CN105294104B - Low-loss dielectric is adjustable intermediary's microwave dielectric ceramic materials and preparation method thereof - Google Patents
Low-loss dielectric is adjustable intermediary's microwave dielectric ceramic materials and preparation method thereof Download PDFInfo
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Abstract
Present invention relates particularly to adjustable intermediary's microwave dielectric ceramic materials of a kind of low-loss dielectric and preparation method thereof.Chemical composition is：aCa(ZrxTi1‑x)O3+(1‑a)La1+yAlO3+ zwt%Al2O3, wherein 0.30≤a≤0.35,0≤x≤0.1,0≤y≤0.01,0≤z≤1.The present invention is a kind of alternative CaTiO3‑NdAlO3It is the inexpensive CaTiO of ceramics3‑LaAlO3Series microwave dielectric ceramic, significantly reduce production cost, it is a kind of with low-loss dielectric tunable characteristic and suitable for the inexpensive microwave dielectric ceramic materials of the microwave devices such as dielectric resonator, wave filter and duplexer, dielectric constant is adjustable, Q × f height and temperature coefficient of resonance frequency τfExcellent, the present invention also provides its preparation method, and low in raw material price, process route are simple and easy.
Description
Technical field
Present invention relates particularly to adjustable intermediary's microwave dielectric ceramic materials of a kind of low-loss dielectric and preparation method thereof.
Background technology
With the rapid propulsion of developing rapidly for modern communication technology, especially 4G, 5G network, miniaturization, it is integrated and
Cost degradation turns into mobile communication and the developing direction of mobile terminal.Realize the miniaturization of communication equipment, high stability and cheap
Approach be the integrated of microwave circuit.Traditional Metal cavity and metal waveguide volume and weight are excessive, limit microwave
The development of integrated circuit, need to develop a series of be suitable in microwave range with high-performance, highly reliable working characteristics for this
Electronically materials and component.Medium dielectric constant, high-quality factor microwave medium ceramic exactly develop rapidly in this context
That gets up is adapted to the optimal dielectric substance of this requirement, and it has low lossy microwave, higher dielectric constant and frequency temperature
Coefficient is small to wait Comprehensive Characteristics, is solution with the wave filter of its making has small volume, in light weight, message transmission rate is high etc. advantage
Certainly current LTE network builds the critical material of frequency spectrum resource bottleneck problem.
At present, the microwave-medium ceramics of Medium dielectric constant, high quality factor are mainly with BaTi4O9、Ba2Ti9O20With
(Zr,Sn)TiO4And MTiO3-LnAlO3(M:Sr,Ca；Ln:La, Nd, Sm) etc. for base microwave dielectric material based on.BaTi4O9、
Ba2Ti9O20(Zr, Sn) TiO4Research is more early, and studies to obtain very system, but these ceramic dielectric constants are relatively low (generally
εr≤ 40), it is unfavorable for the trend of microwave circuit miniaturization.In MTiO3-LnAlO3In system, CaTiO3-NdAlO3Microwave-medium is made pottery
Porcelain is got most of the attention due to the adjustability with excellent microwave dielectric property and perovskite structure.Britain, Russia, Japan
Scholar Deng country researchs and develops performance and reaches ε in successionrFor 43~48, Q × f >=40000GHz, τf≈ 0ppm/'s DEG C
CaTiO3-NdAlO3System microwave-medium ceramics, but at home there is not yet the based material reaches the property of external product in application aspect
Energy index, Q × f values of home products are far below external product, only in 35000GHz or so.Domestic industry production and application
CaTiO3-NdAlO3Series ceramic is mainly that synthetic ceramic powders are bought from Japan, had not only spent a large amount of foreign exchanges but also had been unfavorable for
Proprietary technology progress.In addition, rare earth oxide Nd2O3The costliness of raw material, price is for CaTiO3-NdAlO3Microwave-medium ceramics
Commercial applications promote be a very big limiting factor.Therefore, a kind of alternative CaTiO is obtained3-NdAlO3Ceramics and
It is easy to the inexpensive microwave-medium ceramics of mass production, not only with important social benefit but also with significant economic profit
Benefit.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of adjustable intermediary's microwave-medium pottery of low-loss dielectric
Ceramic material, it is a kind of alternative CaTiO3-NdAlO3It is the inexpensive CaTiO of ceramics3-LaAlO3Series microwave dielectric ceramic, significantly
Production cost is reduced, there is low-loss dielectric tunable characteristic, dielectric constant is adjustable, Q × f height and temperature coefficient of resonance frequency τf
Excellent, the present invention also provides its preparation method.
The adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric of the present invention, chemical composition are：aCa
(ZrxTi1-x)O3+(1-a)La1+yAlO3+ zwt%Al2O3, wherein 0.30≤a≤0.35,0≤x≤0.1,0≤y≤0.01,0≤
z≤1。
Wherein：
Zwt% in chemical composition is Al2O3Account for (aCa (ZrxTi1-x)O3+(1-a)La1+yAlO3) mass fraction.
As a preferred embodiment, 0.30≤a≤0.35,0<X≤0.1,0<Y≤0.01,0<Z≤1, such a chemical composition it is micro-
Ripple medium ceramic material εr=43~48, Q × f >=38500GHz, temperature coefficient of resonance frequency τfIt is excellent, it is that a kind of low-loss is situated between
Electric adjustable intermediary's microwave dielectric ceramic materials.
As a preferred embodiment, a=0.31,0≤x≤0.06,0≤y≤0.005,0≤z≤0.6.
As a preferred embodiment, a=0.31,0<X≤0.06,0<Y≤0.005,0<Z≤0.6, the microwave of such a chemical composition
Medium ceramic material εr=45~46, Q × f >=43500GHz, temperature coefficient of resonance frequency τfIt is excellent.
As a preferred embodiment, a=0.31, x=0.02, y=0.03,0.15<Z≤0.5, the microwave of such a chemical composition are situated between
Ceramics εr=45~46, Q × f >=45000GHz, temperature coefficient of resonance frequency τfIt is excellent.
The preparation method of the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric of the present invention, including following step
Suddenly：
(1) with CaCO3、ZrO2、TiO2、La2O3、Al2O3For raw material, all raw materials are put into ball milling in ball mill, obtained
The slurry that 1.5~2.8 μm of particle diameter；
(2) it is tabletted after the slurry drying crossed ball milling, through 1240~1280 DEG C of pre-burnings 2~6 hours, obtain burning block；
(3) block after pre-burning is crushed, adds the Al of powder quality fraction 0~1%2O3, 0.3%~1% PVA,
PVB or CMC, 0.05%~1% Sodium Polyacrylate and 0.01%~0.2% tbp, using deionized water as ball milling
Medium ball milling, obtain the slurry of 0.6~1.4 μm of particle diameter；
(4) slurry is pressed into cylinder after mist projection granulating；
(5) and then dumping processing is carried out, then heats up and be sintered, you can the adjustable intermediary's microwave-medium of low-loss dielectric is made
Ceramic material.
Wherein：Ball mill is the horizontal ceramic ball mills of 50Kg in step (1), and Ball-milling Time is 12~18 hours.
Being pressed into cylinder in step (4) is：A diameter of 15mm is pressed under 160MPa pressure, is highly 6mm circle
Post.
Step (5) is：Sample is incubated to dumping processing in 2 hours at 650 DEG C, 1450 DEG C~1520 DEG C is then heated to and enters
Row sintering, heating rate is 120-180 DEG C/h, and soaking time is 4~6h, you can the adjustable middle dielectric microwave of low-loss dielectric is made and is situated between
Ceramics.
