CN109796198A - A kind of preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material - Google Patents
A kind of preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material Download PDFInfo
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- CN109796198A CN109796198A CN201910231932.XA CN201910231932A CN109796198A CN 109796198 A CN109796198 A CN 109796198A CN 201910231932 A CN201910231932 A CN 201910231932A CN 109796198 A CN109796198 A CN 109796198A
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- alumina ceramic
- zirconium oxide
- solution
- reinforced alumina
- ceramic material
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 35
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 35
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 43
- 239000011259 mixed solution Substances 0.000 claims abstract description 37
- 230000001376 precipitating effect Effects 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 15
- 239000003463 adsorbent Substances 0.000 claims abstract description 13
- 230000036571 hydration Effects 0.000 claims abstract description 12
- 238000006703 hydration reaction Methods 0.000 claims abstract description 12
- NZSLBYVEIXCMBT-UHFFFAOYSA-N chloro hypochlorite;zirconium Chemical class [Zr].ClOCl NZSLBYVEIXCMBT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 5
- 235000011194 food seasoning agent Nutrition 0.000 claims description 5
- 238000002390 rotary evaporation Methods 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 230000008450 motivation Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 10
- 238000004220 aggregation Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 7
- 239000000470 constituent Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 description 25
- 150000002500 ions Chemical class 0.000 description 20
- 238000005406 washing Methods 0.000 description 18
- 239000002245 particle Substances 0.000 description 15
- 239000000460 chlorine Substances 0.000 description 11
- 238000000975 co-precipitation Methods 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000007791 liquid phase Substances 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000013049 sediment Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 239000002243 precursor Substances 0.000 description 7
- 238000013019 agitation Methods 0.000 description 6
- 239000011268 mixed slurry Substances 0.000 description 6
- 239000012254 powdered material Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- CQGVSILDZJUINE-UHFFFAOYSA-N cerium;hydrate Chemical compound O.[Ce] CQGVSILDZJUINE-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000005056 compaction Methods 0.000 description 3
- 238000010612 desalination reaction Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052574 oxide ceramic Inorganic materials 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- RECVMTHOQWMYFX-UHFFFAOYSA-N oxygen(1+) dihydride Chemical compound [OH2+] RECVMTHOQWMYFX-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material, this method mixes after adding water to be configured to solution respectively eight hydration zirconium oxychlorides and six nitric hydrate ceriums, stirs evenly and ammonium hydroxide is added dropwise after forming mixed solution；After there is flocculent deposit, surfactant is added；Improved electric adsorbent equipment is fixed on to the top for containing precipitating mixed solution container, Cl extra in solution is removed using electric adsorption device stirring and adsorbing—、NH4 +、OH—And NO3 —；Supernatant is dehydrated remainder precipitating after drawing completely, obtains presoma；Dehydrated alcohol is added in presoma, adds nano alumina powder after mixing evenly and carries out ball milling, drying, be ground up, sieved, calcine and obtain Zirconia reinforced alumina ceramic powder；Material is sintered to obtain after molding.Present invention reduces the manufacturing cycles of powder, moreover it is possible to reduce powder because of powder hard aggregation caused by " salt bridge ", uniformity, the purity of powder constituents is effectively ensured.
Description
Technical field
The present invention relates to a kind of preparations of ceramic material, and in particular to a kind of cerium stabilizing zirconium oxide reinforced alumina ceramic material
Preparation method.
Background technique
Coprecipitation is that addition precipitating reagent (can be outer in mixed metal salt solution (i.e. two or more metal salt)
Add or inside generate), the uniform mixed precipitation of chemical composition is obtained, washed, dried, calcined (thermal decomposition) repeatedly, being answered
Close oxide.Compared with solid reaction process, chemical uniformity can be more made well and the powder of easy-sintering in coprecipitation, because of its work
Skill is simple and practical, production cost is not high, and can prepare raw material powder high-purity, ultra-fine, that composition is uniform, sintering character is good,
It is widely used in and prepares various oxide ceramics powders.But coprecipitation prepares the generation that ceramic powder is difficult to avoid that hard aggregation, especially
It is that remaining various salt foreign ion (Cl are remained in the liquid phase that precursor preparation process does not completely remove—、NH4 +、OH—、
NO3 —Deng) " salt bridge " that is formed between particle, it will make by the intergranular adhesion of hydrogen bond close adhesion is stronger can not
Point, and such aggregation procedure be it is irreversible, the compactness of sintered ceramic body is destroyed once being formed serious.
