CN110606732A - Method for preparing oxide ceramic by furnace-free rapid sintering at normal temperature - Google Patents

Method for preparing oxide ceramic by furnace-free rapid sintering at normal temperature Download PDF

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Publication number
CN110606732A
CN110606732A CN201910841475.6A CN201910841475A CN110606732A CN 110606732 A CN110606732 A CN 110606732A CN 201910841475 A CN201910841475 A CN 201910841475A CN 110606732 A CN110606732 A CN 110606732A
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oxide
powder
blank
metal oxide
ceramic
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CN201910841475.6A
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CN110606732B (en
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李焕勇
张春辉
黄欢欢
王乾
唐琦
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Shaanxi Zhihangyu Armor New Materials Co ltd
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Northwest University of Technology
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Abstract

The invention relates to a method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature, in particular to a preparation method for directly and rapidly sintering metal oxide ceramics or oxide solid solution ceramics or composite oxide ceramics or complex oxide ceramics or oxide ceramic matrix or complex phase oxide ceramics by adopting current thermal effect at normal temperature without a high-temperature heating furnace. Compared with the existing ceramic sintering technology, the method can realize densification sintering of various oxide ceramic materials without high-temperature furnace equipment or preheating samples, has the characteristics of short sintering time, high efficiency, small hardware investment, high energy utilization rate, wide application range, simple process, good energy-saving effect and low cost. Is suitable for rapidly preparing oxide ceramics and has wide application prospect.

Description

Method for preparing oxide ceramic by furnace-free rapid sintering at normal temperature
Technical Field
The invention belongs to the technical field of materials, relates to a method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature, and particularly relates to a preparation method for directly and rapidly sintering various metal oxide ceramics or oxide solid solution ceramics or composite oxide ceramics or complex oxide ceramics or oxide ceramic matrix or complex phase oxide ceramics by adopting current thermal effect at normal temperature without a heating furnace.
Background
Oxide ceramic materials can be used as structural or functional ceramic materials and generally have a number of excellent physical and chemical properties such as: the oxide ceramic material has the common characteristics of high chemical stability, high melting point, high temperature resistance, oxidation resistance, corrosion resistance, wear resistance, high-temperature strength, excellent mechanical and mechanical properties and the like, and has wide application in the fields of engineering technology and high technology, and the specific oxide ceramic material has specific application due to composition difference. Common oxide ceramics such as alumina (Al)2O3) Ceramics, magnesium oxide (MgO) ceramics, zinc oxide (ZnO) ceramics, zirconium oxide (ZrO)2) Ceramic, yttrium oxide (Y)2O3) Ceramics, magnesia-alumina spinel (MgO. Al)2O3) Ceramic, mullite (3 Al)2O3·2SiO2) Ceramics, barium titanate (BaTiO)3) Ceramics, and the like.
At present, the conventional preparation technologies of various oxide ceramic materials mostly adopt the traditional preparation technologies of high-temperature sintering, hot-pressing sintering, reaction sintering, hot isostatic pressing sintering, microwave sintering, inductively coupled plasma sintering (SPS) and the like, all of the technologies need to place a formed sample in a high-temperature furnace or heat the formed sample in advance to sinter and prepare the oxide ceramic materials, the sintering needs high-temperature furnace equipment, and the technical defects of large equipment investment, long sintering time, high energy consumption, low energy utilization rate, high cost and the like exist.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature, which is a method for preparing various metal oxide ceramics or oxide solid solution ceramics or composite oxide ceramics or complex oxide ceramics or oxide ceramic matrixes or complex phase oxide ceramics by direct rapid sintering at normal temperature by adopting current thermal effect without a high-temperature heating furnace, and solves the defects of large hardware investment, high-temperature furnace equipment required for sintering, long sintering time, high energy consumption, low energy utilization rate and high cost in the preparation of various oxide ceramic materials at present.
Technical scheme
A method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature is characterized by comprising the following steps:
step 1, weighing oxide superfine powder raw materials:
taking one or more metal oxide powders with the particle size of 5 nm-2000 mu m as raw materials, uniformly mixing the metal oxide powders together, and weighing the total mass of the mixed powder;
the metal oxide powder includes: an alkaline earth metal oxide, a transition metal oxide, or a rare earth metal oxide;
when the prepared unit metal oxide textured ceramic is alkaline earth metal oxide textured ceramic, selecting alkaline earth metal oxide nano powder as a raw material;
when the prepared unit metal oxide textured ceramic is the transition metal oxide textured ceramic, selecting transition metal oxide nano powder as a raw material;
when the prepared unit metal oxide textured ceramic is the rare earth oxide textured ceramic, selecting rare earth metal oxide nano powder as a raw material;
when preparing the oxide solid solution ceramic, two or more kinds of metal oxide superfine powder capable of forming a solid solution are selected from the oxides, and the powder is mixed to be used as a raw material; or the selected oxide powder and an alkali metal oxide form a solid solution, and the solid solution is mixed to be used as a raw material;
when preparing composite metal oxide ceramic or complex oxide ceramic material, selecting two or more metal oxides in the oxides, and mixing the superfine powder of the two or more metal oxides as raw materials; or selecting several kinds of metal oxides and one alkali metal oxide as raw materials, and mixing the superfine powder of the metal oxides and the alkali metal oxide to obtain the raw material;
when preparing a metal oxide ceramic matrix, selecting one metal oxide powder in metal oxides as a raw material, wherein the proportion of the metal oxide in the ingredients is not less than 60 wt%, and the rest of the ingredients which are not more than 40 wt% are prepared by taking one metal oxide powder or a plurality of metal oxide powders or one alkali metal oxide powder or other non-oxide powders as an additive or a sintering aid or a doping agent, mixing the powders to form the raw material, and sintering the raw material by a current thermal effect to finally prepare the ceramic matrix named by the metal oxides with the proportion of the ingredients of not less than 60 wt%;
when the complex phase oxide ceramic or mixed oxide ceramic is prepared, several kinds of oxide powder are selected to be mixed in oxide and alkali metal oxide to be used as raw materials, and the raw materials can form more than two crystal forms or more than two phases or a plurality of unreacted or incompletely reacted oxide ceramic materials through current thermal effect sintering;
step 2, preparation of a water-soluble metal inorganic salt saturated solution: respectively dissolving one or more water-soluble metal salts in distilled water at 4-60 ℃, uniformly stirring by using a magnetic stirrer, adding hydrochloric acid or nitric acid into the salt which is hydrolyzed to generate precipitate to adjust the pH value until the solution is clear, and preparing saturated solution of one or more water-soluble metal inorganic salts;
wherein in the selection of the water-soluble metal salt, the cation of the water-soluble metal salt is different from the valence of the cation of one or more selected metal oxides;
step 3, preparing an oxide superfine powder precursor and forming a wet blank:
respectively adding one or more saturated solutions of water-soluble metal salts into the mixed oxide powder raw materials, adding distilled water to adjust the water content to 50-90%, stirring the mixed powder of the water-containing oxides to be uniform, standing and aging for 0.5-24 hours, and then drying the wet mixed oxide powder at the temperature of 10-60 ℃ until the water content is 2-20% to obtain a metal oxide precursor; then putting the prepared metal oxide precursor into a mold, and applying pressure not more than 50MPa to mold the precursor to prepare a wet blank;
the total mass of the water-soluble metal salt accounts for 0.5-30 wt% of the total mass of the metal oxide superfine powder;
and 4, performing direct current or alternating current densification sintering on the oxide blank:
placing the formed wet blank between two electrodes connected with a direct current power supply or an alternating current power supply at 4-60 ℃, enabling the two electrodes to be in close contact with the blank, applying mechanical pressure to the electrodes to enable the pressure on the blank to be 0.1-30 MPa, turning on the power supply, adjusting the working state of the power supply to be in a constant current mode, adjusting the current limiting value to enable the current intensity applied to the two ends of the blank to be 0.5A/cm2～30A/cm2And heating and sintering the oxide blank under current, and electrifying for 0.1-30 min to obtain the oxide ceramic material with certain density.
The alkali metal oxide is Li2O、Na2O、K2O、Rb2O、Cs2O。
The alkaline earth metal oxide: BeO, MgO, CaO, SrO and BaO.
The transition metal oxide includes: divalent transition metal oxide: ZnO, CuO, CdO, FeO, NiO, CoO, MnO or PbO; trivalent transition metal oxide: al (Al)2O3、Fe2O3、B2O3、V2O3、Cr2O3、In2O3、 Sc2O3Or Ga2O3(ii) a Tetravalent transition metal oxide: ZrO (ZrO)2、TiO2、SiO2、GaO2、GeO2、HfO2、TaO2、 VO2、MnO2Or SnO2(ii) a Pentavalent and hexavalent transition metal oxides: nb2O5、V2O5、Ta2O5Or WO3(ii) a Mixed-valence transition metal oxide: fe3O4、Mn3O4Or Co3O4。
The rare earth metal oxide: y is2O3、Sc2O3、La2O3、Ce2O3、CeO2、Pr2O3、Nd2O3、Er2O3、 EuO、Pm2O3、Eu2O3、Sm2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Tm2O3、Yb2O3Or Lu2O3。
The electrode is a flat plate electrode, wherein tiny circular through holes are uniformly distributed on the flat plate electrode, the diameter of each through hole is 1-5 mm, and the distribution density of the through holes is 0.5-1/cm2。
The water-soluble metal salt is a water-soluble salt of an alkali metal, a water-soluble salt of an alkaline earth metal or various water-soluble salts of transition metal elements.
Water-soluble salts of the alkali metals: including alkali metal halide salts: ACl, a ═ Li, Na, K, Rb, Cs; or alkali metal sulfate: a. the2SO4A ═ Li, Na, K, Rb, Cs; or alkali metal nitrates: ANO3A ═ Li, Na, K, Rb, Cs; or an alkali metal carbonate: a. the2CO3A ═ Li, Na, K, Rb, Cs; or alkali metal phosphates: a. the3PO4A ═ Li, Na, K, Rb, Cs; or a water-soluble organic acid salt of an alkali metal.
Water-soluble salts of the alkaline earth metals: comprises the following halides: BCl2B ═ Mg, Ca, Sr, Ba; or an alkaline earth metal nitrate: b (NO)3)2，B＝Mg、Ca、Sr、Ba。
Various water-soluble salts of the transition metal elements: comprises water-soluble halide salt, water-soluble sulfate, water-soluble nitrate or water-soluble phosphate of the transition metal elements of aluminum Al, zinc Zn, iron Fe, copper Cu, manganese Mn, nickel Ni, cobalt Co, indium In, tin Sn, antimony Sb, bismuth Bi or zirconium Zr.
Advantageous effects
The invention provides a method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature, which is a preparation method for directly and rapidly sintering metal oxide ceramics or oxide solid solution ceramics or composite oxide ceramics or complex oxide ceramics or oxide ceramic matrix or complex phase oxide ceramics by adopting current thermal effect at normal temperature without a high-temperature heating furnace. Compared with the existing ceramic sintering technology, the method can realize densification sintering of various oxide ceramic materials without high-temperature furnace equipment or preheating samples, has the characteristics of short sintering time, high efficiency, small hardware investment, high energy utilization rate, wide application range, simple process, good energy-saving effect and low cost. Is suitable for rapidly preparing oxide ceramics and has wide application prospect.
