CN103121842A - Low-medium low-loss LTCC (Low Temperature Co-Fired Ceramic) microwave ceramic material and preparation method thereof - Google Patents
Low-medium low-loss LTCC (Low Temperature Co-Fired Ceramic) microwave ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000919 ceramic Substances 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 229910004829 CaWO4 Inorganic materials 0.000 claims abstract description 3
- 229910007786 Li2WO4 Inorganic materials 0.000 claims abstract description 3
- QZVSYHUREAVHQG-UHFFFAOYSA-N diberyllium;silicate Chemical group [Be+2].[Be+2].[O-][Si]([O-])([O-])[O-] QZVSYHUREAVHQG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 6
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 4
- 239000003082 abrasive agent Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 4
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 2
- 235000010216 calcium carbonate Nutrition 0.000 abstract 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract 2
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 abstract 2
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000005453 pelletization Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 6
- 238000009766 low-temperature sintering Methods 0.000 description 6
- 230000005496 eutectics Effects 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 229910004283 SiO 4 Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 241000233805 Phoenix Species 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- -1 oxonium ion Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical class [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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Abstract
The invention discloses a low-medium low-loss LTCC (Low Temperature Co-Fired Ceramic) microwave ceramic material and a preparation method thereof. The material is composite ceramic containing double phases, wherein the principal crystalline phase is tetragonal-phase scheelite CaWO4; the auxiliary phase is a trigonal crystal system phenacite structure Li2WO4 with the molecular formula of (1-x) CaWo4-xLi2WO4. The preparation method of the low-medium low-loss LTCC microwave ceramic material comprises the following steps of: with CaCO3, WO3 and Li2CO3 as initial materials, calculating the mass percentages of CaCO3, WO3 and Li2CO3 according to the molar ratio of each element in the molecular formula (1-x)CaWo4-xLi2WO4; weighing the materials, preliminarily ball-milling the materials, drying the materials, pre-sintering, secondarily ball-milling the materials; and obtaining the low-medium low-loss microwave ceramic material by carrying out a series of processes including drying, pelletizing, forming, sintering and the like.
Description
Technical field
The invention belongs to electron ceramic material and manufacturing field thereof, relate to a kind of low sintering low Jie's low-loss microwave stupalith and preparation method thereof.
Background technology
In recent years, be that universal electric complete machine, signal equipment or civilian consumer electronic product are all rapidly to miniaturization, lightweight, integrated, multifunction and high reliability future development in the world.The LTCC(LTCC) technology is as a kind of advanced person's 3 D stereo assembling integrated technology, created condition for passive device and passive/active part mix integrated development, and obtained a wide range of applications in the lamination sheet type passive device rapidly.A lot of internationally recognizable electronically materials and component manufacturing enterprise enters this field one after another, as Murata, Kyocera, TDK, TAIYO YUDAN, the Ferro of Japan, and U.S. Johanson Technology, Dupont company etc.The enterprise such as domestic 999sunlord electronics, phoenix Hua Gaoke, University of Electronic Science and Technology, Tsing-Hua University and colleges and universities have also launched research and development and have produced various LTCC planar passive devices and assembly.And in order to obtain high performance LTCC passive integrated devices and assembly, at first need to have high performance LTCC material.Still monopolized by several major companies such as external Ferro, Dupont, Hereus but the high-performance LTCC material of commercialization at present is main, domesticly fail all the time to obtain key breakthrough in this field, this not only causes LTCC integrated device and the assembly cost of China's research and development very high, be unfavorable for application and the popularization of corresponding product, due under one's control on core key technology, also seriously hindered the development of China LTCC industry on the other hand.Therefore, it is extremely urgent that exploitation has the high-performance LTCC material of independent intellectual property right.