In the prior art application number of invention patent be 200810028209.3,201210218713.6,
201510895338.2,201711179729.X, 201810105686.9 etc. prepare the patent of ceramic powder using coprecipitation
In the step of being all made of water washing and precipitating remove extra Cl—、OH—Equal salts foreign ion finally obtains supernatant without Cl—And its
The presoma of his salt foreign ion is precipitated to carry out subsequent experimental operation.
Water washing and precipitating is " solution left standstill precipitating-precipitation and separation, supernatant-plus deionized water-stirring precipitation solution-
Staticly settle again " process, for preparing 500g cerium stabilizing zirconium oxide reinforced alumina ceramic powder, to make to sink as far as possible
The cerium hydroxide generated in the reaction of shallow lake and precipitated zirconium hydroxide whole sedimentation separation need to staticly settle for a long time；While in order to
Make in infall process in addition to be dispersed in supernatant, can also with sediment settle Cl—Removal effect more preferably, add deionized water
Whipping process afterwards will as far as possible uniformly, therefore (by stirring 4 hours, precipitating 8 was small 20 hours when water washing and precipitating is once at least cost
When estimate), and test the sediment after showing coprecipitation reaction after 8 washings, sedimentation, supernatant remains to examine
Test Cl—Presence.In fact, solution left standstill always has the part Cl for being partly adhered to sediment surface during precipitating—
Container bottom is deposited to sediment, and this part Cl—It can only be by further water-stirring-being added partially to be distributed to
It is possible to be removed in clear liquid, therefore the step of passing through water washing and precipitating reaches the clean extra Cl of removal—、OH—Equal salts are miscellaneous
The purpose of matter ion, it is necessary to just can reach by sufficient number of abundant washing, substantially prolong the experiment of ceramic powder preparation
Period, milling efficiency are extremely low.
Summary of the invention
It is remaining in liquid phase the purpose of the present invention is to provide the step of washing of precipitate, efficiently being removed in a kind of substitution original process
Salt foreign ion the method for preparing cerium stabilizing zirconium oxide reinforced alumina ceramic material.
The present invention utilizes improved electric adsorbent equipment, effectively removes during precursor preparation in supernatant and bottom precipitation
Remaining Cl—、NH4 +、NO3 —、OH—Etc. extra salt foreign ion, the time-consuming tediously long, effect of precipitating washing in the prior art is overcome
The low disadvantage of rate greatly shortens experimental period, improves milling efficiency, while the uniform of powder constituents can be effectively ensured
The consistency of ceramic material structure is obtained after property, purity and powder sintering.
Electro Sorb is potential difference between using the power on two electrode plates as driving force, and charged ion in solution is promoted to be adsorbed
To a kind of liquid desalting purification techniques on charged electrode surface, it is used for sewage treatment field, there is low energy consumption, additive-free, nothing
The features such as secondary pollution, while the electrode after ionic adsorption saturation can also realize secondary use by desorption and regeneration.The prior art
In application No. is disclosing a kind of electric adsorption device in 201811597909.4 patent of invention, device includes shell and is set to shell
The Electro Sorb component in internal portion；Lower part of the housing is equipped with inlet, top is equipped with liquid outlet；It is set in shell and above being located in the liquid inlet
There is liquid distributor, Electro Sorb component is located above liquid distributor, and is fixed with electrode fixing device.When electric adsorption device works, containing dirt
The aqueous solution for contaminating object is flowed into from the inlet of shell, keeps water-flow equation uniform by liquid distributor, passes through Electro Sorb group from top to bottom
After the adsorption treatment of part, flowed out from liquid outlet.Application No. is a kind of electricity suction is disclosed in 201810955489.6 patent of invention
Attached circulating water treatment device, device include circulating water treatment case and interval, are interspersed in the positive electricity of the both ends for the treatment of box energization
Pole and negative electrode, the two sides of circulating water treatment case are respectively equipped with inlet and outlet, positive electrode, negative electrode and circulating water treatment
Case is enclosed water stream channel, when electric adsorption device works, after the aqueous solution containing pollutant flows into treatment box by water inlet, in water
Ion or charged particle to the electrode transfer of oppositely charged and will be attracted, are stored in electrode surface electric double layer respectively,
To the purification desalination for reducing the dissolved salts concentration in the recirculated water in water stream channel, realizing liquid.
