CN102390991B - Microwave dielectric ceramic substrate material sintered at low temperature and preparation thereof - Google Patents
Microwave dielectric ceramic substrate material sintered at low temperature and preparation thereof Download PDFInfo
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Abstract
The invention discloses a microwave dielectric ceramic substrate material sintered at low temperature and a preparation method thereof. The microwave dielectric ceramic substrate material sintered at low temperature has a structural expression as follows: xZnO-(1-x)B2O3, wherein x=0.5-0.75. A solid-phase synthresis process is adopted for preparing powder, the presintering temperature is 750-800 DEG C, and the sintering temperature is 850-960 DEG C. The substrate material disclosed by the invention has the following characteristics of lower dielectric constant, less dielectric loss low sintering temperature, capability of being cofired with Ag or Cu electrodes, simple preparation process and the like, and can be used for preparing low-temperature cofired ceramic (LTCC) substrates.
Description
Technical field
The invention belongs to electronic ceramics and preparation field thereof, particularly a kind of microwave medium ceramic substrate material and preparation thereof of sintering at low temperatures.
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 mainly with Al
2O
3, SiC and AlN etc. be base material, it has good characteristic at aspects such as thermal conductivity, bending strength, thermal expansivity, but the sintering temperature of these materials is basically all more than 1500 ℃, if adopt the method for burning altogether, conductor material can only be selected refractory metal such as W, Mo etc., make cost improve greatly, and new outlet has been opened up in the appearance of LTCC (LTCC) material for this reason.
The LTCC technology can provide high-density, high band, high digitized encapsulation technology and good thermal treatment process.The common burning temperature of LTCC (LTCC) is generally between 800 ℃～950 ℃.Because sintering temperature is low, the low metal of available resistivity is as the conductor material of multilayer wiring, can improve packing density, signaling rate and can in be embedded in the various laminar microwave electronic devices of multilager base plate once-firing, therefore be widely used as high-speed and high-density and interconnect among the polynary ceramic component (MCM).
MCM is on high-density multi-layered interconnect substrates, the various miniature components and parts (IC bare chip and chip components and parts) that adopt microwelding, packaging process will constitute electronic circuit assemble, and form the microelectronic product (comprising assembly, parts, subsystem, system) of high-density, high-performance, high reliability.It is to adapt to short, little, light, the thin and high speed of contemporary electronic systems, high-performance, high reliability, developing direction and the microelectronics Packaging of new generation and the package technique that grow up on the basis of multilayer board (PCB) and surface mounting technique (SMT) are the powerful measure of the realization system integration cheaply.
Being chosen among the MCM of ceramic substrate material is most important, and it influences the performance of MCM, selection and the final cost of associated materials.Generally the requirement to ceramic substrate material is: lower specific inductivity, high quality factor, low resonant frequency temperature factor, high thermal and thermostability, favorable mechanical processing characteristics and chemical stability etc.Adopt the LTCC technology to be convenient to make large size and jumbo substrate, passive devices such as its implantable resistance, electric capacity, inductance, has tangible low loss performance at high frequency band, be particularly suitable for radio frequency, microwave, millimetric wave device, all be widely used at radio communication, military affairs and civil area.
Usually the method that reduces the sintering temperature of microwave dielectric material has: add low melting point oxide or glassy phase as sintering aid, utilize chemical synthesis process, adopt superfine powder as starting material etc.But the general easy decline that causes microwave dielectric property when adding sintering aid, and chemical process is synthetic and adopt superfine powder to cause complex technical process as raw material, manufacturing cost and cycle can rise.Therefore seek a kind of at a lower temperature can sintering and have excellent microwave property, can the simple medium system of burning, chemical constitution and preparation technology be just extremely important altogether with Cu, Ag electrode.And ZnO-B
2O
3System is such individual system just, and the present invention is exactly the low-temperature sintering high performance microwave medium ceramic substrate material of developing in this material system.