The LTCC microwave ceramic material is to use branch very widely in the LTCC material.General microwave ceramic material sintering temperature is all more than 1100 ℃, for its sintering temperature being reduced to and below 950 ℃ of LTCC process compatible (being generally between 800 ℃ ~ 950 ℃), the method for employing comprises that mainly interpolation eutectic oxide compound or glass help burning, introduce chemical synthesis process and adopts superfine powder to do raw material etc.Rear two kinds due to high costs and certain process limitation arranged, therefore add the eutectic oxide compound or glass is the main method that realizes at present the LTCC microwave ceramic material.Even if but take this method, and the sintering temperature of present many microwave ceramic materials is too high, also is difficult to realize low-temperature sintering, and secondly, too much mixing of eutectic oxide compound or glass, also can consist of very large impact to the drain performance of material, causes Q * f to descend very large.Therefore, in order to realize high performance LTCC microwave ceramic material, at first need to select to have lower sintering temperature and the better microwave ceramic material system of dielectric properties, and then realize low-temperature sintering and good microwave dielectric property by various compound or doping way on its basis.
This patent has proposed a kind of with CaWO
4High-performance low-temperature sintered microwave ceramic material for the principal crystalline phase preparation.In the past both at home and abroad about AWO
4The research of (A=Ca, Sr, Ba) stupalith and application mainly concentrate on the aspects such as photo cathode, scintillator detector and fiber optic applications.Discovered in recent years CaWO
4System material also has better microwave dielectric property, has therefore also carried out some research work as microwave dielectric material.CaWO
4Be scheelite-type structure, belong to tetragonal system, the ignore group is I4
1/ a (No.88).For CaWO
4, a=0.524nm, c=1.138nm, its crystalline structure is as shown in Figure 1.Each structure cell contains four CaWO
4Molecule, calcium ion are positioned at (0,0,1/2), and tungsten is from being positioned at (0,0,0), and oxonium ion is positioned at (0.25,0.15,0.075).CaWO
4Sintering temperature be l200 ℃ of left and right, its dielectric properties are as follows: DIELECTRIC CONSTANT ε
rBe about 9~10, Q * f and be about 50,000 ~ 60,000GHz, temperature factor τ
f=(50~-40) ppm/ ° C.CaWO
4An outstanding shortcoming of stupalith is exactly difficult one-tenth porcelain, and the sintered sample hollow air-gap is more, and the people such as Sung HunYoon have studied the employing hot pressing sintering method and improved CaWO
4The one-tenth porcelain density of sample, and obtained the following ceramic ε of microwave property under 1150 ℃ of sintering temperatures
r=10.4, Q * f=63,000GHz, τ
f=-53ppm/ ° C(" Investigation of the relations between structure and microwave dielectric properties of divalent metal tungstate compounds ", J.Eur.Ceram.Soc., 2006,26,2051-2054).I1-Hwan Park has reported CaWO
4With Mg
2SiO
4Carry out compoundly, improved the one-tenth porcelain density of material system and obtained good microwave property: 0.9 CaWO
4-0.1 Mg
2SiO
4Under 1200 ℃ of sintering, ε
r=10.0, Q * f=129,858GHz, τ
f=-49.6ppm/ ° C(" Microwave dielectric properties and mixture behavior of CaWO
4-Mg
2SiO
4Ceramics ", Jpn.J.Appl.Phys.Vol.40 (2001) pp.4956-4960), this composite system has very low dielectric loss, but can only realize high temperature sintering.Eung Soo Kim has reported at CaWO
4In add 0.5wt.%Bi
2O
3-9wt.%H
3BO
3At 850 ℃ of lower sintering, its microwave property is: ε
r=8.7, Q * f=70,220GHz and τ
f=-15ppm/ ° C (" Low-temperature sintering and microwave dielectric properties of CaWO
4Ceramics for LTCC applications ", J.Eur.Ceram.Soc., 26 (2006) 2101 – 2104).By adding eutectic oxide compound and glassy phase can realize low-temperature sintering, but glassy phase add the microwave property that membership reduces pottery, and after being made into device or substrate by LTCC technique, if run into soldering, pottery has the risk of cracking.The existence of glassy phase has simultaneously increased and the interactional possibility of conductor material, has reduced the reliability of substrate, therefore begins to cause people's attention without the stupalith of glass ingredient.Generally speaking, CaWO
4The sintering temperature of material itself is not very high, and has microwave property preferably.If can by reasonably compound or doping design, be expected to realize well low Jie's low-loss LTCC material of over-all properties.