Since ceramic powder precursor solution is precipitating mixed solution, the receiving electrode in solution is easily settled, using existing skill
When electric adsorption device desalination in art, it is difficult to only realize precipitating mixed solution from the bottom up equal by the liquid distributor built in shell
Uniform flow is dynamic, while easily accumulation is deposited in entery and delivery port and cannot normally recycle with solution sediment in circulating water treatment case,
Adsorption effect is had a greatly reduced quality.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material, comprising the following steps:
1) it is mixed after adding water to be configured to solution respectively eight hydration zirconium oxychlorides and six nitric hydrate ceriums, stirs evenly to be formed
Ammonium hydroxide is added dropwise after mixed solution；
2) after there is flocculent deposit in solution, it is eight hydration zirconium oxychlorides and six that quality is added into precipitating mixed solution
The surfactant of nitric hydrate cerium total mass of raw material 2-5% continues stirring until the pH of solution is adjusted to 9.5-10.5, solution sinks
It forms sediment complete；
3) improved electric adsorbent equipment is fixed on to the top for containing precipitating mixed solution container, is stirred using electric adsorption device
It is adsorbed and removed Cl extra in solution—、NH4 +、OH—And NO3 —, to be adsorbed clean rear (with nothing in silver nitrate test solution
Cl—), it staticly settles；The improved electric adsorbent equipment includes that motor, turntable, anode electrode binding post, negative electrode connect
Terminal, negative el, anode electrode plate, motor switch, Electro Sorb switch and power supply, motor are connect with turntable, cathode
Electrode plate and anode electrode plate pass through negative electrode binding post respectively and anode electrode binding post is fixed on turntable bottom, power supply point
Not Lian Jie motor switch and Electro Sorb switch, motor switch is electrically connected with turntable；Electro Sorb switch and negative electrode wiring
Column is connected with anode electrode binding post；
4) after being drawn the supernatant of mixed solution after precipitating completely using siphonage, further centrifugation is precipitated to remainder and is taken off
Water, isolated presoma；
5) dehydrated alcohol is added in presoma, adds nano alumina powder after mixing evenly and carries out ball milling, drying, grinds
Mill, sieving, calcining obtain Zirconia reinforced alumina ceramic powder；
6) it forms；
7) atmospheric air atmosphere sintering obtains Zirconia reinforced alumina ceramic.
To further realize the object of the invention, it is preferable that Ce in mixed solution in step 1)3+With Zr4+Molar ratio be 4:
96~14:86.
Preferably, surfactant described in step 2) is any one in polyethylene glycol and ammonium polyacrylate.
Preferably, the adsorption time of Electro Sorb is 15-30min in step 3).
Preferably, the additive amount of dehydrated alcohol described in step 5) be every 100g presoma in be added 150ml-200ml without
Water-ethanol.
Preferably, the additive amount of alumina powder described in step 5) is the 80-90wt% of ceramic material.
Preferably, it is characterised in that: the revolving speed and Ball-milling Time of ball milling described in step 5) are respectively 400-500r/min
And 6-10h.
Preferably, dry described in step 5) is rotary evaporation seasoning, and drying temperature is 90 DEG C；Mistake described in step 5)
Sieve was 200 meshes.
