CN101148323B - Low-temperature co-fired cordierite series glass-ceramic substance power and preparation method thereof - Google Patents

Low-temperature co-fired cordierite series glass-ceramic substance power and preparation method thereof Download PDF

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CN101148323B
CN101148323B CN2007101214671A CN200710121467A CN101148323B CN 101148323 B CN101148323 B CN 101148323B CN 2007101214671 A CN2007101214671 A CN 2007101214671A CN 200710121467 A CN200710121467 A CN 200710121467A CN 101148323 B CN101148323 B CN 101148323B
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纪箴
张昭瑞
王燕斌
肖治纲
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University of Science and Technology Beijing USTB
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Abstract

The present invention discloses low temperature co-baked MgO-Al2O3-SiO2 glass-ceramic wafer powder and its preparation process. The co-baked MgO-Al2O3-SiO2 glass-ceramic wafer powder is prepared basedon the recipe of cordierite 2MgO.2Al2O3.5SiO2 and through adding baking assistant B2O3 and Bi2O3, and modifiers TiO2, CuO, CaO and/or K2O to improve the crystal chemistry performance. It is preparedthrough a sol-gel synthesis process with roasting temperature of 700-750 deg.c and sintering temperature of 850-900 deg.c. The low temperature co-baked MgO-Al2O3-SiO2 glass-ceramic wafer powder has low sintering temperature, low dielectric constant, low dielectric loss, high insulation resistance, simple preparation process and other advantages. It is applied in making low temperature co-baked wafer.

Description

A kind of low temperature co-fired cordierite series glass-ceramic substance power and preparation method thereof
Technical field
The invention belongs to electronic ceramics substrate and manufacturing field thereof, particularly a kind of low temperature co-fired glass-ceramic substance material and preparation method thereof.
Background technology
Electric substrate is the carrier of semiconductor die package, carries the support of electronic devices and components, constitutes the basal disc of electronic circuit.The tradition inorganic substrate is with Al 2O 3, SiC, BeO and AlN etc. be base material, it has good characteristic at aspects such as thermal conductivity, bending strength, thermal expansivity, but because its sintering temperature is at 1500～1900 ℃, if adopt the method for burning altogether simultaneously, conductor material can only be selected refractory metal W or Mo etc., make cost improve greatly, and new outlet has been opened up in the appearance of LTCC (LTCC) material for this reason.
The common burning temperature of LTCC system is generally between 800～900 ℃.Thereby can replace refractory metals such as W, Mo to do the wiring conductor with the lower metal of fusing points such as Cu, Ag, both can reduce cost, improve specific conductivity, can in atmosphere, burn till again.Adopt LTCC to be convenient to make large size, large vol substrate.Its cost is low, passive elements such as implantable resistance, electric capacity, inductance, particularly the thermal expansivity of glass-ceramic and silicon is complementary, specific inductivity is low, has tangible low loss performance at high frequency band, be particularly suitable for radio frequency, microwave, millimetric wave device, be widely used in wireless communication, military affairs and field such as civilian.
With the trichroite is the MgO-Al of principal crystalline phase 2O 3-SiO 2Microcrystalline glass in series, its thermotolerance height, good (ρ＞10 of electrical insulating property 12Ω cm), high-frequency loss is little, at high frequency (＞specific inductivity very low (ε=5.0～5.5) under 1GHz), and good thermal characteristics (thermalexpansioncoefficient=(1～2) * 10 -6℃ -1), and be close with the performance of silicon, therefore the prospect as substrate and electronic package material is very considerable.
But preparation and performance that present trichroite is the LTCC material can't be satisfactory, have some problems.Research (University Of Science and Technology Of Shandong's journal of document Mg-Al-Si microcrystalline glass in series, September 25 (3) in 2006,78-80), human solid sintering technologies such as Han Ye have made the Mg-Al-Si microcrystalline glass in series, though bending strength is enough big, but sintering temperature height, sintering time are long, and microstructure is fine and close inadequately; The low-temperature sintering of document used for high-frequency chip inductor cordierite ceramic material and performance (Rare Metals Materials and engineering, February 34 (2) in 2005,33-36), it is the LTCC material that human sol-gel methodes such as Wang Shaohong prepare trichroite, though reduced sintering temperature to a certain extent, but sintering temperature is still between 900～1000 ℃, to using silver electrode unfavorable; Document MgO-Al 2O 3-SiO 2-TiO 2-CeO 2The crystallization process of system glass ceramics and microwave dielectric property (Journal of Inorganic Materials, May 18 (3) in 2003,547-552), the king has just waited the people that the crystallization process and the microwave dielectric property of trichroite microcrystalline glass in series are studied, though dielectric loss is less, but specific inductivity is very high, between 8～11.
