CN115521138B - Low dielectric low-loss LTCC material and preparation method thereof - Google Patents
Low dielectric low-loss LTCC material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low dielectric low loss LTCC material, which comprises a part of B-Si-Al glass and B parts of CaSiO 3 Ceramic powder, c parts of SiO 2 Powder, wherein a is 40-55%, b is 45-55%, c is 5-10%, and a+b+c=100%; the preparation method comprises the following steps: 1) Taking the ingredients; 2) Ball milling the ingredients in the step S1, uniformly mixing and drying; 3) Adding adhesive for granulating, pressing and forming, and sintering in air atmosphere at 850-880 ℃. The invention adopts a glass ceramic composite system and adopts the B-Si-Al glass and CaSiO with specific content 3 Ceramic powder and SiO 2 The low dielectric low-loss LTCC material obtained by compounding the powder has lower sintering temperature and better compactness, and can realize low-temperature co-firing with Ag; and the dielectric constant is 5.2-5.7, the dielectric loss is less than 2 thousandths, and the bending strength is more than 170MPa.
Description
Technical Field
The invention relates to the technical field of functional ceramic materials, in particular to a low dielectric low-loss LTCC material and a preparation method thereof.
Background
The low temperature co-fired Ceramic (LTCC) technology is a novel multilayer substrate technology developed in the middle of the 80 s of the last century, and the sintering temperature is generally below 900 ℃ and can be co-fired with Ag.
The LTCC material has the main performance indexes of dielectric constant and dielectric loss, the lower the dielectric constant is, the more favorable for high-speed transmission of signals, and the smaller the dielectric loss is, the better the frequency selection characteristic is. With the advent of the 5G age, the low signal delay requirements of high speed circuits have been met with the need to reduce the dielectric constant and dielectric loss of the materials as much as possible. One proposal is to prepare Ca-B-Si ceramic materials by a solid phase reaction method, but the solid phase method generally has the problems of high sintering temperature (900-1000 ℃), large shrinkage, poor compactness and the like, which can cause the increase of difficulty in low-temperature cofiring (generally less than 900 ℃) with Ag for LTCC materials.
It should be noted that the information disclosed in the above background section is only for understanding the background of the present application and thus may include information that does not form the prior art that is already known to those of ordinary skill in the art.
Disclosure of Invention
In order to solve the problem that low-temperature co-firing of an LTCC material and Ag is difficult in the prior art, the primary purpose of the invention is to provide a low-dielectric low-loss LTCC material.
It is still another object of the present invention to provide a method for preparing the low dielectric low loss LTCC material.
The technical problems of the invention are solved by the following technical scheme:
a low dielectric low-loss LTCC material adopts a glass ceramic composite system material and comprises a part of B-Si-Al glass and B part of CaSiO by mass percent 3 Ceramic powder, c parts of SiO 2 Powder, wherein a is 40-55%, b is 45-55%, c is 5-10%, and a+b+c=100%.
In some embodiments, the raw material components of the B-Si-Al glass are in mass fraction: comprises 60 to 65 percent of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1~2%Na 2 CO 3 ,2~5%ZnO。
In some embodiments, the SiO 2 The powder can be crystalline SiO 2 Or amorphous SiO 2 The purity is more than 99.5 percent, and the granularity is 0.5 to 5 mu m.
In addition, the invention also provides a preparation method of the low dielectric low-loss LTCC material, which comprises the following steps:
1) Taking a parts of B-Si-Al glass and B parts of CaSiO by mass percent 3 Ceramic powder, c parts of SiO 2 Powder is mixed, wherein a is 40-55%, b is 45-55%, c is 5-10%, and a+b+c=100%;
2) Ball milling the ingredients in the step 1), uniformly mixing and drying;
3) Adding adhesive for granulating, pressing and forming, and then sintering in an air atmosphere at 850-880 ℃ to obtain the low dielectric low loss LTCC material.