Detailed Description
The invention will now be further described with reference to the examples:
example 1: non-furnace fast preparation of MgO ceramic material at 20 DEG C
Step 1, weighing MgO superfine powder: taking 25.0 g of MgO superfine powder with the granularity of 5nm to 500 nm.
Step 2, preparation of saturated sodium chloride solution: analytically pure sodium chloride 1.79 g is weighed, and at 20 ℃, the weighed sodium chloride is added into 5.0mL of distilled water and stirred uniformly by a magnetic stirrer until the solution is clear, so as to prepare a saturated solution of the sodium chloride at 20 ℃.
Step 3, preparation of MgO superfine powder precursor and wet blank forming: injecting the saturated sodium chloride solution prepared in the step 2 into a MgO powder raw material, adding 15.0mL of distilled water, stirring the MgO powder to be uniform, standing and aging for 24 hours, and drying the MgO at 40 ℃ until the water content is 20% to obtain a MgO powder precursor; then the prepared MgO precursor is put into a die, and pressure of 40MPa is applied to shape the precursor, so that an MgO wet blank with the diameter of phi 30mm and the thickness of 20mm is prepared.
Step 4, alternating current sintering densification of the MgO blank: horizontally placing the MgO wet blank obtained in the step (3) between two graphite electrodes connected with an alternating current power supply at the temperature of 20 ℃, wherein the graphite electrode at the upper end is uniformly distributed with round through holes with the diameter of phi 1mm, and the distribution density of the through holes is 0.5/cm2. Simultaneously applying mechanical pressure to the electrode to ensure that the pressure on the green body is kept to be 0.1MPa, switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to 210A to ensure that the current intensity applied to two ends of the green body is 30A/cm2Heating and sintering the MgO green body under current, and electrifying for 42s to obtain Mg with the density of 92 percentO ceramic material.
Example 2: non-furnace fast preparation of MgO ceramic material at 20 DEG C
Step 1, weighing MgO superfine powder: 30.00 g of MgO superfine powder with the granularity of 700nm to 1000nm is taken.
Step 2, preparation of saturated solution of sodium sulfate: 0.93 g of analytically pure sodium sulfate powder was weighed, sodium sulfate was added to 5.0mL of distilled water at 20 ℃ and stirred uniformly with a magnetic stirrer until the solution was clear, to prepare a saturated solution of sodium sulfate at 20 ℃.
Step 3, preparation of MgO superfine powder precursor and wet blank forming: injecting the saturated sodium sulfate solution prepared in the step 2 into MgO, adding 15.0mL of distilled water, stirring the MgO powder to be uniform, standing and aging for 0.5 hour, and drying the MgO at 42 ℃ until the water content is 15% to obtain an MgO powder precursor; then the prepared MgO precursor is put into a die, and pressure is applied to 30MPa, so that the precursor is molded to prepare an MgO wet blank with the diameter phi of 40mm and the thickness of 18 mm.
Step 4, alternating current sintering densification of the MgO ceramic blank: horizontally placing the MgO wet blank obtained in the step 3 between two graphite electrodes connected with an alternating current power supply at the temperature of 20 ℃, and enabling the two electrodes to be in close contact with the two end surfaces of the blank, wherein round through holes with the diameter of phi 3mm are uniformly distributed on the graphite electrode at the upper end, and the distribution density of the through holes is 1/cm2. Simultaneously applying mechanical pressure to the electrode to keep the pressure on the green body at 10MPa, switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 175A to ensure that the current intensity applied to two ends of the green body is 25A/cm2And heating and sintering the MgO ceramic blank under current, and electrifying for 96s to obtain the MgO ceramic material with the density of 95.2 percent.
Example 3: BaO ceramic material prepared rapidly at 35 ℃ without furnace
Step 1, weighing BaO superfine powder: 35.00 g of BaO superfine powder with the granularity of 20nm to 300nm is taken.
Step 2, preparing a potassium chloride saturated solution, an aluminum sulfate saturated solution and a ferric nitrate saturated solution respectively: respectively weighing 0.39 g of analytically pure potassium chloride powder, 0.43 g of analytically pure aluminum sulfate powder and 1.66 g of analytically pure ferric nitrate powder, and adding the weighed potassium chloride into 1.0mL of distilled water at 35 ℃ to prepare a potassium chloride saturated solution; dissolving the aluminum sulfate into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 so as to clarify the aluminum sulfate solution, and uniformly stirring by using a magnetic stirrer to prepare an aluminum sulfate saturated solution at the temperature of 35 ℃; the ferric nitrate is dissolved in 1.0mL of distilled water, 1.0mol/L hydrochloric acid is added to adjust the pH value to 3 until the solution is clear, and the solution is stirred uniformly by a magnetic stirrer to prepare a saturated ferric nitrate solution at the temperature of 35 ℃.
Step 3, modulation of a BaO superfine powder precursor and wet blank forming: injecting all the saturated solutions prepared in the step 2 into BaO powder, adding 18.0mL of distilled water, stirring the BaO powder to be uniform, standing and aging for 0.5 hour, and then airing the BaO at 42 ℃ until the water content is 18% to obtain a BaO powder precursor; and then putting the prepared BaO precursor into a mould, and applying pressure of 38MPa to mold the precursor to prepare a BaO wet blank with the diameter of phi 30mm and the thickness of 19 mm.
Step 4, direct current sintering densification of the BaO blank: horizontally placing the wet blank obtained in the step (3) between two graphite electrodes connected with a direct current power supply at 35 ℃, and enabling the positive and negative electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 4mm are uniformly distributed on the graphite electrode at the upper end, and the distribution density of the through holes is 0.5/cm2. Simultaneously applying mechanical pressure to the electrode to ensure that the pressure on the green body is kept at 0.1MPa, switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 50A to ensure that the current intensity applied to two ends of the green body is 7.0A/cm2And heating and sintering the BaO ceramic blank under current, and electrifying for 10min to obtain the BaO ceramic material with the density of 95.8 percent.
Example 4: non-furnace rapid preparation of ZnO ceramic material at 30 DEG C
Step 1, weighing ZnO superfine powder: 40.00 g of ZnO superfine powder with the granularity of 20 nm-100 nm is taken.
Step 2, preparation of saturated potassium chloride solution: 0.12 g of analytically pure potassium chloride powder is weighed, added into 0.5mL of distilled water at 30 ℃, stirred uniformly by a magnetic stirrer and clarified to prepare a saturated solution of potassium chloride at 30 ℃.
Step 3, preparing ZnO superfine powder precursor and forming a wet blank: injecting the potassium chloride saturated solution prepared in the step 2 into ZnO, adding 30.0mL of distilled water, stirring ZnO powder to be uniform, standing and aging for 0.5 hour, and drying ZnO at 60 ℃ until the water content is 5% to obtain a ZnO powder precursor; and then putting the prepared ZnO precursor into a mold, and applying pressure of 10MPa to mold the precursor to prepare a ZnO wet blank with the diameter phi of 40mm and the thickness of 20 mm.
Step 4, alternating current sintering densification of the ZnO green body: placing the blank obtained in the step (3) between two graphite electrodes connected with an alternating current power supply at 30 ℃, enabling the two electrodes to be in close contact with the blank, simultaneously applying mechanical pressure to the electrodes to enable the pressure on the blank to be 0.1MPa, switching on the power supply, adjusting the working state of the power supply to be in a constant current mode, adjusting the current limiting value to be 49A, and enabling the current intensity applied to two ends of the blank to be 3.9A/cm2And heating and sintering the ZnO ceramic blank under current, and electrifying for 9min to obtain the ZnO ceramic material with the density of 97.8 percent.
Example 5: non-furnace rapid preparation of ZnO ceramic material at 20 DEG C
Step 1, weighing ZnO superfine powder: taking 20.00 g of ZnO superfine powder with the granularity of 150-450 nm.
Step 2, preparation of saturated solution of sodium nitrate: 0.87 g of analytically pure sodium nitrate powder is weighed, added into 1.0mL of distilled water at 20 ℃, and stirred uniformly by a magnetic stirrer until the solution is clear, so as to prepare a saturated solution of sodium nitrate at 20 ℃.
Step 3, preparing ZnO superfine powder precursor and forming a wet blank: injecting the saturated solution of sodium nitrate prepared in the step 2 into ZnO, adding 10.0mL of distilled water, stirring ZnO powder to be uniform, standing and aging for 12 hours, and drying ZnO at 42 ℃ until the water content is 5% to obtain a ZnO powder precursor; and then putting the prepared ZnO precursor into a mold, and applying pressure of 5MPa to mold the precursor to prepare a ZnO wet blank with the diameter of phi 20mm and the thickness of 20 mm.
Step 4, direct current densification sintering of the ZnO ceramic blank: horizontally placing the blank obtained in the step (3) between two zirconium-titanium-molybdenum alloy electrodes connected with a direct current power supply at 20 ℃, and enabling the positive electrode and the negative electrode to be in close contact with the blank, wherein circular through holes with the diameter of phi 3mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. Simultaneously applying mechanical pressure to the electrode to ensure that the pressure on the green body is kept at 0.1MPa, switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 1.57A to ensure that the current intensity applied to two ends of the green body is 0.5A/cm2And heating and sintering the ZnO ceramic blank under current, and electrifying for 30min to obtain the ZnO ceramic material with the density of 94.9%.
Example 6: furnace-free rapid preparation of Al at 30 DEG C2O3Ceramic material
Step 1 Al2O3Weighing the superfine powder: taking Al with the particle size of 5-50 nm2O320.00 g of superfine powder.
Step 2, preparation of a saturated calcium chloride solution: weighing 1.00 g of analytically pure calcium chloride powder, adding calcium chloride into 1.0mL of distilled water at 30 ℃, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a saturated solution of calcium chloride at 30 ℃.
Step 3Al2O3Preparing an ultrafine powder precursor and forming a wet blank: injecting the calcium chloride saturated solution prepared in the step 2 into Al2O3In (1), 10.0mL of distilled water was added thereto, and Al was stirred2O3The powder is uniform, placed and aged for 24 hours, and then Al is added at 45 DEG C2O3Drying to water content of 15% to obtain Al2O3A powder precursor; then the prepared Al is added2O3Putting the precursor into a mold, applying pressure of 25MPa to mold the precursor, and preparing Al with the diameter of phi 30mm and the thickness of 20mm2O3And (5) wetting the blank.
Step 4 Al2O3And (3) alternating current densification sintering of the ceramic body: horizontally placing the blank obtained in the step 3 at the temperature of 30 ℃ and connecting with an alternating current power supplyThe two graphite electrodes are in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 1/cm2. Simultaneously applying mechanical pressure to the electrode to keep the pressure on the green body at 50MPa, switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 157A to ensure that the current intensity applied to two ends of the green body is 22.54A/cm2，Al2O3Heating and sintering the ceramic blank under current, electrifying for 85s to obtain Al with the density of 89 percent2O3A ceramic material.
Example 7: non-furnace rapid preparation of Al at 20 DEG C2O3Ceramic material
Step 1 Al2O3Weighing the superfine powder: taking Al with the particle size of 5-50 nm2O320.00 g of superfine powder.
Step 2, preparation of a barium chloride saturated solution and a zinc sulfide saturated solution: weighing 0.50 g of analytically pure barium chloride powder, adding barium chloride into 1.3mL of distilled water at 20 ℃, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a saturated solution of barium chloride at 20 ℃; 0.40 g of analytically pure zinc chloride powder is weighed, added to 1.0mL of distilled water at 20 ℃, added with 1.0mol/L hydrochloric acid to adjust the pH value to 3, and stirred uniformly by a magnetic stirrer until the solution is clarified to prepare a zinc chloride solution at 20 ℃.
