CN102320825A - Low-temperature sintered microwave dielectric ceramic and sintering method thereof - Google Patents
Low-temperature sintered microwave dielectric ceramic and sintering method thereof Download PDFInfo
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Abstract
The invention discloses low-temperature sintered microwave dielectric ceramic and a sintering method thereof. The low-temperature sintered microwave dielectric ceramic comprises Li2MTi3O8 and N, wherein an M element is Zn, Ni, Co or Mg, and N is B2O3, V2O5, CuO or Bi2O3. The performance of a product prepared by adopting a microwave sintering method disclosed by the invention is superior to that of a traditional solid-phase sintered product, the high-frequency dielectric constant (epsilonr) of the product reaches 20 to 30, a Q*f value reaches up to 6000 to 59000GHz, and the temperature coefficient (tauf) of a resonance frequency is small. Moreover, the presintering time and the sintering time can be shortened, and the sintering temperature is decreased, so that the requirements of LTCC (Low Temperature Co-fired Ceramic) production can be met, the performance of the product is improved, energy sources are saved, the production cost is lowered, the low-temperature sintered microwave dielectric ceramic can be used for the manufacture of microwave devices, such as an LTCC system, a multilayer dielectric resonator, a microwave antenna, a filter and the like, the volatilization of low-melting-point substances is inhibited, the environment is protected, and the low-temperature sintered microwave dielectric ceramic has an important industrial application value.
Description
Technical field
The invention belongs to the electronic ceramics manufacturing process technology field, specifically is a kind of low-temperature sintering microwave medium pottery and sintering method thereof.
Background technology
Low temperature co-fired microwave dielectric ceramic material is a key foundation material of making components and parts such as wave filter, resonator, dielectric substrate, medium guided wave loop.Because the low temperature co-fired microwave dielectric pottery need burn with electrode altogether, silver electrode has high conductivity, low cost, especially is being difficult for oxidation in the burning process altogether, is the ideal electrode materials, and its melting temperature is 961 ℃, generally burns temperature altogether and is not higher than 900 ℃.
The microwave sintering technology is a kind of type material technology of preparing, and to be hertzian wave be penetrated into medium inside with the form of ripple to its heating principle causes dielectric loss and generate heat, rather than come from other heating element.Therefore the internal temperature gradient of its material is little, and thermal stresses is also very little, even (500～600 ℃/min) under the situation, generally also can not cause the cracking of material of very high temperature rise rates.Compare with conventional electric heating sintering, microwave heating has quick, efficient, energy-conservation and improve materials microstructure, improve material property, a series of advantages such as environmental protection.
In recent years, along with electronic information technology constantly develops to high frequencyization and digitizing direction,, integrated so that modular requirement is also more and more urgent to the miniaturized of components and parts.LTCC LTCC sintering temperature is low; The low metal of available resistivity is as the conductor material of multilayer wiring; Can improve packing density, signaling rate; And can in be embedded in the various laminar microwave electronic devices of multilager base plate once-firing, therefore be widely used in electronic devices and components fields such as field of wireless communication, aerospace industry and military field, storer, driving mechanism, wave filter, transmitter.Yet the microwave-medium ceramics sintering temperature that much has excellent properties is all very high; Generally all be higher than silver point; Interpolation lower melting point sintering aid reduces sintering temperature and is simply the most practical a kind of way, and is more serious at conventional electric heating sintering process low temperature sintering auxiliary agent volatile ratio, influenced ceramic compactness; Influence performance, and polluted environment.Because the microwave sintering technology has fast, efficiently, special advantages such as energy-saving and environmental protection, more and more receive people's extensive attention.
Summary of the invention
It is not enough that the object of the invention is to overcome above-mentioned conventional electric heating agglomerating, and a kind of low-temperature sintering microwave medium pottery and sintering method thereof are provided.This method adopts microwave sintering preparation technology, and in heat-processed, the material internal thermograde is very little, and thermal stresses is also very little, even under very high temperature rise rate situation, generally also can not cause the cracking of material.And compare with traditional solid state sintering, the volatilization that greatly reduces the low-temperature sintering auxiliary agent is to the infringement that environment causes, and shortened sintering time and microstructure that can control material, improved the material microwave dielectric properties.