Summary of the invention
The objective of the invention is to, a kind of ultra-fine high-performance MgO-Al that can be applicable to prepare ltcc substrate is provided 2O 3-SiO 2The series glass-ceramic substance powder.It is at trichroite (2MgO2Al 2O 35SiO 2) on the basis of prescription, from the angle of crystal chemistry, by in this system, adding sintering agent B 2O 3, Bi 2O 3With properties-correcting agent TiO 2, CuO, CaO, K 2Among the O three kinds or all improve its performance, satisfy the requirement of ltcc substrate material technology.
Another object of the present invention provides above-mentioned MgO-Al 2O 3-SiO 2The process for preparing sol-gel of series low-temperature co-burning substrate powder.Adopt the sol-gel method synthesis technique to prepare precursor, then its roasting is gone out powder, be pressed into circular base substrate again, sintering 2～3h under relatively low temperature (850～900 ℃), can obtain relative permittivity lower (4.6～5.4,1MHz), low (tan δ＜0.17% of dielectric loss, 1MHz), the big (ρ of insulation resistance v〉=4.88 * 10 13Ω cm), density is the high-quality baseplate material of big (ρ 〉=2.82), and preparation technology is simple.
MgO-Al 2O 3-SiO 2The series glass-ceramic substance powder is according to trichroite 2MgO2Al 2O 35SiO 2The packing component design, wherein weighting material comprises sintering agent B 2O 3, Bi 2O 3, and properties-correcting agent TiO 2, CuO, CaO, K 2Among the O three kinds or all, trichroite accounts for 80～90% of total mass in the prescription, and weighting material accounts for 10～20% of total mass in the prescription.Each oxide compound accounts for the per-cent of total mass and is in this powder: 18%～35%Al 2O 3, 40%～50%SiO 2, 8%～15%MgO, 3%～10%B 2O 3, 1%～5%Bi 2O 3, 0.1～10%TiO 2, 0.1～6%CuO, 0.1～4%CaO, 0～3%K 2O.Raw materials used is Al (NO 3) 39H 2O, Mg (NO 3) 2, Si (C 2H 5O) 4, H 3BO 3, Bi (NO 3) 35H 2O, Ti (OC 4H 9) 4, Cu (NO 3) 23H 2O, Ca (NO 3) 24H 2O and KNO 3
Realize above-mentioned MgO-Al 2O 3-SiO 2Be the ltcc substrate preparation methods, carry out according to the following steps:
1) will be 18%～35% Al with mass percent 2O 3With the corresponding Al (NO of 8%～15% MgO quality 3) 39H 2O and Mg (NO 3) 2Being dissolved in the dehydrated alcohol, being stirred to transparent clarification, will be 40%～50% SiO then with mass percent 2With 0.1～10% TiO 2Corresponding Si (the C of quality 2H 5O) 4And Ti (OC 4H 9) 4Join in this solution, stir, form clear soln A;
2) will be 3%～10% B with mass percent 2O 3, 1%～5% Bi 2O 3The corresponding H of quality 3BO 3, Bi (NO 3) 35H 2O and with mass percent be 0.1～6% CuO, 0.1～4% CaO, 0～3% K 2The corresponding KNO of O quality 3, Cu (NO 3) 23H 2O, Ca (NO 3) 24H 2Among the O two kinds or all join in the mixed solution of dehydrated alcohol and deionized water, stir, regulate the pH value between 9～10 with ammoniacal liquor, obtain liquid B;
3) solution A and B are mixed, stir, obtain colloidal sol;
4) colloidal sol is put into 40～60 ℃ baking oven and left standstill to sol-gel takes place and transform, obtain clear gel;
5) gel is placed 80～120 ℃ of oven dry fully;
6) xerogel is ground to form fine powder, place retort furnace, be warming up to 700～750 ℃ of roasting 2～3h then, take out cooling, grind to form powder in 200～250 ℃ of binder removal 1～3h;
7) powder of weighing certain mass, static pressure becomes the circle base under 20～30MPa condition, and sintering 2～3h becomes porcelain under 850～900 ℃ of conditions, can obtain MgO-Al 2O 3-SiO 2It is the ltcc substrate material;
8) be coated with silver electrode on the two sides of base substrate, burn electrode 10～30min at 800～875 ℃.
