CN114315334B - LTCC material and preparation method thereof - Google Patents
LTCC material and preparation method thereof Download PDFInfo
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- CN114315334B CN114315334B CN202111644304.8A CN202111644304A CN114315334B CN 114315334 B CN114315334 B CN 114315334B CN 202111644304 A CN202111644304 A CN 202111644304A CN 114315334 B CN114315334 B CN 114315334B
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Abstract
The invention provides an LTCC material and a preparation method thereof, wherein the main components of the LTCC material are oxides, oxide additives and alkali metal carbonate, so that pure system glass is formed, the LTCC material is a classical glass ceramic, the LTCC material is a glass phase in a green state, and the main components are converted into crystalline phases after the LTCC material is formed into porcelain at 850 ℃. The low-temperature co-fired ceramic material belongs to a CBS system, and the LTCC material has the characteristics of higher crystallization degree and low dielectric loss. By controlling CaCO in LTCC material 3 ，H 3 BO 3 With SiO 2 The dielectric constant of the glass ceramic can be adjusted according to the mass percentage; then the matching of the oxide additive and the gold and silver cofiring can be controlled by controlling the types and the proportions of the oxide additive; the glass melting temperature can be adjusted by controlling the addition amount of the alkali metal carbonate.
Description
Technical Field
The invention belongs to the technical field of LTCC substrates, and particularly relates to an LTCC material and a preparation method thereof.
Background
LTCC (low temperature co-fired ceramic) technology appears in the middle 80 s of the 20 th century, and is an ideal technology for realizing miniaturization, high frequency and integration of electronic components due to incomparable superiority compared with the traditional HTCC (high temperature co-fired ceramic) and thick film technology, and has been widely applied in the field of electronic communication at present.
The LTCC is an ideal technology for realizing miniaturization, high frequency and integration of military electronic components, not only can integrate the passive element R, L, C, but also can integrate the mixed signal design of a microwave transmission line, a logic control line and a power line into the same LTCC three-dimensional microwave transmission structure, thereby maximally reducing the volume and the weight of the component. Meanwhile, the dielectric constant of the material is moderate (4 < epsilon < 8), the loss tangent (tg delta) of the material is about 0.002 below 24GHz frequency, and good conductors such as Au, ag and the like are adopted, so that the high-frequency dielectric loss and the transmission line conductor loss are lower than those of silicon, gallium arsenide and other ceramics. The high-density multilayer interconnection, embedded passive element and airtight ceramic package are integrated based on the LTCC technology, the microwave performance is excellent, the high-density multilayer interconnection, embedded passive element and airtight ceramic package are suitable for the advantages of high-low frequency mixing and digital-analog mixing design, and the LTCC technology has unique technical advantages and wide application prospects in the fields of military electronics such as radars, aerospace, aviation, communication, supercomputers and the like. The LTCC-based system integration technology is a main means for achieving the goal of miniaturization and integration of electronic components, and has become the first choice for the development of miniaturization and higher frequency bands.
In the aspect of millimeter wave low-loss LTCC powder material, a casting technology based on the material and a mass production technology, the system research on ceramic formula composition, casting system composition, casting belt material performance and matching property with gold-silver conductor slurry is lacking, the systematic research on a ceramic formula system is lacking, the system research on the influence rule of casting belt material preparation process parameters on the product performance is lacking, and the preparation process technology of the millimeter wave low-loss material is not mastered.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides an LTCC material and a preparation method thereof, which are used for solving the problems that a proper ceramic formula system and a corresponding preparation process are lacked aiming at millimeter wave low-loss LTCC powder materials in the prior art.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
the LTCC material comprises, by mass, 85-95% of a component A, 2-10% of an oxide additive, and 3-5% of alkali metal carbonate; the component A is a raw material for providing oxide;
the component A comprises CaCO 3 、H 3 BO 3 And SiO 2 ；
The oxidation additive is made of TiO 2 、ZrO 2 、Al 2 O 3 、MgO、ZnO、P 2 O 5 And Cr (V) 2 O 3 M is more than or equal to 4;
the alkali metal carbonate is prepared from Na 2 CO 3 、K 2 CO 3 And Li (lithium) 2 CO 3 The N is more than or equal to 2.