In some embodiments, in the step 1), the raw material components of the B-Si-Al glass are calculated according to mass percentages: comprises 60 to 65 percent of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1~2%Na 2 CO 3 ,2~5%ZnO。
In some embodiments, in the step 2), water is used as a solvent, the ingredients are ball-milled for 6-12 hours by a planet, and the granularity of the slurry is controlled to D 50 0.5-5 mu m; the adhesive is a polyvinyl alcohol PVA adhesive.
In some embodiments, in the step 3), the glue discharging operation is further performed after the pressing and before the sintering.
In some embodiments, the temperature of the glue discharging operation is 450-500 ℃.
In some embodiments, the B-Si-Al glass is prepared using the following method: according to the mass ratio of 60-65% of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1~2%Na 2 CO 3 Preparing 2-5% ZnO, adding zirconia balls and water for ball milling and mixing, and drying; then melting the glass in a corundum mullite crucible at 1550-1600 ℃ for 2 hours to form glass liquid, and quenching the glass liquid by deionized water to obtain glass fragments; grinding again to obtain particle size D 50 B-Si-Al glass powder of 1-5 mu m.
In some embodiments, the CaSiO3 ceramic powder is prepared using a preparation method comprising: according to CaCO 3 :SiO 2 Is 1:1, adding zirconia balls and water, and mixing through planetary ball milling; drying, crushing, sieving, calcining at 1200-1300 deg.c for 2-4 hr, ball milling to obtain CaSiO with granularity of 0.5-2 microns 3 Ceramic powder.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention adopts a glass ceramic composite system and adopts the B-Si-Al glass and CaSiO with specific content 3 Ceramic powder and SiO 2 Compounding the powderCompared with the traditional single solid phase method, the prepared low dielectric low-loss LTCC material has lower sintering temperature (less than 900 ℃), better compactness and can realize low-temperature cofiring with Ag; the dielectric constant of the prepared low dielectric low-loss LTCC material is 5.2-5.7, the dielectric loss is less than 2 thousandths, the bending strength is more than 170MPa, the high-frequency high-speed requirement of the device is facilitated, and the low dielectric low-loss LTCC material can be applied to the device of the LTCC process.
2) The raw material B-Si-Al glass used in the invention can be melted by using a common ceramic crucible, compared with a platinum crucible, the melting cost can be greatly reduced, and the batch production can be realized.
Drawings
FIG. 1 is a flow chart of a preparation method of a low dielectric low loss LTCC material in an embodiment of the invention;
FIG. 2 is a graph of the microscopic morphology of a sintered sample of low dielectric low loss LTCC material prepared in example 3 of the present invention;
fig. 3 is a graph of the microscopic morphology of a sample after sintering of the dielectric material prepared in comparative example 1 of the prior art.
Detailed Description
The invention will be further described with reference to the following drawings in conjunction with the preferred embodiments. It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other.
It should be noted that, in this embodiment, the terms of left, right, upper, lower, top, bottom, etc. are merely relative terms, or refer to the normal use state of the product, and should not be considered as limiting.
Among low dielectric LTCC materials, A6 of Ferro company, 951 of DuPont company and the like are materials with higher commercialization degree at present, wherein the A6 material has low dielectric constant (5.9), low dielectric loss (less than 0.002) and higher bending strength (170 MPa) and is widely applied to high-frequency devices such as T/R components and the like. Although the A6 is Ca-B-Si glass ceramic material and needs to be prepared by a melting-water quenching method, the components of the glass ceramic material are very high in Ca and B, and cannot be melted by a common ceramic crucible, and only a platinum crucible with extremely high price can be used for melting, so that the cost of the glass ceramic material is very high, and on the other hand, the mass production difficulty is also very high, and no mature, commercial and mass-producible substitute material is yet seen at home.