As a kind of optimal technical scheme, the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric of the present invention
Preparation method, comprise the following steps：
(1) with CaCO3、ZrO2、TiO2、La2O3、Al2O3For raw material, all raw materials are put into the horizontal ceramic ball mills of 50KG
Middle ball milling 12~18 hours, obtain the slurry of 1.5~2.8 μm of particle diameter；
(2) after the slurry drying crossed ball milling, diameter 50mm sheet is pressed under 30MPa pressure, through with 4 DEG C/
Min heating rate rises to 1240~1280 DEG C of pre-burnings 2~6 hours, obtains burning block；
(3) 30~80 mesh sieves are crossed after the block after pre-burning is crushed, add the Al of powder quality fraction 0~1%2O3,
0.3%~1% PVA, PVB or CMC, 0.05%~1% Sodium Polyacrylate and 0.01%~0.2% tbp,
Using deionized water as ball-milling medium, with 120L Ball-stirring mills ball milling 2~4 hours, the slurry of 0.6~1.4 μm of particle diameter is obtained；
(4) slurry is pressed into a diameter of 15mm under 160MPa pressure, is highly 6mm cylinder after mist projection granulating；
(5) sample is incubated to dumping processing in 2 hours at 650 DEG C, 1450 DEG C~1520 DEG C is then heated to and is sintered,
Heating rate is 120-180 DEG C/h, and soaking time is 4~6h, you can the adjustable intermediary's microwave-medium ceramics of low-loss dielectric are made
Material.
The present invention is from high-k, the CaTiO of positive temperature coefficient of resonance frequency3With low-k, negative resonance frequency
The inexpensive LaAlO of rate temperature coefficient3It is compound, and by adulterating ZrO into ceramics2, suitably adjust La2O3Content, secondary ball
Al is added after mill2O3Mode regulate and control the microstructure of ceramics, and then provide a kind of adjustable aCa (Zr of low-loss dielectricxTi1-x)O3
+(1-a)La1+yAlO3+ zwt%Al2O3Microwave dielectric ceramic materials.This is that ceramics are that a kind of high-performance of great application value is low
The microwave dielectric ceramic materials of cost.
In summary, the present invention has advantages below：
(1) present invention selects high-k εr≈ 170, positive temperature coefficient of resonance frequency τf≈ 800ppm/ DEG C CaTiO3
With low-k εr≈ 23.4, negative temperature coefficient of resonance frequency τf- 44ppm/ DEG C of ≈ inexpensive LaAlO3It is compound, and pass through
ZrO is adulterated into ceramics2, suitably adjust La2O3Content, add Al after secondary ball milling2O3Mode regulate and control ceramics micro- knot
Structure, and then obtain a kind of with low-loss dielectric tunable characteristic and suitable for microwaves such as dielectric resonator, wave filter and duplexers
The inexpensive microwave dielectric ceramic materials of device.
(2) present invention is a kind of excellent CaTiO of inexpensive microwave dielectric property3-LaAlO3Series ceramic material, the microwave
The dielectric constant of dielectric material, temperature coefficient of resonance frequency can be with chemical constituents than the continuously adjustabe in wider scope, can be with
Structure and performance are adjusted according to the requirement of designed device.
(3) present invention prepares alternative CaTiO using cheap raw material, simple and easy process route3-
NdAlO3It is the inexpensive CaTiO of ceramics3-LaAlO3Series microwave dielectric ceramic, the current domestic material independent research is filled up
Vacancy, significantly reduces production cost, and cost of material compares CaTiO3-NbAlO3Series microwave dielectric ceramic reduces 1/3rd.
