CN116835979B - High-dielectric constant low-temperature co-fired ceramic powder suitable for LTCC filter and preparation method of ceramic powder - Google Patents
High-dielectric constant low-temperature co-fired ceramic powder suitable for LTCC filter and preparation method of ceramic powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 127
- 239000000919 ceramic Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 37
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims description 69
- 239000004677 Nylon Substances 0.000 claims description 23
- 229920001778 nylon Polymers 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- 239000012634 fragment Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 238000007580 dry-mixing Methods 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims 2
- 239000011159 matrix material Substances 0.000 abstract description 6
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 238000009766 low-temperature sintering Methods 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 46
- 239000000463 material Substances 0.000 description 9
- 239000002609 medium Substances 0.000 description 6
- 239000011324 bead Substances 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 239000002612 dispersion medium Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses a high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filter and a preparation method thereof, belonging to the technical field of electronic ceramic materials, and comprising 15.0 to 17.0 weight percent of B 2 O 3 ‑CaO‑SiO 2 ‑MgO‑Al 2 O 3 (BCSMA for short) glass powder, 5.0wt% to 7.0wt% BaZn 2 Ti 4 O 11 Powder and 76.0wt% to 80.0wt% of BaTi 0.89 V 0.07 Zr 0.02 O 3 Powder of BaTi 0.89 V 0.07 Zr 0.02 O 3 The powder is used as a matrix material of low-temperature co-fired ceramic, the BCSMA glass powder is used as a sintering aid, and the BaZn is used as a sintering aid 2 Ti 4 O 11 The powder is used as a regulator phase for regulating the temperature coefficient of the resonant frequency, so that the low-temperature sintering of the low-temperature co-fired ceramic powder is realized, and the low-temperature sintered compact ceramic powder has excellent dielectric property.
Description
Technical Field
The invention belongs to the technical field of electronic ceramic materials, and particularly relates to high-dielectric constant low-temperature co-fired ceramic powder suitable for an LTCC filter and a preparation method thereof.
Background
Low temperature co-fired ceramic technology (LTCC) is a attractive multidisciplinary cross-component technology that has emerged in recent years. With the application of 5G technology, the demands for LTCC microwave passive components, millimeter wave LTCC filters and millimeter wave integrated antennas will be increasing.
The dimensions of the LTCC filter and the dielectric constant of the LTCC material are closely related. For the purpose of miniaturizing the LTCC filter, it is required that the LTCC material has a large dielectric constant. The relevant physical formula is:
where D is the size of the resonator in the filter (in general, the resonance is a cylinder, so here D may represent the diameter of the resonator), f 0 The resonant frequency of the resonator, c is the speed of light in vacuum. It can be seen that the size and dielectric constant of the filter vary inversely. Thus, the dielectric constant ε of LTCC material is improved r It would be advantageous to reduce the size of LTCC filters.
In order to increase the dielectric constant of LTCC materials, a high-dielectric-constant dielectric ceramic material is required as a matrix material. Currently, the relative dielectric constant of the relatively mature medium-high dielectric constant LTCC material is basically smaller than 60. To maintain LTCC material with high dielectric constant (ε) r 70) and a low sintering temperature, the conventional researches have been focused on the use of a Li-based dielectric ceramic matrix as a subject, but Li-based dielectric ceramics are liable to volatilize Li during sintering, and the dielectric loss of Li-based dielectric ceramics is relatively large, which is not advantageous for commercialization.
Disclosure of Invention
The invention aims to provide high-dielectric constant low-temperature co-fired ceramic powder suitable for an LTCC filter and a preparation method thereof, so as to solve the problem of low relative dielectric constant of a high-dielectric constant LTCC material in the prior art.
The aim of the invention can be achieved by the following technical scheme:
a high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filter comprises 15.0wt% -17.0wt% B 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 Glass powder, 5.0wt% to 7.0wt% of BaZn 2 Ti 4 O 11 Powder and 76.0wt% to 80.0wt% of BaTi 0.89 V 0.07 Zr 0.02 O 3 And (3) powder.
Further, the relative dielectric constant of the high dielectric constant low temperature co-fired ceramic powder after sinteringNumber epsilon r 78.7-81.2, a quality factor value of Qxf & gt 5200, and a resonant frequency temperature coefficient tau f -4.6 ppm/. Degree.C.to +5.5 ppm/. Degree.C.