In order to solve the problem of high cost caused by the fact that an expensive platinum crucible is required to be used for melting the calcium-boron-silicon glass ceramics in the prior art, and meanwhile, the low dielectric constant requirement of the material is met for high frequency and high speed of devices, the embodiment of the invention provides the low dielectric constant low-loss LTCC dielectric material and the preparation method thereof, so that the dielectric material which is sintered and compact in an air atmosphere at 850-880 ℃ and has a dielectric constant of 5.2-5.7, dielectric loss less than 2 thousandths and bending strength more than 170MPa is realized. The low-dielectric low-loss LTCC dielectric material adopts a glass ceramic composite system material and comprises a part of B-Si-Al glass and B part of CaSiO by mass percent 3 C parts of SiO 2 Wherein a is 40 to 55%, b is 45 to 55%, c is 5 to 10%, and a+b+c=100%.
The raw material components of the B-Si-Al glass in the embodiment of the invention are as follows in mass percent: comprises 60 to 65 percent of SiO2 and 20 to 25 percent of B 2 O 3 ,5~10%Al 2 O 3 ,1~2%Na 2 CO 3 2-5% ZnO, because the content of alkali metal component contained in B-Si-Al glass is low, can realize melting in corundum mullite ceramic crucible.
SiO in the embodiment of the invention 2 Can be crystalline SiO 2 Or amorphous SiO 2 The purity is more than 99.5 percent, and the granularity is 0.5 to 5 mu m.
The composite material system consists of a low-melting-point B-Si-Al glass phase and a main crystal phase CaSiO 3 SiO with performance adjusting function 2 Phase composition. Wherein, the B-Si-Al glass can form liquid phase at lower temperature, wets and wraps the ceramic powder, promotes the compact arrangement of the ceramic powder and the discharge of air holes, and is the key of the composite material being sintered at low temperature; caSiO (CaSiO) 3 Ceramic is the key of excellent dielectric property and mechanical property as the main crystal phase of the composite material; siO (SiO) 2 The phase is used as a low dielectric constant material, and can play a role in further reducing the dielectric constant and improving the overall dielectric property.
The B-Si-Al glassContent of CaSiO 3 Content of ceramic powder, siO 2 The wettability and compatibility of the phases between the glass phase and the ceramic phase have a great influence on the performance. For composites of glass-ceramic systems, the composition, content, distribution between the phases, softening temperature of the glass, wetting effect between the glass-ceramic phases, and degree of densification of the sintering all affect the final properties.
The embodiment of the invention also provides a preparation method of the low dielectric low-loss LTCC material, which comprises the following steps:
1) Taking a parts of B-Si-Al glass and B parts of CaSiO by mass percent 3 C parts of SiO 2 Batching, wherein a is 40-55%, b is 45-55%, c is 5-10%, and a+b+c=100%;
2) Ball milling and uniformly mixing the ingredients in the step S1, and drying;
3) And pressing the mixture particles, and performing glue discharging and sintering to obtain the low-dielectric low-loss LTCC material.
The raw material components of the B-Si-Al glass in the embodiment of the invention comprise the following components in percentage by mass: 60 to 65 percent of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1-2%Na 2 CO 3 ,2~5%ZnO。
In the step S2, water is used as a solvent, planetary ball milling is adopted, namely, the ingredients are subjected to planetary ball milling for 6-12 hours, and the granularity of the slurry is controlled to D 50 0.5-5 mu m; the binder is a PVA binder.
In the step S3, the glue discharging temperature is 450-500 ℃, and the sintering is carried out in the air atmosphere at 850-880 ℃.
The B-Si-Al glass is prepared by the following method: according to the mass ratio of 60-65% of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1-2%Na 2 CO 3 Preparing 2-5% ZnO, adding zirconia balls and water for ball milling and mixing, and drying; then melting the glass in a corundum mullite crucible at 1550-1600 ℃ for 2 hours to form glass liquid, and quenching the glass liquid by deionized water to obtain glass fragments; grinding again to obtain particle size D 50 B-Si-Al glass powder of 1-5 mu m.