Preferably, calcination temperature described in step 5) is 700 DEG C, and soaking time is 2 hours；Temperature is sintered described in step 7)
Degree is 1350-1550 DEG C, and soaking time is 2 hours.
Preferably, the plate spacing of the negative el and anode electrode plate is 1cm；The negative el and anode
Electrode plate is rectangle tabular.
The present invention has advantageous effect in that compared with prior art:
1) present invention has borrowed the Electro Sorb of sewage treatment field in the technique that coprecipitation prepares oxide ceramics
Mode replaces washing to achieve the purpose that remove salt foreign ion in presoma liquid phase, not only simplifies cerium stabilizing zirconium oxide toughening
The preparation process of aluminium oxide ceramics powder, the manufacturing cycle for shortening powder, the milling efficiency for improving coprecipitation, moreover it is possible to drop
Self raising flour material is effectively ensured after the uniformity, purity and powder sintering of powder constituents because of powder hard aggregation caused by " salt bridge "
To the consistency of ceramic material structure.
2) present invention effectively improves type electric adsorption device, makes it suitable for going for pulverizing process salt foreign ion
It removes, the electrode of the agitation electric adsorption device after modified can be rotated with disk, so that electrode is in uniform agitation precipitating mixed solution
Cleared dissolution salt foreign ion therein utmostly, is most efficiently adsorbed simultaneously.
Detailed description of the invention
Fig. 1 is improved electric adsorbent equipment figure.
Fig. 2 is the burnishing surface scanning electron microscope (SEM) photograph (SEM) of cerium stabilizing zirconium oxide reinforced alumina ceramic prepared by embodiment 1.
Fig. 3 is the burnishing surface scanning electron microscope (SEM) photograph of cerium stabilizing zirconium oxide reinforced alumina ceramic prepared by embodiment 2.
It is shown in figure: motor 1, turntable 2, anode electrode binding post 3, negative electrode binding post 4, negative el 5, just
Pole electrode plate 6, motor switch 7, Electro Sorb switch 8, power supply 9.
Specific embodiment
For a better understanding of the invention, the present invention is further illustrated with reference to the accompanying drawings and examples, but this hair
Bright embodiment is unlimited so.
As shown in Figure 1, a kind of improved electric adsorbent equipment, including motor 1, turntable 2, anode electrode binding post 3, cathode
Electrode terminal 4, negative el 5, anode electrode plate 6, motor switch 7, Electro Sorb switch 8 and power supply 9, motor 1 with
Turntable 2 connects, and negative el 4 and anode electrode plate 5 are solid by negative electrode binding post 4 and anode electrode binding post 3 respectively
Due to 2 bottom of turntable, power supply 9 is separately connected motor switch 7 and Electro Sorb switch 8, and motor switch 7 is electrically connected with turntable 2；
Electro Sorb switch 8 is connect with negative electrode binding post 4 and anode electrode binding post 3；It is preferred that the negative el 5 of rectangle tabular
Plate spacing with anode electrode plate 6 is 1cm.Motor 1 controls turntable rotation, Electro Sorb switch control by motor switch 7
The Electro Sorb of negative el 5 and anode electrode plate 6.
In use, improved electric adsorbent equipment need to be only fixed on to the top for containing precipitating mixed solution container, opened when simultaneously
When opening motor switch and Electro Sorb switch, the turntable 2 being connected with motor is started turning, and is fixed on the negative electricity of turntable bottom
Pole plate 5 and anode electrode plate 6 also rotate agitation precipitating mixed solution with turntable, while the Electro Sorb switch 8 for connecting power supply is opened
After anode electrode binding post 3 and negative electrode binding post 4 are charged, thus negative el 5 and anode electrode plate 6 also band
Electricity, precipitating chloride ion and other salt impurity charged particles in mixed solution will be attracted by the electrode of oppositely charged, is stored in
Cl in electrode surface electric double layer, in mixed solution to be precipitated—、NH4 +、NO3 —、OH—It is complete etc. the absorption of extra salt foreign ion
Afterwards, Electro Sorb process terminates, and the precipitating mixed solution after desalination can be carried out at next step by removing improved electric adsorbent equipment
Reason.
