CN103601490B - A kind of method of low-temperature sintering nozzle zirconium core - Google Patents
A kind of method of low-temperature sintering nozzle zirconium core Download PDFInfo
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- CN103601490B CN103601490B CN201310630497.0A CN201310630497A CN103601490B CN 103601490 B CN103601490 B CN 103601490B CN 201310630497 A CN201310630497 A CN 201310630497A CN 103601490 B CN103601490 B CN 103601490B
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Abstract
The present invention relates to a kind of method of low-temperature sintering nozzle zirconium core, its step is, preparation Al
2o
3-MgO-SiO
2be sintering agent, with the micron-sized ZrO through stabilization treatment
2compression moulding after powder mixing granulation, at 1500 ~ 1650 DEG C after being dried by molding biscuit, is incubated 4 hours, can obtains the zirconium core of densified sintering product.The zirconia powder being mixed with sintering agent during roasting, due to sintering agent fusing, makes biscuit fast densification complete low-temp liquid-phase sintering more than 1300 DEG C.This processing method, compared with the technique of zirconium white biscuit long-time high temperature solid-phase sintering more than 1700 DEG C of routine, can effectively reduce energy consumption, shortens the production cycle, reduces comprehensive cost.
Description
Technical field
The present invention relates to a kind of method of low-temperature sintering nozzle zirconium core, the method is used for making molten steel continuous casting water nozzle zirconium core.
Background technology
Zirconia ceramics material has high tenacity, anti-thermal shock, the good characteristics such as high temperature resistant erosion, in recent years, is widely used in the core pipe making molten steel continuous casting water nozzle.The zirconium core of current continuous casting of molten steel water nozzle adopts 1700 DEG C ~ 1780 DEG C high temperature solid-phase sintering systems sintering 6 ~ 8 hours to burn till substantially.Due to this sintering temperature and flame temperature difference less, cause the stove heating-up time long, therefore at high temperature sinter, energy consumption is high, and the production cycle is long, and equipment loss is large, and production efficiency is lower.When having investigator to propose Zirconium powder particle diameter to be reduced to nanoscale, because nano-powder specific surface area is huge, activity is very high, zirconic sintering can be realized at relatively low temperature, but because the cost preparing nano zirconium oxide powder significantly improves than micro-powder, cause economic benefit to decline to a great extent, therefore, the program cannot be applied in zirconia refractory field.Given this, in order to energy-saving and emission-reduction, reduce the comprehensive production cost of product, need to develop and a kind ofly under the prerequisite keeping zirconium core applied at elevated temperature performance, the method for sintering temperature can be reduced.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of method of low-temperature sintering nozzle zirconium core, the method is by adding sintering agent thus reducing nozzle zirconium core sintering temperature.
Method of the present invention comprises the following steps:
1) Al is configured
2o
3-MgO-SiO
2be sintering agent, the composition of sintering agent is: Al
2o
3content 10 ~ 40%(weight percent); Content of MgO 10 ~ 40%(weight percent); SiO
2content 20 ~ 80%(weight percent); The particle diameter of sintering agent is 0.1 ~ 50 μm;
2) by the sintering agent of grinding and the micron order ZrO of stabilized process
2the abundant mixing granulation of powder, sintering agent add-on is ZrO
20.5 ~ 3% of powder weight;
3) by shaping for the powder pressing after mixing granulation, and molding biscuit is dried 2 ~ 4 hours at 150 ~ 450 DEG C;
4) biscuit after oven dry is sintered 2 ~ 4 hours between 1500 ~ 1650 DEG C.
Described sintering agent fusing point (occurring the temperature of liquid phase) is lower than Zirconium oxide sintering temperature, in zirconium white biscuit, liquid phase is formed after 1300 ~ 1350 DEG C of fusings, wetting Zirconium powder, makes Zirconium powder mutually be close to by capillary force action, realizes densification effectively; On the other hand, the liquid phase that sintering agent is formed has certain solubleness to zirconium dioxide, realizes the interatomic bond between Zirconium powder, thus realize zirconic low-temperature sintering by the mechanism of dissolving-precipitating.Phase after sintering, the liquid phase that sintering agent fusing is formed is due to evaporation and the change of composition, and amount of liquid phase minimizing, remaining a small amount of liquid phase returns to zirconic trident grain boundaries, instead of is present on conventional crystal boundary in a large number, therefore can ensure the performance of the finished product.
