition of deciding, and can make the ceramics powder that makes not only can reduce its sintering temperature in substrate and promote the quartz crystal growth, but also can improve its bending strength at subsequent production electronic package material and chip; In main composition, add silica powder and both can improve the thermal expansivity of material, the problem that is complementary to solve chip bga and pcb board thermal expansivity, also can induce the glassy phase crystallization to be conducive to sinter into porcelain by quartz, in addition, the consumption of regulating silica powder adjustable material high thermal expansion coefficient also, enlarge its scope of application; The present invention namely realizes its goal of the invention with this.Therefore, in this sub-components and parts used for packing material ceramics powder that generates electricity: comprise weight percent be 35-85wt% contain BaO, B 2O 3, SiO 2, Al 2O 3At interior composite oxides and the silica powder of 15-65wt%; Composite oxides take weight percent: BaO as 15-65wt%, B 2O 3Be 5-25wt%, SiO 2Be 20-65wt%, Al 2O 3Be 1-15wt%.
Also contain in the above-mentioned composite oxides be no more than join (system) composite oxides total amount 25wt% comprise MgO, CaO, SrO, ZnO, ZrO 2, TiO 2At interior whole or wherein a kind of, several oxide compound.And described MgO, CaO, SrO, ZnO, ZrO 2, TiO 2In the composite oxides total amount of content after to add of each composition: MgO as 0.5-20wt%, CaO as 0.5-20wt%, SrO as 0.3-18wt%, ZnO as 0.3-18wt%, ZrO 2Be 0.2-16wt%, TiO 2Be 0.2-16wt%, no matter add a kind of, several or whole oxide compounds wherein, its add-on all is no more than the 25wt% of this composite oxides total amount.In order to satisfy packaged material to the requirement of color, in ceramics powder, also be added with the tinting material of its total amount 0.1-2wt%, tinting material is Cr 2O 3, Co 2O 3, Fe 2O 3And Cu 2One or more metal oxides among the O.
The production method of described electronic devices and components used for packing material ceramics powder comprises:
The preparation of step 1. composite oxides:
1a. the preparation of combined oxidation raw material: with BaO, B 2O 3, SiO 2, Al 2O 3Wet-milling mixes or with BaO, B in proportion 2O 3, SiO 2, Al 2O 3And be no more than composite oxides total amount 25wt% comprise MgO, CaO, SrO, ZnO, ZrO 2, TiO 2In a kind of, several or all oxide compounds in proportion wet-milling mixings 2-10 hour be that 1-10 μ m ends to mean particle size, drying, the removal of impurities of sieving get the composite oxides raw material powder;
1b. preparation composite oxide powder: with step 1a gained composite oxides raw material powder place in the sintering oven, under 500-800 ℃ of temperature sintering 1-4 hour, cooling namely gets composite oxide powder by grinding, sieving, and is stand-by;
Step 2. preparation ceramics powder raw material, ball milling mix and drying treatment: the silica powder of technical pure, mean particle size 15-150 μ m and step 1 gained composite oxide powder are placed in proportion wet-milling mixings was that 1-5 μ m ends to mean particle size in 3-12 hour in the ball mill, under 60-110 ℃ of temperature, be dried to water ratio≤1.0% afterwards, sieving namely gets electronic devices and components used for packing material ceramics powder.
It is the zirconium ball that described ball milling mixes its abrading-ball, and ball milling agent is ethanol, deionized water or both mixtures.When need production band look ceramics powder, be as the criterion with the gross weight of combined oxidation raw material at step 1a, add the Cr of its weight 0.2-6wt% 2O 3, Co 2O 3, Fe 2O 3And Cu 2Among the O one or more as tinting material after, again through wet-milling mixing, sintering, grind and sieve and process the composite oxides make respective color, or when step 2 preparation ceramics powder raw material, add the Cr of its gross weight 0.1-2wt% 2O 3, Co 2O 3, Fe 2O 3And Cu 2Among the O one or more as tinting material after, again through wet-milling mixing, sintering, grind and sieve and process the ceramics powder directly make respective color.
The present invention adopts composite oxides+quartz or composite oxides+quartz+tinting material in prescription, and adopt the composite oxides compound carried out sintering processes after, again with the processing methodes such as silica powder mixes, make electronic devices and components packaged material production ceramics powder; In ceramics powder not with the alkalimetal ion of monovalence, stopped the electromigration that after this easily produces as the electronic devices and components packaged material again.Thereby the present invention has that technique is simple, efficient is high, and energy consumption and production cost are low, can carry out the characteristics such as industrialized mass; The ceramics powder that adopts the present invention to make adopts ordinary method, sintering can be produced thermal expansivity (TCE) and is 10-20 * 10 under 800-1000 ℃ of temperature -6/ ℃, high comprehensive performance, reliable electronic devices and components packaged material and chip substrate.