The invention further improves that:
preferably, the component A comprises CaCO in mass fraction 3 : 40~60%，H 3 BO 3 :5~15%，SiO 2 : 55~25%。
Preferably, the mass fraction content range of each substance in the oxide additive is 0-30% in terms of mass fraction.
Preferably, the mass fraction of each substance in the alkali metal carbonate is as follows: na (Na) 2 CO 3 :20~40%；K 2 CO 3 :20~40%；Li 2 CO 3 :20~60%。
A method for preparing an LTCC material as claimed in any one of the preceding claims, comprising the steps of:
step 1, ball-milling and mixing a component A, an oxide additive and alkali metal carbonate, and drying to form mixed powder;
step 3, after the glass powder, the solvent, the binder, the plasticizer and the dispersing agent are subjected to airtight ball milling and uniform mixing, vacuum defoaming is carried out to obtain casting slurry, the casting slurry is injected into a casting machine, and a green ceramic tape is formed after drying;
and 4, pressurizing the green ceramic tape, and sintering to form the LTCC material.
Preferably, in the step 1, the ball milling and mixing mode is wet mixing, and the ball milling and mixing time is 3-5 hours.
Preferably, in the step 2, the smelting temperature is 1350-1550 ℃ and the smelting time is 1-4 h.
Preferably, in step 2, the particle size of D50 in the glass frit is 1.0 to 4.0. Mu.m.
Preferably, in the step 3, the solvent is a mixture of toluene and ethanol, the binder is polyvinyl butyral, the plasticizer is dioctyl phthalate, and the dispersing agent is fish oil.
Preferably, in the step 4, the pressurizing temperature is 60-80 ℃, the pressurizing pressure is 15-25 MPa, and the pressurizing time is 10-15 min;
the sintering process is that the raw porcelain belt is heated to 450 ℃ from the room temperature at the speed of 2 ℃/min, and the temperature is kept for 2 hours; and then heating to 850-900 ℃ at a speed of 5 ℃/min, and preserving heat for 10-15 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a low-temperature co-fired ceramic material, which mainly comprises oxides, oxide additives and alkali metal carbonate, forms simple system glass, is classical glass ceramic, is a glass phase in a green state, and is converted into a crystalline phase after porcelain formation at 850 ℃. The low-temperature co-fired ceramic material belongs to a CBS system, and the LTCC material has the characteristics of higher crystallization degree and low dielectric loss. By controlling CaCO in LTCC material 3 ，H 3 BO 3 With SiO 2 The dielectric constant of the glass ceramic can be adjusted according to the mass percentage; then the matching of the oxide additive and the gold and silver cofiring can be controlled by controlling the types and the proportions of the oxide additive; the glass melting temperature can be adjusted by controlling the addition amount of the alkali metal carbonate. Through formula adjustment, the LTCC material which is sintered and compact at 850 ℃ and has a dielectric constant of 5.0-7.0 and a loss tangent of less than 0.0015 under the condition of 24GHz can be obtained.
The invention also discloses a preparation method of the LTCC material, which comprises the steps of mixing raw materials, smelting to form glass liquid, carrying out water quenching treatment to form glass blocks, and carrying out ball milling and grinding on the glass blocks to form glass powder. The glass powder is used for preparing the birth ceramic tape, and finally the LTCC material is formed.
Drawings
FIG. 1 is an XRD pattern showing the difference between green state and porcelain state of the LTCC material of the CBS system of example 1 of the present invention;
FIG. 2 is a DSC chart of a glass frit of example 1 of the present invention;
FIG. 3 is a surface SEM image of LTCC material of example 1 of the present invention;
FIG. 4 is a co-fired section of LTCC material of example 1 with gold according to the present invention;
FIG. 5 shows the co-fired section of LTCC material of example 1 with silver according to the present invention.
Detailed Description
Aiming at the problems and the demands of the prior art, the invention aims to provide an LTCC material matched with gold and silver conductor slurry and having millimeter wave low loss and a preparation method thereof, so as to meet the application requirements of electronic devices and LTCC substrates.