CaSiO 3 The ceramic powder is prepared by the following method: according to CaCO 3 :SiO 2 Is 1:1, preferably adding zirconia balls and water, and mixing by planetary ball milling; drying, crushing, sieving, calcining at 1200-1300 deg.c for 2-4 hr, ball milling to obtain CaSiO with granularity of 0.5-2 microns 3 Ceramic powder.
The flow chart of the preparation method of the embodiment of the invention is shown in fig. 1, and comprises the following steps:
s1, according to 60 to 65 percent of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1-2%Na 2 CO 3 2-5% ZnO is melted into B-Si-Al glass;
s2, according to 40-55 parts of B-Si-Al glass and 45-55 parts of CaSiO 3 Ceramic powder, 5-10 parts of SiO 2 Ceramic powder batching;
s3, ball-milling and mixing the ingredients, D 50 Controlling the granularity to be 0.5-5 mu m, and then drying;
s4, adding an adhesive to granulate, pressing and forming, and then sintering to obtain the low dielectric low-loss LTCC material.
Example 1
A low dielectric low-loss LTCC material and a preparation method thereof are carried out according to the following steps:
1) B-Si-Al glass powder preparation: the following components are mixed: 65% SiO 2 ,25%B 2 O 3 ,5%Al 2 O 3 ,1%Na 2 CO 3 4% ZnO is prepared, is put into a corundum mullite crucible, is melted at 1550 ℃, is kept for 2 hours, is poured into deionized water for quenching, and is ground to 5 mu m;
2) B-Si-Al glass powder preparation: according to CaCO 3 :SiO 2 Is 1:1, adding zirconia balls and water, and mixing through planetary ball milling; drying, crushing, sieving, calcining at 1250 ℃ for 3 hours, and performing planetary ball milling to obtain CaSiO with granularity of 1 mu m 3 Ceramic powder;
3) Weighing 40% of B-Si-Al glass and 55% of CaSiO by mass percent 3 Ceramic materialPowder, 5% SiO 2 The powder is mixed and ball milled for 6 hours by a planet, and the granularity is controlled D 50 Is 2.0 mu m, and then is dried;
4) Granulating with PVA adhesive, pressing to form, discharging adhesive at 450 deg.C, sintering in 850 deg.C air atmosphere to obtain low dielectric low loss LTCC material;
5) The dielectric properties of the cylindrical sintered body were measured by a resonator method, the three-point bending strength of the sintered long-strip sample was measured by a universal mechanical tester, the thermal expansion coefficient of the sintered sample was measured by a thermal expansion coefficient tester, and the performance results are shown in Table 1.
Example 2
A low dielectric low-loss LTCC material and a preparation method thereof are carried out according to the following steps:
1) B-Si-Al glass powder preparation: the following components are mixed: 65% SiO 2 ,25%B 2 O 3 ,5%Al 2 O 3 ,1%Na 2 CO 3 4% ZnO is prepared, is put into a corundum mullite crucible, is melted at 1550 ℃, is kept for 2 hours, is poured into deionized water for quenching, and is ground to 5 mu m;
2) B-Si-Al glass powder preparation: according to CaCO 3 :SiO 2 Is 1:1, adding zirconia balls and water, and mixing through planetary ball milling; drying, crushing, sieving, calcining at 1250 ℃ for 3 hours, and performing planetary ball milling to obtain CaSiO with granularity of 1 mu m 3 Ceramic powder;
3) Weighing 40% of B-Si-Al glass and 50% of CaSiO by mass percent 3 Ceramic powder, 10% SiO 2 The powder is mixed and ball milled for 6 hours by a planet, and the granularity is controlled D 50 1.5 μm, and then drying;
4) Granulating with PVA adhesive, pressing to form, discharging adhesive at 450 deg.C, sintering in 880 deg.C air atmosphere to obtain low dielectric low loss LTCC material;
5) The dielectric properties of the cylindrical sintered body were measured by a resonator method, the three-point bending strength of the sintered long-strip sample was measured by a universal mechanical tester, the thermal expansion coefficient of the sintered sample was measured by a thermal expansion coefficient tester, and the performance results are shown in Table 1.
