CN106673626A - Low-cost alumina powder material for producing self-toughened wear-resistant alumina ceramic - Google Patents
Low-cost alumina powder material for producing self-toughened wear-resistant alumina ceramic Download PDFInfo
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Abstract
The invention discloses a low-cost alumina powder material for producing self-toughened wear-resistant alumina ceramic. Firstly, industrial-grade gamma-alumina, an additive, oleic acid and other substances are placed into a ball mill together and subjected to dry milling, fine particle powder with D50 smaller than 3 mu m is obtained and calcined at 1200-1400 DEG C for 2-10 h, and alumina powder A with sodium impurities removed is obtained for standby application; then industrial-grade aluminium hydroxide, an additive, oleic acid and other substances are placed into the ball mill together and subjected to dry milling, fine particle powder with D50 smaller than 3 mu m is obtained and calcined at 900-1200 DEG C for 2-10 h, and alumina powder B with sodium impurities removed is obtained for standby application; the alumina powder A and the alumina powder B are mixed in proportion, an additive is added according to the variety of the wear-resistant ceramic, the mixture is sanded and subjected to spray granulation, and the alumina powder material with the sodium mass fraction lower than 0.2%, the median diameter D50 smaller than 2 mu m and suitability for preparing fine ceramic through dry pressing forming or isostatic pressing forming is obtained. The raw material cost is low, the preparation process is simple, the production process is simple and convenient to control, stable and batch production is easy.
Description
Technical field
The present invention relates to aluminium oxide wear-resistant ceramic production raw material, is used to produce self-toughening alumina more particularly, to a kind of
The inexpensive alumina powder jointed material of wear-resistant ceramic.
Background technology
The raw material of country's aluminium oxide wear-resistant ceramic production at present is mainly the gama-alumina or aluminium hydroxide of technical grade,
It is higher that its shortcoming is mainly sodium content, when straight forming is sintered, is difficult to densification due to there is vermiform hole after phase transformation, institute
Generally to need before block ceramic is prepared, first gama-alumina or aluminium hydroxide high-temperature calcination to be transformed into into Alpha-alumina,
The mineralizers such as boride, chloride or fluoride are added in calcination process, with sodium volatile low-melting compound is formed, removed
Sodium impurity in aluminium oxide.In order to ensure that sodium content is sufficiently low, calcining heat is typically greater than 1400 DEG C, therefore the α after calcining-
The former crystalline substance size of aluminium oxide is typically larger than 3 μm, adopts the ceramic microscopic structure that the raw material is prepared Jing after forming and sintering for equiax crystal, and
And crystallite dimension is more than 5 μm.The bending strength of this microstructural aluminium oxide wear-resistant ceramic product, hardness and fracture toughness are equal
It is relatively low.Due at present in wear-resisting field, more and more wider, the traditional wear-resisting alumina ceramic of the milling apparatus application of high speed big load
Because of abrasion greatly, it is broken to have met requirement, it is therefore desirable to improve intensity, hardness and the toughness of aluminium oxide wear-resistant ceramic.
Improving Alumina Ceramics typically has two methods, and one kind is to add the second phase, such as notification number
The Chinese invention patent of CN101508562B discloses a kind of aluminum oxide toughening structure ceramic material, and it adopts and consists of oxidation
78~85wt% of aluminum, 13~20wt% of yttrium stable zirconium oxide, the wherein raw material of 0.5~2wt% of titanium dioxide, yttrium stable zirconium oxide
It is made up of the zirconium oxide of 97mol% and the yittrium oxide of 3mol%.The aluminum oxide toughening structure ceramic material based on aluminium oxide,
And using yttrium stable zirconium oxide as toughener, not only with the excellent in performance of conventional aluminium oxide structural ceramic material, Er Qieyong
There is good toughness, compare relative to self toughening zirconia ceramics material, material cost is relatively low, but relative to alumina material,
It is then relatively costly.It is exactly self toughening that another kind improves the method for Alumina Ceramics, the middle promulgated by the State Council of notification number CN101182193
Bright patent discloses a kind of preparation method of in-situ self-toughening alumina ceramics, adopts nanometer aluminium powder and high-purity alumina powder to be first
Beginning raw material, mix homogeneously；By mixed slurry drying, grind to form powder body；The powder body of acquisition is configured to base substrate；Base substrate is direct
Sinter in common air calcination stove, obtain with the brilliant aluminium oxide ceramics of growth in situ long column shape, tabular, the aluminium oxide is produced
Product have the advantages that high density, high-purity and high tenacity, but its shortcoming adopts nanometer aluminium powder, high cost for raw material, it is difficult to big rule
Mould is produced.