Further, the BaTi 0.89 V 0.07 Zr 0.02 O 3 Powder prepared by the steps of:
according to BaTi 0.89 V 0.07 Zr 0.02 O 3 Stoichiometric ratio BaCO weighing 3 、TiO 2 、V 2 O 5 、ZrO 2 Then absolute ethyl alcohol is added as a dispersion medium, zirconia balls are used as a ball milling medium, ball milling is carried out in a nylon tank, and the slurry is calcined for 2 hours at 1150 ℃ after drying, thus obtaining BaTi 0.89 V 0.07 Zr 0.02 O 3 And (3) powder.
Further, the B is 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 (hereinafter referred to as BCSMA) glass powder, prepared by:
weighing the following raw materials in percentage by weight:
H 3 BO 3 ：67.2wt％；
CaCO 3 ：22.5wt％；
SiO 2 ：5.6wt％；
MgO：3.2wt％；
Al 2 O 3 ：1.5wt％；
will H 3 BO 3 、CaCO 3 、SiO 2 、MgO、Al 2 O 3 Sampling according to the proportion, dry-mixing, and pouring the mixture into a Pt crucible; placing the Pt crucible filled with the mixture into a lifting furnace, and keeping the temperature in a temperature field of 1500 ℃ for 1h to obtain glass liquid; and clamping the Pt crucible out, pouring the glass liquid into water for quenching to obtain glass fragments, and drying, crushing, ball milling and drying the glass fragments by a roller machine to obtain the BCSMA glass powder.
Further, baZn 2 Ti 4 O 11 Powder prepared by the steps of:
according to BaZn 2 Ti 4 O 11 Chemical chemistryThe metering ratio is BaCO 3 、ZnO、TiO 2 After weighing, pouring the mixture into a nylon ball milling tank, and performing ball milling by taking absolute ethyl alcohol as a dispersion medium, wherein the ball milling medium is zirconia balls; drying, calcining at 1050 deg.c for 2 hr to obtain BaZn 2 Ti 4 O 11 And (3) powder.
A preparation method of high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filter comprises the following steps:
weighing B according to the formula 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 Glass powder and BaZn 2 Ti 4 O 11 Powder and BaTi 0.89 V 0.07 Zr 0.02 O 3 And (3) weighing the powder, placing the powder into a nylon ball milling tank, adding deionized water, taking zirconia balls as ball milling media, performing ball milling in the nylon ball milling tank, then sending the obtained slurry into a circulating stirring mill for further ball milling, stopping ball milling, and drying to obtain the low-temperature cofired ceramic powder.
Further, ball milling is carried out in a nylon ball milling tank until the granularity D50 is less than or equal to 7 mu m.
Further, the circulating stirring mill is further ball-milled until the granularity D50 is less than or equal to 1.3 mu m.
The invention has the beneficial effects that:
the invention provides a novel dielectric ceramic powder BaTi 0.89 V 0.07 Zr 0.02 O 3 Powder, using the powder as a matrix material of low-temperature cofiring ceramic, and adding B 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 BaZn is used as sintering aid 2 Ti 4 O 11 The powder is used as a regulator phase for regulating the temperature coefficient of the resonant frequency, so that not only is the low-temperature sintering of the low-temperature co-fired ceramic powder realized, but also the low-temperature co-fired ceramic powder has excellent dielectric property after being sintered compactly.
The dielectric constant of the invention is higher, and can meet the miniaturization requirement of the LTCC filter; the dielectric loss is small, and the use requirement of a 5G frequency band can be met; the temperature coefficient of the resonance frequency is about 0 and can be adjusted in positive and negative values, so that the requirement of stable resonance frequency can be met.
The low-temperature co-fired ceramic powder does not contain Pb and other heavy metal elements, and belongs to environment-friendly materials. The glass powder in the low-temperature co-fired ceramic powder is B 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 The system and the specific composition point are selected, and the component glass has the characteristics of low softening point (Tg temperature is about 580 ℃), strong water resistance and no water absorption after ball milling, so that the sintering densification of the low-temperature cofired ceramic powder of the system is ensured between 940 and 950 ℃.