Embodiment 1
(1) add deionized water to be configured to solution respectively using eight hydration zirconium oxychlorides and six nitric hydrate ceriums as raw material, mix
Stirring 1h obtains mixed solution, Ce in mixed solution3+And Zr4+Molar ratio be 4:96, be added dropwise concentration be 0.1mol/L ammonia
Water.
(2) after there is flocculent deposit in solution, it is eight hydration zirconium oxychlorides and six nitric hydrate cerium raw materials that quality, which is added,
The polyethylene glycol of gross mass 3% continues stirring until the pH of solution is adjusted to 9.5-10.5, solution precipitating completely.
(3) improved electric adsorbent equipment is fixed on to the top for containing precipitating mixed solution container, opens motor switch 7,
The negative el 5 and anode electrode plate 6 for being fixed on 2 bottom of turntable rotate agitation with turntable 2 and precipitate mixed solution, Chlorine in Solution
Ion and other salt impurity charged particles are flowed about with solution in negative el 5 and anode electrode plate 6, open Electro Sorb
The negative el 5 and anode electrode plate 6 charged after switch 8 attracts chloride ion and other salt impurity bands in precipitating mixed solution
Charged particle is simultaneously stored in electrode surface electric double layer, adsorption time 30min, in silver nitrate test solution without Cl—Afterwards, it stands
Precipitating.
(4) after drawing the supernatant of mixed solution after precipitating completely using siphonage, further centrifugation is precipitated to remainder
Dehydration, isolated CeO2-ZrO2Aqueous precursor gel；
(5) dehydrated alcohol is added in presoma by addition 200ml dehydrated alcohol in every 100g aqueous precursor gel；Then it presses
According to ZrO2With Al2O3Molar ratio be 10:90 weigh alumina powder be added presoma in stir 1h；
(6) mixture of presoma, dehydrated alcohol and alumina powder is put into ball milling 6h in the planetary mills of 500r/min, obtained
To mixed slurry.Using rotary evaporation seasoning dry mixed slurry, drying temperature is 90 DEG C.
(7) gained powder after mill-drying, obtains preburning powdered material after crossing 200 meshes；
(8) 700 DEG C calcining preburning powdered material 2 hours, obtain cerium stabilizing zirconium oxide reinforced alumina ceramic powder.
(9) exist again after cerium stabilizing zirconium oxide reinforced alumina ceramic powder in step (8) is dry-pressing formed at 15MPa
Cold isostatic compaction under 200Mpa finally obtains cerium stabilizing zirconium oxide reinforced alumina ceramic in 1350 DEG C of sintering 2h.
After measured, the cerium stabilizing zirconium oxide reinforced alumina ceramic sample that embodiment 1 obtains, density reach 98.3%, by
The microstructure that the SEM characterization result of Fig. 2 obtains shows densification, and zirconia grains are uniformly dispersed, through Electro Sorb in preparation process
Liquid phase afterwards is difficult to detect Cl with silver nitrate—Presence, while the bending strength of material reaches 520MPa, be higher than application No. is
201510895338.2 coprecipitation for reaching removal salt foreign ion purpose by washing prepares cerium stabilizing zirconium oxide and increases
The 414MPa of bending strength peak in tough aluminium oxide ceramics patent, meanwhile, exist according to existing water-washing technique ceramic powder sample
Still there is Cl by 5 washings after precipitation reaction—, and primary complete washing experimentation at least needs 20 hours.The present embodiment
Using 1/200 of Electro Sorb method used time less than WATER-WASHING METHOD, many experiments time has not only been saved, it more can salt effectively in cleared liquid phase
Class foreign ion avoids because of the particle hard aggregation that salt bridge is formed between particle, is higher than existing same type of material mechanical property.
