CN102320825B - 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 a kind of Temperature Firing Microwave Dielectric Ceramics and sintering method thereof.
Background technology
Low temperature co-fired microwave dielectric ceramic material is the key foundation material of making the components and parts such as wave filter, resonator, dielectric substrate, medium guided wave loop.Because the low temperature co-fired microwave dielectric pottery need to burn altogether with electrode, silver electrode has high conductivity, low cost, especially is difficult for oxidation in common burning process, is desirable electrode materials, and its melting temperature is 961 ℃, generally burns altogether temperature and is not higher than 900 ℃.
Microwave Sintering Techniques 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 principle of heating 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) in 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 to high frequency and digitizing future development, to the miniaturization of components and parts, integrated so that modular requirement is also more and more urgent.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 field of wireless communication, aerospace industry and military field, storer, driving mechanism, wave filter, sensor electronic devices and components field.Yet the microwave-medium ceramics sintering temperature that much has excellent properties is all very high, generally all be higher than silver point, it is a kind of the most practical the simplest way that interpolation low melting point sintering aid reduces sintering temperature, more serious at conventional electric heating sintering process low temperature sintering auxiliary agent volatile ratio, affected ceramic compactness, affect performance, and polluted environment.Because the advantage of the uniquenesses such as Microwave Sintering Techniques has fast, efficient, energy-saving and environmental protection more and more attracts widespread attention.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned conventional electric heating sintering, and a kind of Temperature Firing Microwave Dielectric Ceramics and sintering method thereof are provided.The 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 in very high temperature rise rate situation, generally also can not cause the cracking of material.And compare with traditional solid state sintering, greatly reduce the volatilization of low-temperature sintering auxiliary agent to the infringement that environment causes, shorten sintering time and can control the microstructure of material, improved the material microwave dielectric properties.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A kind of Temperature Firing Microwave Dielectric Ceramics 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 Temperature Firing Microwave Dielectric Ceramics 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 4～8 hours post-dryings, powder is put into the sintering alms bowl after the oven dry, 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% batching is mixed by weight percentage, obtain compound, weight ratio by compound and deionized water is 1: 1 adding deionized water, wet ball-milling mixes 4～8 hours post-dryings again, obtains drying compound;
4. step 3 oven dry compound is added mass percentage concentration and be 5% polyvinyl alcohol solution, 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 carry out binder removal, 550～650 ℃ of dump temperatures, 1 ℃～5 ℃/minute of temperature rise rates, insulation 3～8 hours, then the furnace chamber of putting into microwave agglomerating furnace carried out sintering 80 minutes～200 minutes, 825 ℃～925 ℃ of sintering temperatures, soaking time 5 minutes～60 minutes, then be cooled to 600 ℃ with 3～8 ℃/minute 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 ℃ 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 traditional solid reaction process, pre-burning time and sintering time shortened to 1～6 hour by traditional 10～25 hours, had saved widely the energy, had shortened the explained hereafter cycle, had improved production efficiency;
2. solved the poor difficult problem of conventional sintering material grains growth consistence, the product that the quality factor of product is compared conventional sintering method sintering has improved 10%～20%, and namely 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 low 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) the expression time, ordinate zou T (℃) the expression temperature.
Among the figure: X-coordinate t (min) the expression time, ordinate zou T (℃) the expression temperature.The a curve is microwave sintering control curve, and the b curve is the conventional sintering temperature control curve.
Fig. 2 is that the present invention mixes 0.3wt%B
2O
3Li
2ZnTi
3O
8The microwave sintering thetagram of microwave-medium ceramics.
Among the figure: X-coordinate t (min) the expression time, ordinate zou T (℃) the expression temperature.The a curve is 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 again binding agent and granulation after low melting point mixes oven dry, again compression moulding, at last ceramic green is put into resistance furnace and 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.
The invention will be further described below in conjunction with embodiment:
Embodiment 1:Li
2ZnTi
3O
8The microwave sintering method of low temperature microwave medium pottery
Specifically implement according to following steps:
1. at first take by weighing purity and be 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, powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6238.6g, wet ball-milling mixed 4 hours again, interpolation 623.86g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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, powder is put into the sintering alms bowl after the oven dry, 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
5Add deionized water 6346.8g, wet ball-milling mixed 4 hours again, interpolation 634.68g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 6 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 875 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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 again, interpolation 628.27g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding is put into ceramic green at last resistance furnace and is carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours, then puts into the furnace chamber of 2.45GHz microwave agglomerating furnace, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, temperature rise rate is 5 ℃/minute, adds microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, and temperature rise rate is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then be cooled to 600 ℃ with 6 ℃/minute and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6314.60g, wet ball-milling mixed 4 hours again, interpolation 631.46g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2ZnTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6099.36g, wet ball-milling mixed 4 hours again, interpolation 609.94g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