Brief description of the drawings
Fig. 1 is 0.31Ca (Zr prepared by embodiment 130.02Ti0.98)O3+0.69La1.003AlO3+ 0.4wt%Al2O3Ceramics
XRD spectrum during room temperature.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1-5
By formula 0.31Ca (ZrxTi1-x)O3+0.69LaAlO3Dispensing prepares ceramics of the invention by following steps：
(1) using analysis pure chemistry reagent C aCO3、ZrO2、TiO2、La2O3、Al2O3For raw material, by 0.31Ca (ZrxTi1-x)
O3+0.69LaAlO3Chemical general formula mol ratio, wherein 0≤x≤0.06.The raw material prepared is put into the horizontal Ceramic Balls of 50KG
Ball milling 16 hours in grinding machine, obtain the slurry of 2.3 μm of particle diameter；
(2) after the slurry drying crossed ball milling, diameter 50mm sheet is pressed under 30MPa pressure, through with 4 DEG C/
Min heating rate rises to 1260 DEG C of pre-burnings 4 hours, obtains burning block；
(3) 50 mesh sieves excessively after the block after pre-burning is crushed, the PVA (PVB, CMC) of addition powder quality 0.5%,
0.1% Sodium Polyacrylate, 0.05% tbp are small with 120L Ball-stirring mills ball milling 3 using deionized water as ball-milling medium
When, obtain the slurry of 1.1 μm of particle diameter；
(4) slurry is pressed into a diameter of 15mm under 160MPa pressure, is highly 6mm cylinder after mist projection granulating；
(5) sample is incubated to dumping processing in 2 hours at 650 DEG C, 1470 DEG C~1520 DEG C is then heated to and is sintered,
Heating rate is 180 DEG C/h, soaking time 6h, you can 031Ca (Zr are madexTi1-x)O3+0.69LaAlO3Microwave-medium ceramics
Material.
The chemical formula for the microwave dielectric ceramic materials that embodiment 1-5 is prepared is 0.31Ca (ZrxTi1-x)O3+
0.69LaAlO3, wherein x is respectively 0,0.01,0.02,0.04,0.06, corresponds to embodiment 1-5 respectively, prepared by embodiment 1-5
Obtained microwave dielectric ceramic materials carry out performance test, are analyzed using Agilent 8722ET Network Analyzers (open type cell method)
The relative dielectric constant and quality factor of material, with Agilent 8722ET Network Analyzers and exact constant temperature case, measure material
Temperature coefficient of resonance frequency, Range of measuring temp be -40 DEG C~80 DEG C.Test result is shown in Table 1.
0.31Ca (the Zr of table 1xTi1-x)O3+0.69LaAlO3Ceramic microwave dielectric properties
| x | Sintering temperature (DEG C) | εr | Q×f(GHz) | τf(ppm/℃) | |
| Embodiment 1 | 0 | 1470 | 48.1 | 34172 | 7.4 |
| Embodiment 2 | 0.01 | 1480 | 46.6 | 39290 | 4.5 |
| Embodiment 3 | 0.02 | 1490 | 45.3 | 42516 | 2.3 |
| Embodiment 4 | 0.04 | 1500 | 44.1 | 41675 | -2.1 |
| Embodiment 5 | 0.06 | 1520 | 43.1 | 38682 | -4.7 |
Embodiment 6-9
By formula 0.31Ca (Zr0.02Ti0.98)O3+0.69La1+yAlO3Dispensing, using preparation side same as Example 1
Method prepares microwave dielectric ceramic materials, and the chemical formula for the microwave dielectric ceramic materials being prepared is 0.31Ca (Zr0.02Ti0.98)
O3+0.69La1+yAlO3, wherein y is respectively 0,0.01,0.03,0.05, corresponds to embodiment 6-9 respectively, prepared by embodiment 6-9
Obtained microwave dielectric ceramic materials carry out performance test, are analyzed using Agilent 8722ET Network Analyzers (open type cell method)
The relative dielectric constant and quality factor of material, with Agilent 8722ET Network Analyzers and exact constant temperature case, measure material
Temperature coefficient of resonance frequency, Range of measuring temp be -40 DEG C~80 DEG C.Test result is shown in Table 2.