Step 3Al2O3Preparing an ultrafine powder precursor and forming a wet blank: injecting the barium chloride saturated solution and the zinc chloride solution prepared in the step 2 into Al2O3In (1), 100.0mL of distilled water was added thereto, and Al was stirred2O3The powder is uniform, placed and aged for 0.2 hour, and then Al is added at 38 DEG C2O3Drying the powder to water content of 18% to obtain Al2O3A powder precursor; then the prepared Al is added2O3Putting the precursor into a mold, applying pressure of 3.0MPa to mold the precursor, and preparing Al with diameter phi of 30mm and thickness of 20mm2O3And (5) wetting the blank.
Step 4 Al2O3D, direct current densification sintering of the ceramic body: horizontally placing the blank obtained in the step (3) between two tungsten electrodes connected with a direct current power supply at 20 ℃, and enabling the anode and the cathode to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank was 8 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 100A so that the current intensity applied to two ends of the blank is 14.25A/cm2，Al2O3Heating and sintering the ceramic blank under current, electrifying for 150s to obtain compact 97.8 percent Al2O3A ceramic material.
Example 8: rapid preparation of Fe without furnace at 30 DEG C2O3Ceramic material
Step 1 Fe2O3Weighing the superfine powder: taking Fe with the particle size of 520-1000 nm2O335.00 g of superfine powder.
Step 2, preparing saturated solutions of zinc sulfate, lithium nitrate, sodium chloride and barium chloride respectively: weighing 0.50 g of analytically pure zinc sulfate powder, 0.97 g of analytically pure lithium nitrate powder, 0.36 g of analytically pure sodium chloride powder and 0.25 g of analytically pure barium chloride powder, adding the weighed zinc sulfate powder into 0.7mL of distilled water at 30 ℃, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clarified, and uniformly stirring by using a magnetic stirrer to prepare an aluminum sulfate saturated solution at 30 ℃; adding weighed lithium nitrate powder into 0.7mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a lithium nitrate saturated solution at the temperature of 30 ℃; adding weighed sodium chloride powder into 0.7mL of distilled water, and uniformly stirring by using a magnetic stirrer to prepare a sodium chloride saturated solution at the temperature of 30 ℃; the weighed barium chloride powder was added to 0.7mL of distilled water, and stirred uniformly with a magnetic stirrer to prepare a saturated solution of barium chloride at 30 ℃.
Step 3 Fe2O3Preparing an ultrafine powder precursor and forming a wet blank: respectively mixing the saturated solutions prepared in the step 2Partially injecting Fe2O3To the solution, 18.0mL of distilled water was added and Fe was stirred2O3The powder is uniform, placed and aged for 12 hours, and then Fe is added at the temperature of 39 DEG C2O3Drying to water content of 12% to obtain iron oxide powder precursor; then the prepared Fe2O3Putting the precursor into a mold, applying pressure of 5MPa to mold the precursor, and preparing Fe with the diameter of phi 30mm and the thickness of 20mm2O3And (5) wetting the blank.
Step 4 Fe2O3Direct current sintering densification of the ceramic body: placing the blank obtained in the step 3 between two zirconium-titanium-molybdenum alloy electrodes connected with a direct current power supply at 30 ℃, and enabling the positive electrode and the negative electrode to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. Simultaneously applying mechanical pressure to the electrode to keep the pressure on the green body at 50MPa, switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 210A to ensure that the current intensity applied to two ends of the green body is 30A/cm2，Fe2O3Heating and sintering the ceramic blank under current, electrifying for 0.1min to obtain Fe with the average density of 87%2O3A ceramic material.
Example 9: non-furnace rapid preparation of TiO at 30 DEG C2Ceramic material
Step 1 TiO2Weighing the superfine powder: taking TiO with the particle size of 10-150 nm250.00 g of superfine powder.
Step 2, preparation of aluminum chloride saturated solution: weighing 1.41 g of analytically pure aluminum chloride powder, adding the aluminum chloride into 3.0mL of distilled water, uniformly stirring by using a magnetic stirrer, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and preparing a saturated solution of the aluminum chloride at the temperature of 30 ℃.
Step 3TiO2Preparing an ultrafine powder precursor and forming a wet blank: injecting all the aluminum chloride saturated solution prepared in the step 2 into TiO2In (1), 25.0mL of distilled water was added and the TiO was stirred2The powder is homogenized, placed and aged for 16 hours, and then TiO is put into the mixture at the temperature of 45 DEG C2Drying to containThe water content is 13 percent, and TiO is obtained2A powder precursor; then the prepared TiO is mixed2Putting the precursor into a mould, applying pressure of 13MPa to form the precursor, and preparing the TiO with the diameter of phi 40mm and the thickness of 20mm2And (5) wetting the blank.
Step 4 TiO2And (3) alternating current densification sintering of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 30 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 1/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 44A so that the current intensity applied to two ends of the blank is 3.5A/cm2，TiO2Heating and sintering the ceramic blank under current, electrifying for 10min to obtain TiO with the density of 95 percent2A ceramic material.
Example 10: non-furnace rapid preparation of TiO at 20 DEG C2Ceramic material
Step 1 TiO2Weighing the superfine powder: taking TiO with the particle size of 10-100 nm220.00 g of superfine powder.
Step 2, preparation of saturated ferric chloride solution: 0.92 g of analytically pure iron chloride powder is weighed, at 20 ℃, the iron chloride is added into 1.0mL of distilled water, the mixture is stirred uniformly by a magnetic stirrer, 1.0mol/L hydrochloric acid is added to adjust the pH value to 3 until the solution is clear, and a saturated solution of the iron chloride at 20 ℃ is prepared.
Step 3TiO2Preparing an ultrafine powder precursor and forming a wet blank: injecting the ferric chloride saturated solution prepared in the step 2 into TiO2In (1), 10.0mL of distilled water was added and the TiO was stirred2The powder is homogenized, placed and aged for 2 hours, and then TiO is put into the mixture at the temperature of 45 DEG C2Drying to water content of 16% to obtain TiO2A powder precursor; then the prepared TiO is mixed2Putting the precursor into a mould, applying pressure of 3MPa to form the precursor, and preparing the TiO with the diameter of phi 30mm and the thickness of 15mm2And (5) wetting the blank.
Step 4 TiO2Direct current sintering densification of the ceramic body: placing the blank obtained in the step (3) between two graphite electrodes connected with a direct current power supply at 20 ℃, and enabling the positive electrode and the negative electrode to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 7 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 70A so that the current intensity applied to two ends of the blank is 10.0A/cm2，TiO2Heating and sintering the ceramic blank under current, electrifying for 8min to obtain TiO with the density of 96 percent2A ceramic material.
Example 11: rapid preparation of MnO at 30 ℃ without furnace2Ceramic material
Step 1 MnO2Weighing the superfine powder: MnO with the particle size of 20-200 nm is taken227.00 g of superfine powder.
Step 2, preparing saturated solutions of potassium nitrate, lithium sulfate and ferric chloride respectively: weighing 0.45 g of analytically pure potassium nitrate powder, 0.34 g of analytically pure lithium sulfate powder and 1.07 g of analytically pure iron chloride powder, adding the weighed potassium nitrate powder into 5.0mL of distilled water at the temperature of 30 ℃, and uniformly stirring by using a magnetic stirrer to prepare a potassium nitrate saturated solution at the temperature of 30 ℃; adding weighed lithium sulfate powder into 5.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a lithium sulfate saturated solution at the temperature of 30 ℃; the weighed ferric chloride powder is added into 5.0mL of distilled water, 1.0mol/L hydrochloric acid is added to adjust the pH value to 3 until the solution is clear, and the solution is stirred uniformly by a magnetic stirrer to prepare a saturated ferric chloride solution at the temperature of 30 ℃.
Step 3 MnO2Preparing an ultrafine powder precursor and forming a wet blank: respectively and completely injecting the saturated solution prepared in the step 2 into MnO2Adding 5.0mL of distilled water and stirring the MnO2The powder is uniform, placed and aged for 21 hours, and then MnO is added at 46 DEG C2Drying to a water content of 16% to obtain MnO2A powder precursor; then the MnO prepared2Precursor bodyPlacing into a mold, applying pressure of 8MPa to form the precursor, and making into MnO with diameter of 30mm and thickness of 15mm2And (5) wetting the blank.
Step 4 MnO2And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 30 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 40 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 206A so that the current intensity applied to two ends of the blank is 29.51A/cm2，MnO2The ceramic green body is heated and sintered under current for 65s to obtain MnO with the density of 96.2 percent2A ceramic material.
Example 12: non-furnace rapid Nb preparation at 4 DEG C2O5Ceramic material
Step 1 Nb2O5Weighing the superfine powder: taking Nb with the granularity of 20-200 nm2O520.00 g of superfine powder.
Step 2, preparation of saturated sodium chloride solution: weighing 1.06 g of analytically pure sodium chloride powder, adding sodium chloride into 3.0mL of distilled water at 4 ℃, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a saturated solution of sodium chloride at 4 ℃.
Step 3Nb2O5Preparing an ultrafine powder precursor and forming a wet blank: injecting the saturated solution of sodium chloride prepared in the step 2 into the Nb2O5In (1), 10.0mL of distilled water was added and Nb was stirred2O5The powder is uniform, placed and aged for 21 hours, and then Nb is added at 45 DEG C2O5Drying to water content of 10% to obtain Nb2O5A powder precursor; then the prepared Nb is2O5Putting the precursor into a mould, applying pressure of 33MPa to shape the precursor, and preparing the Nb with the diameter of phi 30mm and the thickness of 15mm2O5And (5) wetting the blank.
Step 4 Nb2O5And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in the step (3) between two metal tantalum electrodes connected with an alternating current power supply at 4 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 2 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 175A so that the current intensity applied to two ends of the blank body is 22.6A/cm2，Nb2O5Heating and sintering the ceramic blank under current, electrifying for 166s to obtain Nb with the density of 94.8 percent2O5A ceramic material.
Example 13: non-furnace rapid Nb preparation at 20 DEG C2O5Ceramic material
Step 1 Nb2O5Weighing the superfine powder: taking Nb with the granularity of 30-300 nm2O525.00 g of superfine powder.
Step 2, preparation of zinc bromide saturated solution: weighing 2.23 g of analytically pure zinc bromide powder, adding zinc bromide into 0.5mL of distilled water at 20 ℃, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a saturated solution of zinc bromide at 20 ℃.
Step 3Nb2O5Preparing an ultrafine powder precursor and forming a wet blank: injecting the saturated solution of zinc bromide prepared in the step 2 into Nb2O5In (1), 15mL of distilled water was added and Nb was stirred2O5The powder is uniform, placed and aged for 5 hours, and then Nb is added at 36 DEG C2O5Drying to water content of 15% to obtain Nb2O5A powder precursor; then the prepared Nb is2O5Putting the precursor into a mould, applying pressure of 42MPa to shape the precursor, and preparing the Nb with the diameter of phi 30mm and the thickness of 16mm2O5And (5) wetting the blank.
