CN1935660A - Method for synthesizing ferruginous aluminium titanate solid solution powder - Google Patents
Method for synthesizing ferruginous aluminium titanate solid solution powder Download PDFInfo
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- CN1935660A CN1935660A CN 200610053924 CN200610053924A CN1935660A CN 1935660 A CN1935660 A CN 1935660A CN 200610053924 CN200610053924 CN 200610053924 CN 200610053924 A CN200610053924 A CN 200610053924A CN 1935660 A CN1935660 A CN 1935660A
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Abstract
The invention relates to an iron-containing aluminum titanate solid solution powder, firstly using rutile TiO2 and iron trioxide to synthesize iron titanate; then wet-ball milling and mixing the synthesized iron titanate and industrial-grade alpha-Al2O3 and rutile TiO2 powder raw material, drying, and screening or spray-granulating, and burning to make it, able to be directly used for preparation of aluminum titanate ceramic. And the invention uses the synthesized iron titanate as nucleating agent and stabilizing agent, and promotes synthesis of aluminum titanate solid solution, having high purity and high quality. And the invention changes initial mixture shape from block into powder, convenient to operating and easy to implement industrialized production.
Description
Technical field
The present invention relates to the synthetic method of ferruginous aluminium titanate solid solution powder, belong to field of inorganic nonmetallic material.
Background technology
Non-ferrous alloy such as magnesium, aluminium is owing to have characteristics such as light weight, intensity height, and its goods have obtained using widely in car industry, space flight and aviation industry.Recent years, along with the development of China's car and aerospace industry, the smelting of iron, aluminium alloy and casting have obtained development at full speed, and this smelts iron, aluminium alloy and casts necessary refractory materials or refractory has also proposed increasing demand.For guarantee magnesium, Al-alloy products quality, require to smelt and castingprocesses in used refractory materials or refractory not only to have resistance and high temperature resistance property, and to have characteristics such as nonwetting with the non-ferrous alloy solution, that thermal shock resistance is good.Alumina titanate ceramics be typical low bulk (RT-1000 ℃, 0.2 * 10
-6/ ℃～1 *
-6/ ℃), low thermal conductance stupalith, have good thermal shock resistance, and nonwetting with the non-ferrous alloy solution, therefore be to be applied to that non-ferrous alloys such as magnesium, aluminium are smelted and the good refractory ceramic material of casting.But aluminium titanates is easy to be decomposed into high temperature alumina and rutile titanium dioxide at 700-1280 ℃, causes the low bulk of aluminum titanate ceramic material, thermal shock resistance to reduce, and has limited its application on magnesium, aluminium alloy casting.Fortunately, the solid solution of ferric oxide in the aluminium titanates structure, the formation chemical formula is Al
2 (1-x)Fe
2xTiO
5, the sosoloid of 0.05≤x≤60 can be realized the dynamic stabilization of aluminium titanates improving the thermostability of aluminium titanates in 700 ℃ of-1280 ℃ of temperature ranges, thereby realizes the application of alumina titanate ceramics in iron, aluminium alloy casting industry.
Traditional solid reaction process synthesizes aluminium titanates, is with α-Al
2O
3And rutile TiO
2, and talcum, clay or other additive wet ball grinding are mixed, and oven dry, the granulation of sieving, dry-pressing becomes block, calcines in the temperature that is higher than 1380 ℃.Briquetting and higher calcining temperature all are in order to strengthen the reaction of each stock yard, to realize the synthetic of pure phase aluminium titanates powder.But higher calcining temperature and briquetting are easy to cause the generation of sintering behavior in calcination process, in order to obtain being applied to the powder of aluminum titanate ceramic material preparation, still need and want further fragmentation and ball milling.Not only increase the difficulty of the synthetic aluminium titanates powder of industrialization, also strengthened the cost of synthetic aluminium titanates powder.
Summary of the invention
The objective of the invention is to propose a kind of method of synthetic ferruginous aluminium titanate solid solution powder,, can be directly used in the alumina titanate ceramics preparation to realize the synthetic pure phase ferruginous aluminium titanate solid solution powder of solid state reaction.
The synthetic method of ferruginous aluminium titanate solid solution powder of the present invention, the chemical formula of this ferruginous aluminium titanate solid solution are Al
2 (1-x)Fe
2xTiO
5, 0.05≤x≤60, synthetic method may further comprise the steps:
1) with ferric oxide and rutile TiO
2Be raw material, press chemical formula Fe
2TiO
5The proportioning weighing, it is mixed to place ball mill to add the water wet ball grinding, the pellet water weight ratio is 1: 1: 0.3～1: 5: 1.5, the ball milling time is for being not less than 1 hour, the oven dry of ball milling blended slip is sieved or mist projection granulating, obtains iron titanate Fe 1000 ℃～1300 ℃ calcinings then
2TiO
5
2) with step 1) synthetic iron titanate and technical grade α-Al
2O
3And rutile TiO
2Powder is a raw material, by pre-synthetic sosoloid Al
2 (1-x)Fe
2xTiO
50.05 the chemical constitution proportioning weighing of≤x≤60, placing ball mill to add the water wet ball grinding mixes, the pellet water weight ratio is 1: 1: 0.25～1: 5: 1.2, the ball milling time is for being not less than 4 hours, the oven dry of ball milling blended slip is sieved or mist projection granulating, obtains ferruginous aluminium titanate solid solution powder 1250 ℃～1500 ℃ calcinings then.
