CN102775140B - Method for preparing ion-sieve type conductive ceramic masterbatch - Google Patents
Method for preparing ion-sieve type conductive ceramic masterbatch Download PDFInfo
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Abstract
The invention discloses a method for preparing an ion-sieve type conductive ceramic masterbatch. The ion-sieve type conductive ceramic masterbatch of the nonstoichiometric compound is prepared from montmorillonite which serves as the substrate by subjecting the hydrochloric acid solution of yttrium oxide, barium carbonate and copper oxide to composite reaction with the swollen montmorillonite, washing, drying, forming and roasting. The ion-sieve type conductive ceramic masterbatch prepared by adopting the method has the advantages of oxidation resistance, corrosion resistance, radiation resistance, high temperature resistance and high chemical stability, is provided with a large amount of hole electrons on the surface, is an ideal electrical functional material and can be particularly applied to three-dimensional electrode reactors and other related fields.
Description
Technical field
The present invention relates to a kind of ion(ic)sieve type conductivity ceramics agglomerate preparation method, comprise yttrium oxide, barium carbonate, cupric oxide and hydrochloric acid are made into mixing solutions, sodium-based montmorillonite is distributed to swelling in the ionized water, yttrium oxide, barium carbonate, cupric oxide hydrochloric acid mixed solution are slowly added in the swelling polynite solution, through steps such as pressurize, centrifugation, drying, balling-up, calcinings, obtain ion(ic)sieve type conductivity ceramics master batch.
Background technology
Conducting ceramic material refers to possess ionic conduction in the stupalith, a kind of new function material of electronics, hole conduction.Conductivity ceramics integrates metal electric property and ceramic structure characteristic, have electric properties such as metalloid electroconductibility, the constitutional features that has simultaneously pottery again,, life-span length stable, high temperature resistant as chemical property, radioprotective, corrosion-resistant, anti-oxidant etc. can be widely used in fields such as electrode, gas sensor, ferroelectric material, superconducting material.At present, the preparation method of conductivity ceramics mainly contains sintering process, wet chemistry method, gaseous penetration method, microwave sintering method etc.
Nonstoichiometric compound is a kind of defective compound, is a branch of inorganic solid state chemistry, plays an important role in the type material the reach of science.The reason that nonstoichiometric compound forms has a lot,, metal short defective excessive as the metal of scarce negatively charged ion, the unequal defective of negative ions room number.Nonstoichiometric compound is conducive to the increase of electroconductibility, can be widely used in fields such as semi-conductor, magneticsubstance, optical function material, composite functional material.Utilize nonstoichiometric compound to make conducting ceramic material, will improve the electric property of conductivity ceramics greatly.
Summary of the invention
The technical problem to be solved in the present invention is, a kind of ion(ic)sieve type conductivity ceramics agglomerate preparation method is provided, and can prepare nonstoichiometric conducting ceramic material, improves the electric property of conducting ceramic material.