Step 4 Nb2O5Direct current sintering densification of the ceramic body: at 20 ℃, the product obtained in the step 3The blank is placed between two graphite electrodes connected with a DC power supply, and the positive and negative electrodes are in close contact with the blank, wherein circular through holes with diameter phi of 2mm are uniformly distributed on the upper electrode, and the distribution density of the through holes is 1/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 2 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 178A so that the current intensity applied to two ends of the blank is 25.37A/cm2，Nb2O5Heating and sintering the ceramic blank under current, and electrifying for 78s to obtain Nb with the density of 93.2 percent2O5A ceramic material.
Example 14: rapid preparation of WO at 30 ℃ without furnace3Ceramic material
Step 1 WO3Weighing the superfine powder: taking WO with the particle size of 50-500 nm340.00 g of superfine powder.
Step 2, preparing saturated solutions of potassium chloride, zinc nitrate and aluminum sulfate respectively: weighing 0.37 g of analytically pure potassium chloride powder, 1.38 g of analytically pure zinc nitrate powder and 0.40 g of analytically pure aluminum sulfate powder, adding the weighed potassium chloride powder into 1.0mL of distilled water at 30 ℃, and uniformly stirring by using a magnetic stirrer to prepare a potassium chloride saturated solution at 30 ℃; adding weighed zinc nitrate powder into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a zinc nitrate saturated solution at the temperature of 30 ℃; adding weighed aluminum sulfate powder into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare an aluminum sulfate saturated solution at the temperature of 30 ℃.
Step 3WO3Preparing an ultrafine powder precursor and forming a wet blank: respectively and totally injecting the saturated solutions prepared in the step 2 into WO3In (1), 18.0mL of distilled water was added and the WO was stirred3The powder is homogenized, left to age for 23 hours, and then the WO is put at 37 DEG C3Drying to a water content of 18% to obtain WO3A powder precursor; then the obtained WO is added3Putting the precursor into a mould, applying pressure of 40MPa to form the precursor into a diameterWO of phi 30mm and thickness of 16mm3And (5) wetting the blank.
Step 4 WO3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 30 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 3mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 1/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 40 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 25A so that the current intensity applied to two ends of the blank is 3.5A/cm2，WO3Heating and sintering the ceramic blank under current, electrifying for 300s to obtain WO with the density of 94.7 percent3A ceramic material.
Example 15: non-furnace rapid preparation of Co at 28 DEG C3O4Ceramic material
Step 1 Co3O4Weighing the superfine powder: taking Co with the granularity of 1500-2000 mu m3O440.00 g of superfine powder.
Step 2, preparation of a potassium nitrate saturated solution: 0.20 g of analytically pure potassium nitrate powder was weighed, and potassium nitrate was added to 2.0mL of distilled water at 28 ℃ and stirred uniformly by a magnetic stirrer until the solution was clarified to prepare a saturated solution of potassium nitrate at 28 ℃.
Step 3Co3O4Preparing an ultrafine powder precursor and forming a wet blank: injecting the potassium nitrate saturated solution prepared in the step 2 into Co3O4In (1), 20.0mL of distilled water was added and Co was stirred3O4The powder is homogenized, placed and aged for 23 hours, and then Co is added at 37 DEG C3O4Drying to water content of 2% to obtain Co3O4A powder precursor; then the prepared Co3O4Putting the precursor into a mold, applying pressure of 10MPa to mold the precursor, and preparing Co with the diameter of phi 30mm and the thickness of 25mm3O4And (5) wetting the blank.
Step 4 Co3O4And (3) alternating current sintering densification of the ceramic body:placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 28 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank was 35 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 23A so that the current intensity applied to two ends of the blank is 3.3A/cm2，Fe3O4Heating and sintering the ceramic blank under current, electrifying for 184s to obtain Co with the density of 88.9 percent3O4A ceramic material.
Example 16: non-furnace rapid preparation of Co at 60 DEG C3O4Ceramic material
Step 1 Co3O4Weighing the superfine powder: taking Co with the particle size of 500-1200 mu m3O440.00 g of superfine powder.
Step 2, preparation of lithium chloride saturated solution: 0.28 g of analytically pure lithium chloride powder is weighed, and at 60 ℃, lithium chloride is added into 0.5mL of distilled water and stirred uniformly by a magnetic stirrer until the solution is clear, so that a saturated solution of lithium chloride at 60 ℃ is prepared.
Step 3Co3O4Preparing an ultrafine powder precursor and forming a wet blank: injecting the lithium chloride saturated solution prepared in the step 2 into Co3O4In (1), 20.0mL of distilled water was added and Co was stirred3O4The powder is homogenized, placed and aged for 0.5 hour, and then Co is added at 47 DEG C3O4Drying to water content of 20% to obtain Co3O4A powder precursor; then the prepared Co3O4Putting the precursor into a mold, applying pressure of 5MPa to mold the precursor, and preparing Co with the diameter of phi 30mm and the thickness of 30mm3O4And (5) wetting the blank.
Step 4 Co3O4Direct current sintering densification of the ceramic body: placing the blank obtained in the step (3) between two graphite electrodes connected with a direct current power supply at 60 ℃, and enabling the two electrodes to be in close contact with the blankWherein, the upper electrode is uniformly distributed with round through holes with the diameter phi of 2mm, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 0.5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 100A so that the current intensity applied to two ends of the blank is 14.0A/cm2，Co3O4Heating and sintering the ceramic blank under current, electrifying for 180s to obtain Co with the density of 95.9 percent3O4A ceramic material.
Example 17: rapid preparation of Y at 20 ℃ without furnace2O3Ceramic material
Step 1Y2O3Weighing the superfine powder: taking Y with the particle size of 10-120 nm2O330.00 g of superfine powder.
Step 2, preparation of a barium chloride saturated solution: 0.72 g of analytically pure barium chloride powder is weighed, at the temperature of 20 ℃, the barium chloride is added into 2.0mL of distilled water, and the mixture is stirred uniformly by a magnetic stirrer until the solution is clear, so that a saturated solution of the barium chloride at the temperature of 20 ℃ is prepared.
Step 3Y2O3Preparing an ultrafine powder precursor and forming a wet blank: injecting the barium chloride saturated solution prepared in the step 2 into Y2O3In (1), 20.0mL of distilled water was added and Y was stirred2O3The powder is homogenized, placed and aged for 22 hours, and then Y is put at 48 DEG C2O3Drying to water content of 18% to obtain Y2O3A powder precursor; then the prepared Y2O3Putting the precursor into a mold, applying pressure of 20MPa to mold the precursor, and making into Y with diameter of phi 30mm and thickness of 20mm2O3And (5) wetting the blank.
Step 4Y2O3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in the step 3 between two zirconium-titanium-molybdenum alloy electrodes connected with an alternating current power supply at 20 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. Simultaneous electrode application machineThe mechanical pressure was such that the pressure maintained on the blank was 12 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 31A so that the current intensity applied to two ends of the blank is 4.4A/cm2，Y2O3Heating and sintering the ceramic blank under current, and electrifying for 480s to obtain Y with the density of 95.1 percent2O3A ceramic material.
Example 18: rapid preparation of Y at 40 ℃ without furnace2O3Ceramic material
Step 1Y2O3Weighing the superfine powder: taking Y with the particle size of 10-100 nm2O335.00 g of superfine powder.
Step 2, preparing saturated solutions of sodium chloride and potassium sulfate respectively: weighing 1.08 g of analytically pure sodium chloride powder and 0.39 g of analytically pure potassium sulfate powder, adding the weighed sodium chloride powder into 3.0mL of distilled water at 40 ℃, and uniformly stirring by using a magnetic stirrer to prepare a sodium chloride saturated solution at 30 ℃; the weighed potassium sulfate powder is added into 3.0mL of distilled water, and is stirred uniformly by a magnetic stirrer to prepare a saturated solution of potassium sulfate at the temperature of 30 ℃.
Step 3Y2O3Preparing an ultrafine powder precursor and forming a wet blank: respectively injecting the saturated solutions prepared in the step 2 into Y2O3In (1), 15.0mL of distilled water was added thereto, and Y was stirred2O3The powder is homogenized, placed and aged for 0.5 hour, and then Y is put at 38 DEG C2O3Drying to water content of 12% to obtain Y2O3A powder precursor; then the prepared Y2O3Putting the precursor into a mold, applying pressure of 6MPa to mold the precursor, and making into Y with diameter of phi 30mm and thickness of 25mm2O3And (5) wetting the blank.
Step 4Y2O3Direct current sintering densification of the ceramic body: placing the blank obtained in the step (3) between two graphite electrodes connected with a direct current power supply at 40 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 140A so that the current intensity applied to two ends of the blank is 19.8A/cm2，Y2O3Heating and sintering the ceramic blank under current, electrifying for 120s to obtain Y with the density of 95.9 percent2O3A ceramic material.
Example 19: non-furnace rapid preparation of La at 20 DEG C2O3Ceramic material
Step 1 La2O3Weighing the superfine powder: taking La with the granularity of 20-200 nm2O320.00 g of superfine powder.
Step 2, preparation of saturated solution of sodium nitrate: 0.87 g of analytically pure sodium nitrate powder is weighed, added to 1.0mL of distilled water at 20 ℃, stirred uniformly by a magnetic stirrer until the solution is clear, and prepared into a saturated solution of sodium nitrate at 20 ℃.
Step 3 La2O3Preparing an ultrafine powder precursor and forming a wet blank: fully injecting the saturated solution of sodium nitrate prepared in the step 2 into the La2O3In (1), 10.0mL of distilled water was added thereto, and La was stirred2O3The powder is homogenized, placed and aged for 12 hours, and then the La is put at 38 DEG C2O3Drying to water content of 12% to obtain La2O3A powder precursor; then the prepared La is added2O3Putting the precursor into a mold, applying pressure of 46MPa to mold the precursor, and preparing La with the diameter of phi 20mm and the thickness of 18mm2O3And (5) wetting the blank.
Step 4La2O3Direct current sintering densification of the ceramic body: placing the blank obtained in the step 3 between two molybdenum alloy electrodes connected with a direct current power supply at 20 ℃, and enabling the anode and the cathode to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 1/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 0.5 MPa. Switching on the power supply to regulate the working state of the power supply to be constantCurrent mode, regulating current limiting value to 15.5A to make current intensity applied to two ends of the blank body be 5.0A/cm2，La2O3Heating and sintering the ceramic blank under current, electrifying for 600s to obtain La with the density of 96.1 percent2O3A ceramic material.
Example 20: furnace-free rapid preparation of La at 30 DEG C2O3Ceramic material
Step 1 La2O3Weighing the superfine powder: taking La with the granularity of 20-200 nm2O350.00 g of superfine powder.
Step 2, preparing saturated solutions of magnesium chloride and zinc nitrate respectively: 1.20 g of analytical pure MgCl was weighed2·6H2Adding weighed magnesium chloride powder into 1.0mL of distilled water at 30 ℃ and taking 1.38 g of analytically pure zinc nitrate powder, adding 1.0mol/L hydrochloric acid to regulate the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a magnesium chloride saturated solution at 30 ℃; the weighed zinc nitrate powder was added to 1.0mL of distilled water, and 1.0mol/L hydrochloric acid was added to adjust the pH to 3 until the solution was clear, and the solution was stirred uniformly with a magnetic stirrer to prepare a saturated solution of zinc nitrate at 30 ℃.