Example 3
A low dielectric low-loss LTCC material and a preparation method thereof are carried out according to the following steps:
1) B-Si-Al glass powder preparation: the following components are mixed: 65% SiO 2 ,25%B 2 O 3 ,5%Al 2 O 3 ,1%Na 2 CO 3 4% ZnO is prepared, is put into a corundum mullite crucible, is melted at 1550 ℃, is kept for 2 hours, is poured into deionized water for quenching, and is ground to 5 mu m;
2) B-Si-Al glass powder preparation: according to CaCO 3 :SiO 2 Is 1:1, adding zirconia balls and water, and mixing through planetary ball milling; drying, crushing, sieving, calcining at 1250 ℃ for 3 hours, and performing planetary ball milling to obtain CaSiO with granularity of 1 mu m 3 Ceramic powder;
3) Weighing 45% of B-Si-Al glass and 50% of CaSiO by mass percent 3 Ceramic powder, 5% SiO 2 The powder is mixed and ball milled for 6 hours by a planet, and the granularity is controlled D 50 1.5 μm, and then drying;
4) Granulating with PVA adhesive, pressing to form, discharging adhesive at 450 deg.C, sintering in 880 deg.C air atmosphere to obtain low dielectric low loss LTCC material;
5) The dielectric properties of the cylindrical sintered body were measured by a resonator method, the three-point bending strength of the sintered long-strip sample was measured by a universal mechanical tester, the thermal expansion coefficient of the sintered sample was measured by a thermal expansion coefficient tester, and the performance results are shown in Table 1.
The cross-sectional microscopic morphology diagram of the sample of the low-dielectric low-loss LTCC material prepared in the embodiment 3 after sintering at 880 ℃ is shown in fig. 2, and as can be seen from fig. 2, the prepared low-dielectric low-loss LTCC material has good compactness. Compactness is also a key property of the LTCC material, and if the compactness is deviated, holes are more, the overall extrinsic loss is increased, and the dielectric property of the LTCC material is affected. In addition, the lower the compactibility, the lower the strength of the composite material. Example 3 shows good compactibility, which is also one of the reasons for its excellent dielectric and strength properties.
Example 4
A low dielectric low-loss LTCC material and a preparation method thereof are carried out according to the following steps:
1) B-Si-Al glass powder preparation: the following components are mixed: 60% SiO 2 ,25%B 2 O 3 ,10%Al 2 O 3 ,2%Na 2 CO 3 3% ZnO is prepared, is put into a corundum mullite crucible, is melted at 1550 ℃, is kept for 2 hours, is poured into deionized water for quenching, and is ground to 5 mu m;
2) B-Si-Al glass powder preparation: according to CaCO 3 :SiO 2 Is 1:1, adding zirconia balls and water, and mixing through planetary ball milling; drying, crushing, sieving, calcining at 1300 ℃ for 2 hours, and performing planetary ball milling to obtain CaSiO with granularity of 1.5 mu m 3 Ceramic powder;
3) Weighing 45% of B-Si-Al glass and 45% of CaSiO by mass percent 3 Ceramic powder, 10% SiO 2 The powder is mixed and ball milled for 3 hours by a planet, and the granularity is controlled to D 50 Is 2 mu m, and then is dried;
4) Adding PVA adhesive for granulating, pressing, discharging adhesive at 450 deg.C, and sintering in 880 deg.C air atmosphere to obtain low dielectric low loss LTCC material.
5) The dielectric properties of the cylindrical sintered body were measured by a resonator method, the three-point bending strength of the sintered long-strip sample was measured by a universal mechanical tester, the thermal expansion coefficient of the sintered sample was measured by a thermal expansion coefficient tester, and the performance results are shown in Table 1.