Compared with prior art, the invention has the beneficial effects as follows by ZrO
2add appropriate sintering agent in powder, on the basis ensureing quality product, significantly can reduce the sintering temperature of nozzle zirconium core, shorten firing time, save the energy more than 30%, enhance productivity, reduce the comprehensive production cost of product.
Accompanying drawing explanation
Fig. 1 is that the add-on of sintering agent is too much, the schematic diagram of product tissue after sintering.
Fig. 2 is that the add-on of sintering agent is moderate, the schematic diagram of product tissue after sintering.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1
1) according to the technical scheme the first step configuration sintering agent be ground to ~ 2 μm for subsequent use;
2) take the sintering agent that 5g prepares, add 1Kg particle diameter (D
50) be the ZrO through stabilization treatment of about 6 ~ 40 μm
2among powder, fully after mixing, add a certain amount of deionized water and polyvinyl alcohol (PVA), mixing and ball milling 1h;
3), after being dried by powder and sieving, be pressed into hydropress the biscuit that internal diameter is the nozzle zirconium core of Φ 17mm;
4) biscuit after compacting is dried 3 hours at 150 DEG C;
5) biscuit after oven dry is piled up in kiln, be warming up to 1650 DEG C, be incubated and complete sintering in 2 ~ 4 hours.
Embodiment 2
1) according to the technical scheme the first step configuration sintering agent be ground to ~ 2 μm for subsequent use;
2) take the sintering agent that 10g prepares, add 1Kg particle diameter (D
50) be the ZrO through stabilization treatment of about 6 ~ 40 μm
2among powder, fully after mixing, add a certain amount of deionized water and polyvinyl alcohol (PVA), mixing and ball milling 1h;
3), after being dried by powder and sieving, be pressed into hydropress the biscuit that internal diameter is the nozzle zirconium core of Φ 17mm;
4) biscuit after compacting is dried 3 hours at 150 DEG C;
5) biscuit after oven dry is piled up in kiln, be warming up to 1600 DEG C, be incubated and complete sintering in 2 ~ 4 hours.
Embodiment 3
1) according to the technical scheme the first step configuration sintering agent be ground to ~ 2 μm for subsequent use;
2) take the sintering agent that 20g prepares, add 1Kg particle diameter (D
50) be the ZrO through stabilization treatment of about 6 ~ 40 μm
2among powder, fully after mixing, add a certain amount of deionized water and polyvinyl alcohol (PVA), mixing and ball milling 1h;
3), after being dried by powder and sieving, be pressed into hydropress the biscuit that internal diameter is the nozzle zirconium core of Φ 17mm;
4) biscuit after compacting is dried 3 hours at 150 DEG C;
5) biscuit after oven dry is piled up in kiln, be warming up to 1550 DEG C, be incubated 2 ~ 4 hours.
Embodiment 4
1) according to the technical scheme the first step configuration sintering agent be ground to ~ 2 μm for subsequent use;
2) take the sintering agent that 30g prepares, add 1Kg particle diameter (D
50) be the ZrO through stabilization treatment of about 6 ~ 40 μm
2among powder, fully after mixing, add a certain amount of deionized water and polyvinyl alcohol (PVA), mixing and ball milling 1h;
3), after being dried by powder and sieving, be pressed into hydropress the biscuit that internal diameter is the nozzle zirconium core of Φ 17mm;
4) biscuit after compacting is dried 3 hours at 150 DEG C;
5) biscuit after oven dry is piled up in kiln, be warming up to 1500 DEG C, be incubated 2 ~ 4 hours.
Sintering agent in above-described embodiment can be obtained by composition adjustment by the breeze that composition is close, or passes through Al
2o
3-MgO-SiO
2pure substance proportioning is obtained separately for three kinds of constituent elements.