Step 3 La2O3Preparing an ultrafine powder precursor and forming a wet blank: respectively and completely injecting the saturated solution prepared in the step 2 into the La2O3In (1), 24.0mL of distilled water was added thereto, and La was stirred2O3The powder is homogenized, placed and aged for 12 hours, and then the La is added at 36 DEG C2O3Drying to water content of 15% to obtain La2O3A powder precursor; then the prepared La is added2O3Putting the precursor into a mold, applying pressure of 28MPa to mold the precursor, and preparing La with the diameter of phi 30mm and the thickness of 25mm2O3And (5) wetting the blank.
Step 4La2O3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in the step (3) between two graphite electrodes connected with an alternating current power supply at 30 ℃, and enabling the two electrodes to be in close contact with the blank, wherein the diameter phi 2 is uniformly distributed on the upper end electrodemm round through holes with distribution density of 1/cm2. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 182A so that the current intensity applied to two ends of the blank is 25.98A/cm2，La2O3Heating and sintering the ceramic blank under current, electrifying for 121s to obtain La with the density of 95.5 percent2O3A ceramic material.
Example 21: furnace-free rapid Yb preparation at 40 DEG C2O3Ceramic material
Step 1Yb2O3Weighing the superfine powder: selecting Yb with a particle size of 100-500 nm2O350.00 g of superfine powder.
Step 2, preparing saturated solutions of magnesium chloride, zinc nitrate and potassium sulfate respectively: weighing 1.20 g of analytically pure magnesium chloride powder, 2.11 g of analytically pure zinc nitrate powder and 0.15 g of analytically pure potassium sulfate powder, and weighing MgCl at 40 DEG C2·6H2Adding O powder into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a magnesium chloride saturated solution at the temperature of 30 ℃; adding weighed zinc nitrate powder into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a zinc nitrate saturated solution at the temperature of 30 ℃; adding the weighed potassium sulfate powder into 1.0mL of distilled water, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a saturated potassium sulfate solution at the temperature of 30 ℃.
Step 3Yb2O3Preparing an ultrafine powder precursor and forming a wet blank: respectively injecting the saturated solution prepared in the step 2 into Yb2O3In (1), 23.0mL of distilled water was added thereto, and Yb was stirred2O3The powder is uniform, placed and aged for 22 hours, and then Yb is added at 39 DEG C2O3Drying to a water content of 14% to obtain Yb2O3A powder precursor; then the prepared Yb2O3Putting the precursor into a mold, applying pressure of 45MPa to mold the precursor, and preparing Yb with diameter of phi 30mm and thickness of 20mm2O3Wet blank。
Step 4 Yb2O3And (3) alternating current sintering densification of the ceramic body: horizontally placing the blank obtained in the step (3) between two graphite electrodes connected with an alternating current power supply at 40 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 1/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 25 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 34A so that the current intensity applied to two ends of the blank is 4.8A/cm2，Yb2O3Heating and sintering the ceramic blank under current, electrifying for 620s to obtain Yb with the density of 95 percent2O3A ceramic material.
Example 22: non-furnace fast spinel (MgAl) at 20 DEG C2O4) Ceramic material
Step 1MgO and Al2O3Weighing the superfine powder: weighing 20.00 g of MgO superfine powder with the particle size of 10-100 nm and 7.91 g of alumina superfine powder with the particle size of 5-50 nm, and uniformly mixing the two powders together.
Step 2, preparation of saturated sodium chloride solution: 0.72 g of analytically pure sodium chloride powder is weighed, and at 20 ℃, sodium chloride is added into 2.0mL of distilled water and stirred uniformly by a magnetic stirrer until the solution is clear, so as to prepare a saturated solution of sodium chloride at 20 ℃.
Step 3 MgAl2O4Preparing an ultrafine powder precursor and forming a wet blank: injecting the saturated sodium chloride solution prepared in the step 2 into the mixed powder, adding 10.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 22 hours, and drying the mixed powder at 39 ℃ until the water content is 14% to obtain a mixed powder precursor; then the prepared MgAl2O4Putting the precursor into a mold, applying pressure of 40MPa to mold the precursor, and preparing MgAl with the diameter of phi 30mm and the thickness of 25mm2O4And (5) wetting the blank.
Step 4 MgAl2O4Alternating current sintering densification of ceramic bodies: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 20 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 3mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 20 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 190A so that the current intensity applied to the two ends of the blank is 27A/cm2，MgAl2O4Heating and sintering the ceramic blank under current, electrifying for 122s to obtain MgAl with the density of 97.2 percent2O4A ceramic material.
Example 23: non-furnace fast preparation of spinel (MgAl) at 20 DEG C2O4) Ceramic material
Step 1MgO and Al2O3Weighing the superfine powder: weighing 20.00 g of MgO superfine powder with the particle size of 10-100 nm and 7.91 g of alumina superfine powder with the particle size of 5-50 nm, and uniformly mixing the two powders together.
Step 2, preparation of lithium chloride saturated solution: 1.07 g of analytically pure lithium chloride powder was weighed, and at 20 ℃, lithium chloride was added to 1.5mL of distilled water, and 1.0mol/L hydrochloric acid was added to adjust pH to 3 until the solution was clear, and the solution was stirred uniformly with a magnetic stirrer and cleared to prepare a saturated solution of lithium chloride at 20 ℃.
Step 3 MgAl2O4Preparing an ultrafine powder precursor and forming a wet blank: injecting the lithium chloride saturated solution prepared in the step 2 into the mixed powder, adding 15.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 22 hours, and drying the mixed powder at 45 ℃ until the water content is 16% to obtain a mixed powder precursor; then the prepared MgAl2O4Putting the precursor into a mold, applying pressure of 50MPa to mold the precursor, and preparing MgAl with the diameter of phi 30mm and the thickness of 20mm2O4And (5) wetting the blank.
Step 4 MgAl2O4And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in the step 3 at 20 ℃ and connecting with alternating currentBetween two molybdenum electrodes of the source, and making the two electrodes tightly contact with the blank, wherein the upper electrode is uniformly distributed with round through holes with diameter phi of 2mm, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 10 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 35A so that the current intensity applied to two ends of the blank is 5.0A/cm2，MgO·Al2O3Heating and sintering the ceramic blank under current, electrifying for 560s to obtain MgAl with the density of 95.8 percent2O4A ceramic material.
Example 24: furnace-free rapid preparation of mullite (3 Al) at 60 DEG C2O3·2SiO2) Ceramic material
Step 1 SiO2And Al2O3Weighing the superfine powder: weighing 18.00 g of superfine powder of aluminum oxide with the granularity of 5-50 nm and 7.07 g of superfine powder of silicon oxide with the granularity of 100-500 nm, and uniformly mixing the superfine powder and the silicon oxide.
Step 2, preparing saturated solutions of lithium chloride and zinc sulfate respectively: weighing 0.98 g of analytically pure lithium chloride powder and 0.75 g of analytically pure zinc sulfate powder, adding the weighed lithium chloride powder into 1.0mL of distilled water at 60 ℃, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clarified, and uniformly stirring by using a magnetic stirrer until the solution is clarified to prepare a lithium chloride saturated solution; adding weighed zinc sulfate powder into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a saturated zinc sulfate solution at the temperature of 60 ℃.
Step 33 Al2O3·2SiO2Preparing an ultrafine powder precursor and forming a wet blank: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 14.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 12 hours, and then drying the mixed powder at 45 ℃ until the water content is 15% to obtain a mixed powder precursor; then the prepared 3Al2O3·2SiO2Putting the precursor into a mold, applying pressure of 50MPa to form the precursor into a straight line3Al with diameter of phi 30mm and thickness of 21mm2O3·2SiO2And (5) wetting the blank.
Step 43 Al2O3·2SiO2And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two tungsten electrodes connected with an alternating current power supply at 60 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 70A so that the current intensity applied to two ends of the blank is 9.92A/cm2， 3Al2O3·2SiO2Heating and sintering the ceramic blank under current, electrifying for 10min to obtain 3Al with the density of 95.2 percent2O3·2SiO2A ceramic material.
Example 25: non-furnace rapid BaTiO preparation at 20 DEG C3Ceramic material
Step 1 BaO and TiO2Weighing the superfine powder: weighing 30.00 g of BaO superfine powder with the particle size of 20-200 nm and 15.63 g of titanium oxide superfine powder with the particle size of 10-100 nm, and uniformly mixing the powders together.
Step 2, preparation of a saturated ferric nitrate solution: 1.38 g of analytically pure iron nitrate powder was weighed, and at 20 ℃, iron nitrate was added to 1.0mL of distilled water, stirred uniformly with a magnetic stirrer, and 1.0mol/L nitric acid was added to adjust pH to 2 until the solution was clear, to prepare a saturated solution of iron nitrate at 20 ℃.
Step 3 BaTiO3Preparing an ultrafine powder precursor and forming a wet blank: injecting the ferric nitrate saturated solution prepared in the step 2 into the mixed powder, adding 25.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 22 hours, and then adding BaTiO at 45 DEG C3Drying until the water content is 15% to obtain a mixed powder precursor; then the prepared BaTiO is added3Putting the precursor into a mould, applying pressure of 46MPa to form the precursor, and preparing the cylindrical BaTiO with the diameter of phi 30mm and the thickness of 25mm3Wet blank。
Step 4 BaTiO3Direct current sintering densification of the ceramic body: horizontally placing the blank obtained in the step (3) between two graphite electrodes connected with a direct current power supply at 20 ℃, and enabling the positive electrode and the negative electrode to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 80A so that the current intensity applied to two ends of the blank is 11.3A/cm2，BaTiO3Heating and sintering the ceramic blank under current, electrifying for 300s to obtain the BaTiO with the density of 96.4 percent3A ceramic material.
Example 26: non-furnace rapid BaTiO preparation at 20 DEG C3Ceramic material
Step 1 BaO and TiO2Weighing the superfine powder: weighing 60.00 g of BaO superfine powder with the particle size of 20-200 nm and 31.27 g of titanium oxide superfine powder with the particle size of 10-100 nm, and uniformly mixing the powders together.
Step 2, preparing saturated solutions of lithium chloride, potassium sulfate and aluminum nitrate respectively: weighing 0.84 g of analytically pure lithium chloride powder, 0.11 g of analytically pure potassium sulfate powder and 0.74 g of analytically pure aluminum nitrate powder, adding the weighed lithium chloride powder into 1.0mL of distilled water at 20 ℃, uniformly stirring by using a magnetic stirrer, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and preparing a lithium chloride saturated solution at 20 ℃; adding the weighed potassium sulfate powder into 1.0mL of distilled water, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a saturated potassium sulfate solution at the temperature of 20 ℃; the weighed aluminum nitrate powder is added into 1.0mL of distilled water, stirred uniformly by a magnetic stirrer, added with 1.0mol/L nitric acid to adjust the pH value to 3 until the solution is clear, and prepared into an aluminum nitrate saturated solution at the temperature of 20 ℃.
Step 3 BaTiO3Preparing an ultrafine powder precursor and forming a wet blank: respectively injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 50.0mL of distilled water, stirring the mixed powder to be uniform, and standing for agingDissolving for 11 hours, and then drying the mixed powder at 46 ℃ until the water content is 14% to obtain a mixed powder precursor; then the prepared BaTiO is added3Putting the precursor into a mould, applying pressure of 42MPa to form the precursor, and preparing the BaTiO with the diameter of phi 50mm and the thickness of 20mm3And (5) wetting the blank.