The technical scheme that the present invention solves the problems of the technologies described above is following:
A kind of low-temperature sintering microwave medium pottery is by Li
2MTi
3O
8Form Li with N
2MTi
3O
8With the weight percent of N be: Li
2MTi
3O
8: N=98%～99.8%: 0.2%～2%, wherein M is Zn, Ni, Co or Mg, N is B
2O
3, V
2O
5, CuO or Bi
2O
3
A kind of sintering method of low-temperature sintering microwave medium pottery adopts microwave sintering preparation technology, follows these steps to carry out:
1. at first with analytically pure Li
2CO
3, Co
2O
3, ZnO, MgO, Ni
2O
3And TiO
2Press chemical formula Li
2MTi
3O
8Weighing is mixed with main powder, and wherein M is Zn, Ni, Co or Mg;
2. be to add deionized water at 1: 1 with main powder in the step 1 according to the weight ratio of main powder and deionized water, wet ball-milling mixes oven dry after 4～8 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 40 minutes～150 minutes; 800 ℃～950 ℃ of calcined temperatures, 5～15 ℃/minute of temperature rise rates, soaking time 5 minutes～60 minutes; Naturally cooling obtains the pre-burning powder;
3. after pre-burning powder in the step 2 being pulverized; Add N; Pre-burning powder: N=98%～99.8%: 0.2%～2% batch mixes obtains compound by weight percentage, is to add deionized water at 1: 1 by the weight ratio of compound and deionized water; Wet ball-milling mixes oven dry after 4～8 hours once more, obtains drying compound;
4. step 3 oven dry compound being added mass percentage concentration is 5% polyvinyl alcohol solution, and the polyvinyl alcohol solution amount accounts for Li
2MTi
3O
8With 3%～15% of N gross weight; Mix, granulation, compression moulding, obtain ceramic green, ceramic green is put into resistance furnace carries out binder removal; 550～650 ℃ of dump temperatures, 1 ℃～5 ℃/minute of temperature rise rates, insulation 3～8 hours; The furnace chamber of putting into microwave agglomerating furnace then carried out sintering 80 minutes～200 minutes, and 825 ℃～925 ℃ of sintering temperatures, soaking time 5 minutes～60 minutes are cooled to 600 ℃ with 3～8 ℃/minute then and close microwave source; Naturally cooling obtains low-temperature microwave sintering Li
2MTi
3O
8Microwave dielectric ceramic materials.
The chamber wall of the furnace chamber in the above-mentioned step 2 is the furnace chamber chamber wall that oxide ceramics or oxide ceramic fibre are wrapped to form.
What the temperature measuring equipment in above-mentioned step 2 and the step 3 all adopted is that temperature-measuring range is 385 ℃～1600 ℃ a infrared thermometer.
Pre-burning powder in the above-mentioned step 2 and the Li in the step 3
2MTi
3O
8The phase composite of microwave-medium ceramics is spinel structure.
The inventive method has following characteristics:
1. compare with the conventional solid state reaction method, pre-burning time and sintering time shortened to 1～6 hour by traditional 10～25 hours, had practiced thrift the energy widely, had shortened the explained hereafter cycle, had improved production efficiency;
2. solved the difficult problem of normal sintering method material grains growth consistence difference, the quality factor of product compares conventional sintering method agglomerating product and improved 10%～20%, and promptly Q * f value is up to 6000～59000GHz, high-frequency dielectric constant (ε
r) reach 20～30, and temperature coefficient of resonance frequency (τ
f) little;
3. greatly reduce the volatilization pollution on the environment of lower melting point sintering aid, environmental protection.
Description of drawings
Fig. 1 is Li of the present invention
2ZnTi
3O
8The microwave sintering thetagram of pre-burning powder.
X-coordinate t (min) express time, ordinate zou T (℃) the expression temperature.
Among the figure: X-coordinate t (min) express time, ordinate zou T (℃) the expression temperature.The a curve is a microwave sintering control curve, and the b curve is the conventional sintering temperature control curve.
Fig. 2 mixes 0.3wt%B for the present invention
2O
3Li
2ZnTi
3O
8The microwave sintering thetagram of microwave-medium ceramics.
Among the figure: X-coordinate t (min) express time, ordinate zou T (℃) the expression temperature.The a curve is a microwave sintering control curve, and the b curve is the conventional sintering temperature control curve.
