CN101767982A - Method for improving aluminium oxide ceramic abrasive resistance by precipitation reaction - Google Patents
Method for improving aluminium oxide ceramic abrasive resistance by precipitation reaction Download PDFInfo
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- CN101767982A CN101767982A CN201010004922A CN201010004922A CN101767982A CN 101767982 A CN101767982 A CN 101767982A CN 201010004922 A CN201010004922 A CN 201010004922A CN 201010004922 A CN201010004922 A CN 201010004922A CN 101767982 A CN101767982 A CN 101767982A
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Abstract
The invention relates to a method for preparing aluminium oxide ceramics with good wear-resisting property, that is, low-cost soluble salt is added in slurry which takes water and aluminum oxide as main raw material, and then dehydration pelleting, molding and sintering are carried out; the specific method is that: one working procedure is added after ball-milling procedure and before pelleting procedure in the original preparation process; proper salt which can be dissolved in water and generates metal ions is added in the slurry with qualified fineness and viscosity by ball-milling; the added metal salt can be one, part or all of magnesium salt, calcium salt, yttrium salt, aluminum salt, strontium salt, barium salt, zircon salt, cerium alt and lanthanum salt, the total adding amount accounts for 0.1-30 percent of the alumina powder material, and the optimized adding amount is from 2 percent to 20 percent; the added precipitators can be one, partial or all of sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium fluoride, sodium sulfide, sodium silicate, sodium aluminate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, calcium hydroxide, calcium oxide, barium hydroxide, ammonia, ammonium carbonate, ammonium hydrogencarbonate, ammonium fluoride, ammonium sulfide and carbamide, the total adding amount accounts for 0.05-20 percent of the alumina powder material quantity, and the optimized adding amount is 1-10 percent.
Description
Technical field
The present invention relates to a kind of by generating precipitation at the slurry internal reaction to improve porcelain spare flexible preparation method.More particularly, this patent relate to a kind of with low-cost soluble salt add in the slurry based on water and aluminum oxide, again through dewater granulation, moulding, burn till, make the method for the alumina-ceramic that possesses excellent wear-resisting property.The field that belongs to fine ceramics in the ceramic.
Background technology
Alumina-ceramic is with α-Al
2O
3Be the oxide ceramics that essential mineral is formed, have that Young's modulus is big, the utmost point is not easy distortion, a Heat stability is good, strong, the lower-price characteristic of high temperature oxidation resistance, therefore, be subjected to people's favor deeply.Alumina-ceramic is one of the widest fine ceramics material of present turnout maximum in the world, application surface, is widely used in fields such as aerospace, the energy, biology, metallurgy, electronics, chemistry, chemical industry.In wear resistance applications, the alumina-ceramic ball is widely used in the material ball milling operation of industries such as white cement, mineral and pottery, electronic material, magneticsubstance and coating, paint, makeup, food, pharmacy as grinding medium.
Bonding force between the inner atom of stupalith is based on ionic linkage, and ionic linkage has very strong directivity and very high bound energy, causes viscous deformation difficulty, fragility big; The energy of crack growth is little, in breaking-down process, except increasing new fracture surface energy, the mechanism that does not almost have other dissipation energy, lack that works shifts the viscous deformation mechanism of energy by independently dislocation, sliding system as metal, toughness is very poor, uses in engineering to occur brittle rupture often, the weakness that this is fatal causes it can not stand huge mechanical shock and thermal shocking.
From view point of fracture mechanics, the fragility that overcomes pottery with the key that improves its intensity is: (1) improves the ability of stupalith opposing crack propagation; (2) slow down the stress concentration effect of crack tip.The former mainly is the energy-to-break that improves material, and the latter's key is to reduce the yardstick of the contained crack defect of material internal.At present common several toughness reinforcing mode mainly contains that transformation toughening, particle dispersion are toughness reinforcing, whisker (chopped strand) composite toughening and continuous fibre are toughened and reinforced etc.Crystal whisker toughenedly be difficult to solve whisker toxicity and the uniform distribution in matrix thereof, when the whisker too high levels, the densification of the stupalith difficulty that will become; The fiber reinforced effect that will obtain must be fiber abundant dipping and evenly arranging in matrix, but this be difficult on technology realize that fiber reinforced quality is difficult to control.
The toughness reinforcing mechanism of particle dispersion comprises out-phase (i.e. second phase of introducing in mutually at principal crystalline phase-matrix) particle to the effect of crackle nail nipping bundle, dissipation crackle progressive power; Simultaneously, stop lateral cross section to be shunk when particle is stretched in matrix, consume more energy.