Summary of the invention
The objective of the invention is to overcome above-mentioned prior art deficiency, provide a kind of low-temperature sintering microwave medium ceramic substrate material and preparation method thereof, this stupalith sintering and satisfy the requirement of ltcc substrate material technology at low temperatures just when not adding sintering aid or add a little auxiliary.
First purpose of the present invention provides a kind of low-temperature sintering microwave medium ceramic substrate material, and the relative permittivity behind its sintering is 5.5～8.5, low low-frequency dielectric loss (tan δ＜5 * 10
-41MHz), good microwave property (Qf=13,000GHz～60,000GHz), temperature coefficient of resonance frequency is adjustable (TCF=-20ppm/ ℃～-60ppm/ ℃), and its principal feature is (850 ℃～960 ℃) to carry out sintering under lower sintering temperature in addition, and can burn altogether with Ag or Cu electrode, chemical constitution and preparation technology are simple simultaneously.
Second purpose of the present invention provides the preparation method of above-mentioned low-temperature sintering microwave medium ceramic substrate material, and technology is simple.
The present invention has adopted the method for the most simple and effective solid state reaction sintering to realize the foregoing invention purpose.It at first is the prescription of choosing proper ratio, make raw material mix by a ball milling, make raw material carry out preliminary reaction by the presintering process, by the particle size of secondary ball milling refinement reactant, obtain needed ceramics sample by sintering process at last again.By a kind of so simple effective preparation method, the specific inductivity of the ceramics sample that obtains changes between 5.5～8.5, Qf is distributed in 13,000GHz～60,000GHz, temperature coefficient of resonance frequency-20ppm/ ℃～-60ppm/ ℃ between, sintering temperature is lower than 960 ℃, can burn altogether with Ag or Cu electrode, make it to be applicable to the needs of LTCC technology, enlarge its range of application.
Technical scheme of the present invention is achieved in that
Stupalith structure expression of the present invention is: xZnO-(1-x) B
2O
3, x=0.5～0.75 wherein, this microwave dielectric ceramic materials is based on ZnO-B
2O
3Low fever's compound in the binary system and part of compounds and burn the stupalith of formation with the Zn-B glassy phase of component altogether.
The preparation method of low-temperature sintering microwave medium ceramic substrate material, carry out according to the following steps:
1) with chemical feedstocks ZnO and H
3BO
3By prescription general formula xZnO-(1-x) B
2O
3Preparation, wherein x=0.5～0.75;
2) chemical feedstocks after will preparing mixes, and puts into the nylon jar, adds and the dehydrated alcohol ball milling of weight such as raw material 4～5 hours, fully mixes levigately, takes out the back 100 ℃～120 ℃ flash bakings, is pressed into bulk after crossing 200 mesh sieves;
3) Ya Zhi block is through 750 ℃～800 ℃ pre-burnings, and is incubated 4～8 hours, can obtain sample and burn piece;
4) sample is burnt piece and smash to pieces levigately, and through 4～5 hours secondary ball milling, fully mix levigate, oven dry, add 8～15wt.%PVA tackiness agent, granulation is sieved through 60 orders and 120 eye mesh screens, obtains required porcelain powder;
5) with the compression moulding on demand of porcelain powder, be incubated 4～6 hours to get rid of the PVA tackiness agent at 550 ℃～580 ℃, became porcelain in 4～8 hours at 850～960 ℃ of following sintering, can obtain the low-temperature sintering microwave medium ceramic substrate material.
Described PVA tackiness agent is that mass percent is 5% polyvinyl alcohol water solution.
Low-temperature sintering microwave medium ceramic substrate material of the present invention has following characteristics: relative permittivity lower (ε=5.5～8.5), little (tan δ＜5 * 10 of dielectric loss under the low frequency
-4), temperature coefficient of resonance frequency low (TCF=-20～-60ppm/ ℃), microwave property good (Qf=13,000～60,000GHz), sintering temperature low (850 ℃～960 ℃) can be burnt altogether with Ag or Cu electrode, chemical constitution and preparation technology are simple.