MgO-Al of the present invention 2O 3-SiO 2Be that ltcc substrate powder and preparation method thereof has following characteristics:
1, adopts Prepared by Sol Gel Method MgO-Al 2O 3-SiO 2Be the ltcc substrate powder, and added sintering agent B 2O 3, Bi 2O 3, and properties-correcting agent TiO 2, CuO, CaO, K 2Among the O three kinds or all.TiO 2When high temperature with Ti 4+Participate in the silica network, and temperature is when reducing, TiO 2From the silica network, separate, and form nucleus based on this, promote the glass micritization.And CuO can " induce crystallization " in heat treatment process, promotes the crystalline growth, can form more crystal at identical sintering temperature sample.CaO, K 2O belongs to the glass structure network modifying oxide, can improve the devitrified glass performance.
Prepare the ltcc substrate powder with sol-gel method, its precursor obtains by chemical reaction in solution, its particle size is minimum, Chemical Composition is evenly accurate, activity is very big, can roasting go out ultra-fine, highly active ltcc substrate powder in lesser temps (700～750 ℃) and short time.
2, with sol-gel method preparation, and, can under 850～900 ℃ of low temperature, sinter fine and close ltcc substrate into, can use silver electrode, reduced cost, and preparation technology be simple at ultra-fine, the high reactivity powder of 700～750 ℃ of roastings.
3, with the ltcc substrate of sol-gel method preparation, density is big (ρ 〉=2.82), the low (ε of specific inductivity r=4.6～5.4,1MHz), dielectric loss little (tan δ＜0.17%, 1MHz), sintering temperature low (850～900 ℃), the big (ρ of insulation resistance v〉=4.88 * 10 13Ω cm), satisfied the technical requirements of ltcc substrate material.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1:
The trichroite proportion is 80% of a total mass in the sample, and it is as shown in table 1 below specifically to form mass percent.According to the corresponding chemical feedstocks of prescription weighing, with Al (NO 3) 39H 2O and Mg (NO 3) 3Be dissolved in the dehydrated alcohol, be stirred to transparent clarification, then with Si (C 2H 5O) 4, Ti (C 4H 9O) 4Join in this solution, be stirred to even clarification, obtain liquid A.With stopping composition H 3BO 3, Bi (NO 3) 35H 2O, Ca (NO 3) 24H 2O, Cu (NO 3) 23H 2O joins in the mixed solution of dehydrated alcohol and deionized water, stirs, and regulates its pH value 9.23 with ammoniacal liquor, obtains liquid B.Liquid A is mixed with B, stir, obtain colloidal sol.The baking oven of colloidal sol being put into 40 ℃ leaves standstill, and makes its that sol-gel take place and transforms, and obtains gel.Place 80 ℃ of environment to dry fully gel, after taking-up grinds to form fine powder, place retort furnace, be warming up to 750 ℃ of roasting 2h, take out cooling, grind, obtain the LTCC powder in 250 ℃ of binder removal 3h.It is the round base of 10mm that the powder of weighing certain mass static pressure under the 25MPa condition becomes diameter, and sintering 2h becomes porcelain under 850 ℃ of conditions, can obtain MgO-Al 2O 3-SiO 2It is the ltcc substrate material.Two sides at base substrate is coated with silver electrode, burns electrode 20min at 800 ℃.