A low-loss LTCC material with millimeter wave matched with gold-silver conductor paste is prepared from glass material containing oxide including CaCO 3 、H 3 BO 3 And SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The LTCC material also contains an oxide additive, wherein the oxide additive is prepared from TiO 2 、ZrO 2 、Al 2 O 3 、MgO、ZnO、P 2 O 5 And Cr (V) 2 O 3 M is a natural number greater than or equal to 4. The LTCC material also comprises alkali metal carbonate, in particular K 2 CO 3 、Na2CO 3 And Li (lithium) 2 CO 3 More than two of the substances.
The LTCC material is a glass material, is a CBS (calcium boron silicon) system, and has lower dielectric loss. By controlling CaCO in LTCC material 3 ，H 3 BO 3 With SiO 2 The dielectric constant of the glass-ceramic can be adjusted; then, the matching degree of the oxide additive and gold and silver can be controlled by controlling the types and the proportion of the oxide additive, so that the matching degree of the LTCC material and the gold and silver material in the cofiring process is improved; controlling alkali metal carbonic acidThe amount of salt added can adjust the glass melting temperature. The LTCC material with compact sintering at 850 ℃ and excellent characteristics in millimeter wave frequency band can be obtained through the formula adjustment among the oxide, the oxide additive and the alkali metal carbonate.
For LTCC materials, the influence of the structure and the composition of the materials on the loss is fundamental, and the inorganic medium is mainly the structural loss in the millimeter wave frequency band. The inorganic medium of the LTCC millimeter wave low-loss material is divided into two parts, namely a crystalline phase and a glass phase, and the crystalline phase is converted into the crystalline phase after the glass phase is completely in a green state and is ceramic. The glass ceramic structure not only has the uniformity of a glass phase (compared with a crystal phase, the glass phase has no crystal boundary and no air hole), but also is converted into the crystal phase after porcelain formation, and at the moment, the high loss of the glass phase is avoided (compared with the crystal phase, the lattice arrangement of the internal space of the glass phase is irregular, and the crystal phase is not compact), so that the glass ceramic structure is the first choice material of the LTCC millimeter wave low-loss material.
Specifically, the LTCC material comprises, in mass fraction: 85-95% of oxide, 2-10% of oxide additive and 3-5% of alkali metal carbonate.
As one of the preferred embodiments, the oxide includes CaCO in terms of mass fraction 3 :40~60%、H 3 BO 3 5-15% of SiO 2 :25~55%。
The oxide additive consists of M substances, wherein M is a natural number more than or equal to 4; the specific substances and the mass fraction thereof are as follows: tiO (titanium dioxide) 2 :0~30%；ZrO 2 : 0~30%；Al 2 O 3 :0 ~30%; MgO: 0~30%; ZnO : 0~30%; P 2 O 5: 0-30% of Cr 2 O 3 :0~30%。
The alkali metal carbonate consists of the following N substances, wherein N is a natural number more than or equal to 2, and the specific substances and mass ratio thereof are as follows: na (Na) 2 CO 3 :20~40%；K 2 CO 3 :20~40%；Li 2 CO 3 :20~60%。
The preparation method of the LTCC material in the embodiment comprises the following steps:
step 1, caCO is processed 3 、H 3 BO 3 、SiO 2 Wet mixing the oxide additive and alkali metal carbonate, and stoving to form mixed powder;
specifically, the wet mixing is performed by ball milling with deionized water by a ball mill for 3-5 hours, and more preferably for 4 hours.
And 2, sieving the mixed powder, melting the mixed powder into glass liquid, carrying out water quenching treatment on the glass liquid to form glass blocks, and then crushing the glass blocks into glass powder to obtain the glass powder.
Specifically, the mixed powder is sieved by a 120-mesh sieve, and the melting temperature of the mixed powder is 1350-1550 ℃, more preferably 1400-1500 ℃; the melting time is 1-4 h, more preferably 2h; then the glass liquid is water quenched into glass blocks, and then the glass blocks are crushed into glass powder through wet ball milling. In the glass powder, the D50 particle size is 1.0-4.0 μm, more preferably 2-3 μm.
