CN109704779A - A kind of modified boron nitride composite and preparation method thereof and a kind of side seal board - Google Patents
A kind of modified boron nitride composite and preparation method thereof and a kind of side seal board Download PDFInfo
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- CN109704779A CN109704779A CN201910086738.7A CN201910086738A CN109704779A CN 109704779 A CN109704779 A CN 109704779A CN 201910086738 A CN201910086738 A CN 201910086738A CN 109704779 A CN109704779 A CN 109704779A
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Abstract
The present invention provides a kind of modified boron nitride composites and preparation method thereof and a kind of side seal board, belong to technical field of inorganic nonmetallic materials, are prepared by the raw material for including following mass percentage: boron nitride 50~80%；Zirconium oxide 8~20%；Sialon 5~15%；Silicon carbide 5~15%；Additive 1~5%.In the present invention, when generating volume expansion during phase transformation when zirconium oxide, Sialon plays the role of pinning, and zirconium oxide crystal face is inhibited to crack, and guarantees that cracking phenomena will not be generated under modified boron nitride composite high temperature；Meanwhile the elasticity modulus of Sialon, in 250GPa or so, the elasticity modulus of zirconium oxide is 150GPa or so, and the Sialon material of such high elastic modulus can promote the lesser zirconium oxide transformation stress of elasticity modulus to significantly improve, and reduces the generation of crystal face crackle.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, in particular to a kind of modified boron nitride composite and its system
Preparation Method and a kind of side seal board.
Background technique
Twin-roll thin strip continuous casting technology is a kind of novel Thin Strip Steel production technology, can save continuous casting, heating and hot rolling etc.
Cumbersome process, the technique that solid-state strip is become from metal liquid in a relatively short period of time.With iron and steel smelting technology level
It is continuously improved, thin strap continuous casting level also needs to improve, and side seal board is strip continuous casting technology critical component, therefore improves side seal board
Performance be improve thin strap continuous casting level key factor.
Continuous casting side seal board is required to have high temperature resistant, not chemically reacted with molten steel, good anti-molten steel, steel slag
Aggressivity, good thermal shock resistance is to resist the erosion of molten steel, it is necessary to have wearability to cope with the mill of roll and steel band
Damage.Meanwhile also to have easy machining property, accurately to process the geometric dimension of side seal board, adapt to side seal board assembly and
Use process is easy to operate.
Raw material used in production thin-strip casting side sealing plate are boron nitride, zirconium oxide, silicon carbide both at home and abroad at present, outside
Add some additives, however these product anti-thermal shock produced is poor, is easy to appear crackle at high temperature causes service life short.
Summary of the invention
In view of this, it is an object of that present invention to provide a kind of modified boron nitride composites and preparation method thereof and a kind of side
Sealing plate.Modified boron nitride composite provided by the invention is not good as thin-strip casting side sealing plate thermal shock resistance, at high temperature not
It is easy to crack.
The present invention provides a kind of modified boron nitride composites, are prepared by the raw material for including following mass percentage
It arrives:
Preferably, by including that the raw material of following mass percentage is prepared:
Preferably, the Sialon is β-sialon, α-sialon or O '-sialon.
Preferably, the additive includes one of aluminium oxide, magnesia and oxidation hundred million or a variety of.
The present invention also provides the preparation methods of above-mentioned modified boron nitride composite, comprising the following steps:
Boron nitride, zirconium oxide, Sialon, silicon carbide and additive are subjected to ground and mixed, obtain mixed powder；
By the mixed powder Thermocompressed sintering and forming, modified boron nitride composite is obtained.
Preferably, after the ground and mixed gained powder partial size≤200 mesh.