Each sample of table 1 is formed mass percent
Oxide compound Al 2O 3 SiO 2 MgO B 2O 3 Bi 2O 3 TiO 2 CuO CaO
Mass percent 31.89 41.08 11.03 6 4 0.2 5.2 0.6
Corresponding raw material Al(NO 3) 3 ·9H 2O Si(C 2H 5O) 4 Mg(NO 3) 3 H 3B 2O 3 Bi(NO 3) 3 ·5H 2O Ti(C 4H 9O) 4 Cu(NO 3) 2 ·3H 2O Ca(NO 3) 2 ·4H 2O
The performance of this glass ceramic material reaches following index behind 850 ℃ of following sintering:
Density p=2.84gcm -3, DIELECTRIC CONSTANT r=4.6 (1MHz), dielectric loss tan δ=1.7 * 10 -3(1MHz), insulation resistance ρ v=4.88 * 10 13Ω cm.
Embodiment 2:
The trichroite proportion is 85% of a total mass in the sample, and it is as shown in table 2 below specifically to form mass percent.According to the corresponding chemical feedstocks of prescription weighing, with Al (NO 3) 39H 2O and Mg (NO 3) 3Be dissolved in the dehydrated alcohol, be stirred to transparent clarification, then with Si (C 2H 5O) 4, Ti (C 4H 9O) 4Join in this solution, be stirred to even clarification, obtain liquid A.With stopping composition H 3BO 3, Bi (NO 3) 35H 2O, Ca (NO 3) 24H 2O, Cu (NO 3) 23H 2O joins in the mixed solution of dehydrated alcohol and deionized water, stirs, and regulates its pH value 9.45 with ammoniacal liquor, obtains liquid B.Liquid A is mixed with B, stir, obtain colloidal sol.The baking oven of colloidal sol being put into 50 ℃ leaves standstill, and makes its that sol-gel take place and transforms, and obtains gel.Place 100 ℃ of environment to dry fully gel, after taking-up grinds to form fine powder, place retort furnace, be warming up to 750 ℃ of roasting 2h, take out cooling, grind, obtain the LTCC powder in 250 ℃ of binder removal 1h.It is the round base of 10mm that the powder of weighing certain mass static pressure under the 25MPa condition becomes diameter, and sintering 2h becomes porcelain under 850 ℃ of conditions, can obtain MgO-Al 2O 3-SiO 2It is the ltcc substrate material.Two sides at base substrate is coated with silver electrode, burns electrode 15min at 850 ℃.
Each sample of table 2 is formed mass percent
Oxide compound Al 2O 3 SiO 2 MgO B 2O 3 Bi 2O 3 TiO 2 CuO CaO
Mass percent 29.63 43.65 11.72 4.5 3 0.15 3.9 0.45
Corresponding raw material Al(NO 3) 3 ·9H 2O Si(C 2H 5O) 4 Mg(NO 3) 3 H 3B 2O 3 Bi(NO 3) 3 ·5H 2O Ti(C 4H 9O) 4 Cu(NO 3) 2 ·3H 2O Ca(NO 3) 2 ·4H 2O
This glass ceramic material performance behind 850 ℃ of following sintering reaches following index:
Density p=2.82gcm -3, DIELECTRIC CONSTANT r=4.8 (1MHz), dielectric loss tan δ=1.3 * 10 -3(1MHz), insulation resistance ρ v=1.20 * 10 15Ω cm.
Embodiment 3:
The trichroite proportion is 90% of a total mass in the sample, and it is as shown in table 3 below specifically to form mass percent.According to the corresponding chemical feedstocks of prescription weighing, with Al (NO 3) 39H 2O and Mg (NO 3) 3Be dissolved in the dehydrated alcohol, be stirred to transparent clarification, then with Ti (OC 4H 9) 4And Si (C 2H 5O) 4Join in this solution, stir, form clear soln A.With weighting material H 3BO 3, Bi (NO 3) 35H 2O, Ca (NO 3) 24H 2O, KNO 3, Cu (NO 3) 23H 2O joins in the mixed solution of dehydrated alcohol and deionized water, stirs, and regulates its pH value 9.43 with ammoniacal liquor, obtains liquid B.Solution A is mixed with B, stir, obtain colloidal sol.The baking oven of colloidal sol being put into 60 ℃ leaves standstill, and makes its that sol-gel take place and transforms, and obtains gel.Place 120 ℃ of environment to dry fully gel, after taking-up grinds to form fine powder, place retort furnace, be warming up to 700 ℃ of roasting 3h, take out cooling, grind, obtain the LTCC powder in 200 ℃ of binder removal 2h.It is the round base of 10mm that the powder of weighing certain mass static pressure under the 30MPa condition becomes diameter, and sintering 2h becomes porcelain under 900 ℃ of conditions, can obtain MgO-Al 2O 3-SiO 2It is the ltcc substrate material.Two sides at base substrate is coated with silver electrode, burns electrode 10min at 875 ℃.