Example 5
A low dielectric low-loss LTCC material and a preparation method thereof are carried out according to the following steps:
1) B-Si-Al glass powder preparation: the following components are mixed: 60% SiO 2 ,25%B 2 O 3 ,10%Al 2 O 3 ,2%Na 2 CO 3 3% ZnO is prepared, is put into a corundum mullite crucible, is melted at 1550 ℃, is kept for 2 hours, is poured into deionized water for quenching, and is ground to 5 mu m;
2) B-Si-Al glass powder preparation: according to CaCO 3 :SiO 2 Is 1:1, adding zirconia balls and water, and mixing through planetary ball milling; drying, crushing, sieving, calcining at 1300 ℃ for 2 hours, and performing planetary ball milling to obtain CaSiO with granularity of 1.5 mu m 3 Ceramic powder;
3) Weighing 50% of B-Si-Al glass and 45% of CaSiO by mass percent 3 Ceramic powder, 5% SiO 2 The powder is mixed and ball milled for 3 hours by a planet, and the granularity is controlled to D 50 Is 2 mu m, and then is dried;
4) Granulating with PVA adhesive, pressing to form, discharging adhesive at 450 deg.C, sintering in 880 deg.C air atmosphere to obtain low dielectric low loss LTCC material;
5) The dielectric properties of the cylindrical sintered body were measured by a resonator method, the three-point bending strength of the sintered long-strip sample was measured by a universal mechanical tester, the thermal expansion coefficient of the sintered sample was measured by a thermal expansion coefficient tester, and the performance results are shown in Table 1.
Comparative example 1
Comparative example 1 differs from example 1 in the ratio of glass to ceramic, comparative example 1 weighed 35% of B-Si-Al glass, 60% of CaSiO in mass fraction 3 Ceramic powder, 5% SiO 2 The powder is mixed and ball milled for 3 hours by a planet, and the granularity is controlled to D 50 And (3) drying the mixture to be 2.0 mu m, adding PVA adhesive for granulating, pressing and forming, discharging glue at 450 ℃, and sintering in an air atmosphere at 850 ℃ to obtain a sintered sample. Fig. 3 is a microscopic morphology of the cross section of the sintered sample of comparative example 1, and it can be seen that the cross section of comparative example 1 has more holes and has poor compactness. As can be seen from the results of the properties shown in Table 1, the poor sintering densification results in a sharp increase in extrinsic loss, deterioration in dielectric properties, and a significant decrease in flexural strength.
Comparative example 2
Comparative example 2 differs from example 1 in that the B-Si-Al glass and CaSiO 3 The proportion of the ceramic powder is calculated according to the mass fraction of comparative example 2, 60 percent of B-Si-Al glass and 35 percent of CaSiO are weighed 3 Ceramic powder, 5% SiO 2 The powder is mixed and passes through the planetary ballGrinding for 3h, controlling granularity D 50 And (3) drying the mixture to be 2.0 mu m, adding PVA for granulating, pressing and forming, discharging glue at 450 ℃, and sintering in an air atmosphere at 850 ℃ to obtain a sintered sample. As can be seen from the performance results of Table 1, when the B-Si-Al glass is too high, the dielectric loss increases to 2.8 thousandths, although the prepared material still has higher flexural strength and lower dielectric constant, because the B-Si-Al glass has a loss greater than that of CaSiO 3 The loss of the ceramic powder is high, and the increase of the content of the B-Si-Al glass can lead to the increase of the overall loss. In addition, if the B-Si-Al glass component in the composite material is too high, too much liquid phase may be formed during sintering, and the "overburning" phenomenon may occur, and problems such as deterioration of compactibility may occur, and further, performance may be degraded.