A little less than the particle at stupalith crystal boundary place was got in touch than intragranular particle, it destroyed always based on intercrystalline fracture; Stressed during at material along intercrystalline failure, the crack propagation distance be make a circulation, zigzag.Crystal grain is more little, and the expansion distance is longer, and therefore toughness be improved, and wear resistance is also just good more, so wear-resistant ceramic just develops towards the micritization direction.The porcelain ball that wear resistance is good requires not only that crystal grain is little and even, intercrystalline bonding strength height, density height, few, the smooth surface of pore, and will have higher fracture toughness property and hardness, lower Young's modulus.
The ceramics personnel have proposed several different methods increases ceramics toughness, but wherein the good method of toughening effect often cost is very high.As seen ceramic toughening method research cheaply is task a kind of not only heavy but also that need to adhere to long-term endeavour.
Application number is that 200510024330.5 Chinese invention patent relates to a kind of nano crystal adding alumina ceramic material and low temperature liquid phase sintering process, although can low-temperature sintering, needs to add the nanocrystalline aluminum oxide that adds the wet chemistry method preparation, cost height.Application number is that 200710118742.4 Chinese invention patent relates to a kind of alumina-ceramic and preparation method thereof, is 99.9% or above alpha's alumina raw material but need purity, and the sintering temperature height.Application number is 200810021162.8 Chinese invention patent proposition: by the meticulous control to impurity in the alumina-ceramic and sintering process, make part crystal grain at some specific direction preferential growths, form crystal grain big L/D ratio, similar whisker, reach the crystal whisker excess weld metal effect, can solve the insufficient shortcoming of wear-resisting alumina ceramic toughness, but need in advance with aluminium hydroxide or boehmite and acidic cpd reaction carrying out part solation, again water is evaporated the generation xerogel, this just consumes too many water and evaporation institute heat requirement.Application number is 200710178148.4 Chinese invention patent proposition, with nanometer aluminium powder and high purity aluminium oxide powder is initial feed, grind, be configured as base substrate, with base substrate sintering in common air calcination stove, obtain having the alumina-ceramic of growth in situ long column shape, tabular crystalline substance, keep traditional fibre and the tangible toughened and reinforced effect of whisker, solve fiber, whisker and carbon nanotube simultaneously and using the difficulty of bringing on the technology.But its nanometer aluminium powder that needs also is the higher raw material of cost.
The objective of the invention is to adopt lower-cost raw material and preparation technology to make the fine-grain that has contained toughening effect, thereby the alumina-ceramic of higher toughness and wear resisting property is arranged.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of method new, that increase aluminium oxide ceramic abrasive resistance.Generally adopt in the industry, existing processes comprises seven procedures: batching=＞ball milling=＞granulation=＞old=＞moulding=＞dry=＞burn till; Technology of the present invention be after ball milling and granulation before increase by a procedure: in the ball milling slurry qualified, add salt and the precipitation agent thereof that an amount of water soluble produces metal ion to fineness, viscosity; In other words, technology of the present invention comprises eight procedures: batching=＞ball milling=＞add metal-salt and precipitation agent thereof=＞granulation=＞old=＞moulding=＞dry=＞burn till.
The metal-salt that the present invention adds in grinding qualified slurry can be following salt a kind of, part or all:
Magnesium chloride, magnesium nitrate, calcium chloride, nitrocalcite, Yttrium trichloride, Yttrium trinitrate, aluminum chloride, aluminum nitrate, strontium chloride, strontium nitrate, bariumchloride, nitrate of baryta, zirconium oxychloride, zirconium nitrate, zirconium sulfate, ceric ammonium nitrate, lanthanum nitrate.
Total dosage of various metal-salts accounts for 0.1% to 30% of alumina powder quality, and preferred dosage is 2% to 20%.
The precipitation agent that the present invention adds in grinding qualified slurry can be following salt, bases a kind of, part or all:
Sodium hydroxide, yellow soda ash, sodium bicarbonate, Sodium Fluoride, sodium sulphite, water glass, sodium aluminate, potassium hydroxide, salt of wormwood, potassium silicate, lithium hydroxide, Quilonum Retard, calcium hydroxide, calcium oxide, hydrated barta, ammoniacal liquor, volatile salt, ammonium hydrogencarbonate, Neutral ammonium fluoride, ammonium sulfide, urea.
The precipitation agent dosage accounts for 0.05% to 20% of alumina powder quality, and preferred dosage is 1% to 10%.