And 3, adding 70% by weight of solvent, 8% by weight of binder, 3.5% by weight of plasticizer and 2% by weight of dispersing agent into the glass powder, ball-milling and mixing uniformly in a closed environment, vacuum defoaming to obtain casting slurry of the LTCC material, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape. The solvent is a mixture of toluene and ethanol according to a volume ratio of 1:1, the binder is polyvinyl butyral, the plasticizer is dioctyl phthalate, and the dispersing agent is fish oil.
And 4, cutting the dried green porcelain belt into a required shape, placing the green porcelain belt into a hot press, pressurizing at 60-80 ℃ and 15-25 MPa, maintaining the pressure for 10-15 min, and then placing the green porcelain belt into an electric furnace for sintering. The specific sintering process is as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw ceramic tape after glue discharging to 850-900 ℃ from 450 ℃ at a speed of 5 ℃/min, and preserving heat for 10-15 min to obtain the LTCC material.
The LTCC material prepared by the preparation method can be co-fired with gold and silver conductor slurry, and has good matching property.
The invention provides a preparation method of an LTCC material. Experimental results show that the LTCC material with the dielectric constant of 5.0-7.0 and the loss tangent of less than 0.0015 can be obtained by adjusting the formula, and the preferable formula can be co-fired with gold and silver conductor paste under the condition of 850 ℃ sintering densification and 24 GHz.
For a further understanding of the present invention, the LTCC materials provided by the present invention are described in detail below in connection with specific examples.
Example 1
Step 1, calculating a formula according to 90% of oxide, 6% of oxide additive and 4% of alkali metal carbonate; specific oxides include CaCO 3 :55%、H 3 BO 3 10% and SiO 2 35 percent; the oxide additive comprises TiO 2 :30%、ZrO 2 :30%、Al 2 O 3 :10%、MgO:10%、ZnO :10%、P 2 O 5 5% and Cr 2 O 3 5 percent; the alkali metal carbonate includes: na (Na) 2 CO 3 :30%、K 2 CO 3 30% and Li 2 CO 3 :40%。
Correspondingly weigh 1237.5g CaCO 3 225g of H 3 BO 3 787.5g of SiO 2 45g of TiO 2 45g of ZrO 2 15g of Al 2 O 3 15g MgO, 15g ZnO, 7.5g P 2 O 5 7.5g of Cr 2 O 3 30g of Na 2 CO 3 K of 30g 2 CO 3 And 40g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 4 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a melting furnace at 1500 ℃, melting for 2 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained. The glass DSC is shown in FIG. 2, and the glass transition point (Tg) of the glass has two crystallization peaks at 676 ℃, 839 ℃ and 878 ℃ respectively, and the crystallization starting point is 816 ℃. Upon elevated temperature sintering, the glass will soften and sinter rapidly to a dense state, starting at 816 ℃, where the dense glass phase will be converted to a crystalline phase to achieve good dielectric properties, typical characteristics of glass ceramics being clearly demonstrated in the DSC of FIG. 2.
Step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into 1KG glass frit, ball milling and mixing uniformly in a closed environment, vacuum defoaming to obtain casting slurry of low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape;
and 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; and (3) starting from 450 ℃, heating to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 10min to obtain the LTCC material.
As can be seen from SEM analysis of FIG. 3, the LTCC material was sinter dense at 850 ℃. In the millimeter wave band (24 GHz), the dielectric constant was 5.823 and the loss tangent was 0.00113. By analyzing the difference between the green state and the porcelain state of the LTCC material of the CBS system through an X-ray diffractometer (XRD) technique in the attached figure 1, the LTCC material prepared in the embodiment is a pure glass phase, and the main component is converted into a crystalline phase after porcelain formation.
The LTCC material prepared by the embodiment is respectively co-fired with gold conductor slurry and silver conductor slurry, so that the formed substrates have good matching degree and no warpage. FIG. 4 is an SEM of a cofiring cross section of LTCC material with gold, showing no diffusion; FIG. 5 is an SEM image of a co-fired section of LTCC material and silver, showing no diffusion.