5Add deionized water 6205.17g, wet ball-milling mixed 4 hours again, interpolation 620.52g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 6 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 875 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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 again, interpolation 614.25g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding is put into ceramic green at last resistance furnace and is carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours, then puts into the furnace chamber of 2.45GHz microwave agglomerating furnace, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, temperature rise rate is 5 ℃/minute, adds microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, and temperature rise rate is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then be cooled to 600 ℃ with 6 ℃/minute and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6173.67g, wet ball-milling mixed 6 hours again, interpolation 617.37g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2NiTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6099.92g, wet ball-milling mixed 4 hours again, interpolation 609.99g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
5Add deionized water 6205.74g, wet ball-milling mixed 4 hours again, interpolation 620.57g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 6 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 875 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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 again, interpolation 614.31g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding is put into ceramic green at last resistance furnace and is carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours, then puts into the furnace chamber of 2.45GHz microwave agglomerating furnace, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, temperature rise rate is 5 ℃/minute, adds microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, and temperature rise rate is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then be cooled to 600 ℃ with 6 ℃/minute and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6174.23g, wet ball-milling mixed 4 hours again, interpolation 617.42g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2CoTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6147.69g, wet ball-milling mixed 4 hours again, interpolation 614.77g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
5Add deionized water 6254.33g, wet ball-milling mixed 4 hours again, interpolation 625.43g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 6 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 875 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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 again, interpolation 619.12g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding is put into ceramic green at last resistance furnace and is carried out binder removal, 600 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate is incubated 4 hours, then puts into the furnace chamber of 2.45GHz microwave agglomerating furnace, adding microwave power at room temperature to 600 a ℃ warm area is 1.0kW, temperature rise rate is 5 ℃/minute, adds microwave power 1.5～2.2kW at 600～900 ℃ of warm areas, and temperature rise rate is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then be cooled to 600 ℃ with 6 ℃/minute and close microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The relative 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 take by weighing purity and be 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 powder is put into the sintering alms bowl after the oven dry, 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
3Add deionized water 6222.58g, wet ball-milling mixed 4 hours again, interpolation 622.26g mass concentration is 5% polyvinyl alcohol solution after the oven dry, and granulation, again compression moulding, at last ceramic green is put into resistance furnace and carried out binder removal, 650 ℃ of dump temperatures, 1 ℃/minute of temperature rise rate, be incubated 4 hours, then put into the furnace chamber of 2.45GHz microwave agglomerating furnace, 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 is 15 ℃/minute, 900 ℃ of insulations 40 minutes, then is cooled to 600 ℃ with 6 ℃/minute and closes microwave source, naturally cooling can obtain low-temperature microwave sintering Li
2MgTi
3O
8Microwave dielectric ceramic materials.The relative 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, above-described embodiment can also be enumerated many, the results show a large amount of according to the applicant, the scope in that claims of the present invention propose all can reach purpose of the present invention.
Claims (2)
1. the sintering method of a Temperature Firing Microwave Dielectric Ceramics is characterized in that,
Described Temperature Firing Microwave Dielectric Ceramics 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
Described Temperature Firing Microwave Dielectric Ceramics 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 4～8 hours post-dryings, powder is put into the sintering alms bowl after the oven dry, 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% batching is mixed by weight percentage, obtain compound, weight ratio by compound and deionized water is 1: 1 adding deionized water, wet ball-milling mixes 4～8 hours post-dryings again, 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 carry out binder removal, 550～650 ℃ of dump temperatures, 1 ℃～5 ℃/minute of temperature rise rates, insulation 3～8 hours, then the furnace chamber of putting into microwave agglomerating furnace carried out sintering 80 minutes～200 minutes, 825 ℃～925 ℃ of sintering temperatures, soaking time 5 minutes～60 minutes, then be cooled to 600 ℃ with 3～8 ℃/minute and close microwave source, naturally cooling obtains low-temperature microwave sintering Li
2MTi
3O
8Microwave dielectric ceramic materials.
2. the sintering method of a kind of Temperature Firing Microwave Dielectric Ceramics according to claim 1 is characterized in that, described step 2) in the chamber wall of furnace chamber be the furnace chamber chamber wall that oxide ceramics is wrapped to form.
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| CN102603292B (en) * | 2012-03-20 | 2014-11-05 | 广西新未来信息产业股份有限公司 | Composite oxide used for sintering microwave dielectric ceramics at low temperature |
| CN102875129B (en) * | 2012-10-12 | 2014-12-10 | 西安交通大学 | Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof |
| CN104557019B (en) * | 2014-12-27 | 2016-09-28 | 桂林理工大学 | Sintered at ultra low temperature temperature-stable microwave dielectric ceramic LiBiB2o5and preparation method thereof |
| CN104692795B (en) * | 2015-02-09 | 2017-07-11 | 陕西师范大学 | A kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof |
| CN104844193B (en) * | 2015-04-08 | 2017-04-05 | 天津大学 | High q-factor lithium magnesium titanium series microwave dielectric ceramic and its low sintering implementation method |
| CN105859281B (en) * | 2016-04-26 | 2018-07-31 | 济南大学 | A kind of low Jie's ceramics as low-loss microwave medium and preparation method |
| CN108191426B (en) * | 2018-01-17 | 2020-01-17 | 天津大学 | Medium-temperature sintered high-Q-value microwave dielectric material |
| 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 |
| CN109133871B (en) * | 2018-09-12 | 2021-05-25 | 桂林理工大学 | Low-cost, low-density and low-sintering-temperature microwave dielectric material and preparation method thereof |
| CN110137482B (en) * | 2019-06-17 | 2021-02-19 | 桑顿新能源科技(长沙)有限公司 | Carbon-coated negative electrode material, preparation method thereof and battery |
| CN110229002B (en) * | 2019-07-04 | 2022-04-22 | 贵州振华电子信息产业技术研究有限公司 | Low-temperature co-fired ceramic material and preparation method thereof |
| CN111170733A (en) * | 2020-01-15 | 2020-05-19 | 三桥惠(佛山)新材料有限公司 | Low dielectric loss dielectric ceramic and preparation method thereof |
| CN111778458A (en) * | 2020-07-09 | 2020-10-16 | 苏州市高科百年工贸有限公司 | Formula and preparation process of ceramic material for 5G communication ceramic dielectric filter |
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