CN1693286A - Low temp. coburning ceramic and its preparation process - Google Patents
Low temp. coburning ceramic and its preparation process Download PDFInfo
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- CN1693286A CN1693286A CN 200510076888 CN200510076888A CN1693286A CN 1693286 A CN1693286 A CN 1693286A CN 200510076888 CN200510076888 CN 200510076888 CN 200510076888 A CN200510076888 A CN 200510076888A CN 1693286 A CN1693286 A CN 1693286A
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- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000000919 ceramic Substances 0.000 title abstract description 20
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 3
- 230000004907 flux Effects 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- 229910011255 B2O3 Inorganic materials 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 42
- 239000000758 substrate Substances 0.000 description 25
- 238000005516 engineering process Methods 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 229910052709 silver Inorganic materials 0.000 description 10
- 239000004332 silver Substances 0.000 description 10
- 239000012298 atmosphere Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 230000001590 oxidative effect Effects 0.000 description 8
- 238000007796 conventional method Methods 0.000 description 7
- 230000008602 contraction Effects 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 239000006112 glass ceramic composition Substances 0.000 description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 description 4
- 238000007729 constrained sintering Methods 0.000 description 3
- 239000006124 glass-ceramic system Substances 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000005388 borosilicate glass Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000007766 curtain coating Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
A low-temp calcined ceramic for electronic device and package is proportionally prepared from Bi2O3, B2O3, SiO2, flux and ceramic material through mixing, adding alcohol or water, grinding, baking, grinding, calcining at 500-600 deg.C for 2-4 hr, and grinding.
Description
Technical field
The present invention relates to a kind of sintering temperature below 700 ℃, sintering shrinkage can be controlled in LTCC between the 0-20% and preparation method thereof.
Background technology
LTCC (Low Temperature Co-fired Ceramic, LTCC) be in nineteen eighty-two type material by Hughes Electronics's exploitation, it adopts thick-film material, according to the structure that designs in advance, with disposable burning till such as electrode materials, substrate, electron devices, can be used to realize high integration, high performance electronic encapsulation technology.At present, the LTCC technology be widely used in the fields such as radio frequency or microwave wireless communication, semi-conductor, photoelectron, MEMS as multi-layered ceramic substrate, encapsulation and multilayer ceramic unicircuit (multilayer ceramic integrated circuits, MCIC).In MCIC, the welding process of discrete assembling is adopted in the integrated encapsulation of semi-conductor and ceramic substrate usually, and because of the high-temperature damage semi-conductor, scolder generally selects for use softening temperature to be lower than 600 ℃ flux powder during for fear of welding; This technology shows many deficiencies especially along with the IC integrated level improves constantly: (1) along with chip size is more and more littler, the mode of this discrete combined can not satisfy processing requirement; (2) Chang Yong flux component contains toxicant Pb mostly, does not meet environmental requirement; (3) thermal expansivity of glass solder higher and be not easy control.And adopt the glass ceramic material of sintered at ultra low temperature (sintering temperature is at 700 ℃) can overcome above-mentioned some deficiency, utilize the LTCC technology that semi-conductor chip and ceramic substrate is integrated, simultaneously again can integrated multiple passive device on the ceramic substrate, thereby make the integration density of system higher.
The ltcc substrate material of current use mainly is compound system, devitrified glass system and the amorphous glass system of pottery+glass stopping composition.People have been developed a lot of sintering temperature and lows, low-k system on the compound system and devitrified glass that focus on glass+pottery of research in recent years.People such as Kumar made composition in 1977 be Al
2O
3-SiO
2-MgO-B
2O
3-P
2O
5Devitrified glass after, the glass-ceramic system of relevant LTCC has obtained flourish.People such as Kondo have developed ZnO-MgO-Al
2O
3-SiO
2System glass ceramic material, Kawakamf have been studied silicate glass and have been added Al
2O
3It is baseplate material; Also have borosilicate glass pottery (BSGC) and high silica glass pottery (HSGC) system etc. in addition.
Compare with other encapsulation technologies, although the LTCC technology has the superiority of not replacing, still there is the problem of substrate heat radiation and shrinking percentage control in the LTCC technology.The substrate heat radiation can solve by heat through-hole, and the development of zero shrinkage type LTCC material then can solve shrinks a control difficult problem.The zero-shrinkage theory is at first by propositions such as H.Nisbikawa, that is: place the dry-pressing raw cook as the shrinking percentage key-course in top and bottom that LTCC burns layer altogether during sintering, shrinking percentage by cohesive action certain between key-course and the multilayer and frictional force and key-course strictness, limited of the contraction behavior of LTCC multilayered structure along X, Y direction (two-dimensional directional of substrate surface), in order to compensate the contraction losses of substrate along the X-Y direction, substrate will carry out shrinkage-compensating along the Z direction.As a result, the dimensional change of LTCC structure on X, Y direction has only about 0.1%, thereby guaranteed the position and the precision of wiring and through hole behind the sintering, guaranteed the quality of device.The shrinking percentage key-course is mainly mixed by some non-metal powders and forms with fluidizer, solvent and binding agent, and the sintering temperature of non-metal powder requires the sintering temperature far above substrate, as adopting Al
2O
3, TiO
2Powder.Non-metal powder in the key-course is pressed very solidly, and this makes its shrinking percentage less than the shrinking percentage of LTCC substrate.