Example 2
Step 1, 88% oxygenA formulation calculated from the oxide, 7% oxide additive and 5% alkali carbonate; specific oxides include CaCO 3 :55%、H 3 BO 3 10% and SiO 2 35 percent; the oxide additive comprises TiO 2 :30%、ZrO 2 :30%、Al 2 O 3 :10%、MgO:10%、ZnO :10%、P 2 O 5 5% and Cr 2 O 3 5 percent; the alkali metal carbonate includes: na (Na) 2 CO 3 :30%、K 2 CO 3 30% and Li 2 CO 3 :40%。
Correspondingly weigh 1210g of CaCO 3 220g of H 3 BO 3 770g of SiO 2 52.5g of TiO 2 52.5g of ZrO 2 17.5g of Al 2 O 3 17.5g MgO, 17.5g ZnO, 8.75g P 2 O 5 8.75g of Cr 2 O 3 37.5g of Na 2 CO 3 37.5g of K 2 CO 3 And 50g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 4 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a 1450 ℃ melting furnace, melting for 2 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
Step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into 1KG glass frit, ball milling and mixing uniformly in a closed environment, vacuum defoaming to obtain casting slurry of low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape;
and 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; and (3) starting from 450 ℃, heating to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 10min to obtain the LTCC material.
The LTCC material produced in this example was tested to have a dielectric constant of 6.214 and a loss tangent of 0.00144 at 24 GHz.
Example 3
Step 1, calculating a formula according to 92% of oxide, 5% of oxide additive and 3% of alkali metal carbonate; specific oxides include CaCO 3 :55%、H 3 BO 3 10% and SiO 2 35 percent; the oxide additive comprises TiO 2 :30%、ZrO 2 :30%、Al 2 O 3 :10%、MgO:10%、ZnO :10%、P 2 O 5 5% and Cr 2 O 3 5 percent; alkali metal carbonates including Na 2 CO 3 :30%、K 2 CO 3 30% and Li 2 CO 3 :40%。。
1265g CaCO was weighed out 3 230g of H 3 BO 3 805g of SiO 2 37.5g of TiO 2 37.5g of ZrO 2 12.5g of Al 2 O 3 12.5g MgO, 12.5g ZnO, 6.25g P 2 O5, 6.25g of Cr 2 O 3 22.5g of Na 2 CO 3 22.5g of K 2 CO 3 And 30g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 4 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a melting furnace at 1520 ℃, melting for 4 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
Step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into 1KG glass frit, ball milling and mixing uniformly in a closed environment, vacuum defoaming to obtain casting slurry of low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape;
and 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw porcelain belt after glue discharging to 860 ℃ from 450 ℃ at a speed of 5 ℃/min, and preserving heat for 12min to obtain the LTCC material.
The LTCC material obtained in this example was tested to have a dielectric constant of 5.768 and a loss tangent of 0.00085 at 24 GHz.
Example 4
Step 1, calculating a formula according to 90% of oxide, 6% of oxide additive and 4% of alkali metal carbonate; specific oxides include CaCO 3 :52%、H 3 BO 3 10% and SiO 2 38 percent; the oxide additive comprises TiO 2 :30%、ZrO 2 :30%、Al 2 O 3 :10%、MgO:10%、ZnO:10%、P 2 O 5 5% and Cr 2 O 3 5 percent; the alkali metal carbonate includes: na (Na) 2 CO 3 :30%、K 2 CO 3 30% and Li 2 CO 3 :40%。
1170g of CaCO was weighed out 3 225g of H 3 BO 3 855g of SiO 2 45g of TiO 2 45g of ZrO 2 15g of Al 2 O 3 15g MgO, 15g ZnO, 7.5g P 2 O 5 7.5g of Cr 2 O 3 30g of Na 2 CO 3 K of 30g 2 CO 3 And 40g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 4 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a 1475 ℃ melting furnace, melting for 2 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
And step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into the 1KG glass frit, performing ball milling and mixing uniformly in a closed environment, performing vacuum deaeration to obtain casting slurry of the low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape.
And 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw porcelain belt after glue discharging from 450 ℃ to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 15min to obtain the LTCC material.
The LTCC material prepared in this example was tested for a dielectric constant of 5.683 and loss tangent of 0.00092 at 24 GHz.