Embodiment
The present invention is with the analytical pure raw material Li
2CO
3, Co
2O
3, ZnO, MgO, Ni
2O
3And TiO
2Press chemical formula Li
2MTi
3O
8Main powder is prepared in weighing; The microwave pre-burning; Then the pre-burning powder is added and add sticker and granulation again after low melting point mixes oven dry, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; Then be put into microwave oven and carry out microwave sintering, can obtain the microwave sintering low-temperature sintered microwave dielectric ceramic material.
Below in conjunction with embodiment the present invention is further described:
Embodiment 1:Li
2ZnTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31308.72g, ZnO 1447.66g and TiO
24243.62g, be hybridly prepared into main powder.
2. main powder in the step 1 being added deionized water 7kg wet ball-milling mixed 4 hours; Oven dry back powder is put into the sintering alms bowl, and the furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 79 minutes, 825 ℃ of calcined temperatures; 15 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling is shown in microwave sintering curve a in the accompanying drawing 1.
3. after pre-burning powder in the step 2 being pulverized, add 18.73g B
2O
3, adding deionized water 6238.6g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 623.86g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 96.5%, and microwave dielectric property is: ε
r=25.8, Q * f=58900GHz, τ
f=-9.7ppm/ ℃.
Embodiment 2:Li
2ZnTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31308.72g, ZnO 1447.66g and TiO
24243.62g, be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg wet ball-milling and mixed 4 hours, oven dry back powder is put into the sintering alms bowl, and the furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes; 850 ℃ of calcined temperatures; 15 ℃/minute of temperature rise rates, soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 126.94gV
2O
5, adding deionized water 6346.8g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 634.68g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 6 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～875 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 875 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.3%, and microwave dielectric property is: ε
r=25.1, Q * f=47400GHz, τ
f=-12.3ppm/ ℃.
Embodiment 3:Li
2ZnTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31308.72g, ZnO 1447.66g and TiO
24243.62g, be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 6 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 89 minutes, 900 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 30 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 62.83gCuO, add deionized water 6282.7g, wet ball-milling mixed 6 hours once more; Oven dry back interpolation 628.27g mass concentration is 5% polyvinyl alcohol solution, and granulation, and compression moulding is again put into resistance furnace with ceramic green at last and carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 5 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 96.4%, and microwave dielectric property is: ε
r=25.8, Q * f=36900GHz, τ
f=-7.7ppm/ ℃.
Embodiment 4:Li
2ZnTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31308.72g, ZnO 1447.66g and TiO
24243.62g, be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 108 minutes, 850 ℃ of calcined temperatures, 10 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 94.72gBi
2O
3, adding deionized water 6314.60g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 631.46g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 96.4%, and microwave dielectric property is: ε
r=25.4, Q * f=42900GHz, τ
f=-15.9ppm/ ℃.
Embodiment 5:Li
2NiTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31303.08g, Ni
2O
31471.56g and TiO
24225.36g, be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes, 850 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 18.298g B
2O
3, adding deionized water 6099.36g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 609.94g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.4%, and microwave dielectric property is: ε
r=24.6, Q * f=10900GHz, τ
f=24ppm/ ℃.
Embodiment 6:Li
2NiTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31303.08g, Ni
2O
31471.56g and TiO
24225.36g, be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes, 850 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 124.10gV
2O
5, adding deionized water 6205.17g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 620.52g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 6 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～875 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 875 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.3%, and microwave dielectric property is: ε
r=23.8, Q * f=7400GHz, τ
f=21.1ppm/ ℃.
Embodiment 7:Li
2NiTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31303.08g, Ni
2O
31471.56g and TiO
24225.36g, be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 6 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 89 minutes, 900 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 30 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 61.42gCuO, add deionized water 6142.50g, wet ball-milling mixed 6 hours once more; Oven dry back interpolation 614.25g mass concentration is 5% polyvinyl alcohol solution, and granulation, and compression moulding is again put into resistance furnace with ceramic green at last and carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 5 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 94.8%, and microwave dielectric property is: ε
r=24.3, Q * f=9900GHz, τ
f=17ppm/ ℃.
Embodiment 8:Li
2NiTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31303.08g, Ni
2O
31471.56g and TiO
24225.36g, be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes, 850 ℃ of calcined temperatures, 10 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 92.61gBi
2O
3, adding deionized water 6173.67g, wet ball-milling mixed 6 hours once more, and oven dry back interpolation 617.37g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.1%, and microwave dielectric property is: ε
r=23.8, Q * f=11900GHz, τ
f=15ppm/ ℃.