At present, the means of restriction LTCC shrinking percentage are mainly controlled by sintering process, method commonly used has: sintering process (self constrained sintering is shunk in restriction certainly, SCS), less pressure is assisted limit sintering (pressureless assisted constrained sintering, PLAS), pressure assist the limit sintering (pressureassisted constrained sintering, PAS) etc.The two kinds of technologies in back all are to realize by the sintering oven of special device, and PAS technology can be restricted to the LTCC multilayered structure and approach 0 along the contraction of X, Y direction, but technology is loaded down with trivial details, and cost is higher; The SCS method that has then is by the more organism of interpolation in the ltcc substrate material, make its more pore of generation during sintering and limit the sintering contraction, but the LTCC intensity of this method preparation is not high, and substrate surface is coarse, and dielectric loss is also bigger.
Along with the chip-count of assembling on substrate is more and more, substrate size is also done bigger and bigger, and the NEC Corporation of Japan has made the large substrates of 225mm * 225mm, and 100 chips can be installed above, and packing density is increased substantially.Yet along with the expansion of substrate area, in order to guarantee the setting accuracy of chip, it is extremely important that the sintering shrinkage of control basal plate just becomes, and sintering shrinkage is inconsistent or inhomogeneous, all can't be at its surface mount chip.It mainly is by the granularity of control powder, the ratio of curtain coating tackiness agent that the sintering of common ltcc substrate shrinks, and means such as the pressure of hot pressing lamination, sintering curre realize.
Summary of the invention
The purpose of this invention is to provide a kind of sintering and shrink controlled, that sintering temperature is low LTCC material and preparation method thereof.
Low-temperature co-burning ceramic material provided by the present invention, contain following components by weight portion:
Bi
2O
3 40-80，
B
2O
3 5-20，
SiO
2 5-30，
Fusing assistant 0-2,
Stupalith 1-50.
Wherein, fusing assistant can be selected from Li
2CO
3, CaF
2With LiF etc.; Stupalith can be selected from ZnO, Al
2O
3, TiO
2, CaO, P
2O
5, Nb
2O
3, V
2O
5, La
2O
3, Sb
2O
3And As
2O
3Deng oxide compound.
The preparation method of this low-temperature co-burning ceramic material comprises the steps:
1) in the mixture that contains the following portions by weight component, adds ethanol or water, grind the back oven dry, then grind into powder again;
Bi
2O
3 40-80，
B
2O
3 5-20，
SiO
2 5-30，
Fusing assistant 0-2,
Stupalith 1-50;
2) the gained powder was calcined 2-4 hour down at 500-600 ℃, obtained described low-temperature co-burning ceramic material after the grinding.
Wherein, ethanol or water be described mixture gross weight 1.5-2.5 doubly.
The resulting low-temperature co-burning ceramic material of this method is easy to use, as make base sheet or device after wherein adding an amount of binding agent and through dry-pressing or cold isostatic compaction, burns till under 550-700 ℃ of oxidizing atmosphere, and being incubated 2-4 hour can use; Perhaps, with the material preparation form slurry, be prepared into the single or multiple lift ceramic substrate behind the casting film-forming, burn till under 550-700 ℃ behind the binder removal, being incubated 2-4 hour can use; Or slurry is coated on the surface that needs the sealing-in assembly, 600-700 ℃ of thermal treatment gets final product.
The present invention adopts bismuth borosilicate glass+pottery (ZnO, Al
2O
3, TiO
2Deng), replace high-temperature fusion technology with powder calcination in the preparation, by regulating the proportioning of heterogeneity in the glass-ceramic, the sintering temperature of material is reduced to below 700 ℃, and composition and proportioning by ceramic phase in the feed glass ceramic systems, adjust the organic content in the curtain coating prescription, make sintering shrinkage controlled between 0-20%, specific inductivity is between 5-20 (1GHz), and dielectric loss coefficient is at the LTCC composition material below 0.002.The method of the control shrinking percentage that low-temperature co-burning ceramic material of the present invention adopts is by regulating the mark of high-melting-point pottery in the glass-ceramic, make it to constitute the ceramic frame that is difficult for contraction, make space between the flowable glassy phase material fill frame by wicking action, can control sintering shrinkage, can reach the glass-ceramic system again has uniform microtexture and more slick surface, and the composition and the proportioning of other stupalith of the dielectric properties of this stupalith system and heat physical properties and admixture are closely related.