Each sample of table 3 is formed mass percent (wt%)
Oxide compound Al 2O 3 SiO 2 MgO B 2O 3 Bi 2O 3 TiO 2 CuO CaO K 2O
Mass percent 30.5 49.0 10.5 3.5 2.0 2.1 1.0 0.3 0.1
Corresponding raw material Al(NO 3) 3 ·9H 2O (C 2H 5O) 4Si Mg(OH) 2 ·4MgCO 3 B 2O 3 Bi(NO 3) 3 ·5H 2O Ti(OC 4H 9) 4 Cu(NO 3) 2 ·3H 2O Ca(NO 3) 2 ·4H 2O KNO 3
This glass ceramic material performance behind 900 ℃ of following sintering reaches following index:
Density p=2.99gcm -3, DIELECTRIC CONSTANT r=5.4 (1MHz), dielectric loss tan δ=1.0 * 10 -4(1MHz), insulation resistance ρ v=1.41 * 10 14Ω cm.

Claims (2)

1. a low temperature co-fired cordierite series glass-ceramic substance power is characterized in that, according to trichroite 2MgO2Al 2O 35SiO 2The packing component design, wherein weighting material comprises sintering agent B 2O 3, Bi 2O 3, and properties-correcting agent TiO 2, CuO, CaO, K 2Among the O three kinds or all, trichroite accounts for 80～90% of total mass in the prescription, and weighting material accounts for 10～20% of total mass in the prescription;
Each oxide compound accounts for the per-cent of total mass and is in the described powder: 18%～35%Al 2O 3, 40%～50%SiO 2, 8%～15%MgO, 3%～10%B 2O 3, 1%～5%Bi 2O 3, 0.1～10%TiO 2, 0.1～6%CuO, 0.1～4%CaO, 0～3%K 2O, raw materials used is Al (NO 3) 39H 2O, Mg (NO 3) 2, Si (C 2H 5O) 4, H 3BO 3, Bi (NO 3) 35H 2O, Ti (OC 4H 9) 4, Cu (NO 3) 23H 2O, Ca (NO 3) 24H 2O and KNO 3
2. realize the preparation method of the described cordierite series glass-ceramic substance power of claim 1, it is characterized in that, carry out according to the following steps:
1) will be 18%～35% Al with mass percent 2O 3With the corresponding Al (NO of 8%～15% MgO quality 3) 39H 2O and Mg (NO 3) 2Being dissolved in the dehydrated alcohol, being stirred to transparent clarification, will be 40%～50% SiO then with mass percent 2With 0.1～10% TiO 2Corresponding Si (the C of quality 2H 5O) 4And Ti (OC 4H 9) 4Join in this solution, stir, form clear soln A;
2) will be 3%～10% B with mass percent 2O 3, 1%～5% Bi 2O 3The corresponding H of quality 3BO 3, Bi (NO 3) 35H 2O and with mass percent be 0.1～6% CuO, 0.1～4% CaO, 0～3% K 2The corresponding KNO of O quality 3, Cu (NO 3) 23H 2O, Ca (NO 3) 24H 2Among the O two kinds or all join in the mixed solution of dehydrated alcohol and deionized water, stir, regulate the pH value between 9～10 with ammoniacal liquor, obtain liquid B;
3) solution A and B are mixed, stir, obtain colloidal sol;
4) colloidal sol is put into 40～60 ℃ baking oven and left standstill to sol-gel takes place and transform, obtain clear gel;
5) gel is placed 80～120 ℃ of oven dry fully;
6) xerogel is ground to form fine powder, place retort furnace, be warming up to 700～750 ℃ of roasting 2～3h then, take out cooling, grind to form powder in 200～250 ℃ of binder removal 1～3h.
CN2007101214671A 2007-09-06 2007-09-06 Low-temperature co-fired cordierite series glass-ceramic substance power and preparation method thereof Expired - Fee Related CN101148323B (en)

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