The anti-thermal shock of above 4 embodiment products (meeting molten steel not burst) performance and the erosion performance of resistance to molten steel are (to be washed away the mouth of a river that internal diameter after 6h is Φ 17mm by 1600 DEG C of molten steel, its internal diameter extensive magnitude characterizes, and it is qualified that internal diameter extensive magnitude is less than 1mm) be summarized in following table:
It should be noted that the add-on of described sintering agent can not be too much, with non-sintered rear generation Continuous Liquid Phase.Under the add-on of sintering agent shown in Fig. 1 is greater than 4% situation; the schematic diagram of product tissue after sintering; as seen from Figure 1; on zirconia particles matrix, continuous print glassy phase is there is after sintering; this glassy phase can melt with steel contacts in product use procedure; cause zirconia particles by molten steel rapid erosion, reduce product work-ing life.
Fig. 2 is the add-on of sintering agent is in 2% situation, the schematic diagram of product tissue after sintering, and under sintering agent add-on moderated case, after completing sintering, residue glass liquid phase is present in zirconic trident grain boundaries, can ensure the performance that the resistance to molten steel of product corrodes.
The add-on of described sintering agent can not be very few, if the add-on of sintering agent is lower than 0.5%, do not have the effect reducing sintering temperature.
Claims (5)
1. a method for low-temperature sintering nozzle zirconium core, its feature comprises the following steps:
1) Al is configured
2o
3-MgO-SiO
2be sintering agent, after sintering agent melting being cooled, be ground to 0.1 ~ 50 μm; The composition of sintering agent is: Al
2o
3content 10 ~ 40%(weight percent); Content of MgO 10 ~ 40%(weight percent); SiO
2content 20 ~ 80%(weight percent);
2) by the micron order ZrO of described sintering agent and stabilized process
2the abundant mixing granulation of powder, sintering agent add-on is ZrO
20.5 ~ 3% of powder weight;
3) by shaping for the powder pressing after mixing granulation, and molding biscuit is dried 0.5 ~ 2.5 hour at 150 ~ 450 DEG C;
4) biscuit after oven dry is sintered 2 ~ 4 hours between 1500 ~ 1650 DEG C.
2. the method for low-temperature sintering nozzle zirconium core according to claim 1, is characterized in that: described sintering agent add-on is ZrO
21 ~ 2.5% of powder weight, the particle diameter of sintering agent is 2 μm.
3. the method for low-temperature sintering nozzle zirconium core according to claim 1, is characterized in that: described sintering agent add-on is ZrO
22% of powder weight, the particle diameter of sintering agent is 2 μm.
4. the method for low-temperature sintering nozzle zirconium core according to any one of claim 1 to 3, is characterized in that: described ZrO
2diameter of particle is 6 ~ 40 μm.
5. the method for low-temperature sintering nozzle zirconium core according to claim 1, is characterized in that: sintering agent is obtained by composition adjustment by the breeze that composition is close, or passes through Al
2o
3-MgO-SiO
2pure substance proportioning is obtained separately for three kinds of constituent elements.
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| CN103601490B true CN103601490B (en) | 2015-08-05 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638317A (en) * | 2008-08-02 | 2010-02-03 | 比亚迪股份有限公司 | Fully stabilized zirconia ceramic material and preparation method thereof |
| CN102863213A (en) * | 2012-09-14 | 2013-01-09 | 钟祥市中原电子有限责任公司 | High-density magnesium-stabilized zirconia ceramic |
-
2013
- 2013-12-02 CN CN201310630497.0A patent/CN103601490B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638317A (en) * | 2008-08-02 | 2010-02-03 | 比亚迪股份有限公司 | Fully stabilized zirconia ceramic material and preparation method thereof |
| CN102863213A (en) * | 2012-09-14 | 2013-01-09 | 钟祥市中原电子有限责任公司 | High-density magnesium-stabilized zirconia ceramic |
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Application publication date: 20140226 Assignee: JIANGSU HIGH-XIN HIGH-TEMPERATURE NEW MATERIALS TECHNOLOGY CO.,LTD. Assignor: TAIZHOU CITY WANGXIN REFRACTORY MATERIAL CO.,LTD. Contract record no.: X2023980041210 Denomination of invention: A Method for Low Temperature Sintering of Zirconium Cores with Water Mouth Granted publication date: 20150805 License type: Common License Record date: 20230905 |
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