The technical solution adopted for the present invention to solve the technical problems is: a kind of ion(ic)sieve type conductivity ceramics agglomerate preparation method is provided, it is characterized in that, earlier prepare ion(ic)sieve type conductive powder with sodium-based montmorillonite, yttrium oxide powder, barium carbonate powder, cupric oxide powder, hydrochloric acid and deionized water, again this ion(ic)sieve type conductive powder is made a kind of ion(ic)sieve type conductivity ceramics master batch;
Described preparation ion(ic)sieve type conductive powder step is as follows:
A1, difference slowly add yttrium oxide powder 5%～8%, barium carbonate powder 13%～18%, cupric oxide powder 12%～18% in 1mol/L～3mol/L hydrochloric acid by weight percentage, constantly stir, make the hydrochloric acid mixed solution of yttrium oxide, barium carbonate, cupric oxide, the weight percent of hydrochloric acid is 20%～30%;
A2,80 orders～100 order sodium-based montmorillonites are evenly spread in the deionized water, fully stir, leave standstill 12h～24h and make it swelling, weight percent is sodium-based montmorillonite 10%～20%, deionized water 30%～40%;
A3, above-mentioned hydrochloric acid mixed solution is slowly added in the above-mentioned swelling polynite solution, leave standstill 12h～24h after constantly stirring;
A4, the solution after will leaving standstill are put into container, keep 3h～6h under 180 ℃～360 ℃ conditions;
A5, with above-mentioned solidliquid mixture cooling back centrifugation, being solid to deionized water wash does not have chlorion;
A6, above-mentioned solid is dry under 80 ℃～160 ℃ crosses 100 orders～120 mesh sieves and gets ion(ic)sieve type conductive powder;
Described preparation ion(ic)sieve type conductivity ceramics master batch step is as follows:
B1, above-mentioned ion(ic)sieve type conductive powder is added in the nodulizer, under the condition that constantly sprays into water smoke, is rotated into ball, the bead particle diameter more than or equal to 4 millimeters, smaller or equal to 9 millimeters;
B2, above-mentioned bead is put into retort furnace calcine, 600 ℃ to 800 ℃ of calcining temperatures, calcination time 2h～4h, then, press following program preserving temperature and reducing temperature: 600 ℃ to 800 ℃ of holding temperatures, soaking time 1h～2h, 400 ℃ to 600 ℃ of holding temperatures, soaking time 1h～2h, 200 ℃ to 400 ℃ of holding temperatures, soaking time 1h～2h;
B3, the bead after will calcining take out, and naturally cooling obtains ion(ic)sieve type conductivity ceramics master batch.
In ion(ic)sieve type conductivity ceramics agglomerate preparation method of the present invention, in steps A 3, " above-mentioned hydrochloric acid mixed solution is slowly added in the above swelling polynite solution " adopts separating funnel that slowly dropping mode of described hydrochloric acid mixed solution is realized.
In ion(ic)sieve type conductivity ceramics agglomerate preparation method of the present invention, in step B2, at 600 ℃ or 800 ℃ of calcining 2h～4h.
Implement ion(ic)sieve type conductivity ceramics agglomerate preparation method of the present invention, compared with the prior art, its beneficial effect is: adopting montmorillonite is matrix, utilizes ion-exchange with yttrium oxide (Y
2O
3), barium carbonate (BaCO
3), the hydrochloric acid soln of cupric oxide (CuO) and the reaction of the montmorillonite Composite after the swelling, again through processing such as washing, drying, moulding, roastings, make a kind of ion(ic)sieve type conductivity ceramics master batch of nonstoichiometric compound, have anti-oxidant, anticorrosive, radioprotective, high temperature resistant, chemical stability advantages of higher, there are a large amount of both hole and electrons in its surface, be as the ideal material of electric work energy material, be specially adapted to 3 D electrode reactor and other association areas.
Embodiment
The invention will be further described below in conjunction with embodiment.
Ion(ic)sieve type conductivity ceramics agglomerate preparation method of the present invention prepares ion(ic)sieve type conductive powder with sodium-based montmorillonite, yttrium oxide powder, barium carbonate powder, cupric oxide powder, hydrochloric acid and deionized water earlier, this ion(ic)sieve type conductive powder is made a kind of ion(ic)sieve type conductivity ceramics master batch again.
Embodiment one
(1) slowly add yttrium oxide (Y2O3) powder 5%, barium carbonate (BaCO3) powder 13%, cupric oxide (CuO) powder 12% in the hydrochloric acid 20% of 3mol/L respectively, constantly stir, the hydrochloric acid mixed solution of yttrium oxide, barium carbonate, cupric oxide (above-mentioned per-cent is weight percentage, down together).
(2) 80 order sodium-based montmorillonites 10% are evenly spread in the deionized water 40%, fully stir, leave standstill 24h and make it swelling.
(3) with separating funnel above-mentioned hydrochloric acid mixed solution slowly is added dropwise in the above-mentioned swelling polynite solution, constantly stirs, leave standstill 24h after evenly.
(4) solution after will leaving standstill is put into container, keeps 5h under 240 ℃ of conditions.