By as seen above-mentioned, metal-salt of the present invention mainly is some more common, common cheap water-soluble inorganic salts, its effect is to generate the fine precipitation that contains coherent element with the precipitation agent reaction, these precipitations are entrained in the gap of alumina particle or attached on the alumina particle surface, and its dispersed uniform and stability are than for toughness reinforcing and to add fiber, whisker, nano-powder etc. in slip much easier; In sintering process, these precipitations can be converted into magnesium oxide, magnesium fluoride, calcium oxide, Calcium Fluoride (Fluorspan), strontium oxide, strontium fluoride, barium fluoride, barium oxide, zirconium white, yttrium oxide, cerium oxide, Calucium Silicate powder, Calucium Silicate powder, Magnesium Silicate q-agent, strontium silicate, barium silicate, lanthanum trioxide, spinel, the fine-grain of mullite etc., these crystal grain on the one hand can the promotes oxidn aluminium grain sintering and stop alumina grain excessively to be grown up, can hinder on the other hand owing to the extension of the stressed tiny crack that produces of pottery between alumina grain, promptly to the effect of crackle nail nipping bundle, dissipation crackle progressive power; Simultaneously, these fine-grains also stop lateral cross section to be shunk when pottery is stretched, and consume more energy.More than the effect of three aspects all help increasing the toughness and the wear resistance of aluminium oxide ceramic products.
Some personage can be talkative in the industry, for microstructure and the use properties of improving product, the prior art of alumina-ceramic preparation just usually adds an amount of magnesium oxide in first procedure (batching), barium oxide, zirconium white, yttrium oxide, cerium oxide, Magnesium Silicate q-agent, mullite etc., the application also utilizes these oxide compounds and salt, does this overlap with prior art? if overlap, does the method that the application proposed possess novelty so? in order to illustrate that the method that the application proposes possesses novelty, here point out emphatically: the material that prior art is added is water-insoluble oxide compound and salt, be at burden process the opportunity of adding, and adds the back and grind jointly with aluminum oxide; And the material that the present invention adds is water miscible industrial chemicals, the opportunity of interpolation be after grinding step with the dehydration granulating working procedure before.Method of the present invention is compared with the prior art of adding oxide compound and salt, has the following points difference at least: the substance classes difference that add (1); (2) difference on opportunity of Tian Jiaing, operation difference; (3) there was the form difference in the material that is added before sintering, thereby the effect difference in the material embryo.
Embodiment
Below the specific embodiment of the present invention is illustrated, used various starting material all are the industrial goods bought of hook from the market.
Embodiment 1
The first step: take by weighing 1000kg alpha aluminum oxide, 51kg kaolin, 19kg talcum powder, other auxiliary material of 7kg by existing processes, wet ball grinding 48 hours, slip meta particle diameter is 1.49 microns after measured, being coated with-4 viscosity is 13 " 86; Slip is put into the stirring material storage container from the ball milling filling.
Second step:, take by weighing following raw materials according successively and add and stir material storage container: Magnesium dichloride hexahydrate 35kg, six hydration calcium chloride 3kg, Yttrium trichloride 0.8kg, Aluminium chloride hexahydrate 4kg, water glass (modulus is 2.4 bubble flower alkali) 10kg by technology of the present invention.
The 3rd step: add polyvinyl alcohol water solution (5wt%) 60kg by existing processes in slip, carry out mist projection granulating, old after stirring, rolling is shaped to the ball of diameter 6-16 millimeter, and burn till at 1460 ℃ dry back.
More than prepared porcelain ball be 0.15% from abrasion, and do not adopt above-mentioned second step add metal-salt with precipitation agent, only to adopt the above the first step and prepared porcelain ball of the 3rd step be 0.39% from wearing away.
Embodiment 2
The first step: take by weighing 1000kg alpha aluminum oxide, 51kg kaolin, 19kg talcum powder, other auxiliary material of 7kg by existing processes, wet ball grinding 48 hours, slip meta particle diameter is 1.43 microns after measured, being coated with-4 viscosity is 13 " 98; Slip is put into the stirring material storage container from the ball milling filling.
Second step:, take by weighing following raw materials according successively and add and stir material storage container: Magnesium dichloride hexahydrate 8kg, six hydration calcium chloride 2kg, six hydration Yttrium trichloride 1.5kg, eight hydration zirconium oxychloride 75kg, Neutral ammonium fluoride 5kg, volatile salt 27kg by technology of the present invention.