The present invention improves and controls the performances such as dielectric properties, thermal expansivity, sintering temperature and sintering contraction of LTCC material by the stupalith of admixture heterogeneity and proportioning; By combining, obtain that dielectric properties satisfy application requiring, sintering shrinks controlled low-temperature co-fired glass ceramic composition material with traditional LTCC technology.Low-temperature co-burning ceramic material of the present invention has the following advantages:
(1) sintering temperature is low, and according to the difference of forming proportioning, sintering temperature is between 550-700 ℃, and sintering atmosphere is an oxidizing atmosphere, and pressure condition is a normal pressure; This sintering temperature shrinking percentage is controlled between 0-20%, and the glass ceramic material surfacing is smooth, and intensity is higher;
(2) specific inductivity can be regulated between 5-20 (1GHz), and dielectric loss coefficient is below 0.002; By adding other stupalith composition or adjusting the dielectric properties that the method for forming can change material;
(3) preparation technology is simple, cost is low, do not have toxic side effect, does not need to fire in advance, fusion, directly can use after ball mill mixing, the calcining;
(4) can be applied to electron device and the semi-conductor and the microelectronic packaging material field such as ceramic substrate, resonator, wave filter of high frequency circuit, integrability.
Embodiment
Embodiment 1,
As follows by following each component of dosage weighing:
Bi
2O
3：75g，
B
2O
3：5g，
SiO
2：7g，
Fusing assistant (LiF, 1g; Li
2CO
3, 0.5g): 1.5g,
Other stupalith (ZnO:4.5g; Al
2O
3: 8g): 12.5g.
Above-mentioned compound is placed ball grinder, add deionized water (be about compound gross weight 1.5 times), ball milling was dried in baking oven after 24 hours, and grinding is sieved; The powder of gained is calcined 2h at 550 ℃, promptly obtain the stupalith powder.
According to a conventional method above-mentioned powder is made the base sheet, insulation is 2 hours under 650 ℃, oxidizing atmosphere, and the ceramics behind the sintering is carried out electric performance test after by silver, silver ink firing, and the performance of this composition porcelain reaches following index:
Specific inductivity (1GHz) ε
rBe about 11.0, dielectric loss coefficient tg δ (1GHz) is 0.002; Behind the compressing tablet radially sintering shrinkage be about 0.
According to a conventional method above-mentioned powder is prepared into cast sheet, prints electrode after the film forming, lamination and cutting are burnt till under 600 ℃, oxidizing atmosphere behind the binder removal, are incubated and can obtain prototype multilayer low-temperature co-fired ceramic substrate after 2-4 hour.After tested, this substrate meets the industry service requirements.
Embodiment 2,
As follows by following each component of dosage weighing:
Bi
2O
3：70g，
B
2O
3：10g，
SiO
2：12g，
Fusing assistant (LiF): 0.5g,
Other stupalith (V
2O
5: 3.5g; Nb
2O
5: 4g): 7.5g.
Above-mentioned compound is placed ball grinder, add ethanol (be about compound gross weight 2.5 times), ball milling was dried in baking oven after 24 hours, and grinding is sieved; The powder of gained is calcined 4h at 500 ℃, promptly obtain the stupalith powder.
According to a conventional method above-mentioned powder is made the base sheet, insulation is 3 hours under 650 ℃, oxidizing atmosphere, and the ceramics behind the sintering is carried out electric performance test after by silver, silver ink firing, and the performance of this composition porcelain reaches following index:
Specific inductivity (1GHz) ε
rBe 10.5, dielectric loss coefficient tg δ (1GHz) is about 0.002, behind the compressing tablet radially sintering shrinkage be about 10%.If this powder preparing is become tape casting diaphragm, its sintering shrinkage can reach about 20%.
Embodiment 3,
As follows by following each component of dosage weighing:
Bi
2O
3：68g，
B
2O
3：12g，
SiO
2：10g，
Other stupalith: Sb
2O
3: 4.5g; ZnO:3g, CaO:2.5g.
Above-mentioned compound is placed ball grinder, add deionized water (be about compound gross weight 2 times), ball milling was dried in baking oven after 24 hours, and grinding is sieved; The powder of gained is calcined 2h at 600 ℃, promptly obtain the stupalith powder.
According to a conventional method above-mentioned powder is made the base sheet, insulation is 3 hours under 650 ℃, oxidizing atmosphere, and the ceramics behind the sintering is carried out electric performance test after by silver, silver ink firing, and the performance of this composition porcelain reaches following index:
Specific inductivity (1GHz) ε
rBe about 7.8, dielectric loss coefficient tg δ (1GHz) is about 0.002; Behind the compressing tablet radially sintering shrinkage be about 0.