Description of drawings
The electronic devices and components encapsulation that Fig. 1 makes for the employing example 1 gained ceramics powder electron micrograph of stupalith section;
The electronic devices and components encapsulation that Fig. 2 makes for the employing example 2 gained ceramics powders electron micrograph of stupalith section;
The electronic devices and components encapsulation that Fig. 3 makes for the employing example 3 gained ceramics powders electron micrograph of stupalith section;
The electronic devices and components encapsulation that Fig. 4 makes for the employing example 4 gained ceramics powders electron micrograph of stupalith section;
The electronic devices and components encapsulation that Fig. 5 makes for the employing example 5 gained ceramics powders electron micrograph of stupalith section;
Fig. 6 uses the thermal expansion curve of stupalith for the real electronic devices and components encapsulation of adopting routine 1-5 gained ceramics powder to make.
Embodiment
Embodiment 1: weighing 60kg BaO, 9kg B 2O 3, 23kg SiO 2, 3kg Al 2O 3, 5kg TiO 2, place in the lump in the ball mill, take ethanol as ball milling agent, the zirconium ball is abrading-ball, through 3 hours ball millings, oven dry under 70 ℃ of temperature, sieving obtained the powder of mean particle size 4.3 μ m; At sintering under 750 ℃ of temperature and after being incubated 1.5 hours, be composite oxides through the powder after grinding, sieving again; Then weighing 45kg composite oxides, 55kg quartzy (125 μ m) still place the interior wet-milling of ball mill after 11 hours, dry to water ratio≤0.5% under 70 ℃ of temperature, and the white powder that obtains mean particle size 3.0 μ m that sieves is the electronic package material ceramics powder.
Adopt above-mentioned ceramics powder after 20MPa compression moulding, sintering and to be incubated 1 hour, namely to obtain thermal expansivity be 18.3 * 10 under air and 970 ℃ of temperature -6The encapsulation of the electronic devices and components of/℃ (25-400 ℃) stupalith, the specific inductivity 6.2(1MHz of this stupalith), dielectric loss 3 * 10 -4(1MHz), insulation resistivity 4.0 * 10 13Ω cm, bending strength 153MPa; Accompanying drawing 1 is the electromicroscopic photograph of this stupalith structure, and the curve S 1 in the accompanying drawing 6 is its thermal expansion graphic representation.
Embodiment 2: weighing 52kg BaO, 10kg B 2O 3, 30kg SiO 2, 5kg Al 2O 3, 3kg ZrO 2With 1kg Co 2O 3Place in the lump in the ball mill, take deionized water as ball milling agent, the zirconium ball is abrading-ball, through 5 hours ball millings, under 100 ℃ of temperature, dry, sieve and obtain the powder of mean particle size 3.5 μ m, then sintering and be incubated 2 hours under 750 ℃ of temperature is composite oxides through the powder after grinding, sieving again; Then these composite oxides of weighing 57kg, 43kg quartzy (105 μ m), still place in the ball mill wet-milling after 9 hours, dry to water ratio≤1% under 100 ℃ of temperature, the blue powder of the averaging of income granularity of sieving 2.5 μ m is the electronic package material ceramics powder.
Adopt above-mentioned ceramics powder after 20MPa compression moulding, at reducing atmosphere N 2+ H 2In and sintering and be incubated 1.5 hours and obtain thermal expansivity 14.2 * 10 under 950 ℃ of temperature -6The encapsulation of the electronic devices and components of/℃ (25-400 ℃) stupalith, the specific inductivity 6.5(1MHz of this stupalith), dielectric loss 4 * 10 -4(1MHz), insulation resistivity 3.9 * 10 13Ω cm, bending strength 171MPa; Accompanying drawing 2 is the electromicroscopic photograph of this stupalith structure, and the curve S 2 in the accompanying drawing 6 is its thermal expansion graphic representation.
Embodiment 3: weighing 16kg BaO, 5kg B 2O 3, 52kg SiO 2, 5kg Al 2O 3, 15kg MgO, 7kg ZrO 2Place in the lump in the ball mill, take ethanol and deionized water by the mixed solution of 7:3 as ball milling agent, zirconium ball as abrading-ball, through 7 hours ball millings, under 80 ℃ of temperature, dry, sieving obtains the powder of mean particle size 2.8 μ m; Then sintering and be incubated 2.5 hours under 750 ℃ of temperature, again through grinding, sieving, i.e. composite oxide powder; Then quartzy (74 μ m) and 0.5kg Cr of weighing 73kg composite oxides, 27kg 2O 3Take ethanol and deionized water by the 7:3 mixed solution as ball milling agent, take the zirconium ball as abrading-ball, through 7 hours ball millings, under 80 ℃ of temperature, dry to water ratio≤1%, the green powder that obtains mean particle size 2.1 μ m of sieving is the electronic package material ceramics powder.