In the past, li-containing phase powder is often used as a matrix material of high dielectric constant LTCC powder, but Li-containing materials often have disadvantages such as water absorption during ball milling and Li volatilization during sintering. Therefore, the invention adopts a brand new phase BaTi 0.89 V 0.07 Zr 0.02 O 3 The powder is used as a matrix material of the LTCC powder with high dielectric constant. The BaTi is 0.89 V 0.07 Zr 0.02 O 3 Powder and BCSMA glass powder and BaZn 2 Ti 4 O 11 After the powder is sintered after being sintered at a low temperature, the relative dielectric constant epsilon of the sintered body r The dielectric loss and the temperature coefficient performance of the resonant frequency are excellent and can meet the requirements of the LTCC filter with high dielectric constant between 78.7 and 81.2.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a BCSMA glass powder, which is prepared by the following steps:
weighing the following raw materials in percentage by weight:
H 3 BO 3 ：67.2wt％；
CaCO 3 ：22.5wt％；
SiO 2 ：5.6wt％；
MgO：3.2wt％；
Al 2 O 3 ：1.5wt％；
will H 3 BO 3 、CaCO 3 、SiO 2 、MgO、Al 2 O 3 Sampling according to the proportion, dry-mixing, and pouring the mixture into a Pt crucible; placing the Pt crucible filled with the mixture into a lifting furnace, and keeping the temperature in a temperature field of 1500 ℃ for 1h to obtain glass liquid; and clamping the Pt crucible out, pouring the glass liquid into water for quenching to obtain glass fragments, and drying, crushing, ball milling and drying the glass fragments by a roller machine to obtain the BCSMA glass powder.
Example 2
The present example provides a BaZn 2 Ti 4 O 11 Powder prepared by the steps of:
according to BaZn 2 Ti 4 O 11 Stoichiometric ratio will BaCO 3 、ZnO、TiO 2 After weighing, pouring the mixture into a nylon ball milling tank, and performing ball milling by taking absolute ethyl alcohol as a dispersion medium, wherein the ball milling medium is zirconia balls. Drying, calcining at 1050 deg.c for 2 hr to obtain BaZn 2 Ti 4 O 11 And (3) powder.
Example 3
The present embodiment provides a BaTi 0.89 V 0.07 Zr 0.02 O 3 Powder prepared by the steps of:
according to BaTi 0.89 V 0.07 Zr 0.02 O 3 Stoichiometric ratio BaCO weighing 3 、TiO 2 、V 2 O 5 、ZrO 2 Then absolute ethyl alcohol is added as a dispersion medium, zirconia balls are used as a ball milling medium, ball milling is carried out in a nylon tank, and the slurry is calcined for 2 hours at 1150 ℃ after drying, thus obtaining BaTi 0.89 V 0.07 Zr 0.02 O 3 And (3) powder.
Example 4
The embodiment provides a high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filters, which is prepared by the following steps:
15.0wt% of BCSMA glass powder prepared in example 1 and BaZn prepared in example 2 are weighed according to weight percentage 2 Ti 4 O 11 7.0wt% of powder, baTi prepared in example 3 0.89 V 0.07 Zr 0.02 O 3 And (3) weighing 78.0wt% of powder, placing the powder into a nylon ball milling tank, adding deionized water, performing ball milling in the nylon ball milling tank by taking zirconia balls as ball milling media, sending the obtained slurry into a circulating stirring mill (the lining is made of zirconia, the grinding beads are zirconia balls with the diameter of 1 mm) for further ball milling after the granularity D50 reaches 7 mu m, stopping ball milling when the granularity D50 reaches 1.3 mu m, and drying the slurry to obtain the low-temperature co-fired ceramic powder.
Granulating and tabletting the ceramic powder, and sintering at 940 ℃ for 3 hours to compact the ceramic. Its relative dielectric constant epsilon r 79.1, Q×f value 5235, and resonant frequency temperature coefficient of-0.1 ppm/. Degree.C.
Example 5
The embodiment provides a high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filters, which is prepared by the following steps:
15.0wt% of BCSMA glass powder prepared in example 1 and BaZn prepared in example 2 are weighed according to weight percentage 2 Ti 4 O 11 5.0wt% of powder, baTi prepared in example 3 0.89 V 0.07 Zr 0.02 O 3 80.0wt% of powder, weighing each powder, placing the powder into a nylon ball milling tank, adding a proper amount of deionized water, taking zirconia balls as ball milling media, performing ball milling in the nylon ball milling tank, after the granularity D50 reaches 7 mu m, sending the obtained slurry into a circulating stirring mill (the lining is made of zirconia, the grinding beads are zirconia balls with the diameter of 1 mm) for further ball milling, after the granularity D50 reaches 1.3 mu m, stopping ball milling, and drying the slurry to obtain the low-temperature co-fired ceramic powder.
Granulating, tabletting, sintering at 950 deg.C for 3 hr, and sinteringAnd (5) sealing. Its relative dielectric constant epsilon r The Q×f value was 5210 at 81.2, and the temperature coefficient of resonance frequency was +5.5 ppm/. Degree.C.