According to a conventional method above-mentioned powder is prepared into the slurry that can be used for printing, is coated on the ceramic substrate surface that needs connection, superimposed back can obtain the good package of stopping property at 650-700 ℃ of thermal treatment 2h.
Embodiment 4,
As follows by following each component of dosage weighing:
Bi
2O
3：67g，
B
2O
3：5g，
SiO
2：5g，
Fusing assistant CaF
2: 0.5g,
Other stupalith: TiO
2: 20g; Al
2O
3: 2.5g.
Above-mentioned compound is placed ball grinder, add deionized water (be about compound gross weight 2 times), ball milling was dried in baking oven after 24 hours, and grinding is sieved; The powder of gained is calcined 2h at 600 ℃, promptly obtain the stupalith powder.
According to a conventional method above-mentioned powder is made the base sheet, insulation is 3 hours under 650 ℃, oxidizing atmosphere, and the ceramics behind the sintering is carried out electric performance test after by silver, silver ink firing, and the performance of this composition porcelain reaches following index:
Specific inductivity (1GHz) ε
rBe about 18.8, dielectric loss coefficient tg δ (1GHz) is about 0.002; Sintering behind the compressing tablet, radial shrinkage ratio is about 0.
Embodiment 5,
As follows by following each component of dosage weighing:
Bi
2O
3：50g，
B
2O
3：10g，
SiO
2：21g，
Fusing assistant (Li
2CO
3): 0.5g
Other stupalith (P
2O
5: 8.5g; As
2O
3: 8g; La
2O
3: 2.0g): 18.5g,
Above-mentioned compound is placed ball grinder, add deionized water (be about compound gross weight 1.5 times), ball milling was dried in baking oven after 24 hours, and grinding is sieved; The powder of gained is calcined 2h at 550 ℃, promptly obtain the stupalith powder.
According to a conventional method above-mentioned powder is made the base sheet, insulation is 2 hours under 580 ℃, oxidizing atmosphere, and the ceramics behind the sintering is carried out electric performance test after by silver, silver ink firing, and the performance of this composition porcelain reaches following index:
Specific inductivity (1GHz) ε
rBe about 5.8, dielectric loss coefficient tg δ (1GHz) is 0.002; Behind the compressing tablet radially sintering shrinkage be about 10%.
Claims (6)
1, a kind of low-temperature co-burning ceramic material, contain following components by weight portion:
Bi
2O
3 40-80，
B
2O
3 5-20，
SiO
2 5-30，
Fusing assistant 0-2,
Stupalith 1-50.
2, low-temperature co-burning ceramic material according to claim 1 is characterized in that: described fusing assistant is selected from Li
2CO
3, CaF
2With among the LiF one or more.
3, low-temperature co-burning ceramic material according to claim 1 and 2 is characterized in that: described stupalith is selected from ZnO, Al
2O
3, TiO
2, CaO, P
2O
5, Nb
2O
5, V
2O
5, La
2O
3, Sb
2O
3And As
2O
3In one or more.
4, the preparation method of the described low-temperature co-burning ceramic material of claim 1 comprises the steps:
1) in the mixture that contains the following portions by weight component, add ethanol or water, grind the back oven dry, then grind into powder again:
Bi
2O
3 40-80，
B
2O
3 5-20，
SiO
2 5-30，
Fusing assistant 0-2,
Stupalith 1-50;
2) the gained powder was calcined 2-4 hour down at 500-600 ℃, obtained described low-temperature co-burning ceramic material after the grinding.
5, preparation method according to claim 4 is characterized in that: described fusing assistant is selected from Li
2CO
3, CaF
2With among the LiF one or more; Described stupalith is selected from ZnO, Al
2O
3, TiO
2, CaO, P
2O
5, Nb
2O
5, V
2O
5, La
2O
3, Sb
2O
3And As
2O
3In one or more.
6, according to claim 4 or 5 described preparation methods, it is characterized in that: described ethanol or water are 1.5-2.5 times of described mixture gross weight.
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|---|---|---|---|
| CNB2005100768888A CN1304335C (en) | 2005-06-20 | 2005-06-20 | Low temp. coburning ceramic and its preparation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100768888A CN1304335C (en) | 2005-06-20 | 2005-06-20 | Low temp. coburning ceramic and its preparation process |
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|---|---|
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| CN1304335C CN1304335C (en) | 2007-03-14 |
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ID=35352431
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|---|---|---|---|
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| CN1267376C (en) * | 2004-02-19 | 2006-08-02 | 清华大学 | Composite material of glass ceramics cosintered by low temp |
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