The content of the invention
It is an object of the invention to provide a kind of inexpensive alumina powder for producing self-toughening alumina wear-resistant ceramic
Body material.
For achieving the above object, the present invention can take following technical proposals：
Inexpensive alumina powder jointed material for producing self-toughening alumina wear-resistant ceramic of the present invention includes following systems
Standby step：
The first step, is entered in ball mill from technical grade gama-alumina, adds adding for gama-alumina total mass fraction 0.1 ~ 3%
Plus agent and 0.2 ~ 2% Oleic acid, stearic acid or sodium stearate are dry grinded together with gama-alumina and are mixed and break up agglomerates, are obtained
The fine grained mixed powder of 3 μm of median particle diameter D50 ＜, the additive is appointing in boric acid, calcium fluoride, ammonium chloride and aluminium fluoride
One or two and thing mixed above；Additive therein can play a part of to remove impurity and inhibiting grain growth；Oleic acid,
Stearic acid or sodium stearate can play a part of grinding aid, avoid fine grained from reuniting；
Second step, by fine grained mixed powder obtained in the first step in 1200 DEG C ~ 1400 DEG C temperature lower calcinations 2 ~ 10 hours, obtains
The alumina powder jointed A for removing sodium impurity is standby；
3rd step, is entered in ball mill from technical grade aluminium hydroxide, adds the additive of aluminium hydroxide total mass fraction 0.1 ~ 3%
Oleic acid, stearic acid or sodium stearate with 0.2 ~ 2% is dry grinded together with aluminium hydroxide and is mixed and break up agglomerates, obtains intermediate value grain
The fine grained mixed powder of 3 μm of footpath D50 ＜, the additive is boric acid, calcium fluoride, ammonium chloride, aluminium fluoride, magnesium chloride and fluorination
One or two and thing mixed above in magnesium；Likewise, additive therein can play removing impurity and suppress crystal grain long
Big effect；Oleic acid, stearic acid or sodium stearate can play a part of grinding aid, avoid fine grained from reuniting；
4th step, by fine grained mixed powder obtained in the 3rd step in 900 DEG C ~ 1200 DEG C temperature lower calcinations 2 ~ 10 hours, obtains
The alumina powder jointed B for removing sodium impurity is standby；
5th step, by alumina powder jointed A obtained in second step and alumina powder jointed B obtained in the 4th step 1 is pressed:0.5 ~ 3 weight
After part mixing, according to the species of wear-resistant ceramic, different additives are added（Its objective is to play reduction sintering temperature and improve to make pottery
The effect of porcelain performance）, Jing sand millings and mist projection granulating, that is, obtain sodium mass fraction less than 0.2%, 2 μm of median particle diameter D50 ＜, be adapted to
Dry-pressing or isostatic pressing prepare the alumina powder jointed material of fine ceramics；95 aluminium oxidies obtained using the powder body material sintering
The ＞ 13GPa of vickers hardness hv 5 and fracture toughness of ceramics is higher than 3.8MPam1/2。
The additive added in 5th step is CaO, MgO, SiO2、TiO2、La2O3、CAS(CaO-Al2O3-SiO2) in glass
The mixture of one or two kinds of and the above so as to glass is formed in follow-up sintering process to reduce sintering temperature.
Impurity total mass fraction ＜ 2% of the technical grade gama-alumina；The total matter of impurity of the technical grade aluminium hydroxide
Amount fraction ＜ 2%.
When reality prepares alumina powder jointed A and alumina powder jointed B, there is phase when addition Oleic acid, stearic acid or sodium stearate
Same effect；
When preparing alumina powder jointed A, the additive of employing can be any one in boric acid, calcium fluoride, ammonium chloride and aluminium fluoride
Or two kinds and thing mixed above, effect is identical；
When preparing alumina powder jointed B, the additive of employing can be boric acid, calcium fluoride, ammonium chloride, aluminium fluoride, magnesium chloride and fluorine
Change one or two and the thing mixed above in magnesium, effect is identical.