The 3rd step: add polyvinyl alcohol water solution (5wt%) 60kg by existing processes in slip, carry out mist projection granulating, old after stirring, rolling is shaped to the ball of diameter 6-16 millimeter, and burn till at 1500 ℃ dry back.
More than prepared porcelain ball be 0.13% from abrasion.
Embodiment 3
The first step: take by weighing 1000kg alpha aluminum oxide, 51kg kaolin, 19kg talcum powder, other auxiliary material of 7kg by existing processes, wet ball grinding 48 hours, slip meta particle diameter is 1.62 microns after measured, being coated with-4 viscosity is 13 " 27; Slip is put into the stirring material storage container from the ball milling filling.
Second step:, take by weighing following raw materials according successively and add and stir material storage container: magnesium nitrate hexahydrate 38kg, six nitric hydrate yttrium 1.8kg, water glass (modulus is 2.4 bubble flower alkali) 9kg by technology of the present invention.。
The 3rd step: add polyvinyl alcohol water solution (5wt%) 60kg by existing processes in slip, carry out mist projection granulating, old after stirring, rolling is shaped to the ball of diameter 6-16 millimeter, and burn till at 1450 ℃ dry back.
More than prepared porcelain ball be 0.18% from abrasion.
Comparative Examples
The first step: take by weighing 1000kg alpha aluminum oxide, 51kg kaolin, 19kg talcum powder, other auxiliary material of 7kg by existing processes; Magnesium oxide 5.9kg (the magnesium elements mole number that provides with the added magnesium nitrate hexahydrate of second step of embodiment 3 is identical); Yttrium oxide 0.4kg (the yttrium mole number that provides with embodiment 3 added six nitric hydrate yttriums is identical); White carbon black (nano silicon oxide) 2.7kg, sodium bicarbonate 7.3kg (element silicon, the sodium element mole number that provides with embodiment 3 added water glass is identical respectively).Wet ball grinding 48 hours, slip meta particle diameter is 1.60 microns after measured, being coated with-4 viscosity is 13 " 29; Slip is put into the stirring material storage container from the ball milling filling.
Second step: add polyvinyl alcohol water solution (5wt%) 60kg by existing processes in slip, carry out mist projection granulating, old after stirring, rolling is shaped to the ball of diameter 6-16 millimeter, and burn till at 1450 ℃ dry back.
More than prepared porcelain ball be 0.31% from abrasion.The porcelain ball of this Comparative Examples preparation is identical with the porcelain ball composition of embodiment 3 preparations, ball milling, granulation, moulding, firing process are identical, only be physical form difference, the interpolation difference on opportunity of adding for magnesium, yttrium, silicon, these four kinds of elements of sodium are provided in the porcelain ball, it is more very different than embodiment 3 that obviously this Comparative Examples improves the effect of porcelain ball wear resistance.
By above embodiment, Comparative Examples as seen, the present invention adds the product of metal-salt and precipitation agent and compares with the product that does not only add metal-salt and precipitation agent by existing technology between this two procedures of ball milling-granulation, and abrasion reduce by more than 50 certainly.It is above to be that wear resisting property doubles, and this is the practicality place of method therefor of the present invention.
The foregoing description is used for the explanation to claim, but is not the qualification that is used for claim, and protection scope of the present invention should be as the criterion with claims.
Claims (5)
1. method that improves aluminium oxide ceramic abrasive resistance by precipitin reaction, it is characterized in that and generally to adopt in the industry, existing processes seven procedures (refer to: batching=ball milling=granulation=old=moulding=dry=burn till) change into eight procedures: batching=ball milling=add metal-salt and precipitation agent thereof=granulation=old=moulding=dry=burn till i.e. increase by one procedure ball milling after and before the granulation: to ball milling to fineness, interior salt and the precipitation agent thereof that adds an amount of water soluble generation metal ion of the slurry that viscosity is qualified.
2. according to claim 1ly a kind ofly improve the method for aluminium oxide ceramic abrasive resistance by precipitin reaction, it is characterized in that the metal-salt that in grinding qualified slurry, adds be following salt a kind of, part or all:
Magnesium chloride, magnesium nitrate, calcium chloride, nitrocalcite, Yttrium trichloride, Yttrium trinitrate, aluminum chloride, aluminum nitrate, strontium chloride, strontium nitrate, bariumchloride, nitrate of baryta, zirconium oxychloride, zirconium nitrate, zirconium sulfate, ceric ammonium nitrate, lanthanum nitrate.