(5) with above-mentioned solidliquid mixture cooling back centrifugation, be solid to deionized water wash and do not have chlorion.
(6) above-mentioned solid is dry under 100 ℃, cross 120 mesh sieves and obtain ion(ic)sieve type conductive powder.
(7) above-mentioned ion(ic)sieve type conductive powder is added in the nodulizer, under the condition that constantly sprays into water smoke, is rotated into ball, the bead particle diameter more than or equal to 4 millimeters, smaller or equal to 9 millimeters.
(8) above-mentioned bead is put into retort furnace, behind 600 ℃ of calcining 4h, cooling process is as follows: 600 ℃ of insulation 2h, 400 ℃ of insulation 2h, 200 ℃ of insulation 2h.
(9) bead after will calcining takes out, and naturally cooling obtains ion(ic)sieve type conductivity ceramics master batch.
In step (3), except adopting separating funnel that hydrochloric acid mixed solution slowly is added dropwise to swelling polynite solution China and foreign countries, also can adopt other common methods that hydrochloric acid mixed solution is slowly added in the swelling polynite solution, down together.
Embodiment two
(1) slowly add yttrium oxide (Y2O3) powder 5%, barium carbonate (BaCO3) powder 13%, cupric oxide (CuO) powder 12% in the hydrochloric acid 30% of 2mol/L respectively, constantly stir, the hydrochloric acid mixed solution of yttrium oxide, barium carbonate, cupric oxide (above-mentioned per-cent is weight percentage, down together).
(2) 90 order sodium-based montmorillonites 10% are evenly spread in the deionized water 30%, fully stir, leave standstill 18h and make it swelling.
(3) with separating funnel above-mentioned hydrochloric acid mixed solution slowly is added dropwise in the above-mentioned swelling polynite solution, constantly stirs, leave standstill 18h after evenly.
(4) solution after will leaving standstill is put into container, keeps 6h under 360 ℃ of conditions.
(5) with above-mentioned solidliquid mixture cooling back centrifugation, be solid to deionized water wash and do not have chlorion.
(6) above-mentioned solid is dry under 80 ℃, cross 100 mesh sieves and obtain ion(ic)sieve type conductive powder.
(7) above-mentioned ion(ic)sieve type conductive powder is added in the nodulizer, under the condition that constantly sprays into water smoke, is rotated into ball, the bead particle diameter more than or equal to 4 millimeters, smaller or equal to 9 millimeters.
(8) above-mentioned bead is put into retort furnace, behind 700 ℃ of calcining 3h, cooling process is as follows: 700 ℃ of insulation 1.5h, 500 ℃ of insulation 1.5h, 300 ℃ of insulation 1.5h.
(9) bead after will calcining takes out, and naturally cooling obtains ion(ic)sieve type conductivity ceramics master batch.
Embodiment three
(1) slowly add yttrium oxide (Y2O3) powder 5%, barium carbonate (BaCO3) powder 13%, cupric oxide (CuO) powder 12% in the hydrochloric acid 20% of 1mol/L respectively, constantly stir, the hydrochloric acid mixed solution of yttrium oxide, barium carbonate, cupric oxide (above-mentioned per-cent is weight percentage, down together).
(2) 100 order sodium-based montmorillonites 20% are evenly spread in the deionized water 30%, fully stir, leave standstill 12h and make it swelling.
(3) with separating funnel above-mentioned hydrochloric acid mixed solution slowly is added dropwise in the above-mentioned swelling polynite solution, constantly stirs, leave standstill 12h after evenly.
(4) solution after will leaving standstill is put into container, keeps 3h under 180 ℃ of conditions.
(5) with above-mentioned solidliquid mixture cooling back centrifugation, be solid to deionized water wash and do not have chlorion.
(6) above-mentioned solid is dry under 160 ℃, cross 110 mesh sieves and obtain ion(ic)sieve type conductive powder.
(7) above-mentioned ion(ic)sieve type conductive powder is added in the nodulizer, under the condition that constantly sprays into water smoke, is rotated into ball, the bead particle diameter more than or equal to 4 millimeters, smaller or equal to 9 millimeters.