Summary of the invention
The purpose of this invention is to provide a kind of with CaWO
4For principal crystalline phase preparation, without glass ingredient and can realize 900 ℃ of low-temperature sinterings, specific inductivity is about 9.0, and has the preparation method of the LTCC microwave dielectric ceramic material of extremely low microwave loss.This microwave ceramics can significantly reduce the loss of microwave device or module as LTCC microwave-medium substrate or device material the time.
The present invention is to achieve these goals by the following technical solutions:
A kind of low Jie's low-loss LTCC microwave ceramic material, it is characterized in that: the composite ceramic material that comprises two-phase, wherein principal crystalline phase is Tetragonal sheelite CaWO4, and auxiliary phase is trigonal system phenakite structure Li2WO4, and its formula molecular formula is (1-x) CaWO4-xLi2WO4.Can realize extremely low dielectric loss when sintering temperature is 900 ℃ of left and right, its Q * f value can reach 117,600GHz.
A kind of low Jie's low-loss LTCC microwave ceramic material in such scheme, its formula molecular formula is 0.08~0.12 for the span of x in (1-x) CaWO4-xLi2WO4.
Adopt Tetragonal sheelite CaWO in the present invention
4Be principal crystalline phase, its have lower sintering temperature (1200 ℃ of left and right), less specific inductivity (<12) and lower microwave dielectric loss (Q * f〉50,000GHz).The Li of trigonal system
2WO
4Be mainly because its fusing point lower (742 ℃) can produce the liquid phase parcel to main phase grain when sintering, can effectively impel grain growth, improve densification degree, reduce crystal boundary and defective, to reach the purpose that reduces sintering temperature, reduces dielectric loss.While Li
2WO
4Itself also has microwave dielectric property preferably: ε
rBe about 5.5, Q * f and be about 60,000GHz, therefore a small amount of Li
2WO
4Introducing can be as not adding other eutectic sintering agents the microwave property of obvious reduction principal phase material, also may improve because of densification degree on the contrary, microtexture improves the low loss performance when making material system obtain even to surpass high temperature sintering.
In such scheme, a kind of preparation method of low Jie's low-loss LTCC microwave ceramic material is characterized in that comprising the following steps:
Step 1: with CaCO
3, WO
3, Li
2CO
3Be initial feed, according to (1-x) CaWO
4-xLi
2WO
4In the ceramic formula molecular formula, the molar ratio of each element is converted out CaCO
3, WO
3And Li
2CO
3Mass percent, carry out weighing, ball milling, the even post-drying of batch mixing;
Step 2: put into crucible and compacting after the oven dry material of step 1 gained is sieved, rise to 850~950 ℃ by the temperature rise rates of 2 ℃/minutes and carry out pre-burning, be incubated 2~3 hours, furnace cooling obtains Preburning material;
Step 3: the block Preburning material of step 2 gained is taken out from crucible to put into mortar first levigate roughly, then carry out secondary ball milling in ball mill;
Step 4: after the oven dry of the resulting secondary ball abrasive material of step 3, adding massfraction is that 10%~20% PVA solution carries out granulation and dry-pressing formedly is cylinder;
Step 5: the sample of step 4 gained is put into sintering oven, slowly rise to 600 ℃ and be incubated 2 hours by the temperature rise rate of 1 ~ 2 ℃/minute, to get rid of moisture and the glue in green compact, and then be warming up to 850 ℃~950 ℃ and carry out sintering by the temperature rise rate of 2 ℃~5 ℃/minutes, be incubated 2~3 hours, be cooled to 600 ℃ by the rate of temperature fall of 2 ℃~5 ℃/minutes again, furnace cooling obtains low Jie's low-loss microwave stupalith subsequently.