Example 5
Step 1, calculating a formula according to 85% of oxide, 10% of oxide additive and 5% of alkali metal carbonate; specific oxides include CaCO 3 :50%、H 3 BO 3 12% and SiO 2 38 percent; oxide additive packageIncluding TiO 2 :30%、ZrO 2 :20%、Al 2 O 3 30% and 20% of ZnO; the alkali metal carbonate includes: na (Na) 2 CO 3 40% and Li 2 CO 3 :60%。
Weigh 1062.5 g CaCO 3 H of 255, 255 g 3 BO 3 SiO of 807.5 g 2 TiO 75/75 g 2 ZrO of 50. 50g 2 Al of 75, 75g 2 O 3 50g ZnO, 50g Na 2 CO 3 75g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 3 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a melting furnace at 1400 ℃, melting for 3 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
And step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into the 1KG glass frit, performing ball milling and mixing uniformly in a closed environment, performing vacuum deaeration to obtain casting slurry of the low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape.
And 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw porcelain belt after glue discharging to 900 ℃ from 450 ℃ at a speed of 5 ℃/min, and preserving heat for 10min to obtain the LTCC material.
The LTCC material prepared in this example was tested to have a dielectric constant of 6.332 and a loss tangent of 0.00189 at 24 GHz.
Example 6
Step 1, calculating a formula according to 95% of oxide, 2% of oxide additive and 3% of alkali metal carbonate; specific oxides include CaCO 3 :60%、H 3 BO 3 15% and SiO 2 25 percent; the oxide additive comprises ZrO 2 :10%、Al 2 O 3 :30%、MgO:20%、ZnO:20%、P 2 O 5 10% and Cr 2 O 3 10 percent; the alkali metal carbonate includes: k (K) 2 CO 3 40% and Li 2 CO 3 :60%。
1425g CaCO was weighed out 3 356.3g of H 3 BO 3 593.8g of SiO 2 5g of ZrO 2 15g of Al 2 O 3 10g MgO, 10g ZnO, 5g P 2 O 5 5g of Cr 2 O 3 K of 30g 2 CO 3 45g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 5h at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a melting furnace at 1500 ℃, melting for 2 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
And step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into the 1KG glass frit, performing ball milling and mixing uniformly in a closed environment, performing vacuum deaeration to obtain casting slurry of the low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape.
Step 4, cutting the dried green porcelain belt into a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa for 10min, and then placing the green porcelain belt into an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; and heating the raw porcelain belt after glue discharging to 880 ℃ from 450 ℃ at a speed of 5 ℃/min, and preserving heat for 13min to obtain the LTCC material.
The LTCC material prepared in this example was tested to have a dielectric constant of 6.552 and a loss tangent of 0.00245 at 24 GHz.
Example 7
Step 1, calculating a formula according to 86% of oxide, 10% of oxide additive and 4% of alkali metal carbonate; specific oxides include CaCO 3 :40%、H 3 BO 3 5% and SiO 2 55 percent; the oxide additive comprises TiO 2 :30%、Al 2 O 3 20 percent of MgO, 20 percent of ZnO, 20 percent of P 2 O 5 10 percent; the alkali metal carbonate includes: na (Na) 2 CO 3 :40%、K 2 CO 3 40% and Li 2 CO 3 :20%。
860g CaCO was weighed out 3 107.5g of H 3 BO 3 1182.5g of SiO 2 75g of TiO 2 50g of Al 2 O 3 50g MgO, 50g ZnO, 25g P 2 O 5 40g of Na 2 CO 3 40g of K 2 CO 3 20g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 3 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a 1550 ℃ melting furnace, melting for 1h, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
Step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into 1KG glass frit, ball milling and mixing uniformly in a closed environment, vacuum defoaming to obtain casting slurry of low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape;
and 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw porcelain belt after glue discharging from 450 ℃ to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 15min to obtain the LTCC material.
The LTCC material prepared in this example was tested for a dielectric constant of 5.563 and loss tangent of 0.00216 at 24 GHz.