Embodiment
Below content of the present invention is further described.
According to this clearly demarcated technical scheme, the structure expression of low-temperature sintered ceramics baseplate material of the present invention is: xZnO-(1-x) B
2O
3, x=0.5～0.75 wherein.
The concrete preparation process of low-temperature sintering microwave medium ceramic substrate material of the present invention is: with chemical feedstocks ZnO and H
3BO
3By prescription general formula xZnO-(1-x) B
2O
3Preparation, wherein x=0.5～0.75.Fully mixing and ball milling is 4～5 hours, dries after levigate, sieves, briquetting, then through 750 ℃～800 ℃ pre-burnings, and be incubated 4～8 hours, the block after the pre-burning is carried out secondary ball milling, granulation after the levigate oven dry, sieve through 60 orders and 120 eye mesh screen bilayers, can obtain required powder.With powder compression moulding on demand, got rid of the PVA tackiness agent in 4～6 hours 550 ℃～580 ℃ insulations, became porcelain in 4～8 hours at 850 ℃～960 ℃ following sintering then, can obtain the low-temperature sintering microwave medium ceramic substrate material.
Low-temperature sintering microwave medium ceramic substrate material of the present invention is owing to adopted low-melting H
3BO
3As main starting raw material, make that sintering medium ceramic material of the present invention becomes possibility at low temperatures.The present invention is relevant with dielectric medium theoretical according to the crystal chemistry principle, with ZnO-B
2O
3Low fever's compound in the binary system is the basis, come the microwave medium ceramic substrate material is carried out modification with the method for chemical component glassy phase by adding a small amount of low melting point, can go out densification and the baseplate material of good microwave dielectric property is arranged at lower temperature (being lower than 960 ℃) sintering.
Embodiment 1:
Raw material ZnO and H with purity assay
3BO
3Be mixed with main powder by x=0.5, then with the abundant mixing and ball milling of main powder 4 hours, drying, sieve, behind the briquetting 800 ℃ of pre-burnings 4 hours, carried out secondary ball milling again 5 hours after then the bulk sample after the pre-burning being pulverized, levigate oven dry back granulation, sieve through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand (sheet or column), sintering 6～8h becomes porcelain under 950 ℃ of air then, can obtain the low-temperature sintering microwave medium ceramic substrate material.
The performance of this group stupalith reaches following index:
Sinter porcelain in 950 ℃ of air, dielectric properties ε r～5.7 (11.89GHz) under the microwave, quality factor q～1200, Qf～14, the temperature coefficient of resonance frequency TCF under the 298GHz, microwave～-25.6ppm/ ℃ (25 ℃～85 ℃).
Embodiment 2:
Raw material ZnO and H with purity assay
3BO
3Be mixed with main powder by x=0.5, then with the abundant mixing and ball milling of main powder 4 hours, drying, sieve, behind the briquetting 800 ℃ of pre-burnings 4 hours, carry out secondary ball milling again 5 hours after then will the bulk sample after the pre-burning pulverizing, it is 4% ZnB that the oven dry back adds weight percent
2O
4Glassy phase, abundant mixing and ball milling was dried after 4 hours, granulation, sieved through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand (sheet or column), sintering 4～6h becomes porcelain under 925 ℃ of air then, can obtain the low-temperature sintering microwave medium ceramic substrate material.
The performance of this group stupalith reaches following index:
Sinter porcelain in 925 ℃ of air, the dielectric properties ε under the microwave
r～6.6 (11.98GHz), quality factor q～1800, Qf～21, the temperature coefficient of resonance frequency TCF under the 960GHz, microwave～-35.1ppm/ ℃ (25 ℃～85 ℃).