(8) above-mentioned bead is put into retort furnace, behind 800 ℃ of calcining 2h, cooling process is as follows: 800 ℃ of insulation 1h, 600 ℃ of insulation 1h, 400 ℃ of insulation 1h.
(9) bead after will calcining takes out, and naturally cooling obtains ion(ic)sieve type conductivity ceramics master batch.
In other embodiments, the weight percent of yttrium oxide powder, barium carbonate powder, cupric oxide powder, hydrochloric acid, sodium-based montmorillonite, deionized water also can adopt and include but not limited to following ratio combination:
Yttrium oxide powder 8%, barium carbonate powder 14%, cupric oxide powder 18%, hydrochloric acid 20%, sodium-based montmorillonite 10%, deionized water 30%.
Yttrium oxide powder 8%, barium carbonate powder 18%, cupric oxide powder 14%, hydrochloric acid 20%, sodium-based montmorillonite 10%, deionized water 30%.
Claims (3)
1. ion(ic)sieve type conductivity ceramics agglomerate preparation method, it is characterized in that, earlier prepare ion(ic)sieve type conductive powder with sodium-based montmorillonite, yttrium oxide powder, barium carbonate powder, cupric oxide powder, hydrochloric acid and deionized water, again this ion(ic)sieve type conductive powder is made a kind of ion(ic)sieve type conductivity ceramics master batch;
Described preparation ion(ic)sieve type conductive powder step is as follows:
A1, difference slowly add yttrium oxide powder 5%～8%, barium carbonate powder 13%～18%, cupric oxide powder 12%～18% in 1mol/L～3mol/L hydrochloric acid by weight percentage, constantly stir, make the hydrochloric acid mixed solution of yttrium oxide, barium carbonate, cupric oxide, the weight percent of hydrochloric acid is 20%～30%;
A2,80 orders～100 order sodium-based montmorillonites are evenly spread in the deionized water, fully stir, leave standstill 12h～24h and make it swelling, weight percent is sodium-based montmorillonite 10%～20%, deionized water 30%～40%;
A3, above-mentioned hydrochloric acid mixed solution is slowly added in the above-mentioned swelling polynite solution, leave standstill 12h～24h after constantly stirring;
A4, the solution after will leaving standstill are put into container, keep 3h～6h under 180 ℃～360 ℃ conditions;
A5, with above-mentioned solidliquid mixture cooling back centrifugation, being solid to deionized water wash does not have chlorion;
A6, above-mentioned solid is dry under 80 ℃～160 ℃ crosses 100 orders～120 mesh sieves and gets ion(ic)sieve type conductive powder;
Described preparation ion(ic)sieve type conductivity ceramics master batch step is as follows:
B1, above-mentioned ion(ic)sieve type conductive powder is added in the nodulizer, under the condition that constantly sprays into water smoke, is rotated into ball, the bead particle diameter more than or equal to 4 millimeters, smaller or equal to 9 millimeters;
B2, above-mentioned bead is put into retort furnace calcine, 600 ℃ to 800 ℃ of calcining temperatures, calcination time 2h～4h, then, press following program preserving temperature and reducing temperature: 600 ℃ to 800 ℃ of holding temperatures, soaking time 1h～2h, 400 ℃ to 600 ℃ of holding temperatures, soaking time 1h～2h, 200 ℃ to 400 ℃ of holding temperatures, soaking time 1h～2h;
B3, the bead after will calcining take out, and naturally cooling obtains ion(ic)sieve type conductivity ceramics master batch.
2. ion(ic)sieve type conductivity ceramics agglomerate preparation method as claimed in claim 1, it is characterized in that, in steps A 3, " above-mentioned hydrochloric acid mixed solution is slowly added in the above swelling polynite solution " adopts separating funnel that slowly dropping mode of described hydrochloric acid mixed solution is realized.
3. ion(ic)sieve type conductivity ceramics agglomerate preparation method as claimed in claim 1 or 2 is characterized in that, in step B2, at 600 ℃ or 800 ℃ of calcining 2h～4h.
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