TABLE 1
Wherein @15GHz represents the operating frequency of the processor core, the above table 1 gives the material components, dielectric properties, flexural strength, thermal expansion coefficients and other properties of examples 1-5 and comparative examples 1-2, and as can be seen from comparison of the results in table 1, examples 1-5 of the present invention can be sintered compactly in an air atmosphere at 850-880 ℃ and can realize low-temperature cofiring with Ag paste; the dielectric constant is 5.2-5.7, the dielectric loss is less than 2 thousandths, and the requirements of high frequency and high speed of the device are met; the bending strength is more than 170MPa, and can be applied to devices such as filters, antennas, substrates and the like in the LTCC process.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several equivalent substitutions and obvious modifications can be made without departing from the spirit of the invention, and the same should be considered to be within the scope of the invention.
Claims (8)
1. A low dielectric low loss LTCC material is characterized by using glassThe ceramic composite system material comprises, by mass, a parts of B-Si-Al glass and B parts of CaSiO 3 Ceramic powder, c parts of SiO 2 Powder, wherein a is 40-55%, b is 45-55%, c is 5-10%, and a+b+c=100%;
the raw material components of the B-Si-Al glass are as follows in mass percent: comprises 60 to 65 percent of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1~2%Na 2 CO 3 ,2~5%ZnO。
2. The low dielectric low loss LTCC material of claim 1, wherein the SiO 2 The powder can be crystalline SiO 2 Or amorphous SiO 2 The purity is more than 99.5 percent, and the granularity is 0.5 to 5 mu m.
3. The preparation method of the low dielectric low-loss LTCC material is characterized by comprising the following steps of:
1) Taking a parts of B-Si-Al glass and B parts of CaSiO by mass percent 3 Ceramic powder, c parts of SiO 2 Powder is mixed, wherein a is 40-55%, b is 45-55%, c is 5-10%, and a+b+c=100%;
2) Ball milling the ingredients in the step 1), uniformly mixing and drying;
3) Adding adhesive for granulating, pressing and forming, and then sintering in an air atmosphere at 850-880 ℃ to obtain a low dielectric low loss LTCC material;
in the step 1), the raw material components of the B-Si-Al glass are calculated according to mass percent: comprises 60 to 65 percent of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1~2%Na 2 CO 3 ,2~5%ZnO。
4. The method for preparing low dielectric loss LTCC material according to claim 3, wherein in the step 2), water is used as solvent, the ingredients are ball milled for 6-12 hours by a planet, and the size of the slurry is controlled to D 50 0.5-5 mu m; the adhesive in the step 3) is a polyvinyl alcohol PVA adhesive.
5. The method for preparing low dielectric loss LTCC material of claim 3 wherein in step 3), the step of removing the adhesive is performed after the compression molding and before the sintering.
6. The method for preparing low dielectric low loss LTCC material of claim 5, wherein the temperature of the glue discharging operation is 450-500 ℃.
7. The method for preparing a low dielectric low loss LTCC material according to any of claims 3-6, wherein the B-Si-Al glass is prepared by: according to the mass ratio of 60-65% of SiO 2 ,20~25%B 2 O 3 ,5~10%Al 2 O 3 ,1~2%Na 2 CO 3 Preparing 2-5% ZnO, adding zirconia balls and water for ball milling and mixing, and drying; then melting the glass in a corundum mullite crucible at 1550-1600 ℃ for 2 hours to form glass liquid, and quenching the glass liquid by deionized water to obtain glass fragments; grinding again to obtain particle size D 50 B-Si-Al glass powder of 1-5 mu m.
8. The method for preparing a low dielectric low loss LTCC material according to any of claims 3 to 6, wherein the CaSiO 3 The ceramic powder is prepared by the following preparation method: according to CaCO 3 :SiO 2 Is 1:1, adding zirconia balls and water, and mixing through planetary ball milling; drying, crushing, sieving, calcining at 1200-1300 deg.c for 2-4 hr, ball milling to obtain CaSiO with granularity of 0.5-2 microns 3 Ceramic powder.
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