Embodiment 9:Li
2CoTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31302.29g, Co
2O
31474.93g and TiO
24222.78g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes, 850 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 18.30gB
2O
3, adding deionized water 6099.92g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 609.99g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 97.1%, and microwave dielectric property is: ε
r=28.4, Q * f=52900GHz, τ
f=7.1ppm/ ℃.
Embodiment 10:Li
2CoTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31302.29g, Co
2O
31474.93g and TiO
24222.78g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes, 850 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 124.11gV
2O
5, adding deionized water 6205.74g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 620.57g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 6 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～875 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 875 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 96.9%, and microwave dielectric property is: ε
r=25.1, Q * f=41400GHz, τ
f=16.4ppm/ ℃.
Embodiment 11:Li
2CoTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31302.29g, Co
2O
31474.93g and TiO
24222.78g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 6 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 89 minutes, 900 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 30 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 61.43g CuO, add deionized water 6143.05g, wet ball-milling mixed 6 hours once more; Oven dry back interpolation 614.31g mass concentration is 5% polyvinyl alcohol solution, and granulation, and compression moulding is again put into resistance furnace with ceramic green at last and carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 5 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.8%, and microwave dielectric property is: ε
r=25.8, Q * f=29600GHz, τ
f=12.1ppm/ ℃.
Embodiment 12:Li
2CoTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31302.29g, Co
2O
31474.93g and TiO
24222.78g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 108 minutes, 850 ℃ of calcined temperatures, 10 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 92.61g Bi
2O
3, adding deionized water 6174.23g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 617.42g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.8%, and microwave dielectric property is: ε
r=25.5, Q * f=36900GHz, τ
f=9.5ppm/ ℃.
Embodiment 13:Li
2MgTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31461.31g, MgO 800.29g and TiO
24738.41g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes, 850 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 18.44g B
2O
3, adding deionized water 6147.69g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 614.77g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.4%, and microwave dielectric property is: ε
r=26.8, Q * f=39800GHz, τ
f=3.5ppm/ ℃.
Embodiment 14:Li
2MgTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31461.31g, MgO 800.29g and TiO
24738.41g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 80 minutes, 850 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 125.09gV
2O
5, adding deionized water 6254.33g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 625.43g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 6 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～875 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 875 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.3%, and microwave dielectric property is: ε
r=26.3, Q * f=29000GHz, τ
f=1.1ppm/ ℃.
Embodiment 15:Li
2MgTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31461.31g, MgO 800.29g and TiO
24738.41g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 6 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 89 minutes, 900 ℃ of calcined temperatures, 15 ℃/minute of temperature rise rates; Soaking time 30 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 61.91gCuO, add deionized water 6191.16g, wet ball-milling mixed 6 hours once more; Oven dry back interpolation 619.12g mass concentration is 5% polyvinyl alcohol solution, and granulation, and compression moulding is again put into resistance furnace with ceramic green at last and carried out binder removal; 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 5 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 94.9%, and microwave dielectric property is: ε
r=27.3, Q * f=27900GHz, τ
f=2.4ppm/ ℃.
Embodiment 16:Li
2MgTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first taking by weighing purity is the analytical pure raw material Li more than 99%
2CO
31461.31g, MgO 800.29g and TiO
24738.41g be hybridly prepared into main powder;
2. main powder in the step 1 is added deionized water 7kg, wet ball-milling mixed 4 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 108 minutes, 850 ℃ of calcined temperatures, 10 ℃/minute of temperature rise rates; Soaking time 25 minutes, naturally cooling.
3. after pre-burning powder in the step 2 being pulverized, add 93.34gBi
2O
3, adding deionized water 6222.58g, wet ball-milling mixed 4 hours once more, and oven dry back interpolation 622.26g mass concentration is 5% polyvinyl alcohol solution; And granulation, compression moulding is again put into resistance furnace with ceramic green at last and is carried out binder removal; 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours; Put into the furnace chamber of 2.45GHz microwave agglomerating furnace then, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, and temperature rise rate is 10 ℃/minute; Add microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, temperature rise rate was 15 ℃/minute, 900 ℃ of insulations 40 minutes; Be cooled to 600 ℃ with 6 ℃/minute then and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The specific density of this material reaches 95.8%, and microwave dielectric property is: ε
r=27.1, Q * f=28400GHz, τ
f=5.2ppm/ ℃.