Preferably, the Thermocompressed sintering and forming the following steps are included:
The mixed powder is fitted into mold, from room temperature the first heating to the first holding temperature, carries out the first heat preservation；Institute
The temperature for stating the first heat preservation is 1550~1650 DEG C, and the time of first heat preservation is 20~40min, the pressure of first heat preservation
It is by force 3~5MPa；
Mixed powder second after first heat preservation is warming up to the second holding temperature, carries out the second heat preservation；Described second protects
Temperature temperature be 1700~1800 DEG C, it is described second heat preservation time be 50~70min, it is described second heat preservation pressure be 8~
12MPa；
Mixed powder third after second heat preservation is warming up to third holding temperature, carries out third heat preservation；The third is protected
The when temperature of temperature is 1850~1950 DEG C, and the time of the third heat preservation is 50~70min, and the pressure of the third heat preservation is 14
~20MPa.
Preferably, the first heating is that the mixed powder is fitted into mold, from room temperature with 10~20 DEG C/min liter
Then temperature is warming up to 1500~1600 DEG C to 800~1000 DEG C with 5~10 DEG C/min, be then warming up to 5~10 DEG C/min
One holding temperature；
Second heating is to be warming up to the second holding temperature from the first holding temperature with 3~5 DEG C/min；
The third heating is to be warming up to third holding temperature from the second holding temperature with 3~5 DEG C/min.
The present invention also provides a kind of side seal board, the material of side seal board provided by the invention is that above-mentioned modified boron nitride is compound
The modification boron nitride composite that material or above-mentioned preparation method are prepared.
Advantageous effects: the present invention provides a kind of modified boron nitride composites, by including that following quality percentage contains
The raw material of amount is prepared: boron nitride 50~80%；Zirconium oxide 8~20%；Sialon 5~15%；Silicon carbide 5~15%；Addition
Agent 1~5%.In the present invention, boron nitride is with high temperature resistant, and anti-thermal shock, thermal expansion coefficient are small, do not melt with metal, easily machinery adds
The performances such as work, the addition of zirconium oxide makes material have good strengthening and toughening effect, but zirconium oxide is in sintered body cooling down
Process generates martensitic traoformation, volume expansion is generated in phase transition process, and cause surface to crack therewith, will cause in this way
Resulting materials thermal shock resistance reduces.And Sialon has very with superior thermal shock resistance, inoxidizability and with molten metal
The aggressivity of good compatibility and resist melt metal.Especially Sialon thermal expansion coefficient is small by (2.4 × 10-6~3.2 × 10-6/ K),
And the thermal expansion coefficient big (9.6 × 10 of zirconium oxide-6~10.5 × 10-6/ K), when zirconium oxide generates volume during phase transformation
Expansion, Sialon play the role of pinning, and zirconium oxide crystal face is inhibited to crack, and guarantee under modified boron nitride composite high temperature not
Cracking phenomena can be generated；Meanwhile the elasticity modulus of Sialon, in 250GPa or so, the elasticity modulus of zirconium oxide is 150GPa or so,
The Sialon material of high elastic modulus in this way can promote the lesser zirconium oxide transformation stress of elasticity modulus to significantly improve, and reduce crystal face
The generation of crackle.Embodiment experimental data shows that modified boron nitride composite thermal shock resistance provided by the invention is good, heating
To 1000 DEG C, do not rupture for water cooling 40 times.
Specific embodiment
The present invention provides a kind of modified boron nitride composites, are prepared by the raw material for including following mass percentage
It arrives:
In the present invention, unless otherwise specified, raw materials used to be using commercial goods well-known to those skilled in the art
It can.
In terms of mass percentage, modified boron nitride composite provided by the invention includes boron nitride 50~80%, more
Preferably 62~70%, most preferably 65~68%.
In terms of mass percentage, modified boron nitride composite provided by the invention includes zirconium oxide 8~20%, more excellent
It is selected as 10~15%.
In terms of mass percentage, modified boron nitride composite provided by the invention includes Sialon 5~15%, more preferably
It is 8~10%.In the present invention, the Sialon is preferably β-sialon, α-sialon or O '-sialon, more preferably O '-
sialon。
In the present invention, the boron nitride has high temperature resistant, and thermal shock resistance, thermal expansion coefficient are small, do not melt with metal, easy machine
The performances such as tool processing；Zirconium oxide has high intensity, high rigidity, high temperature resistant, alkali corrosion resistance, wearability etc., and in hot pressed sintering
During, as the temperature rises, have the characteristics that crystal transfer.It is thus possible to improve the intensity and toughness of side seal board, from
And enhance the ability that resistance to molten steel washes away.But zirconium oxide generates martensitic traoformation in sintered body cool down, in phase transformation
Volume expansion is generated in journey, and causes material surface to crack therewith, will cause the reduction of resulting materials thermal shock resistance in this way.