3. according to claim 1ly a kind ofly improve the method for aluminium oxide ceramic abrasive resistance by precipitin reaction, it is characterized in that the precipitation agent that in grinding qualified slurry, adds be following salt, bases a kind of, part or all:
Sodium hydroxide, yellow soda ash, sodium bicarbonate, Sodium Fluoride, sodium sulphite, water glass, sodium aluminate, potassium hydroxide, salt of wormwood, potassium silicate, lithium hydroxide, Quilonum Retard, calcium hydroxide, calcium oxide, hydrated barta, ammoniacal liquor, volatile salt, ammonium hydrogencarbonate, Neutral ammonium fluoride, ammonium sulfide, urea.
4. a kind of method that improves aluminium oxide ceramic abrasive resistance by precipitin reaction according to claim 1, the total dosage that it is characterized in that the metal-salt that adds in grinding qualified slurry accounts for 0.1% to 30% of alumina powder quality, and preferred dosage is 2% to 20%.
5. a kind of method that improves aluminium oxide ceramic abrasive resistance by precipitin reaction according to claim 1, it is characterized in that the total dosage of precipitation agent that adds in grinding qualified slurry accounts for 0.05% to 20% of alumina powder quality, preferred dosage is 1% to 10%.
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| CN102821550A (en) * | 2012-08-25 | 2012-12-12 | 佛山市煜丰机械有限公司 | Nanostructure composite LED (Light Emitting Diode) ceramic substrate and manufacturing method thereof |
| CN104845584A (en) * | 2015-01-06 | 2015-08-19 | 朱晖 | Nonmetal grinding medium for cement grinding, and application thereof |
| CN105536662A (en) * | 2015-12-30 | 2016-05-04 | 西安科技大学 | Preparation method of microcapsules |
| CN107032818A (en) * | 2017-02-28 | 2017-08-11 | 韦尧天 | A kind of heat-insulation and heat-preservation ceramics and preparation method thereof |
| CN109437930A (en) * | 2018-12-13 | 2019-03-08 | 云南大学 | The utilization of the uniform dispersing method of sintering aid and the sintering aid in this method |
| CN111410538A (en) * | 2020-05-08 | 2020-07-14 | 潍坊工商职业学院 | Toughened silicon carbide ceramic and preparation method thereof |
| CN112062548A (en) * | 2020-09-28 | 2020-12-11 | 成都万士达瓷业有限公司 | Production method of Al2O3 ceramic green body |
| CN115572151A (en) * | 2022-10-10 | 2023-01-06 | 淄博和润马科托矿业技术有限公司 | Microcrystalline alumina grinding medium and preparation method thereof |
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2010
- 2010-01-18 CN CN201010004922A patent/CN101767982A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102821550A (en) * | 2012-08-25 | 2012-12-12 | 佛山市煜丰机械有限公司 | Nanostructure composite LED (Light Emitting Diode) ceramic substrate and manufacturing method thereof |
| CN102821550B (en) * | 2012-08-25 | 2014-12-10 | 佛山市煜丰机械有限公司 | Nanostructure composite LED (Light Emitting Diode) ceramic substrate and manufacturing method thereof |
| CN104845584A (en) * | 2015-01-06 | 2015-08-19 | 朱晖 | Nonmetal grinding medium for cement grinding, and application thereof |
| CN105536662A (en) * | 2015-12-30 | 2016-05-04 | 西安科技大学 | Preparation method of microcapsules |
| CN105536662B (en) * | 2015-12-30 | 2017-12-12 | 西安科技大学 | A kind of preparation method of microcapsules |
| CN107032818A (en) * | 2017-02-28 | 2017-08-11 | 韦尧天 | A kind of heat-insulation and heat-preservation ceramics and preparation method thereof |
| CN109437930A (en) * | 2018-12-13 | 2019-03-08 | 云南大学 | The utilization of the uniform dispersing method of sintering aid and the sintering aid in this method |
| CN109437930B (en) * | 2018-12-13 | 2021-07-02 | 云南大学 | Method for homogeneously dispersing sintering aid and use of sintering aid in such method |
| CN111410538A (en) * | 2020-05-08 | 2020-07-14 | 潍坊工商职业学院 | Toughened silicon carbide ceramic and preparation method thereof |
| CN112062548A (en) * | 2020-09-28 | 2020-12-11 | 成都万士达瓷业有限公司 | Production method of Al2O3 ceramic green body |
| CN115572151A (en) * | 2022-10-10 | 2023-01-06 | 淄博和润马科托矿业技术有限公司 | Microcrystalline alumina grinding medium and preparation method thereof |
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Application publication date: 20100707 |