Embodiment 3:
Raw material ZnO and H with purity assay
3BO
3Be mixed with main powder by x=0.57, then with the abundant mixing and ball milling of main powder 4 hours, drying, sieve, behind the briquetting 800 ℃ of pre-burnings 4 hours, carried out secondary ball milling again 5 hours after then the bulk sample after the pre-burning being pulverized, levigate oven dry back granulation, sieve through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand (sheet or column), sintering 4～6h becomes porcelain under 900 ℃ of air then, can obtain the low-temperature sintering microwave medium ceramic substrate material.
The performance of this group stupalith reaches following index:
Sinter porcelain in 900 ℃ of air, the dielectric properties ε under the microwave
r～6.5 (11.97GHz), quality factor q～1970, Qf～23, the temperature coefficient of resonance frequency TCF under the 543GHz, microwave～-58.3ppm/ ℃ (25 ℃～85 ℃).
Embodiment 4:
Raw material ZnO and H with purity assay
3BO
3Be mixed with main powder by x=0.75, then with the abundant mixing and ball milling of main powder 4 hours, drying, sieve, behind the briquetting 780 ℃ of pre-burnings 4 hours, carried out secondary ball milling again 5 hours after then the bulk sample after the pre-burning being pulverized, levigate oven dry back granulation, sieve through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand (sheet or column), sintering 4～6h becomes porcelain under 900 ℃ of air then, can obtain the low-temperature sintering microwave medium ceramic substrate material.
The performance of this group stupalith reaches following index:
Sinter porcelain in 900 ℃ of air, the dielectric properties ε under the microwave
r～5.7 (10.97GHz), quality factor q～5300, Qf～58, the temperature coefficient of resonance frequency TCF under the 534GHz, microwave～-52.4ppm/ ℃ (25 ℃～85 ℃).
It is pointed out that according to technical scheme of the present invention, above-described embodiment can also be enumerated many, prove according to applicant's lot of experiment results that the scope in that claims of the present invention propose all can reach purpose of the present invention.
Claims (3)
1. a low-temperature sintering microwave medium ceramic substrate material is characterized in that, this stupalith structure expression is: xZnO-(1-x) B
2O
3, x=0.5～0.75 wherein, this microwave dielectric ceramic materials is based on ZnO-B
2O
3Low fever's compound in the binary system and part low fever compound with burn the stupalith of formation altogether with the Zn-B glassy phase of component, wherein, accounting for part low fever compound weight percent with the Zn-B glassy phase of component is 4%.
2. the preparation method of low-temperature sintering microwave medium ceramic substrate material as claimed in claim 1 is characterized in that, carries out according to the following steps:
1) with chemical feedstocks ZnO and H
3BO
3By prescription general formula xZnO-(1-x) B
2O
3Preparation, wherein x=0.5～0.75;
2) chemical feedstocks after will preparing mixes, and puts into the nylon jar, adds and the dehydrated alcohol ball milling of weight such as raw material 4～5 hours, fully mixes levigately, takes out the back in ° C flash baking of 100 ° of C～120, is pressed into bulk after crossing 200 mesh sieves;
3) Ya Zhi block is through ° C pre-burning of 750 ° of C～800, and is incubated 4～8 hours, can obtain sample and burn piece;
4) sample is burnt piece and smash to pieces levigately, add the Zn-B glassy phase with component, and through 4～5 hours secondary ball milling, fully mix levigate, oven dry, add 8～15wt.%PVA tackiness agent, granulation is sieved through 60 orders and 120 eye mesh screens, obtains required porcelain powder; Wherein, accounting for the weight percent that sample burns piece with the Zn-B glassy phase of component is 4%;
5) with the compression moulding on demand of porcelain powder, sintering became porcelain in 4～8 hours under 850～960 ° of C, can obtain the low-temperature sintering microwave medium ceramic substrate material to get rid of the PVA tackiness agent in 4～6 hours in ° C insulation 550 ° of C～580.
3. method according to claim 2 is characterized in that, described PVA tackiness agent is that mass percent is 5% polyvinyl alcohol water solution.
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