Employed raw material can be commercially available industrial raw material, α-Al among the present invention
2O
3Purity (wt%) 〉=95, granularity d (μ m) 0.5≤d≤5.Rutile TiO
2Purity (wt%) 〉=95, granularity d (μ m) 0.5≤d≤5.The purity of ferric oxide (wt%) 〉=86, granularity d (μ m) 0.2≤d≤2.
In order to reduce water consumption and to strengthen grinding efficiency, can be in the building-up process in step 2) wet ball grinding in introduce dispersion agent, said dispersion agent can be polyacrylate, sodium humate or soda ash.
Beneficial effect of the present invention is:
Compare with the solid reaction process that synthesized the aluminium titanates powder in the past, the present invention has many advantages.At first, the present invention is by synthesizing the stablizer Fe of heterogeneous isomorphism in advance
2TiO
5, as the crystal seed that forms aluminium titanate solid solution, having reduced the potential barrier that aluminium titanates forms, speed of response is accelerated, and just can realize by the fully conversion of initial feed to aluminium titanates in the time that lower temperature calcining is short.Because being easy to of building-up reactions finished, make the present invention can change the initial proterties of the compound of synthetic aluminium titanates, by the briquetting proterties of traditional synthesis method, change powder proterties of the present invention into, being easy to post-production is the fine powder raw material that is applicable to the pottery preparation.In addition, the used raw material of the present invention is industrial raw material, and technological operation is convenient, and cost is low, and universality is strong, is applicable to industrialized production.
Description of drawings
Fig. 1 is synthetic Fe
2TiO
5The XRD figure spectrum of powder;
Fig. 2 is synthetic Al
1.6Fe
0.4TiO
5The XRD figure spectrum of solid solution powder.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Example 1:
1) starting material adopt technical grade α-Al
2O
3, rutile TiO
2And Fe
2O
3At first with rutile TiO
2And Fe
2O
3Be raw material synthesizing stable agent Fe
2TiO
5, its proportioning is Fe: Ti=2: 1, and the pellet water weight ratio is: 1: 5: 1.5,10 hours ball milling time, go out to grind back 100 ℃ of oven dry, cross 30 mesh sieves, 1150 ℃ of insulations calcining in 4 hours, XRD detects and has synthesized pure Fe
2TiO
5Powder (Fig. 1).
2) with synthetic Fe
2TiO
5Be stablizer and nucleus and technical grade α-Al
2O
3And rutile TiO
2The powder ball milling mixes synthetic Al
1.6Fe
0.4TiO
5Solid solution powder, its proportioning is: Al: Fe: Ti=1.6: 0.4: 1.0, the pellet water weight ratio was: 1: 4: 0.8.In order to reduce water consumption and to strengthen grinding efficiency, add the dispersion agent polyacrylic acid ammonia of the 0.2wt% of material quantity, ball milling 24 hours goes out to grind back 100 ℃ of oven dry, crosses 30 mesh sieves, and 1350 ℃ of insulations calcining in 5 hours is synthetic, and XRD detects and is pure phase Al
1.6Fe
0.4TiO
5Solid solution powder (Fig. 2).Can be directly used in the preparation alumina titanate ceramics.
Example 2:
1) starting material adopt technical grade α-Al
2O
3, rutile TiO
2And Fe
2O
3At first with rutile TiO
2And Fe
2O
3Be raw material synthesizing stable agent Fe
2TiO
5, its proportioning is Fe: Ti=2: 1, and pellet water ratio is: 1: 1: 1.2,18 hours ball milling time, go out to grind back 100 ℃ of oven dry, cross 30 mesh sieves, 1150 ℃ of insulations calcining in 4 hours, XRD detects and has synthesized pure Fe
2TiO
5Powder.
2) with synthetic Fe
2TiO
5Be stablizer and nucleus and technical grade α-Al
2O
3And rutile TiO
2The powder ball milling mixes synthetic Al
1.8Fe
0.2TiO
5Solid solution powder, its proportioning is: Al: Fe: Ti=1.8: 0.2: 1.0, the pellet water weight ratio was: 1: 5: 1.2.Ball milling 24 hours goes out to grind back 100 ℃ of oven dry, crosses 30 mesh sieves, and 1420 ℃ of insulations calcining in 5 hours is synthetic, and XRD detects and is pure phase Al
1.8Fe
0.2TiO
5Solid solution powder.