Embodiment 2
(1) add deionized water to be configured to solution respectively using eight hydration zirconium oxychlorides and six nitric hydrate ceriums as raw material, mix
Stirring 1h obtains mixed solution, Ce in mixed solution3+And Zr4+Molar ratio be 14:86, be added dropwise concentration be 0.1mol/L ammonia
Water.
(2) after there is flocculent deposit in solution, it is eight hydration zirconium oxychlorides and six nitric hydrate cerium raw materials that quality, which is added,
The ammonium polyacrylate of gross mass 3% continues stirring until the pH of solution is adjusted to 9.5-10.5, solution precipitating completely.
(3) improved electric adsorbent equipment is fixed on to the top for containing precipitating mixed solution container, opens motor switch 7,
The negative el 5 and anode electrode plate 6 for being fixed on 2 bottom of turntable rotate agitation with turntable 2 and precipitate mixed solution, Chlorine in Solution
Ion and other salt impurity charged particles are flowed about with solution in negative el 5 and anode electrode plate 6, open Electro Sorb
The negative el 5 and anode electrode plate 6 charged after switch 8 attracts chloride ion and other salt impurity bands in precipitating mixed solution
Charged particle is simultaneously stored in electrode surface electric double layer, adsorption time 15min, in silver nitrate test solution without Cl—, it is heavy to stand
It forms sediment.
(4) after drawing the supernatant of mixed solution after precipitating completely using siphonage, further centrifugation is precipitated to remainder
Dehydration, isolated CeO2-ZrO2Aqueous precursor gel；
(5) dehydrated alcohol is added in presoma by addition 150ml dehydrated alcohol in every 100g presoma, then according to m
(ZrO2): m (Al2O3)=20:80 is weighed in alumina powder addition presoma and is stirred 1h；
(6) mixture of presoma, dehydrated alcohol, alumina powder is put into ball milling 10h in the planetary mills of 400r/min, obtained
To mixed slurry.Using rotary evaporation seasoning dry mixed slurry, drying temperature is 90 DEG C；
(7) gained powder after mill-drying, obtains preburning powdered material after crossing 200 meshes；
(8) 700 DEG C calcining preburning powdered material 2 hours, obtain cerium stabilizing zirconium oxide reinforced alumina ceramic powder.
(9) after cerium stabilizing zirconium oxide reinforced alumina ceramic powder described in step (8) is dry-pressing formed at 15MPa again
The cold isostatic compaction at 200Mpa finally obtains cerium stabilizing zirconium oxide reinforced alumina ceramic in 1450 DEG C of sintering 2h.
After measured, the cerium stabilizing zirconium oxide reinforced alumina ceramic sample that embodiment 2 obtains, density reach 98.5%, by
The microstructure material that the SEM characterization result of Fig. 3 obtains is fine and close, and the liquid phase in preparation process after Electro Sorb is difficult to silver nitrate
Detect Cl—Presence, while material three-point bending resistance intensity reaches 599MPa；Application No. is 201510895338.2 Chinese inventions
Patent application cerium stabilizing zirconium oxide reinforced alumina ceramic as made from the coprecipitation of washing removal salt foreign ion is anti-
Curved intensity highest is just 414MPa, and 1/400 of the present embodiment Electro Sorb method used time less than WATER-WASHING METHOD, has not only been saved a large amount of
Experimental period, more can salt foreign ion effectively in cleared liquid phase, avoid because of the particle hard aggregation that salt bridge is formed between particle, it is high
In existing same type of material mechanical property.
Embodiment 3
(1) add deionized water to be configured to solution respectively using eight hydration zirconium oxychlorides and six nitric hydrate ceriums as raw material, mix
Stirring 1h obtains mixed solution, Ce in mixed solution3+And Zr4+Molar ratio be 8:92, be added dropwise concentration be 0.1mol/L ammonia
Water.
(2) after there is flocculent deposit in solution, it is eight hydration zirconium oxychlorides and six nitric hydrate cerium raw materials that quality, which is added,
The ammonium polyacrylate of gross mass 3% continues stirring until the pH of solution is adjusted to 9.5-10.5, solution precipitating completely.