In such scheme, a kind of preparation method of low Jie's low-loss LTCC microwave ceramic material, described formula molecular formula is 0.08~0.12 for the span of x in (1-x) CaWO4-xLi2WO4.
In such scheme, a kind of preparation method of low Jie's low-loss LTCC microwave ceramic material, the concentration of described PVA solution is 10%.
Through above five steps, just can obtain low Jie's low-loss LTCC microwave ceramic material of the present invention.After tested, low Jie's low-loss LTCC microwave ceramic material provided by the invention, its specific inductivity between 8.38~9.01, Q * f value all 44,000GHz GHz above (be up to 117,600GHz), temperature coefficient of resonance frequency τ
fBe about-60ppm/ ° C.
The major advantage of low Jie's low-loss LTCC microwave ceramic material provided by the invention is:
1, specific inductivity in 8.38~9.01 left and right, can be widely used in LTCC microwave base plate, laminated microwave device and module.
2, have extremely low dielectric loss, Q * f reaches as high as 117,600GHz GHz when 900 ℃ of low-temperature sinterings.
3, do not add glass to fall burning in material system, occur the problem of crackle when having avoided when making LTCC device or module easily in soldering, be conducive to improve processing compatibility and the yield rate of product.
4, raw materials for production are cheap, and process engineering is simple, and handled easily and being beneficial to reduces costs.
Description of drawings
Fig. 1 is this CaWO
4The crystalline structure schematic diagram;
Fig. 2 is preparation technology's schematic flow sheet of low Jie's low-loss LTCC microwave ceramic material provided by the invention;
The microwave dielectric property of material system when Fig. 3 is x variation and sintering temperature variation.
Embodiment
Below described be a kind of specific embodiments of LTCC microwave ceramic material of the present invention.As shown in Figure 2, the concrete preparation method of this material is as follows:
Step 1: with CaCO
3, WO
3, Li
2CO
3Be initial feed, according to 0.9 CaWO
4-0.1 Li
2WO
4In the formula molecular formula, the molar ratio of each element is converted out CaCO
3, WO
3And Li
2CO
3Mass percent, carry out accurate weighing, ball milling is 12 hours in planetary ball mill, after ball milling, material is placed in baking oven and dries under 100 ℃.
Step 2: the oven dry of step 1 gained was expected to put into crucible and compacting after 40 mesh sieve, rise to 900 ℃ of pre-burnings by the temperature rise rates of 2 ℃/minutes, and be incubated 2 hours, it is standby that furnace cooling obtains Preburning material.
Step 3: the resulting block Preburning material of step 2 is first levigate roughly in mortar, secondary ball milling 12 hours in planetary ball mill then, after ball milling, material is placed in baking oven and dries under 100 ℃.
Step 4: add the PVA solution (PVA concentration is 10%) about 15wt% to carry out granulation after the secondary ball abrasive material oven dry with the step 3 gained, being pressed into diameter is 12mm, and height is the cylindric green compact sample of 6mm.
Step 5: the green compact sample that step 4 obtains is put into sintering oven, slowly rise to 600 ℃ and be incubated 2 hours by the temperature rise rate of 1 ℃/minute, to get rid of moisture and the glue in green compact, and then be warming up to 900 ℃ and carry out sintering by the temperature rise rate of 5 ℃/minutes, be incubated 2 hours, and then being cooled to 600 ℃ by the rate of temperature fall of 5 ℃/minutes, furnace cooling obtains low Jie's low-loss microwave ceramic material sample subsequently.This development type is tested through XRD, and most of crystalline phase is CaWO
4, a small amount of Li is arranged in addition
2WO
4Crystalline phase exists, without other third phase.The LTCC material property that this specific embodiments obtains is DIELECTRIC CONSTANT ε
rBe that 9.01, Q * f is 117,600GHz GHz, temperature factor τ
f=-60 ppm/ ° C.This dielectric material loss is very low, but the temperature factor performance is also not so good, and next step can consider that the compound pottery that has in right amount positive temperature coefficient improves whole temperature factor performance on this material system basis.