Example 8
Step 1, calculating a formula according to 94% of oxide, 2% of oxide additive and 4% of alkali metal carbonate; specific oxides include CaCO 3 :60%、H 3 BO 3 5% and SiO 2 35 percent; the oxide additive comprises TiO 2 :20%、ZrO 2 :20%、Al 2 O 3 30%, mgO 10%, znO 10% and P 2 O 5 10 percent; the alkali metal carbonate includes: na (Na) 2 CO 3 :20%、K 2 CO 3 20% and Li 2 CO 3 :60%。
Weighing 1410g of CaCO 3 117.5g of H 3 BO 3 822.5g of SiO 2 10g of TiO 2 10g of ZrO 2 15g of Al 2 O 3 5g MgO, 5g ZnO, 5g P 2 O 5 20g of Na 2 CO 3 K of 20g 2 CO 3 60g of Li 2 CO 3 Placing in a 10L vertical ball millAdding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 5h at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a melting furnace at 1350 ℃, melting for 4 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
And step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into the 1KG glass frit, performing ball milling and mixing uniformly in a closed environment, performing vacuum deaeration to obtain casting slurry of the low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape.
And 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw porcelain belt after glue discharging from 450 ℃ to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 10min to obtain the LTCC material.
The LTCC material prepared in this example was tested to have a dielectric constant of 6.382 and a loss tangent of 0.00267 at 24 GHz.
Example 9
Step 1, calculating a formula according to 88% of oxide, 7% of oxide additive and 5% of alkali metal carbonate; specific oxides include CaCO 3 :60%、H 3 BO 3 10% and SiO 2 30 percent; the oxide additive comprises TiO 2 :5%、ZrO 2 :5%、Al 2 O 3 :20%、MgO:10%、ZnO:30%、P 2 O 5 10% and Cr 2 O 3 20 percent; the alkali metal carbonate includes: na (Na) 2 CO 3 :30%、K 2 CO 3 25% and Li 2 CO 3 :45%。
1320g CaCO was weighed out 3 220g of H 3 BO 3 660g of SiO 2 8.75g of TiO 2 8.75g of ZrO 2 35g of Al 2 O 3 17.5g MgO, 52.5g ZnO, 17.5g P 2 O 5 37.5g of Na 2 CO 3 K of 31.25g 2 CO 3 56.25g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 4 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a melting furnace at 1400 ℃, melting for 3 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
And step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into the 1KG glass frit, performing ball milling and mixing uniformly in a closed environment, performing vacuum deaeration to obtain casting slurry of the low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape.
And 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw porcelain belt after glue discharging from 450 ℃ to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 10min to obtain the LTCC material.
The LTCC material prepared in this example was tested for a dielectric constant of 6.414 and loss tangent of 0.00164 at 24 GHz.
Example 10
Step 1, calculating a formula according to 92% of oxide, 4% of oxide additive and 4% of alkali metal carbonate; specific oxides include CaCO 3 :52%、H 3 BO 3 8% and SiO 2 40 percent; the oxide additive comprises ZrO 2 :30%、MgO:30%、P 2 O 5 20% and Cr 2 O 3 20 percent; the alkali metal carbonate includes: na (Na) 2 CO 3 :35%、K 2 CO 3 25% and Li 2 CO 3 :40%。
Weighing 1196g of CaCO 3 184g of H 3 BO 3 920g of SiO 2 30g of ZrO 2 30g MgO, 20g P 2 O 5 20g of Cr 2 O 3 35g of Na 2 CO 3 K of 25g 2 CO 3 40g of Li 2 CO 3 Placing the mixture in a 10L vertical ball mill, adding 2.5kg of deionized water and 10kg of zirconia balls with the diameter of 5mm, ball milling for 4 hours at the stirring speed of 250r/min, filtering the zirconia balls by a 20-mesh sieve, and then placing the mixed slurry in a blast oven at 130 ℃ for drying to obtain mixed powder.
And 2, placing the dried mixed powder in a 1450 ℃ melting furnace, melting for 2 hours, and finally, water-quenching the glass liquid into glass blocks. After water is filtered off from the glass block, the glass block is placed in a 10L vertical ball mill, 10KG of zirconia balls with the diameter of 5mm are added, 2KG of deionized water is added, the ball milling is carried out for 4 hours at the stirring speed of 250r/min, and finally, the glass slurry is screened and dried, so that the glass powder with the granularity of 2-3 mu m is obtained.