(3) improved electric adsorbent equipment is fixed on to the top for containing precipitating mixed solution container, opens motor switch 7,
The negative el 5 and anode electrode plate 6 for being fixed on 2 bottom of turntable rotate agitation with turntable 2 and precipitate mixed solution, Chlorine in Solution
Ion and other salt impurity charged particles are flowed about with solution in negative el 5 and anode electrode plate 6, open Electro Sorb
The negative el 5 and anode electrode plate 6 charged after switch 8 attracts chloride ion and other salt impurity bands in precipitating mixed solution
Charged particle is simultaneously stored in electrode surface electric double layer, adsorption time 25min, in silver nitrate test solution without Cl—, it is heavy to stand
It forms sediment.
(4) after drawing the supernatant of mixed solution after precipitating completely using siphonage, further centrifugation is precipitated to remainder
Dehydration, isolated CeO2-ZrO2Aqueous precursor gel；
(5) dehydrated alcohol is added in presoma by addition 175ml dehydrated alcohol in every 100g presoma, then according to m
(ZrO2): m (Al2O3)=15:85 is weighed in alumina powder addition presoma and is stirred 1h；
(6) mixture of presoma, dehydrated alcohol, alumina powder is put into ball milling 8h in the planetary mills of 450r/min, obtained
To mixed slurry.Using rotary evaporation seasoning dry mixed slurry, drying temperature is 90 DEG C；
(7) gained powder after mill-drying, obtains preburning powdered material after crossing 200 meshes；
(8) 700 DEG C calcining preburning powdered material 2 hours, obtain cerium stabilizing zirconium oxide reinforced alumina ceramic powder.
(9) after cerium stabilizing zirconium oxide reinforced alumina ceramic powder described in step (8) is dry-pressing formed at 15MPa again
The cold isostatic compaction at 200Mpa finally obtains cerium stabilizing zirconium oxide reinforced alumina ceramic in 1450 DEG C of sintering 2h.
After measured, the cerium stabilizing zirconium oxide reinforced alumina ceramic sample that embodiment 3 obtains, density reach 98.5%, material
Expect that microstructure is fine and close, the liquid phase in preparation process after Electro Sorb is difficult to detect Cl with silver nitrate—Presence, while material
Three-point bending resistance intensity reaches 705MPa；Application No. is reached when 201510895338.2 Chinese invention patent application by washing
Cerium stabilizing zirconium oxide reinforced alumina ceramic bending strength peak made from coprecipitation except salt foreign ion
414MPa, and the Electro Sorb method used time of the present embodiment less than the 1/250 of prior art WATER-WASHING METHOD, not only saved many experiments
Time, more can salt foreign ion effectively in cleared liquid phase, avoid because of the particle hard aggregation that salt bridge is formed between particle, be higher than existing
There is same type of material mechanical property.
Embodiment of the present invention are not limited by the above embodiments, other any real without departing from spirit of the invention
Made changes, modifications, substitutions, combinations, simplifications under matter and principle, should be equivalent substitute mode, are included in the present invention
Protection scope within.