In addition, by appropriate change (1-x) CaWO
4-xLi
2WO
4The value of x in (wherein the span of x is 0.08~0.12), and final sintering temperature (850 ~ 950 ° of C), the microwave property of material system has certain variation.Specifically as shown in Figure 3, but work as x=0.10, when sintering temperature is 900 ° of C, dielectric loss is minimum.
Claims (5)
1. one kind low Jie's low-loss LTCC microwave ceramic material, it is characterized in that: the composite ceramic material that comprises two-phase, wherein principal crystalline phase is Tetragonal sheelite CaWO4, and auxiliary phase is trigonal system phenakite structure Li2WO4, and its formula molecular formula is (1-x) CaWO4-xLi2WO4.
2. a kind of low Jie's low-loss LTCC microwave ceramic material according to claim 1 is characterized in that: the formula molecular formula is 0.08~0.12 for the span of x in (1-x) CaWO4-xLi2WO4.
3. the preparation method of one kind low Jie's low-loss LTCC microwave ceramic material is characterized in that comprising the following steps:
Step 1: with CaCO
3, WO
3, Li
2CO
3Be initial feed, according to (1-x) CaWO
4-xLi
2WO
4In the formula molecular formula, the molar ratio of each element is converted out CaCO
3, WO
3And Li
2CO
3Mass percent, carry out weighing, ball milling, the even post-drying of batch mixing;
Step 2: put into crucible and compacting after the oven dry material of step 1 gained is sieved, rise to 850~950 ℃ by the temperature rise rates of 2 ℃/minutes and carry out pre-burning, be incubated 2~3 hours, furnace cooling obtains Preburning material;
Step 3: the block Preburning material of step 2 gained is taken out from crucible to put into mortar first levigate roughly, then carry out secondary ball milling in ball mill;
Step 4: after the oven dry of the resulting secondary ball abrasive material of step 3, adding massfraction is that 10%~20% PVA solution carries out granulation and dry-pressing formedly is cylinder;
Step 5: the sample of step 4 gained is put into sintering oven, slowly rise to 600 ℃ and be incubated 2 hours by the temperature rise rate of 1 ~ 2 ℃/minute, to get rid of moisture and the glue in green compact, and then be warming up to 850 ℃~950 ℃ and carry out sintering by the temperature rise rate of 2 ℃~5 ℃/minutes, be incubated 2~3 hours, be cooled to 600 ℃ by the rate of temperature fall of 2 ℃~5 ℃/minutes again, furnace cooling obtains low Jie's low-loss microwave stupalith subsequently.
4. the preparation method of a kind of low Jie's low-loss LTCC microwave ceramic material described according to claim 3, it is characterized in that: described formula molecular formula is 0.08~0.12 for the span of x in (1-x) CaWO4-xLi2WO4.
5. the preparation method of a kind of low Jie's low-loss LTCC microwave ceramic material described according to claim 3, it is characterized in that: the concentration of described PVA solution is 10%.
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CN105801119A (en) * | 2016-05-11 | 2016-07-27 | 电子科技大学 | Microwave dielectric LTCC material and preparation method thereof |
CN106699179A (en) * | 2016-12-09 | 2017-05-24 | 陈忠燕 | Low-dielectric low-loss LTCC microwave dielectric ceramic material and preparation method thereof |
CN108298982A (en) * | 2018-04-11 | 2018-07-20 | 长安大学 | A method of AWO4 one-component ceramics are prepared based on high-energy ball milling method |
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CN103539449B (en) * | 2013-10-07 | 2015-11-25 | 桂林理工大学 | Low temperature sintering microwave dielectric ceramic BiNbW 2o 10and preparation method thereof |
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