Example 6
The embodiment provides a high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filters, which is prepared by the following steps:
17.0wt% of BCSMA glass powder prepared in example 1 and BaZn prepared in example 2 are weighed according to weight percentage 2 Ti 4 O 11 7.0wt% of powder, baTi prepared in example 3 0.89 V 0.07 Zr 0.02 O 3 And (3) weighing 76.0wt% of powder, placing the powder into a nylon ball milling tank, adding a proper amount of deionized water, performing ball milling in the nylon ball milling tank by taking zirconia balls as a ball milling medium, sending the obtained slurry into a circulating stirring mill (the lining is made of zirconia, the grinding beads are zirconia balls with the diameter of 1 mm) for further ball milling after the granularity D50 reaches 7 mu m, stopping ball milling when the granularity D50 reaches 1.3 mu m, and drying the slurry to obtain the low-temperature co-fired ceramic powder.
Granulating and tabletting the ceramic powder, and sintering at 940 ℃ for 3 hours to compact the ceramic. Its relative dielectric constant epsilon r The Q×f value was 5336 and the temperature coefficient of resonance frequency was-4.6 ppm/. Degree.C.at 78.7.
Example 7
The embodiment provides a high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filter, which is prepared by the following steps
17.0wt% of BCSMA glass powder prepared in example 1 and BaZn prepared in example 2 are weighed according to weight percentage 2 Ti 4 O 11 5.0wt% of powder, baTi prepared in example 3 0.89 V 0.07 Zr 0.02 O 3 78.0wt% of powder, weighing each powder, placing the powder into a nylon ball milling tank, adding a proper amount of deionized water, taking zirconia balls as ball milling media, performing ball milling in the nylon ball milling tank, after the granularity D50 reaches 7 mu m, sending the obtained slurry into a circulating stirring mill (the lining is made of zirconia, the milling balls are zirconia balls with the diameter of 1 mm) for further ball milling, and stopping when the granularity D50 reaches 1.3 mu mStopping ball milling, and drying the slurry to obtain the low-temperature co-fired ceramic powder.
Granulating and tabletting the ceramic powder, and sintering at 950 ℃ for 3 hours to compact the ceramic. Its relative dielectric constant epsilon r The Q×f value was 5325 at 78.9, and the temperature coefficient of resonance frequency was +1.2 ppm/. Degree.C.
Example 8
The embodiment provides a high dielectric constant low temperature co-fired ceramic powder suitable for LTCC filters, which is prepared by the following steps:
16.0wt% of BCSMA glass powder prepared in example 1 and BaZn prepared in example 2 are weighed according to weight percentage 2 Ti 4 O 11 6.0wt% of powder, baTi prepared in example 3 0.89 V 0.07 Zr 0.02 O 3 And (3) weighing 78.0wt% of powder, placing the powder into a nylon ball milling tank, adding a proper amount of deionized water, performing ball milling in the nylon ball milling tank by taking zirconia balls as a ball milling medium, sending the obtained slurry into a circulating stirring mill (the lining is made of zirconia, the grinding beads are zirconia balls with the diameter of 1 mm) for further ball milling after the granularity D50 reaches 7 mu m, stopping ball milling when the granularity D50 reaches 1.3 mu m, and drying the slurry to obtain the low-temperature co-fired ceramic powder.
Granulating and tabletting the ceramic powder, and sintering at 950 ℃ for 3 hours to compact the ceramic. Its relative dielectric constant epsilon r The Q×f value was 5217, and the temperature coefficient of resonance frequency was +1.2 ppm/. Degree.C.
Comparative example 1
15.0wt% of BCSMA glass powder prepared in example 1 and BaZn prepared in example 2 are weighed according to weight percentage 2 Ti 4 O 11 5.0wt% of powder and BaTiO 3 80.0wt% of powder, weighing each powder, placing the powder into a nylon ball milling tank, adding a proper amount of deionized water, taking zirconia balls as ball milling media, performing ball milling in the nylon ball milling tank, after the granularity D50 reaches 7 mu m, sending the obtained slurry into a circulating stirring mill (the lining is made of zirconia, the grinding beads are zirconia balls with the diameter of 1 mm) for further ball milling, after the granularity D50 reaches 1.3 mu m, stopping ball milling, drying the slurry, and obtainingTo low temperature co-firing ceramic powder.
Granulating and tabletting the ceramic powder, and sintering at 950 ℃ for 3 hours to compact the ceramic. The relative dielectric constant εr was 57.8, the Q×f value was 4830, and the temperature coefficient of resonance frequency was +53.9 ppm/. Degree.C.