It is pointed out that according to technical scheme of the present invention, the foregoing description can also be enumerated many, prove,, all can reach the object of the invention in the scope that claims of the present invention proposed according to applicant's lot of experiment results.
Claims (5)
1. a low-temperature sintering microwave medium pottery is characterized in that it is by Li
2MTi
3O
8Form Li with N
2MTi
3O
8Weight percent with N: Li
2MTi
3O
8: N=98%～99.8%: 0.2%～2%, wherein M is Zn, Ni, Co or Mg, N is B
2O
3, V
2O
5, CuO or Bi
2O
3
2. the sintering method of a low-temperature sintering microwave medium pottery is characterized in that, adopts microwave sintering preparation technology may further comprise the steps:
1) at first with analytically pure Li
2CO
3, Co
2O
3, ZnO, MgO, Ni
2O
3And TiO
2Starting material are pressed chemical formula Li
2MTi
3O
8Weighing is mixed with main powder, and wherein M is Zn, Ni, Co or Mg;
2) be to add deionized water at 1: 1 with main powder in the step 1) according to the weight ratio of main powder and deionized water, wet ball-milling mixes oven dry after 4～8 hours, and oven dry back powder is put into the sintering alms bowl; The furnace chamber of the sintering alms bowl being put into microwave agglomerating furnace carried out pre-burning 40 minutes～150 minutes; 800 ℃～950 ℃ of calcined temperatures, 5～15 ℃/minute of temperature rise rates, soaking time 5 minutes～60 minutes; Naturally cooling obtains the pre-burning powder;
3) with step 2) in after the pre-burning powder pulverizes; Add N; Pre-burning powder: N=98%～99.8%: 0.2%～2% batch mixes obtains compound by weight percentage, is to add deionized water at 1: 1 by the weight ratio of compound and deionized water; Wet ball-milling mixes oven dry after 4～8 hours once more, obtains drying compound;
4) step 3) being dried compound, to add mass percentage concentration be 5% polyvinyl alcohol solution, and the polyvinyl alcohol solution amount accounts for Li
2MTi
3O
8With 3%～15% of N gross weight; Mix, granulation, compression moulding, obtain ceramic green, ceramic green is put into resistance furnace carries out binder removal; 550～650 ℃ of dump temperatures, 1 ℃～5 ℃/minute of temperature rise rates, insulation 3～8 hours; The furnace chamber of putting into microwave agglomerating furnace then carried out sintering 80 minutes～200 minutes, and 825 ℃～925 ℃ of sintering temperatures, soaking time 5 minutes～60 minutes are cooled to 600 ℃ with 3～8 ℃/minute then and close microwave source; Naturally cooling obtains low-temperature microwave sintering Li
2MTi
3O
8Microwave dielectric ceramic materials.
3. the microwave sintering method of a kind of low-temperature sintering microwave medium pottery according to claim 2 is characterized in that described step 2) in the chamber wall of furnace chamber be the furnace chamber chamber wall that oxide ceramics or oxide ceramic fibre are wrapped to form.
4. the microwave sintering method of a kind of low-temperature sintering microwave medium pottery according to claim 2 is characterized in that described step 2) and step 3) in temperature measuring equipment all adopts is that temperature-measuring range is 385 ℃～1600 ℃ a infrared thermometer.
5. the microwave sintering method of a kind of low-temperature sintering microwave medium pottery according to claim 2 is characterized in that described step 2) in pre-burning powder and the Li in the step 3)
2MTi
3O
8The phase composite of microwave-medium ceramics is spinel structure.
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| CN102875129A (en) * | 2012-10-12 | 2013-01-16 | 西安交通大学 | Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof |
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| CN110272263B (en) * | 2018-03-13 | 2022-05-27 | 浙江矽瓷科技有限公司 | Low-temperature co-fired ceramic dielectric material and preparation method thereof |
| CN109133871A (en) * | 2018-09-12 | 2019-01-04 | 桂林理工大学 | Low cost, low-density, sintering temperature and low type microwave dielectric material and preparation method |
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