And Sialon has good compatibility and resist melt metal with superior thermal shock resistance, inoxidizability and with molten metal
Aggressivity；Especially Sialon thermal expansion coefficient is small by (2.4 × 10-6~3.2 × 10-6/ K), and the thermal expansion coefficient of zirconium oxide is big
(9.6×10-6~10.5 × 10-6/ K), when zirconium oxide generates volume expansion during phase transformation, Sialon plays the work of pinning
With inhibition zirconium oxide crystal face cracks, and guarantees that cracking phenomena will not be generated under modified boron nitride composite high temperature；Meanwhile
The elasticity modulus of Sialon is 150GPa or so, the Sialon of such high elastic modulus in 250GPa or so, the elasticity modulus of zirconium oxide
Material can promote the lesser zirconium oxide transformation stress of elasticity modulus to significantly improve, and reduce the generation of crystal face crackle.
In terms of mass percentage, modified boron nitride composite provided by the invention includes silicon carbide 5~15%, more excellent
It is selected as 8~10%.In the present invention, silicon carbide intensity with higher, the ability of anti-metal corroded by liquid are added a certain amount of
Silicon carbide is conducive to the heat-resistant knocking stability for improving material, improves the inoxidizability of material, and enhancing side seal board resists molten steel
Ability, extend the service life of side seal board.
In terms of mass percentage, modified boron nitride composite provided by the invention includes additive 1~5%, more excellent
It is selected as 2~3%.In the present invention, the additive preferably includes one of aluminium oxide, magnesia and oxidation hundred million or a variety of,
More preferably oxidation hundred million.The present invention reduces firing temperature by the way that additive is added, and forming liquid phase densifies material more.
The present invention also provides the preparation methods of above-mentioned modified boron nitride composite, comprising the following steps:
Boron nitride, zirconium oxide, Sialon, silicon carbide and additive are subjected to ground and mixed, obtain mixed powder；
By the mixed powder Thermocompressed sintering and forming, modified boron nitride composite is obtained.
Boron nitride, zirconium oxide, Sialon, silicon carbide and additive are carried out ground and mixed by the present invention, obtain mixed powder.
The present invention is not particularly limited mixed method, selects mixed method well known to those skilled in the art.
The present invention is not particularly limited the method for ground and mixed, selects the method for ground and mixed well known to those skilled in the art i.e.
Can, such as ball milling.In the present invention, gained mixed powder partial size is preferably≤200 mesh after the ground and mixed, more preferably≤
150 mesh.
After obtaining mixed powder, obtained mixed powder is carried out Thermocompressed sintering and forming by the present invention, obtains modified boron nitride
Composite material.
In the present invention, the Thermocompressed sintering and forming preferably includes following steps:
Mixed powder is fitted into mold, from room temperature the first heating to the first holding temperature, carries out the first heat preservation；Described
The temperature of one heat preservation is 1550~1650 DEG C, and the time of first heat preservation is 20~40min, and the pressure of first heat preservation is
3~5MPa；
Mixed powder second after first heat preservation is warming up to the second holding temperature, carries out the second heat preservation；Described second protects
Temperature temperature be 1700~1800 DEG C, it is described second heat preservation time be 50~70min, it is described second heat preservation pressure be 8~
12MPa；
Mixed powder third after second heat preservation is warming up to third holding temperature, carries out third heat preservation；The third is protected
The when temperature of temperature is 1850~1950 DEG C, and the time of the third heat preservation is 50~70min, and the pressure of the third heat preservation is 14
~20MPa.