In this comparative example, compared with example 5, conventional BaTiO was used 3 The powder is BCSMA glass powder and BaZn 2 Ti 4 O 11 Powder, baTiO 3 The dielectric constant of the mixed powder of the powder can only reach 57.8 after sintering.
Inventive examples 4 to 5 will be described as B 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 BaZn is used as sintering aid 2 Ti 4 O 11 The powder is used as a regulator phase for regulating the temperature coefficient of the resonant frequency, so that not only is the low-temperature sintering of the low-temperature co-fired ceramic powder realized, but also the low-temperature co-fired ceramic powder has excellent dielectric property after being sintered compactly.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. High dielectric constant suitable for LTCC filterThe low temperature co-fired ceramic powder is characterized by comprising 15.0 to 17.0 weight percent of B 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 Glass powder, 5.0wt% to 7.0wt% of BaZn 2 Ti 4 O 11 Powder and 76.0wt% to 80.0wt% of BaTi 0.89 V 0.07 Zr 0.02 O 3 And (3) powder.
2. The high-dielectric constant low-temperature co-fired ceramic powder for LTCC filter according to claim 1, wherein the high-dielectric constant low-temperature co-fired ceramic powder has a relative dielectric constant ε after sintering r 78.7-81.2, a quality factor value of Qxf & gt 5200, and a resonant frequency temperature coefficient tau f -4.6 ppm/. Degree.C.to +5.5 ppm/. Degree.C.
3. The high dielectric constant low temperature co-fired ceramic powder for LTCC filter according to claim 1, wherein the BaTi 0.89 V 0.07 Zr 0.02 O 3 Powder prepared by the steps of:
according to BaTi 0.89 V 0.07 Zr 0.02 O 3 Stoichiometric ratio BaCO weighing 3 、TiO 2 、V 2 O 5 、ZrO 2 Adding absolute ethyl alcohol, ball milling in nylon pot, drying after ball milling, calcining at 1150 deg.c for 2 hr to obtain BaTi 0.89 V 0.07 Zr 0.02 O 3 And (3) powder.
4. The high dielectric constant low temperature co-fired ceramic powder for LTCC filter according to claim 1, wherein the B 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 Glass powder prepared by the following steps:
weighing the following raw materials in percentage by weight: h 3 BO 3 ：67.2wt％、CaCO 3 ：22.5wt％、SiO 2 :5.6wt%, mgO:3.2wt% and Al 2 O 3 ：1.5wt％；Dry-mixing, and pouring the mixture into a Pt crucible; placing the Pt crucible filled with the mixture into a lifting furnace, and keeping the temperature in a temperature field of 1500 ℃ for 1h to obtain glass liquid; pouring the glass liquid into water for quenching to obtain glass fragments, drying the glass fragments, crushing the glass fragments by a pair of rollers, ball-milling the glass fragments, and drying the glass fragments to obtain B 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 Glass powder.
5. The high dielectric constant low temperature co-fired ceramic powder for LTCC filter according to claim 1, wherein BaZn 2 Ti 4 O 11 Powder prepared by the steps of:
according to BaZn 2 Ti 4 O 11 Stoichiometric ratio will BaCO 3 、ZnO、TiO 2 Weighing, adding absolute ethyl alcohol, ball milling in a nylon ball milling tank, drying, calcining at 1050 ℃, and preserving heat for 2h to obtain BaZn 2 Ti 4 O 11 And (3) powder.
6. The method for preparing the high dielectric constant low temperature co-fired ceramic powder suitable for the LTCC filter according to claim 1, comprising the following steps:
weighing B according to the formula 2 O 3 -CaO-SiO 2 -MgO-Al 2 O 3 Glass powder and BaZn 2 Ti 4 O 11 Powder and BaTi 0.89 V 0.07 Zr 0.02 O 3 Placing the powder in a nylon ball milling tank, adding deionized water for ball milling, then sending the obtained slurry into a circulating stirring mill for further ball milling, stopping ball milling, and drying to obtain the low-temperature co-fired ceramic powder.
7. The method for preparing the high-dielectric constant low-temperature co-fired ceramic powder for the LTCC filter according to claim 6, wherein the ball milling is carried out in a nylon ball milling tank until the particle size D50 is less than or equal to 7 μm.
8. The method for preparing high dielectric constant low temperature co-fired ceramic powder for LTCC filter according to claim 6, wherein the particle size D50 is less than or equal to 1.3 μm by a circulating stirring mill.
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