It is an advantage of the current invention that phase inversion remove impurity additive will be added in the industrial raw material of low cost, ground by ball milling
Destruction is reunited and controls pre-sintering temperature, eliminates the sodium impurity remained in gama-alumina and aluminium hydroxide, obtains difference
The Alpha-alumina of sintering activity；Subsequently the alumina powder jointed ratio as required for preparing is mixed and added into into specific addition
After agent, the elongated grain formed in powder body microscopic structure is controlled, there is the finished product aluminium oxide wear-resistant ceramic for making sintering self toughening to make
With.Cost of material of the present invention is low, preparation process is simple, and technique produces easy to control, it is easy to stable and batch production.
Require to ensure that the quality of the alumina powder jointed material of finished product meets, the impurity gross mass point of the gama-alumina of selection
Number ＜ 2%；From technical grade aluminium hydroxide impurity total mass fraction ＜ 2%.
Specific embodiment
Below by specific embodiment to the low cost for producing self-toughening alumina wear-resistant ceramic of the present invention
The preparation method of alumina powder jointed material is described in detail.
Embodiment 1
1）By technical grade gama-alumina 800kg（The total mass fraction 0.6% of impurity）, account for total quality of alumina fraction 0.4%
Boric acid, the sodium stearate for accounting for total quality of alumina fraction 0.5% are put into together in ball mill, dry grinding mixing 8 hours and broken reunion
Body, obtains the gama-alumina fine grained mixed powder that median particle diameter D50 is 2.8 μm；
2）By obtained gama-alumina mixed powder in 1400 DEG C of temperature lower calcinations 4 hours, sodium impurity mass fraction is obtained little
In 0.1% alumina powder jointed A；
3）By technical grade aluminium hydroxide 200kg（Total mass fraction ＜ 0.6% of impurity）, account for aluminium hydroxide mass fraction 0.1%
Calcium fluoride, 0.2% ammonium chloride and account for the Oleic acid of aluminium hydroxide mass fraction 0.5% and be put into together in ball mill, dry grinding mixing 8 is little
When and break up agglomerates, it is 2.6 μm of aluminium hydroxide fine grained mixed powder to obtain median particle diameter D50；
4）By obtained aluminium hydroxide fine grained mixed powder in 1150 DEG C of temperature lower calcinations 6 hours, sodium impurity quality point is obtained
The alumina powder jointed B less than 0.1% is standby for number；
5）Alumina powder jointed A and alumina powder jointed B is mixed, addition accounts for total mixed powder mass fraction 1%CaO+2%MgO+2%
SiO2The additive package of composition, Jing sand millings and mist projection granulating, the median particle diameter D50 for obtaining being tested under laser particle analyzer is
1.6 μm of alumina powder jointed material；
6）The dry-pressing or isostatic pressing method that above-mentioned powder body material is routinely adopted is sintered, and hardness height (HV5 is obtained
13 GPa) and toughness height (3.8MPam1/2) 95 porcelain aluminium oxide wear-resistant ceramics.
Embodiment 2
1）By technical grade gama-alumina 700kg（The total mass fraction 0.6% of impurity）, account for total quality of alumina fraction 0.3%
Boric acid, the sodium stearate for accounting for total quality of alumina fraction 0.6% are put into together in ball mill, dry grinding mixing 12 hours and broken group
Aggressiveness, obtains the gama-alumina fine grained mixed powder that median particle diameter D50 is 2.8 μm；
2）By obtained gama-alumina mixed powder in 1380 DEG C of temperature lower calcinations 6 hours, sodium impurity mass fraction is obtained little
In 0.1% alumina powder jointed A；
3）By technical grade aluminium hydroxide 300kg（Total mass fraction ＜ 0.6% of impurity）, account for aluminium hydroxide mass fraction 0.3%
Afluon (Asta), 0.1% ammonium chloride and account for the stearic acid of aluminium hydroxide mass fraction 0.6% and be put into together in ball mill, dry grinding mixing
And break up agglomerates, obtain the aluminium hydroxide fine grained mixed powder that median particle diameter D50 is 2.6 μm；
4）By obtained aluminium hydroxide fine grained mixed powder in 1100 DEG C of temperature lower calcinations 4 hours, sodium impurity quality point is obtained
The alumina powder jointed B less than 0.1% is standby for number；
5）Alumina powder jointed A and alumina powder jointed B is mixed, addition accounts for total mixed powder mass fraction 2%MgO+1%SiO2Group
Into additive package, Jing sand millings and mist projection granulating, the median particle diameter D50 for obtaining being tested under laser particle analyzer is 1.4 μm
Alumina powder jointed material；
6）The dry-pressing or isostatic pressing method that above-mentioned powder body material is routinely adopted is sintered, and hardness height (HV5 is obtained