Example 3:
1) starting material adopt technical grade α-Al
2O
3, rutile TiO
2And Fe
2O
3At first with rutile TiO
2And Fe
2O
3Be raw material synthesizing stable agent Fe
2TiO
5, its proportioning is Fe: Ti=2: 1, and pellet water ratio is: 1: 2.6: 0.3,10 hours ball milling time, go out to grind back 100 ℃ of oven dry, cross 30 mesh sieves, 1200 ℃ of insulations calcining in 4 hours, XRD detects and has synthesized pure Fe
2TiO
5Powder.
2) with synthetic Fe
2TiO
5Be stablizer and nucleus and technical grade α-Al
2O
3And rutile TiO
2The powder ball milling mixes synthetic Al
1.6Fe
0.4TiO
5Solid solution powder, its proportioning is: Al: Fe: Ti=1.6: 0.4: 1.0, pellet water ratio was: 1: 1: 0.25.In order to reduce water consumption and to strengthen grinding efficiency, add the dispersion agent polyacrylic acid ammonia of the 0.4wt% of material quantity, ball milling 24 hours goes out to grind back 100 ℃ of oven dry, crosses 30 mesh sieves, and 1400 ℃ of insulations calcining in 5 hours is synthetic, and XRD detects and is pure phase Al
1.6Fe
0.4TiO
5Solid solution powder.
In the foregoing description, employed raw material is commercially available industrial raw material, α-Al
2O
3Purity (wt%) 〉=95, granularity d (μ m) 0.5≤d≤5.Rutile TiO
2Purity (wt%) 〉=95, granularity d (μ m) 0.5≤d≤5.The purity of ferric oxide (wt%) 〉=86, granularity d (μ m) 0.2≤d≤2.
Claims (6)
1. the synthetic method of ferruginous aluminium titanate solid solution powder, the chemical formula of this ferruginous aluminium titanate solid solution is Al
2 (1-x)Fe
2xTiO
5, 0.05≤x≤60, synthetic method may further comprise the steps:
1) with ferric oxide and rutile TiO
2Be raw material, press chemical formula Fe
2TiO
5The proportioning weighing, it is mixed to place ball mill to add the water wet ball grinding, the pellet water weight ratio is 1: 1: 0.3～1: 5: 1.5, the ball milling time is for being not less than 1 hour, the oven dry of ball milling blended slip is sieved or mist projection granulating, obtains iron titanate Fe 1000 ℃～1300 ℃ calcinings then
2TiO
5
2) with step 1) synthetic iron titanate and technical grade α-Al
2O
3And rutile TiO
2Powder is a raw material, by pre-synthetic sosoloid Al
2 (1-x)Fe
2xTiO
50.05 the chemical constitution proportioning weighing of≤x≤60, placing ball mill to add the water wet ball grinding mixes, the pellet water weight ratio is 1: 1: 0.25～1: 5: 1.2, the ball milling time is for being not less than 4 hours, the oven dry of ball milling blended slip is sieved or mist projection granulating, obtains ferruginous aluminium titanate solid solution powder 1250 ℃～1500 ℃ calcinings then.
2. according to the synthetic method of right 1 described ferruginous aluminium titanate solid solution powder, it is characterized in that in step 2) introduce dispersion agent in the said wet ball grinding.
3. according to the synthetic method of right 2 described ferruginous aluminium titanate solid solution powders, it is characterized in that said dispersion agent is polyacrylate, sodium humate or soda ash.
4. according to the synthetic method of right 1 described ferruginous aluminium titanate solid solution powder, it is characterized in that α-Al
2O
3Purity (wt%) 〉=95, granularity d (μ m) 0.5≤d≤5.
5. according to the synthetic method of right 1 described ferruginous aluminium titanate solid solution powder, it is characterized in that rutile TiO
2Purity (wt%) 〉=95, granularity d (μ m) 0.5≤d≤5.
6. according to the synthetic method of right 1 described ferruginous aluminium titanate solid solution powder, it is characterized in that the purity (wt%) 〉=86 of ferric oxide, granularity d (μ m) 0.2≤d≤2.
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|---|---|---|---|
| CN 200610053924 CN1935660A (en) | 2006-10-23 | 2006-10-23 | Method for synthesizing ferruginous aluminium titanate solid solution powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936133A (en) * | 2012-12-10 | 2013-02-20 | 青岛海诺水务科技股份有限公司 | Preparation method of aluminium titanate material |
| CN102936134A (en) * | 2012-12-11 | 2013-02-20 | 青岛森淼实业有限公司 | Preparation method of aluminium titanate sintering body |
-
2006
- 2006-10-23 CN CN 200610053924 patent/CN1935660A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936133A (en) * | 2012-12-10 | 2013-02-20 | 青岛海诺水务科技股份有限公司 | Preparation method of aluminium titanate material |
| CN102936134A (en) * | 2012-12-11 | 2013-02-20 | 青岛森淼实业有限公司 | Preparation method of aluminium titanate sintering body |
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