Step 4 BaTiO3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 20 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 10 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 285A so that the current intensity applied to two ends of the blank is 14.5A/cm2，BaTiO3Heating and sintering the ceramic blank under current, electrifying for 180s to obtain BaTiO with the density of 94.2 percent3A ceramic material.
Example 27: non-furnace fast preparation of LiNbO at 20 DEG C3Ceramic material
Step 1Li2O and Nb2O5Weighing the superfine powder: weighing 5.06 g of lithium oxide superfine powder with the granularity of 50-500 nm and 45.00 g of niobium oxide superfine powder with the granularity of 20-200 nm, and uniformly mixing the two powders together.
Step 2, preparation of lithium chloride saturated solution: 1.67 g of analytically pure lithium chloride powder was weighed, and at 20 ℃, lithium chloride was added to 2.0mL of distilled water, and 1.0mol/L hydrochloric acid was added to adjust pH to 3 until the solution was clear, and the solution was stirred uniformly with a magnetic stirrer to prepare a saturated solution of lithium chloride at 20 ℃.
Step 3 LiNbO3Preparing an ultrafine powder precursor and forming a wet blank: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 30.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 1 hour, and drying the mixed powder at 48 ℃ until the water content is 13% to obtain a mixed powder precursor; then the prepared LiNbO3Precursor body is putPutting the precursor into a mould, applying pressure of 32MPa to form the precursor, and preparing the LiNbO with the diameter of phi 50mm and the thickness of 20mm3And (5) wetting the blank.
Step 4 LiNbO3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 20 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 1 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 285A so that the current intensity applied to two ends of the blank is 14.5A/cm2，LiNbO3Heating and sintering the ceramic blank under current, electrifying for 250s to obtain LiNbO with the density of 95.7 percent3A ceramic material.
Example 28: method for rapidly preparing 8 mol% yttria stabilized zirconia (8YSZ) ceramic material at 20 ℃ without furnace
Step 1 ZrO2And Y2O3Weighing the superfine powder: weighing 20.00 g of superfine powder of zirconium oxide with the particle size of 5-100 nm and 2.93 g of superfine powder of yttrium oxide with the particle size of 10-100 nm, and uniformly mixing the superfine powder and the yttrium oxide;
step 2, preparation of a saturated calcium chloride solution: weighing 0.75 g of analytically pure calcium chloride powder, adding calcium chloride into 1.0mL of distilled water at 20 ℃, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a saturated solution of calcium chloride at 20 ℃;
step 38, preparing a YSZ superfine powder precursor and forming a wet blank: injecting the calcium chloride saturated solution prepared in the step 2 into the mixed powder, adding 12.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 21 hours, and drying the mixed powder at 48 ℃ until the water content is 14% to obtain a mixed powder precursor; and then putting the prepared 8YSZ precursor into a mold, and applying pressure of 28MPa to mold the precursor to prepare an 8YSZ wet blank with the diameter of phi 30mm and the thickness of 20 mm.
Step 48 alternating current electrogenerated ceramic body of YSZDensification and sintering: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 20 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 3mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 2 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 70A so that the current intensity applied to two ends of the blank is 10A/cm2And heating and sintering the 8YSZ ceramic blank under current, and electrifying for 400s to obtain the 8YSZ ceramic material with the density of 93.8 percent.
Example 29: rapid preparation of 3 mol% yttria stabilized zirconia (3YSZ) ceramic material at 40 ℃ without furnace
Step 1 ZrO2And Y2O3Weighing the superfine powder: weighing 36.00 g of superfine powder of zirconium oxide with the particle size of 5-100 nm and 2.0 g of superfine powder of yttrium oxide with the particle size of 10-100 nm, and uniformly mixing the superfine powder and the yttrium oxide;
step 2, preparing saturated solutions of barium chloride, sodium nitrate and lithium sulfate respectively: weighing 0.41 g of analytically pure barium chloride powder, 1.02 g of analytically pure sodium nitrate powder and 0.34 g of analytically pure lithium sulfate powder, adding the weighed barium chloride powder into 1.0mL of distilled water at 40 ℃, and uniformly stirring by using a magnetic stirrer to prepare a barium chloride saturated solution at 40 ℃; adding weighed sodium nitrate powder into 1.0mL of distilled water, and uniformly stirring by using a magnetic stirrer to prepare a sodium nitrate saturated solution at the temperature of 40 ℃; and adding weighed lithium sulfate powder into 1.0mL of distilled water, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a lithium sulfate saturated solution at the temperature of 40 ℃.
Step 33, preparing a YSZ powder precursor and forming a wet blank: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 23.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 2 hours, and drying the mixed powder at 50 ℃ until the water content is 13% to obtain a mixed powder precursor; and then putting the prepared 3YSZ precursor into a mold, and applying pressure of 46MPa to mold the precursor to prepare a 3YSZ wet blank with the diameter of phi 30mm and the thickness of 20 mm.
Step 43 direct current sintering densification of the YSZ ceramic body: placing the blank obtained in the step (3) between two graphite electrodes connected with a direct current power supply at 40 ℃, and enabling the positive electrode and the negative electrode to be in close contact with the blank, wherein circular through holes with the diameter of phi 3mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 170A so that the current intensity applied to two ends of the blank is 24.05A/cm2And heating and sintering the YSZ ceramic blank under current, and electrifying for 125s to obtain the 3YSZ ceramic material with the density of 97.8 percent.
Example 30: method for rapidly preparing 8 mol% yttria-stabilized zirconia 8YSZ ceramic material at 20 ℃ without furnace
Step 1 ZrO2And Y2O3Weighing the superfine powder: weighing 20.00 g of superfine powder of zirconium oxide with the particle size of 5-100 nm and 2.93 g of superfine powder of yttrium oxide with the particle size of 10-100 nm, and uniformly mixing the superfine powder and the yttrium oxide;
step 2, preparing saturated solutions of calcium chloride and potassium sulfate respectively: weighing 0.75 g of analytically pure calcium chloride powder and 0.11 g of analytically pure potassium sulfate powder, adding the weighed calcium chloride powder into 1.0mL of distilled water at the temperature of 20 ℃, and uniformly stirring by using a magnetic stirrer to prepare a calcium chloride saturated solution at the temperature of 20 ℃; adding the weighed potassium sulfate powder into 1.0mL of distilled water, and uniformly stirring by using a magnetic stirrer to prepare a saturated potassium sulfate solution at the temperature of 20 ℃.
Step 38, preparing a YSZ superfine powder precursor and forming a wet blank: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 14.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 20 hours, and then drying the mixed powder at 40 ℃ until the water content is 18% to obtain a mixed powder precursor; and then putting the prepared 8YSZ precursor into a mold, and applying pressure of 30MPa to mold the precursor to prepare an 8YSZ wet blank with the diameter of phi 30mm and the thickness of 19 mm.
48, alternating current sintering densification of the YSZ ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 20 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 3mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 25 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 210A so that the current intensity applied to two ends of the blank is 30A/cm2And 8YSZ ceramic blank is heated and sintered under current, and electrified for 30s to obtain the 8YSZ ceramic material with the density of 94.5 percent.
Example 31: non-furnace rapid preparation of 95 aluminum oxide based ceramic material at 20 DEG C
Step 195, weighing raw material powder of the alumina-based ceramic material: weighing the following raw materials in sequence: al with a particle size of 3-9 μm2O365 g of superfine powder, 0.42 g of MgO superfine powder with the granularity of 500-900 nm and ZrO with the granularity of 100-500 nm20.28 g of superfine powder and SiO with the granularity of 1-3 mu m21.20 g of superfine powder and La with the granularity of 80-300 nm2O30.80 g of superfine powder and TiO with the granularity of 80-500 nm20.5 g of superfine powder, and uniformly mixing the weighed powder together to obtain 68.2 g of raw material powder of the 95 alumina-based ceramic material;
step 2, preparing saturated solutions of calcium chloride and potassium sulfate respectively: weighing 18.46 g of analytically pure calcium chloride powder and 2.0 g of analytically pure potassium sulfate powder, adding the weighed calcium chloride powder into 24.6mL of distilled water at the temperature of 20 ℃, and uniformly stirring by using a magnetic stirrer to prepare a calcium chloride saturated solution at the temperature of 20 ℃; adding the weighed potassium sulfate powder into 15.0mL of distilled water, and uniformly stirring by using a magnetic stirrer to prepare a saturated potassium sulfate solution at the temperature of 20 ℃.
Step 395, preparation of an alumina superfine powder precursor and wet blank forming: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 50.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 2 hours, and then drying the mixed powder at 40 ℃ until the water content is 15% to obtain a mixed powder precursor; and then putting the prepared 95 aluminum oxide precursor into a mold, and applying pressure of 40MPa to mold the precursor to prepare a 95 aluminum oxide wet blank with the diameter of phi 40mm and the thickness of 22 mm.
Step 495 alternating current sintering densification of an alumina ceramic body: horizontally placing the blank obtained in the step (3) between two zirconium-titanium-molybdenum alloy electrodes connected with an alternating current power supply at 20 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank was 9 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 240A so that the current intensity applied to two ends of the blank is 19.1A/cm2And heating and sintering the 95 aluminum oxide ceramic blank under current, and electrifying for 100s to obtain the 95 aluminum oxide-based ceramic material with the density of 95.4 percent.
Example 32: furnace-free rapid preparation of BaZr at 40 DEG C0.1Ce0.7Y0.1Yb0.1O3Ceramic material
Step 1 BaO, ZrO2、CeO2、Y2O3And Yb2O3Weighing the superfine powder: weighing 20.00 g of BaO superfine powder with the particle size of 10-100 nm, 1.61 g of zirconia superfine powder with the particle size of 20-100 nm, 15.72 g of cerium oxide superfine powder with the particle size of 10-100 nm, 2.95 g of yttria superfine powder with the particle size of 5-100 nm and 5.14 g of ytterbium oxide superfine powder with the particle size of 20-200 nm, and uniformly mixing the two powders together;
step 2, preparation of saturated solution of sodium nitrate: weighing 1.05 g of analytically pure sodium nitrate powder, adding sodium nitrate into 1.0mL of distilled water at 40 ℃, and uniformly stirring by using a magnetic stirrer until the solution is clear to prepare a saturated solution of sodium nitrate at 40 ℃;
step 3 BaZr0.1Ce0.7Y0.1Yb0.1O3Preparation of superfine powder precursor and wet blank formationType (2): injecting the saturated solution of sodium nitrate prepared in the step 2 into the mixed powder, adding 25.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 20 hours, and drying the mixed powder at 45 ℃ until the water content is 15% to obtain a mixed powder precursor; then the BaZr0.1Ce0.7Y0.1Yb0.1O3And putting the precursor into a mold, and applying pressure of 40MPa to mold the precursor to prepare a wet blank with the diameter of phi 30mm and the thickness of 25 mm.
Step 4BaZr0.1Ce0.7Y0.1Yb0.1O3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 40 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 35A so that the current intensity applied to two ends of the blank is 4.9A/cm2，BaZr0.1Ce0.7Y0.1Yb0.1O3Heating and sintering the ceramic blank under current, electrifying for 10min to obtain BaZr with the density of 96.8 percent0.1Ce0.7Y0.1Yb0.1O3A ceramic material.