14.5 GPa) and toughness height (4.6MPam1/2) 97 porcelain aluminium oxide wear-resistant ceramics.
Claims (3)
1. a kind of inexpensive alumina powder jointed material for producing self-toughening alumina wear-resistant ceramic, it is characterised in that：Including
Following preparation processes：
The first step, is entered in ball mill from technical grade gama-alumina, adds adding for gama-alumina total mass fraction 0.1 ~ 3%
Plus agent and 0.2 ~ 2% Oleic acid, stearic acid or sodium stearate are dry grinded together with gama-alumina and are mixed and break up agglomerates, are obtained
The fine grained mixed powder of 3 μm of median particle diameter D50 ＜, the additive is appointing in boric acid, calcium fluoride, ammonium chloride and aluminium fluoride
One or two and thing mixed above；
Second step, by fine grained mixed powder obtained in the first step in 1200 DEG C ~ 1400 DEG C temperature lower calcinations 2 ~ 10 hours, obtains
The alumina powder jointed A for removing sodium impurity is standby；
3rd step, is entered in ball mill from technical grade aluminium hydroxide, adds the additive of aluminium hydroxide total mass fraction 0.1 ~ 3%
Oleic acid, stearic acid or sodium stearate with 0.2 ~ 2% is dry grinded together with aluminium hydroxide and is mixed and break up agglomerates, obtains intermediate value grain
The fine grained mixed powder of 3 μm of footpath D50 ＜, the additive is boric acid, calcium fluoride, ammonium chloride, aluminium fluoride, magnesium chloride and fluorination
One or two and thing mixed above in magnesium；
4th step, by fine grained mixed powder obtained in the 3rd step in 900 DEG C ~ 1200 DEG C temperature lower calcinations 2 ~ 10 hours, obtains
The alumina powder jointed B for removing sodium impurity is standby；
5th step, by alumina powder jointed A obtained in second step and alumina powder jointed B obtained in the 4th step 1 is pressed:0.5 ~ 3 weight
After part mixing, according to the species of wear-resistant ceramic, additive, Jing sand millings and mist projection granulating are added, obtain 2 μm of median particle diameter D50 ＜
Alumina powder jointed material.
2. the inexpensive alumina powder jointed material for producing self-toughening alumina wear-resistant ceramic according to claim 1,
It is characterized in that：The additive added in 5th step is CaO, MgO, SiO2、TiO2、La2O3、CAS(CaO-Al2O3-SiO2) glass
The mixture of one or two kinds of and the above in glass.
3. the inexpensive alumina powder jointed material for producing self-toughening alumina wear-resistant ceramic according to claim 1 and 2
Material, it is characterised in that：Impurity total mass fraction ＜ 2% of the technical grade gama-alumina；The technical grade aluminium hydroxide it is miscellaneous
Matter total mass fraction ＜ 2%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805838A (en) * | 2017-10-25 | 2018-03-16 | 盐城师范学院 | A kind of electrochemical method for synthesizing of out-of-plane orientation phosphate aluminium molecular sieve film |
| CN108298964A (en) * | 2018-04-10 | 2018-07-20 | 淄博启明星新材料股份有限公司 | High-purity fine grain wear-resisting alumina liner plate and preparation method thereof |
| CN108840668A (en) * | 2018-07-05 | 2018-11-20 | 中国铝业股份有限公司 | A kind of wear-resistant material |
| CN112028098A (en) * | 2019-06-04 | 2020-12-04 | 北京化工大学 | Preparation method of gamma-alumina nano dispersion |
| CN112430104A (en) * | 2020-12-07 | 2021-03-02 | 娄底市安地亚斯电子陶瓷有限公司 | Composite additive for preparing ceramic and preparation method and application thereof |
| CN112717963A (en) * | 2019-10-28 | 2021-04-30 | 中国石油化工股份有限公司 | Hydrogenation pretreatment catalyst, and preparation method and application thereof |
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| CN108298964B (en) * | 2018-04-10 | 2021-03-02 | 淄博启明星新材料股份有限公司 | High-purity fine-grain wear-resistant alumina lining plate and preparation method thereof |
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| CN112717963B (en) * | 2019-10-28 | 2022-03-04 | 中国石油化工股份有限公司 | Hydrogenation pretreatment catalyst, and preparation method and application thereof |
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