Claims (10)
1. a kind of preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material, it is characterised in that the following steps are included:
1) it is mixed after adding water to be configured to solution respectively eight hydration zirconium oxychlorides and six nitric hydrate ceriums, stirs evenly to form mixing
Ammonium hydroxide is added dropwise after solution；
2) after there is flocculent deposit in solution, it is eight hydration zirconium oxychlorides and six hydrations that quality is added into precipitating mixed solution
The surfactant of cerous nitrate total mass of raw material 2-5% continues stirring until the pH of solution is adjusted to 9.5-10.5, solution has precipitated
Entirely；
3) improved electric adsorbent equipment is fixed on to the top for containing precipitating mixed solution container, using electric adsorption device stirring and adsorbing
Remove Cl extra in solution—、NH4 +、OH—And NO3 —, to be adsorbed completely (to use in silver nitrate test solution without Cl afterwards—), it is quiet
Set precipitating；The improved electric adsorbent equipment includes motor, turntable, anode electrode binding post, negative electrode binding post, bears
Pole electrode plate, anode electrode plate, motor switch, Electro Sorb switch and power supply, motor connect with turntable, negative el with
Anode electrode plate passes through negative electrode binding post respectively and anode electrode binding post is fixed on turntable bottom, and power supply is separately connected electricity
Motivation switch and Electro Sorb switch, motor switch are electrically connected with turntable；Electro Sorb switch and negative electrode binding post and anode
Electrode terminal connection；
4) after drawing the supernatant of mixed solution after precipitating completely using siphonage, further centrifugal dehydration is precipitated to remainder,
Isolated presoma；
5) dehydrated alcohol is added in presoma, adds nano alumina powder after mixing evenly and carries out ball milling, drying, grinding, mistake
Sieve, calcining obtain Zirconia reinforced alumina ceramic powder；
6) it forms；
7) atmospheric air atmosphere sintering obtains Zirconia reinforced alumina ceramic.
2. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
Ce in mixed solution in step 1)3+With Zr4+Molar ratio be 4:96~14:86.
3. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
Surfactant described in step 2) is any one in polyethylene glycol and ammonium polyacrylate.
4. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
The adsorption time of Electro Sorb is 15-30min in step 3).
5. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
The additive amount of dehydrated alcohol described in step 5) is that 150ml-200ml dehydrated alcohol is added in every 100g presoma.
6. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
The additive amount of alumina powder described in step 5) is the 80-90wt% of ceramic material.
7. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
It is characterized by: the revolving speed and Ball-milling Time of ball milling described in step 5) are respectively 400-500r/min and 6-10h.
8. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
Dry described in step 5) is rotary evaporation seasoning, and drying temperature is 90 DEG C；Sieving was 200 meshes described in step 5).
9. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, it is characterised in that:
Calcination temperature described in step 5) is 700 DEG C, and soaking time is 2 hours；Sintering temperature described in step 7) is 1350-1550
DEG C, soaking time is 2 hours.
10. the preparation method of cerium stabilizing zirconium oxide reinforced alumina ceramic material according to claim 1, feature exist
In: the plate spacing of the negative el and anode electrode plate is 1cm；The negative el and anode electrode plate are rectangular
Shape plate.
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| CN112876272A (en) * | 2021-02-07 | 2021-06-01 | 新化县新天地精细陶瓷有限公司 | Preparation method of heterogeneous core-shell structure toughening agent, alumina ceramic material, preparation method and application |
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| CN103290353A (en) * | 2013-06-18 | 2013-09-11 | 张关莲 | Method for preparing corrosion-resistant zirconium oxide thermal barrier coating |
| CN103708831A (en) * | 2013-09-28 | 2014-04-09 | 雅安远创陶瓷有限责任公司 | Yttria-stabilized zirconia powder and preparation method thereof |
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| CN102718470A (en) * | 2012-06-29 | 2012-10-10 | 华南理工大学 | Spray granulation preparation method for zirconium oxide toughened aluminum oxide powder |
| CN103290353A (en) * | 2013-06-18 | 2013-09-11 | 张关莲 | Method for preparing corrosion-resistant zirconium oxide thermal barrier coating |
| CN103708831A (en) * | 2013-09-28 | 2014-04-09 | 雅安远创陶瓷有限责任公司 | Yttria-stabilized zirconia powder and preparation method thereof |
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| CN112876272A (en) * | 2021-02-07 | 2021-06-01 | 新化县新天地精细陶瓷有限公司 | Preparation method of heterogeneous core-shell structure toughening agent, alumina ceramic material, preparation method and application |
| CN112876272B (en) * | 2021-02-07 | 2022-06-10 | 新化县新天地精细陶瓷有限公司 | Preparation method of heterogeneous core-shell structure toughening agent, alumina ceramic material, preparation method and application |
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