Example 33: furnace-free rapid preparation of BaZr at 40 DEG C0.1Ce0.7Y0.1Yb0.1O3Ceramic material
Step 1 BaO, ZrO2、CeO2、Y2O3And Yb2O3Weighing the superfine powder: weighing 20.00 g of BaO superfine powder with the granularity of 25nm, 1.61 g of zirconia superfine powder with the granularity of 35nm, 15.72 g of cerium oxide superfine powder with the granularity of 45nm, 2.95 g of yttrium oxide superfine powder with the granularity of 30nm and 5.14 g of ytterbium oxide superfine powder with the granularity of 55nm, and uniformly mixing the powders together;
step 2, preparation of saturated solution of potassium chloride, sodium sulfate and lithium nitrate: weighing 0.40 g of analytically pure potassium chloride powder, 0.49 g of analytically pure sodium sulfate powder and 1.52 g of analytically pure lithium nitrate powder, adding the weighed potassium chloride powder into 1.0mL of distilled water at 40 ℃, and uniformly stirring by using a magnetic stirrer to prepare a calcium chloride saturated solution at 40 ℃; adding weighed sodium sulfate powder into 1.0mL of distilled water, and uniformly stirring by using a magnetic stirrer to prepare a sodium sulfate saturated solution at the temperature of 40 ℃; the weighed lithium nitrate powder was added to 1.0mL of distilled water, 1.0mol/L of nitric acid was added to adjust the pH to 3 until the solution was clear, and the solution was stirred uniformly with a magnetic stirrer to prepare a saturated solution of lithium nitrate at 40 ℃.
Step 3 BaZr0.1Ce0.7Y0.1Yb0.1O3Preparing an ultrafine powder precursor and forming a wet blank: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 23.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 20 hours, and then drying the mixed powder at 45 ℃ until the water content is 5% to obtain a mixed powder precursor; then the BaZr0.1Ce0.7Y0.1Yb0.1O3Putting the precursor into a mould, applying pressure of 45MPa to form the precursor, and preparing the BaZr with the diameter of phi 30mm and the thickness of 20mm0.1Ce0.7Y0.1Yb0.1O3And (5) wetting the blank.
Step 4BaZr0.1Ce0.7Y0.1Yb0.1O3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 40 ℃, and enabling the positive electrode and the negative electrode to be in close contact with the blank, wherein circular through holes with the diameter of phi 4mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 2 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 32A so that the current intensity applied to two ends of the blank is 4.5A/cm2，BaZr0.1Ce0.7Y0.1Yb0.1O3Ceramic body is under currentHot sintering, electrifying for 20min to obtain BaZr with the density of 98.2 percent0.1Ce0.7Y0.1Yb0.1O3A ceramic material.
Example 34: rapid preparation of lanthanum chromate (LaCrO) at 60 ℃ without furnace3) Ceramic material
Step 1 La2O3And Cr2O3Weighing the superfine powder: weighing 30.00 g of lanthanum oxide superfine powder with the granularity of 20-200 nm and 14.00 g of chromium oxide superfine powder with the granularity of 50-500 nm, and uniformly mixing the two powders together.
Step 2, preparing saturated solutions of lithium chloride and zinc sulfate respectively: weighing 0.98 g of analytically pure lithium chloride powder and 0.75 g of analytically pure zinc sulfate powder, adding the weighed lithium chloride powder into 1.0mL of distilled water at 60 ℃, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clarified, and uniformly stirring by using a magnetic stirrer to prepare a lithium chloride saturated solution at 60 ℃; adding weighed zinc sulfate powder into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a saturated zinc sulfate solution at the temperature of 60 ℃.
Step 3 LaCrO3Preparing an ultrafine powder precursor and forming a wet blank: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 28.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 0.5 hour, and drying the mixed powder at 46 ℃ until the water content is 4% to obtain a mixed powder precursor; then the prepared LaCrO is added3Putting the precursor into a mold, applying pressure of 48MPa to mold the precursor, and preparing the LaCrO with the diameter of phi 30mm and the thickness of 20mm3A green body.
Step 4 LaCrO3And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 60 ℃, and enabling the two electrodes to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 1/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 3 MPa. Power-on, regulationThe working state of the power supply is in a constant current mode, and the current limiting value is adjusted to be 170A, so that the current intensity applied to the two ends of the blank body is 24A/cm2，LaCrO3Heating and sintering the ceramic blank under current, electrifying for 180s to obtain LaCrO with the density of 95.6 percent3A ceramic material.
Example 35: furnace-free rapid preparation of lanthanum zirconate (La) at 20 DEG C2Zr2O7) Ceramic material
Step 1 La2O3And ZrO2Weighing the superfine powder: weighing 33.05 g of lanthanum oxide superfine powder with the particle size of 10-100 nm and 25.00 g of zirconium oxide superfine powder with the particle size of 10-100 nm, and uniformly mixing the two powders together.
Step 2, preparation of lithium chloride saturated solution: 1.67 g of analytically pure lithium chloride powder was weighed, added to 2.0mL of distilled water at 20 ℃, stirred uniformly with a magnetic stirrer, added with 1.0mol/L hydrochloric acid to adjust the pH to 3 until the solution was clear, and made into a saturated solution of lithium chloride at 20 ℃.
Step 3 La2Zr2O7Preparing an ultrafine powder precursor and forming a wet blank: injecting the lithium chloride saturated solution prepared in the step 2 into the mixed powder, adding 30.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 0.5 hour, and drying the mixed powder at 45 ℃ until the water content is 6% to obtain a mixed powder precursor; then the prepared La is added2Zr2O7Putting the precursor into a mold, applying pressure of 48MPa to mold the precursor, and preparing La with the diameter of phi 30mm and the thickness of 25mm2Zr2O7And (5) wetting the blank.
Step 4La2Zr2O7Direct current sintering densification of the ceramic body: placing the blank obtained in the step (3) between two graphite electrodes connected with a direct current power supply at 20 ℃, and enabling the positive electrode and the negative electrode to be in close contact with the blank, wherein circular through holes with the diameter of phi 2mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 2 MPa. Switching on the power supply to regulate the working state of the power supply to be constantCurrent mode, regulating current limiting value to 35A to make current intensity applied to two ends of blank body be 5.0A/cm2，La2Zr2O7Heating and sintering the ceramic blank under current, electrifying for 10min to obtain La with the density of 97.5 percent2Zr2O7A ceramic material.
Example 36: non-furnace rapid preparation of Al at 60 DEG C2O3·SiO2Ceramic material
Step 1 SiO2And Al2O3Weighing the superfine powder: weighing 18.00 g of superfine powder of aluminum oxide with the granularity of 5-50 nm and 10.61 g of superfine powder of silicon oxide with the granularity of 50-500 nm, and uniformly mixing the superfine powder and the silicon oxide;
step 2, preparing saturated solutions of lithium chloride and zinc sulfate respectively: weighing 0.98 g of analytically pure lithium chloride powder and 0.75 g of analytically pure zinc sulfate powder, adding the weighed lithium chloride powder into 1.0mL of distilled water at 60 ℃, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clarified, and uniformly stirring by using a magnetic stirrer to prepare a lithium chloride saturated solution at 60 ℃; the weighed zinc sulfate powder is added into 1.0mL of distilled water, and is stirred uniformly by a magnetic stirrer to prepare a saturated zinc sulfate solution at the temperature of 60 ℃.
Step 3Al2O3·SiO2Preparing an ultrafine powder precursor and forming a wet blank: respectively and completely injecting the saturated solutions prepared in the step 2 into the mixed powder, adding 14.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 2 hours, and then drying the mixed powder at 45 ℃ until the water content is 15% to obtain a mixed powder precursor; then the prepared Al is added2O3·SiO2Putting the precursor into a mold, applying pressure of 50MPa to mold the precursor, and preparing Al with the diameter of phi 30mm and the thickness of 25mm2O3·SiO2And (5) wetting the blank.
Step 4 Al2O3·SiO2And (3) alternating current sintering densification of the ceramic body: placing the blank obtained in the step (3) between two graphite electrodes connected with an alternating current power supply at 60 ℃, and enabling the two electrodes to be tightly connected with the blankContact, wherein the upper end electrode is uniformly distributed with round through holes with the diameter phi of 2mm, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the blank is 5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 170A so that the current intensity applied to two ends of the blank is 24.10A/cm2， Al2O3·SiO2Heating and sintering the ceramic blank under current, electrifying for 180s to obtain Al with the density of 95.3 percent2O3·SiO2A ceramic material.
Example 37: furnace-free rapid preparation of La (Fe) at 60 DEG C0.6Co0.4)O3-FeCo complex phase ceramic material
Step 1 La2O3、Co2O3And Cr2O3Weighing the superfine powder: weighing 30.00 g of lanthanum oxide superfine powder with the particle size of 20-200 nm, 6.11 g of cobalt oxide superfine powder with the particle size of 10-100 nm and 8.40 g of chromium oxide superfine powder with the particle size of 20-200 nm, and uniformly mixing the two powders together;
step 2, preparing saturated solutions of lithium chloride and zinc sulfate respectively: weighing 0.98 g of analytically pure lithium chloride powder and 0.75 g of analytically pure zinc sulfate powder, adding the weighed lithium chloride powder into 1.0mL of distilled water at 60 ℃, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clarified, and uniformly stirring by using a magnetic stirrer to prepare a lithium chloride saturated solution at 60 ℃; adding weighed zinc sulfate powder into 1.0mL of distilled water, adding 1.0mol/L hydrochloric acid to adjust the pH value to 3 until the solution is clear, and uniformly stirring by using a magnetic stirrer to prepare a saturated zinc sulfate solution at the temperature of 60 ℃.
Step 3 La (Fe)0.6Co0.4)O3Preparing FeCo superfine powder precursor and forming a wet blank: injecting all the mixed saturated solution prepared in the step 2 into the mixed powder, adding 28.0mL of distilled water, stirring the mixed powder to be uniform, standing and aging for 1 hour, and drying the mixed powder at 46 ℃ until the water content is 8% to obtain a mixed powder precursor; then the prepared La (Fe)0.6Co0.4)O3FeCo precursor is put into a mould, pressure is applied to 45MPa, so that the precursor is molded to prepare La (Fe) with the diameter of phi 30mm and the thickness of 20mm0.6Co0.4)O3-a FeCo green body.
Step 4La (Fe)0.6Co0.4)O3-alternating current sintering densification of FeCo ceramic body: placing the blank obtained in step 3 between two graphite electrodes connected with an alternating current power supply at 60 deg.C, and making the two electrodes closely contact with the blank, wherein circular through holes with diameter of phi 3mm are uniformly distributed on the upper end electrode, and the distribution density of the through holes is 0.5/cm2. While applying mechanical pressure to the electrode so that the pressure maintained on the green body was 0.5 MPa. Switching on a power supply, adjusting the working state of the power supply to be in a constant current mode, and adjusting the current limiting value to be 115A so that the current intensity applied to two ends of the blank is 16.0A/cm2， La(Fe0.6Co0.4)O3Heating and sintering the FeCo complex phase ceramic blank under current, electrifying for 30min to obtain La (Fe) with the density of 97.1 percent0.6Co0.4)O3-FeCo complex phase ceramic material.