0.31Ca (the Zr of table 20.02Ti0.98)O3+0.69La1+yAlO3Ceramic microwave dielectric properties
| y | Sintering temperature (DEG C) | εr | Q×f(GHz) | τf(ppm/℃) | |
| Embodiment 6 | 0 | 1490 | 45.3 | 42516 | 2.3 |
| Embodiment 7 | 0.001 | 1490 | 45.4 | 42832 | 2.5 |
| Embodiment 8 | 0.003 | 1480 | 45.5 | 43938 | 2.6 |
| Embodiment 9 | 0.005 | 1480 | 45.1 | 43156 | 3.2 |
Embodiment 10-14
By formula 0.31Ca (Zr0.02Ti0.98)O3+0.69La1.003AlO3+ zwt%Al2O3This hair is prepared through following steps
Bright ceramics：
(1) using analysis pure chemistry reagent C aCO3、ZrO2、TiO2、La2O3、Al2O3For raw material, by 0.31Ca
(Zr0.02Ti0.98)O3+0.69La1.003AlO3Chemical general formula mol ratio, the raw material prepared is put into the horizontal Ceramic Balls of 50KG
Ball milling 16 hours in grinding machine, obtain the slurry of 2.3 μm of particle diameter；
(2) after the slurry drying crossed ball milling, diameter 50mm sheet is pressed under 30MPa pressure, through with 4 DEG C/
Min heating rate rises to 1260 DEG C of pre-burnings 4 hours, obtains burning block；
(3) 50 mesh sieves are crossed after the block after pre-burning is crushed, add the Al of powder quality 0~0.6%2O3, 0.5% PVA
(PVB, CMC), 0.1% Sodium Polyacrylate, 0.05% tbp, using deionized water as ball-milling medium, use
120L Ball-stirring mills ball milling 2 hours, obtain the slurry of 1.1 μm of particle diameter；
(4) slurry is pressed into a diameter of 15mm under 160MPa pressure, is highly 6mm cylinder after mist projection granulating；
(5) sample is incubated to dumping processing in 2 hours at 650 DEG C, 1480 DEG C is then heated to and is sintered, heating rate
For 180 DEG C/h, soaking time 6h, you can 0.31Ca (Zr are made0.02Ti0.98)O3+0.69La1.003AlO3+ zwt%Al2O3It is micro-
Ripple medium ceramic material.
The chemical formula for the microwave dielectric ceramic materials that embodiment 10-14 is prepared is 0.31Ca (Zr0.02Ti0.98)O3+
0.69La1.003AlO3+ zwt%Al2O3, wherein z is respectively 0,0.1,0.2,0.4,0.6, embodiment 10-14 is corresponded to respectively, to reality
Apply the microwave dielectric ceramic materials that a 10-14 is prepared and carry out performance test, using Agilent 8722ET Network Analyzers
The relative dielectric constant and quality factor of (open type cell method) analysis of material, it is permanent with Agilent 8722ET Network Analyzers and precision
Incubator, measures the temperature coefficient of resonance frequency of material, and Range of measuring temp is -40 DEG C~80 DEG C.Test result is shown in Table 3.
0.31Ca (the Zr of table 30.02Ti0.98)O3+0.69La1.003AlO3+ zwt%Al2O3Ceramic microwave dielectric properties
| z | Sintering temperature (DEG C) | εr | Q×f(GHz) | τf(ppm/℃) | |
| Embodiment 10 | 0 | 1480 | 45.5 | 43938 | 2.6 |
| Embodiment 11 | 0.1 | 1480 | 45.6 | 44752 | 1.5 |
| Embodiment 12 | 0.2 | 1480 | 45.5 | 45362 | -0.4 |
| Embodiment 13 | 0.4 | 1480 | 45.3 | 46136 | -1.7 |
| Embodiment 14 | 0.6 | 1480 | 45.1 | 43854 | -3.2 |
Claims (6)
- A kind of 1. adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric, it is characterised in that：Chemical composition is：aCa (ZrxTi1-x)O3+(1-a)La1+yAlO3+ zwt%Al2O3, wherein a=0.31,0<X≤0.06,0<Y≤0.005,0<z≤0.6.
