Multiphase rock-salt structure ultra-low loss microwave dielectric ceramic material and preparation method thereof

A microwave dielectric ceramic and microwave ceramic technology are applied in the field of electronic information functional materials and devices, which can solve the problems of increasing dielectric loss of materials, increasing industrial production costs, and being difficult to meet industrial applications, achieving stable performance, saving time and energy costs. , the effect of increasing the complexity of the process

Active Publication Date: 2021-01-22
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although Li 3 Mg 2 NbO 6 Microwave dielectric ceramics have lower losses, but have the same defects as most pristine microwave ceramics
First, in a high-temperature sintering environment around 1300 °C, Li + The severe volatilization of ions leads to Li 3 Mg 2 NbO 6 There are more pores in the structure, which increases the dielectric loss of the material; second, the large negative frequency temperature coefficient makes Li 3 Mg 2 NbO 6 Raw ceramic materials are difficult to meet industrial applications; third, higher firing temperatures increase the cost of industrial production
Sintering the material in an atmosphere rich in Li volatiles or calcining in a closed space to suppress the volatilization of lithium are two commonly used methods. The former is often complex in process, and the latter generally uses platinum crucibles or buried sintered powders that do not react with raw materials. However, due to the high price of platinum and the complicated burying process, it is difficult to apply it in actual industrial production.

Method used

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  • Multiphase rock-salt structure ultra-low loss microwave dielectric ceramic material and preparation method thereof
  • Multiphase rock-salt structure ultra-low loss microwave dielectric ceramic material and preparation method thereof
  • Multiphase rock-salt structure ultra-low loss microwave dielectric ceramic material and preparation method thereof

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preparation example Construction

[0034] Its preparation method comprises the following steps:

[0035] Step 1: Add basic magnesium carbonate Mg(OH) 2 4MgCO 3 ·5H 2 O, Li 2 CO 3 , rare earth oxides of Nb or Ta, oxides of titanium, tin or zirconium, according to Li 3+a Mg 2-b / 3 x 1-2b / 3 Y b+c o 6+2c The molar ratio of the general chemical formula is prepared, wherein X is Nb 5+ or Ta 5+ , Y is Ti 4+ , Sn 4+ or Zr 4+ , 0.03 ≤ a ≤ 0.12, 0.12 ≤ b ≤ 0.38, 0 ≤ c ≤ 0.15, the obtained mixture is milled with zirconia balls, and absolute ethanol is used as the solvent, according to the weight of the mixture: grinding balls: ethanol The ratio is 1:(5~7):(2~4) for grinding for 5~8 hours, and finally a uniformly mixed mixture is obtained;

[0036] Step 2: Dry the ball-milled mixture at 100°C and pass through a 60-mesh sieve to obtain a dry powder, then pre-fire and keep it warm at 900-1050°C for 3-5 hours to obtain a sample briquette;

[0037] Step 3: Pulverize the sample sintered block, do not add dopant or...

Embodiment 1

[0048] Step 1: Magnesium carbonate basic (Mg(OH) 2 4MgCO 3 ·5H 2 O), Li 2 CO 3 , Nb 2 o 5 and TiO 2 , prepare materials according to the mass ratio of 43.66%, 25.93%, 27.09% and 3.32% respectively, the resulting mixture is milled with zirconia balls, and absolute ethanol is used as a solvent. The weight ratio was 1:5:2 for grinding for 6 hours, and finally a homogeneous mixture was obtained;

[0049] Step 2: Dry the ball-milled mixture at 100°C and pass through a 60-mesh sieve to obtain a dry powder, then pre-sinter at 1000°C for 3 hours to obtain a sample briquette;

[0050] Step 3: Pulverize the sample burnt block, use zirconia balls as the ball milling medium, use dehydrated ethanol as the solvent, grind for 2 hours according to the weight ratio of mixture: balls: ethanol is 1:5:2, and dry, Granulation treatment, the size of the granulation is controlled at 120 mesh, and the granules are put into the forming mold for dry pressing to form a green body;

[0051] Step...

Embodiment 2

[0053] Step 1: Magnesium carbonate basic (Mg(OH) 2 4MgCO 3 ·5H 2 O), Li 2 CO 3 , Nb 2 o 5 and TiO 2 , prepare materials according to the mass ratio of 43.34%, 26.27%, 25.94% and 4.45% respectively, the obtained mixture is milled with zirconia balls, and absolute ethanol is used as solvent, according to the mixture: grinding ball: ethanol Grind for 7 hours at a weight ratio of 1:6:3, and finally obtain a homogeneous mixture;

[0054] Step 2: Dry the ball-milled mixture at 100°C and pass through a 60-mesh sieve to obtain a dry powder, and then pre-sinter at 900°C for 4 hours to obtain a sample briquette;

[0055] Step 3: Pulverize the sample sintered block, weigh it, add 0.8wt% ZnO dopant to the sample sintered block, use zirconia balls as the ball milling medium, and use dehydrated ethanol as the solvent, according to the mixture: grinding balls: ethanol The weight ratio was 1:6:3 and ground for 3 hours, dried and granulated, and the granulated size was controlled at 12...

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Abstract

The invention provides a multi-phase rock-salt structure ultra-low loss microwave dielectric ceramic material and a preparation method thereof, the general formula of which is Li 3+ a Mg 2‑b / 3 x 1‑2b / 3 Y b+c o 6+2c · dZ, X is Nb 5+ or Ta 5+ , Y is Ti 4+ , Sn 4+ or Zr 4+ , Z is ZnO or LiF, 0.03≤a≤0.12, 0.12≤b≤0.38, 0≤c≤0.15, 0wt%≤d≤5wt%, the preparation method is according to the general formula ingredients, after the first ball mill mixing, drying, Screening, pre-calcination, and second ball milling, drying, granulation, debinding, and sintering in air; the crystal phase of the finished product is an ordered orthorhombic phase rock salt structure and a disordered cubic phase rock salt The composite phase of the structure; the microwave dielectric ceramic material provided by the present invention shows excellent performance under the condition of two different rock salt structural components adjustable: its relative permittivity ε r Adjustable between 8.8~17.9, Q×f value is 82000GHz~128000GHz, resonant frequency temperature coefficient τ f It can be adjusted between -33ppm / ℃~+11ppm / ℃, the preparation process is simple, and the performance is stable, which meets the application requirements of modern microwave devices.

Description

technical field [0001] The invention belongs to the technical field of electronic information functional materials and devices, and in particular relates to an ultra-low loss microwave dielectric ceramic material with an adjustable frequency temperature coefficient near zero end and a preparation method thereof. Background technique [0002] Microwave dielectric ceramics are key materials for microwave components such as resonators, filters, and dielectric substrates used in modern mobile communications, satellite communications, and military radars. As early as 2009, the State Council put forward the importance of developing dielectric ceramics with serialized dielectric constant and excellent microwave dielectric properties in the document "Outline of Electronic Information Industry Adjustment and Revitalization Plan" in 2009. High frequency is an inevitable trend in the development of digital products. With the continuous development of electronic information technology t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/495C04B35/465C04B35/453C04B35/48
CPCC04B35/457C04B35/465C04B35/48C04B35/495C04B2235/3284C04B2235/442C04B2235/445C04B2235/96
Inventor 唐斌张星袁颖钟朝位张树人
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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