In the present invention,
the metal oxide superfine powder relates to the following 7 types of oxide powder:
alkaline earth metal oxide: BeO, MgO, CaO, SrO, BaO;
divalent transition metal oxide: ZnO, CuO, CdO, FeO, NiO, CoO, MnO, PbO, etc.;
③ oxide of trivalent transition metal: al (Al)2O3、Fe2O3、B2O3、V2O3、Cr2O3、In2O3、Sc2O3、Ga2O3Etc.;
tetravalent transition metal oxide: ZrO (ZrO)2、TiO2、SiO2、GaO2、GeO2、HfO2、TaO2、VO2、MnO2、 SnO2Etc.;
pentavalent and hexavalent transition metal oxides: nb2O5、V2O5、Ta2O5、WO3Etc.;
sixthly, mixed valence transition metal oxide: fe3O4、Mn3O4、Co3O4；
Seventh, rare earth metal oxide: y is2O3、Sc2O3、La2O3、Ce2O3、CeO2、Pr2O3、Nd2O3、Er2O3、EuO、 Pm2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Tm2O3、Yb2O3、Lu2O3Etc.;
the material form of the oxide superfine powder is crystalline state or amorphous state.
When preparing metal oxide ceramics, including alkaline earth metal oxide ceramics or transition metal oxide ceramics or rare earth oxide ceramics, one oxide ultrafine powder in the 7 types of oxides is selected as a raw material;
when preparing the oxide solid solution ceramic, two or more kinds of metal oxide superfine powder capable of forming a solid solution are selected from the 7 oxides, and the powder is mixed to be used as a raw material; or selected oxide powders among the above 7-type oxides may be mixed with an alkali metal oxide (including Li)2O、Na2O、K2O、Rb2O、Cs2O) to form a solid solution, and mixing them as a raw material.
When preparing the composite metal oxide ceramic or the complex oxide ceramic material, two or more metal oxides in the 7 types of oxides are selected and mixed to be used as raw materials; or selecting several of the above 7 kinds of metal oxides and one alkali metal oxide (including Li)2O、Na2O、K2O、Rb2O、Cs2O) as a raw material, and finely pulverizing the sameThe mixture was used as a raw material.
When preparing the metal oxide ceramic matrix, one metal oxide powder in the 7 metal oxides listed above is selected as a raw material, the proportion of the metal oxide in the ingredients is not less than 60 wt%, the rest of the ingredients which are not more than 40 wt% are prepared by taking one metal oxide powder or a plurality of metal oxide powders or one alkali metal oxide powder or other non-oxide powders as an additive or a sintering aid or a dopant, and the like, and the powders are mixed to form the raw material, and the raw material is sintered by the current thermal effect to finally prepare the ceramic matrix named by the metal oxide with the ingredient proportion of not less than 60 wt%.
The preparation method comprises selecting several oxide powders from the above 7 oxides and alkali metal oxides, mixing, and sintering by current thermal effect to obtain two or more crystal forms or two or more phases or multiple unreacted or incompletely reacted oxide ceramic materials.
The alkali metal oxides (including Li)2O、Na2O、K2O、Rb2O、Cs2O) the particle size of the raw material powder is also 5nm to 2000 μm.
The water-soluble metal salt involved in the step 2 refers to the following water-soluble metal salts, including: alkali metal halides (AX, a ═ Li, Na, K, Rb, Cs, X ═ F, Cl, Br, I), or alkali metal sulfates (a)2SO4A ═ Li, Na, K, Rb, Cs), or alkali metal nitrate (ANO)3A ═ Li, Na, K, Rb, Cs), or an alkali metal carbonate (a)2CO3A ═ Li, Na, K, Rb, Cs), or alkaline earth metal halide (BCl)2，BBr2B ═ Mg, Ca, Sr, Ba), or zinc salts (ZnSO)4、ZnNO3、ZnX2X ═ F, Cl, Br, I), or iron salts (FeCl)3、 Fe2(SO4)3、Fe(NO3)3) Or indium salts (InCl)3，In2(SO4)3，In(NO3)3) Or bismuth salts (BiCl)3、Bi(NO3)3) Or aluminium salts (AlCl)3、Al2(SO4)3、Al(NO3)3) And the like.
Wherein, in the selection of the water-soluble metal salt, the cation of the water-soluble metal salt has different valence with the cation of one or more oxides in the selected metal oxides. The water-soluble metal salt may or may not have crystal water or adsorbed water.

Claims (10)

1. A method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature is characterized by comprising the following steps:
step 1, weighing oxide superfine powder raw materials:
taking one or more metal oxide powders with the particle size of 5 nm-2000 mu m as raw materials, uniformly mixing the metal oxide powders together, and weighing the total mass of the mixed powder;
the metal oxide powder includes: an alkaline earth metal oxide, a transition metal oxide, or a rare earth metal oxide;
when the prepared unit metal oxide textured ceramic is alkaline earth metal oxide textured ceramic, selecting alkaline earth metal oxide nano powder as a raw material;
when the prepared unit metal oxide textured ceramic is the transition metal oxide textured ceramic, selecting transition metal oxide nano powder as a raw material;
when the prepared unit metal oxide textured ceramic is the rare earth oxide textured ceramic, selecting rare earth metal oxide nano powder as a raw material;
when preparing the oxide solid solution ceramic, two or more kinds of metal oxide superfine powder capable of forming a solid solution are selected from the oxides, and the powder is mixed to be used as a raw material; or the selected oxide powder and an alkali metal oxide form a solid solution, and the solid solution is mixed to be used as a raw material;
when preparing composite metal oxide ceramic or complex oxide ceramic material, selecting two or more metal oxides in the oxides, and mixing the superfine powder of the two or more metal oxides as raw materials; or selecting several kinds of metal oxides and one alkali metal oxide as raw materials, and mixing the superfine powder of the metal oxides and the alkali metal oxide to obtain the raw material;
when preparing a metal oxide ceramic matrix, selecting one metal oxide powder in metal oxides as a raw material, wherein the proportion of the metal oxide in the ingredients is not less than 60 wt%, and the rest of the ingredients which are not more than 40 wt% are prepared by taking one metal oxide powder or a plurality of metal oxide powders or one alkali metal oxide powder or other non-oxide powders as an additive or a sintering aid or a doping agent, mixing the powders to form the raw material, and sintering the raw material by a current thermal effect to finally prepare the ceramic matrix named by the metal oxides with the proportion of the ingredients of not less than 60 wt%;
when the complex phase oxide ceramic or mixed oxide ceramic is prepared, several kinds of oxide powder are selected to be mixed in oxide and alkali metal oxide to be used as raw materials, and the raw materials can form more than two crystal forms or more than two phases or a plurality of unreacted or incompletely reacted oxide ceramic materials through current thermal effect sintering;
step 2, preparation of a water-soluble metal inorganic salt saturated solution: respectively dissolving one or more water-soluble metal salts in distilled water at 4-60 ℃, uniformly stirring by using a magnetic stirrer, adding hydrochloric acid or nitric acid into the salt which is hydrolyzed to generate precipitate to adjust the pH value until the solution is clear, and preparing saturated solution of one or more water-soluble metal inorganic salts;
wherein in the selection of the water-soluble metal salt, the cation of the water-soluble metal salt is different from the valence of the cation of one or more selected metal oxides;
step 3, preparing an oxide superfine powder precursor and forming a wet blank:
respectively adding one or more saturated solutions of water-soluble metal salts into the mixed oxide powder raw materials, adding distilled water to adjust the water content to 50-90%, stirring the mixed powder of the water-containing oxides to be uniform, standing and aging for 0.5-24 hours, and then drying the wet mixed oxide powder at the temperature of 10-60 ℃ until the water content is 2-20% to obtain a metal oxide precursor; then putting the prepared metal oxide precursor into a mold, and applying pressure not more than 50MPa to mold the precursor to prepare a wet blank;
the total mass of the water-soluble metal salt accounts for 0.5-30 wt% of the total mass of the metal oxide superfine powder;
and 4, performing direct current or alternating current densification sintering on the oxide blank:
placing the formed wet blank between two electrodes connected with a direct current power supply or an alternating current power supply at 4-60 ℃, enabling the two electrodes to be in close contact with the blank, applying mechanical pressure to the electrodes to enable the pressure on the blank to be 0.1-30 MPa, turning on the power supply, adjusting the working state of the power supply to be in a constant current mode, adjusting the current limiting value to enable the current intensity applied to the two ends of the blank to be 0.5A/cm2～30A/cm2And heating and sintering the oxide blank under current, and electrifying for 0.1-30 min to obtain the oxide ceramic material with certain density.
2. The method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature according to claim 1, which is characterized in that: the alkali metal oxide is Li2O、Na2O、K2O、Rb2O、Cs2O。
3. The method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature according to claim 1, which is characterized in that: the alkaline earth metal oxide: BeO, MgO, CaO, SrO and BaO.
4. The method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature according to claim 1, which is characterized in that: the transition metal oxide includes: divalent transition metal oxide: ZnO, CuO, CdO, FeO, NiO, CoO, MnO or PbO; trivalent transition metal oxide: al (Al)2O3、Fe2O3、B2O3、V2O3、Cr2O3、In2O3、Sc2O3Or Ga2O3(ii) a Tetravalent transition metal oxide: ZrO (ZrO)2、TiO2、SiO2、GaO2、GeO2、HfO2、TaO2、VO2、MnO2Or SnO2(ii) a Pentavalent and hexavalent transition metal oxides: nb2O5、V2O5、Ta2O5Or WO3(ii) a Mixed-valence transition metal oxide: fe3O4、Mn3O4Or Co3O4。
5. The method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature according to claim 1, which is characterized in that: the rare earth metal oxide: y is2O3、Sc2O3、La2O3、Ce2O3、CeO2、Pr2O3、Nd2O3、Er2O3、EuO、Pm2O3、Eu2O3、Sm2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Tm2O3、Yb2O3Or Lu2O3。
6. The method for the oven-free rapid preparation of building blocks according to claim 1, wherein: the electrode is a flat plate electrode, wherein tiny circular through holes are uniformly distributed on the flat plate electrode, the diameter of each through hole is 1-5 mm, and the distribution density of the through holes is 0.5-1/cm2。
7. The method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature according to claim 1, which is characterized in that: the water-soluble metal salt is a water-soluble salt of an alkali metal, a water-soluble salt of an alkaline earth metal or various water-soluble salts of transition metal elements.
8. The composition according to claim 7, wherein the composition is at room temperatureThe method for preparing the oxide ceramic by furnace-free rapid sintering is characterized by comprising the following steps: water-soluble salts of the alkali metals: including alkali metal halide salts: ACl, a ═ Li, Na, K, Rb, Cs; or alkali metal sulfate: a. the2SO4A ═ Li, Na, K, Rb, Cs; or alkali metal nitrates: ANO3A ═ Li, Na, K, Rb, Cs; or an alkali metal carbonate: a. the2CO3A ═ Li, Na, K, Rb, Cs; or alkali metal phosphates: a. the3PO4A ═ Li, Na, K, Rb, Cs; or a water-soluble organic acid salt of an alkali metal.
9. The method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature according to claim 7, wherein: water-soluble salts of the alkaline earth metals: comprises the following halides: BCl2B ═ Mg, Ca, Sr, Ba; or an alkaline earth metal nitrate: b (NO)3)2，B＝Mg、Ca、Sr、Ba。
10. The method for preparing oxide ceramics by furnace-free rapid sintering at normal temperature according to claim 7, wherein: various water-soluble salts of the transition metal elements: comprises water-soluble halide salt, water-soluble sulfate, water-soluble nitrate or water-soluble phosphate of the transition metal elements of aluminum Al, zinc Zn, iron Fe, copper Cu, manganese Mn, nickel Ni, cobalt Co, indium In, tin Sn, antimony Sb, bismuth Bi or zirconium Zr.
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