- 2. a kind of preparation method of the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric described in claim 1, its feature It is：Comprise the following steps：（1）With CaCO3、ZrO2、TiO2、La2O3、Al2O3For raw material, all raw materials are put into ball milling in ball mill, obtain particle diameter 1.5~2.8 μm of slurry；（2）It is tabletted after the slurry drying that ball milling is crossed, through 1240~1280 DEG C of pre-burnings 2~6 hours, obtain burning block；（3）Block after pre-burning is crushed, adds the Al of powder quality fraction 0~1%2O3, 0.3%~1% PVA, PVB or CMC, 0.05%~1% Sodium Polyacrylate and 0.01%~0.2% tbp, using deionized water as ball-milling medium ball milling, Obtain the slurry of 0.6~1.4 μm of particle diameter；（4）Slurry is pressed into cylinder after mist projection granulating；（5）Then dumping processing is carried out, then heats up and is sintered, you can the adjustable intermediary's microwave-medium ceramics of low-loss dielectric are made Material.
- 3. the preparation method of the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric according to claim 2, its feature It is：Step（1）Middle ball mill is the horizontal ceramic ball mills of 50Kg, and Ball-milling Time is 12~18 hours.
- 4. the preparation method of the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric according to claim 2, its feature It is：Step（4）In be pressed into cylinder and be：A diameter of 15 mm is pressed under 160 MPa pressure, is highly 6 mm circle Post.
- 5. the preparation method of the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric according to claim 2, its feature It is：Step（5）For：Sample is incubated to dumping processing in 2 hours at 650 DEG C, then heats to 1450 DEG C~1520 DEG C progress Sintering, heating rate is 120-180 DEG C/h, and soaking time is 4~6h, you can the adjustable intermediary's microwave-medium of low-loss dielectric is made Ceramic material.
- 6. the preparation method of the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric according to claim 2, its feature It is：Comprise the following steps：（1）With CaCO3、ZrO2、TiO2、La2O3、Al2O3For raw material, all raw materials are put into ball in the horizontal ceramic ball mills of 50Kg Mill 12~18 hours, obtains the slurry of 1.5~2.8 μm of particle diameter；（2）After the slurry drying that ball milling is crossed, the mm of diameter 50 sheet is pressed under 30 MPa pressure, through with 4 DEG C/min Heating rate rise to 1240~1280 DEG C of pre-burnings 2~6 hours, obtain burning block；（3）30~80 mesh sieves are crossed after block after pre-burning is crushed, add the Al of powder quality fraction 0~1%2O3, 0.3%~1% PVA, PVB or CMC, 0.05%~1% Sodium Polyacrylate and 0.01%~0.2% tbp, using deionized water as ball Grinding media, with 120L Ball-stirring mills ball milling 2~4 hours, obtain the slurry of 0.6~1.4 μm of particle diameter；（4）Slurry is pressed into a diameter of 15 mm under 160 MPa pressure, is highly 6 mm cylinder after mist projection granulating；（5）Sample is incubated to dumping processing in 2 hours at 650 DEG C, 1450 DEG C~1520 DEG C is then heated to and is sintered, heat up Speed is 120-180 DEG C/h, and soaking time is 4~6h, you can the adjustable intermediary's microwave dielectric ceramic materials of low-loss dielectric are made.
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| CN105837213B (en) * | 2016-03-29 | 2019-03-29 | 电子科技大学 | Add ReAlO3Microwave dielectric ceramic materials and preparation method thereof |
| CN110734284A (en) * | 2019-11-11 | 2020-01-31 | 深圳顺络电子股份有限公司 | medium high Q microwave medium ceramic material and preparation method thereof |
| CN112851344B (en) * | 2021-01-26 | 2023-03-10 | 山东丁鼎科技发展有限公司 | Microwave dielectric ceramic with medium dielectric constant and preparation method thereof |
| CN112898010B (en) * | 2021-03-10 | 2022-08-12 | 苏州瑞玛精密工业股份有限公司 | Microwave dielectric ceramic material for 5G communication base station and preparation method and application thereof |
| CN113480303B (en) * | 2021-07-27 | 2023-01-17 | 华中科技大学温州先进制造技术研究院 | Aluminate-based low-dielectric microwave dielectric ceramic and preparation method thereof |
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