Adopt above-mentioned ceramics powder after 20MPa compression moulding, at reducing atmosphere N 2+ H 2Sintering and be incubated 2 hours and obtain thermal expansivity 11.0 * 10 among the O and under 930 ℃ of temperature -6The encapsulation of the electronic devices and components of/℃ (25-400 ℃) stupalith, its specific inductivity 5.9(1MHz), dielectric loss 4 * 10 -4(1MHz), insulation resistivity 3.6 * 10 13Ω cm, bending strength 155MPa; Accompanying drawing 3 is the electromicroscopic photograph of this stupalith structure, and the curve S 3 in the accompanying drawing 6 is its thermal expansion graphic representation.
Embodiment 4: weighing 22kg BaO, 8kg B 2O 3, 44kg SiO 2, 7kg Al 2O 3, 9kg CaO, 10kg ZrO 2And 1kgCo 2O 3Place in the lump in the ball mill, take ethanol and deionized water by the mixed solution of 5:5 as ball milling agent, zirconium ball as abrading-ball, through 8 hours ball millings, 85 ℃ of oven dry, sieve and obtain the powder of mean particle size 2.4 μ m, sintering and be incubated 3 hours under 600 ℃ of temperature is composite oxides through the powder after grinding, sieving again; Then quartzy (53 μ m) and 0.5kg Cu of weighing 70kg composite oxides, 30kg 2O, take ethanol and deionized water by the 5:5 mixed solution as ball milling agent, zirconium ball as abrading-ball, through 5 hours ball millings, under 85 ℃ of temperature, dry to water ratio≤1%, sieving obtains the black powder of mean particle size 1.7 μ m, and this black powder is the electronic package material ceramics powder.
Adopt the gained ceramics powder after 20MPa compression moulding, at reducing atmosphere N 2+ H 2+ H 2Among the O and under 900 ℃ of temperature sintering and be incubated 2.5 hours thermal expansivity 11.5 * 10 -6The encapsulation of the electronic devices and components of/℃ (25-400 ℃) stupalith, its specific inductivity 6.2(1MHz), dielectric loss 5 * 10 -4(1MHz), insulation resistivity 4.0 * 10 13Ω cm, bending strength 166MPa; Accompanying drawing 4 is the electromicroscopic photograph of this stupalith structure, and the curve S 4 in the accompanying drawing 6 is its thermal expansion graphic representation.
Embodiment 5: weighing 27kg BaO, 12kg B 2O 3, 39kg SiO 2, 10kg Al 2O 3, 5kg SrO, 1kg ZnO, 6kgZrO 2Place in the lump in the ball mill, take ethanol and deionized water by the mixed solution of 3:7 as ball milling agent, zirconium ball as abrading-ball, through 9 hours ball millings, under 90 ℃ of temperature, dry, sieve and obtain the powder of mean particle size 2.1 μ m, at sintering under 550 ℃ of temperature and after being incubated 3.5 hours, be composite oxides through the powder after grinding, sieving again; Then quartzy (37 μ m), 0.5kg Fe of weighing 64kg composite oxides, 36kg 2O 3Batch mixing evenly after, take ethanol and deionized water by the 3:7 mixed solution as ball milling agent, zirconium ball as abrading-ball, through 5 hours ball millings, dry to water ratio≤1% under 90 ℃ of temperature, the red powder that obtains mean particle size 1.5 μ m that sieves is the electronic package material ceramics powder.
This powder body material is after 20MPa compression moulding, in nitrogen N 2In and sintering and be incubated 4 hours and obtain thermal expansivity 12.7 * 10 under 850 ℃ of temperature -6The encapsulation of the electronic devices and components of/℃ (25-400 ℃) stupalith, this ceramic dielectric constant 5.7(1MHz), dielectric loss 5 * 10 -4(1MHz), insulation resistivity 3.4 * 10 13Ω cm, bending strength 151MPa; Accompanying drawing 5 is the electromicroscopic photograph of this stupalith structure, and the curve S 5 in the accompanying drawing 6 is its thermal expansion graphic representation.

Claims (7)

1. electronic devices and components used for packing material ceramics powder, it is characterized in that comprising in the ceramics powder weight percent be 35-85wt% contain BaO, B 2O 3, SiO 2, Al 2O 3At interior composite oxides and the silica powder of 15-65wt%; Composite oxides take weight percent: BaO as 15-65wt%, B 2O 3Be 5-25wt%, SiO 2Be 20-65wt%, Al 2O 3Be 1-15wt%.