And step 3, adding 700g of solvent (toluene: ethanol volume ratio is 1:1), 80g of binder (polyvinyl butyral), 35g of plasticizer (dioctyl phthalate) and 20g of dispersing agent (fish oil) into the 1KG glass frit, performing ball milling and mixing uniformly in a closed environment, performing vacuum deaeration to obtain casting slurry of the low-temperature cofired ceramic, injecting the casting slurry into a casting machine to form a thin-layer green ceramic tape, and naturally drying at room temperature to form a compact green ceramic tape.
And 4, cutting the dried green porcelain belt to form a required shape, placing the green porcelain belt into a hot press, pressurizing at 70 ℃ and 20MPa, and maintaining the pressure for 10min. Then placing the mixture in an electric furnace for sintering, wherein the specific conditions are as follows: heating the raw porcelain belt to 450 ℃ from room temperature at a speed of 2 ℃/min, and preserving heat for 2 hours for glue discharging; heating the raw porcelain belt after glue discharging from 450 ℃ to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 10min to obtain the LTCC material.
The LTCC material prepared in this example was tested for a dielectric constant of 5.723 and loss tangent of 0.00097 at 24 GHz.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. The LTCC material is characterized by comprising, by mass, 85-95% of a component A, 2-10% of an oxide additive and 3-5% of alkali metal carbonate; the component A is a raw material for providing oxide;
the component A comprises CaCO 3 、H 3 BO 3 And SiO 2 ；
The oxide additive is made of TiO 2 、ZrO 2 、Al 2 O 3 、MgO、ZnO、P 2 O 5 And Cr (V) 2 O 3 Composition;
the alkali metal carbonate is prepared from Na 2 CO 3 、K 2 CO 3 And Li (lithium) 2 CO 3 Composition;
the component A comprises CaCO 3 : 40~60%，H 3 BO 3 :5~15%，SiO 2 : 25~55%；
The mass fraction content range of each substance in the oxide additive is 0-30%;
the mass fraction of each substance in the alkali metal carbonate is as follows: na (Na) 2 CO 3 :20~40%；K 2 CO 3 :20~40%；Li 2 CO 3 :20~60%。
2. A method of preparing an LTCC material as claimed in claim 1, comprising the steps of:
step 1, ball-milling and mixing a component A, an oxide additive and alkali metal carbonate, and drying to form mixed powder;
step 2, sieving the mixed powder, smelting to obtain glass liquid; carrying out water quenching treatment on the glass liquid to form glass blocks, and ball-milling and crushing the glass blocks to obtain glass powder;
step 3, after the glass powder, the solvent, the binder, the plasticizer and the dispersing agent are subjected to airtight ball milling and uniform mixing, vacuum defoaming is carried out to obtain casting slurry, the casting slurry is injected into a casting machine, and a green ceramic tape is formed after drying;
and 4, pressurizing the green ceramic tape, and sintering to form the LTCC material.
3. The preparation method of the LTCC material according to claim 2, wherein in the step 1, the ball milling mixing mode is wet mixing, and the ball milling mixing time is 3-5 hours.
4. The method for producing LTCC materials according to claim 2, wherein in step 2, the melting temperature is 1350 to 1550 ℃ and the melting time is 1 to 4 hours.
5. The method for preparing LTCC material according to claim 2, wherein in the step 2, the particle size of D50 in the glass frit is 1.0-4.0 μm.
6. The method of preparing LTCC materials according to claim 2, wherein in step 3, the solvent is a mixture of toluene and ethanol, the binder is polyvinyl butyral, the plasticizer is dioctyl phthalate, and the dispersant is fish oil.
7. The preparation method of the LTCC material according to claim 2, wherein in the step 4, the pressurizing temperature is 60-80 ℃, the pressurizing pressure is 15-25 MPa, and the pressurizing time is 10-15 min;
the sintering process is that the raw porcelain belt is heated to 450 ℃ from the room temperature at the speed of 2 ℃/min, and the temperature is kept for 2 hours; and then heating to 850-900 ℃ at a speed of 5 ℃/min, and preserving heat for 10-15 min.
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