2. by the described electronic devices and components used for packing material of claim 1 ceramics powder, it is characterized in that also can containing in the described composite oxides add be no more than join composite oxides total amount 25wt% comprise MgO, CaO, SrO, ZnO, ZrO 2, TiO 2At interior whole or wherein a kind of, several oxide compound.
3. by the described electronic devices and components used for packing material of claim 2 ceramics powder, it is characterized in that described MgO, CaO, SrO, ZnO, ZrO 2, TiO 2In the composite oxides total amount of content after to add of each composition: MgO as 0.5-20wt%, CaO as 0.5-20wt%, SrO as 0.3-18wt%, ZnO as 0.3-18wt%, ZrO 2Be 0.2-16wt%, TiO 2Be 0.2-16wt%, no matter add a kind of, several or whole oxide compounds wherein, its add-on all is no more than the 25wt% of this composite oxides total amount.
4. by the described electronic devices and components used for packing material of claim 1 ceramics powder, it is characterized in that also containing the tinting material that total amount is ceramics powder 0.1-2wt% in ceramics powder, tinting material is Cr 2O 3, Co 2O 3, Fe 2O 3And Cu 2One or more metal oxides among the O.
5. by the production method of the described electronic devices and components used for packing material of claim 1 ceramics powder, comprising:
The preparation of step 1. composite oxides:
1a. the preparation of combined oxidation raw material: with BaO, B 2O 3, SiO 2, Al 2O 3Wet-milling mixes or with BaO, B in proportion 2O 3, SiO 2, Al 2O 3And be no more than composite oxides total amount 25wt% comprise MgO, CaO, SrO, ZnO, ZrO 2, TiO 2In a kind of, several or all oxide compounds in proportion wet-milling mixings 2-10 hour be that 1-10 μ m ends to mean particle size, drying, the removal of impurities of sieving get the composite oxides raw material powder;
1b. preparation composite oxide powder: with step 1a gained composite oxides raw material powder place in the sintering oven, under 500-800 ℃ of temperature sintering 1-4 hour, cooling namely gets composite oxide powder by grinding, sieving, and is stand-by;
Step 2. preparation ceramics powder raw material, ball milling mix and drying treatment: the silica powder of technical pure, mean particle size 15-150 μ m and step 1 gained composite oxide powder are placed in proportion wet-milling mixings was that 1-5 μ m ends to mean particle size in 3-12 hour in the ball mill, under 60-110 ℃ of temperature, be dried to water ratio≤1.0% afterwards, sieving namely gets electronic devices and components used for packing material ceramics powder.
6. by the production method of the described ceramics powder of claim 5, it is characterized in that it is the zirconium ball that described ball milling mixes its abrading-ball, ball milling agent is ethanol, deionized water or both mixtures.
7. by the production method of the described ceramics powder of claim 5, it is characterized in that the gross weight with the combined oxidation raw material in step 1a is as the criterion, and adds the Cr of its weight 0.2-6wt% when producing band look ceramics powder 2O 3, Co 2O 3, Fe 2O 3And Cu 2Among the O one or more as tinting material after, again through wet-milling mixing, sintering, grind and sieve and process the composite oxides make respective color; Or when step 2 preparation ceramics powder raw material, add the Cr of its gross weight 0.1-2wt% 2O 3, Co 2O 3, Fe 2O 3And Cu 2Among the O one or more as tinting material after, again through wet-milling mixing, sintering, grind and sieve and process the ceramics powder directly make respective color.
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CN106045323A (en) * 2016-05-27 2016-10-26 电子科技大学 High thermal expansion coefficient ceramic material and preparation method thereof
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CN108424132A (en) * 2018-05-24 2018-08-21 电子科技大学 A kind of high fever expansion high strength ceramic packaging material and preparation method thereof
CN110190210A (en) * 2019-03-12 2019-08-30 华电电力科学研究院有限公司 A kind of solid oxide fuel cell structure convenient for edge sealing-in
CN114171479A (en) * 2022-02-14 2022-03-11 潮州三环(集团)股份有限公司 Ceramic packaging base and preparation method and application thereof

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CN108424132A (en) * 2018-05-24 2018-08-21 电子科技大学 A kind of high fever expansion high strength ceramic packaging material and preparation method thereof
CN108424132B (en) * 2018-05-24 2021-04-30 电子科技大学 High-thermal-expansion high-strength ceramic packaging material and preparation method thereof
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CN114171479A (en) * 2022-02-14 2022-03-11 潮州三环(集团)股份有限公司 Ceramic packaging base and preparation method and application thereof
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