Mixed powder is fitted into mold by the present invention, from room temperature the first heating to the first holding temperature, carries out the first heat preservation；
The temperature of first heat preservation is 1550~1650 DEG C, and the time of first heat preservation is 20~40min, first heat preservation
Pressure is 3~5MPa.
It in the present invention, further include being granulated before the mixed powder is packed into mold.The present invention does not have the method for the granulation
There is particular determination, selects prilling process well known to those skilled in the art.The present invention makes preferably by isostatic pressing machine
Grain.In the present invention, the partial size of particle obtained by the granulation is preferably 1~5mm, more preferably 3~4mm.
In the present invention, the temperature of first heat preservation is preferably 1550~1650 DEG C, and further preferably 1600 DEG C；Institute
The time for stating the first heat preservation is preferably 20~40min, further preferably 30~35min；The pressure of first heat preservation is preferred
For 3~5MPa, further preferably 4MPa.
In the present invention, the first heating is preferably warming up to 800~1000 DEG C from room temperature with 10~20 DEG C/min, so
1500~1600 DEG C are warming up to 5~10 DEG C/min afterwards, the first holding temperature is then warming up to 5~10 DEG C/min；More preferably
To be warming up to 900~950 DEG C from room temperature with 15 DEG C/min, 1550 DEG C then are warming up to 7 DEG C/min, then with 7 DEG C/min
It is warming up to the first holding temperature.In the present invention, the pressure of first heat preservation is preferably provided by inflated with nitrogen in confined conditions.
In the present invention, start the pressure of inflated with nitrogen to the first heat preservation after being warming up to 1500~1600 DEG C with 5~10 DEG C/min.This hair
The bright rate to inflated with nitrogen is not particularly limited, and selects rate well known to those skilled in the art.The present invention is filled with nitrogen
When in order to prevent boron nitride occur oxidation reaction.The pressure for being forced into the first heat preservation carries out precompressed, prevents mixed powder under high temperature
Rebound.
After first heat preservation, the mixed powder second after the first heat preservation is warming up to the second holding temperature by the present invention, carries out the
Two heat preservations；The temperature of second heat preservation is 1700~1800 DEG C, and the time of second heat preservation is 50~70min, described the
The pressure of two heat preservations is 8~12MPa.
In the present invention, the temperature of second heat preservation is 1700~1800 DEG C, preferably 1750 DEG C；Second heat preservation
Time be 50~70min, preferably 60~65min；The pressure of second heat preservation is 8~12MPa, preferably 10MPa.
In the present invention, second heating is preferably warming up to the second heat preservation from the first holding temperature with 3~5 DEG C/min
Temperature.In the present invention, continue inflated with nitrogen while the described second heating, pressure is made to rise to the pressure of the second holding temperature.This
Invention is not particularly limited the rate of inflated with nitrogen, selects rate well known to those skilled in the art.The present invention passes through liter
The pressure that temperature was kept the temperature and be forced into the second holding temperature to the second holding temperature enables additive adequately to form liquid phase,
It is distributed more evenly across in material.
After second heat preservation, the mixed powder third after the second heat preservation will be warming up to third holding temperature by the present invention, be carried out
Third heat preservation；The when temperature of the third heat preservation is 1850~1950 DEG C, and the time of the third heat preservation is 50~70min, institute
The pressure for stating third heat preservation is 14~20MPa.
In the present invention, the temperature of the third heat preservation is 1850~1950 DEG C, preferably 1900 DEG C；The third heat preservation
Time be 50~70min, preferably 60~65min；The pressure of the third heat preservation is preferably 15~17MPa.
In the present invention, the third heating is preferably warming up to third heat preservation from the second holding temperature with 3~5 DEG C/min
Temperature.In the present invention, continue inflated with nitrogen while the third heats up, pressure is made to rise to the pressure of the second holding temperature.This
Invention is not particularly limited the rate of inflated with nitrogen, selects rate well known to those skilled in the art.The present invention passes through liter
Temperature kept the temperature and boosted to the third holding temperature pressure of third holding temperature processed keeps the oxide in material sufficient
Reaction.
After the third heat preservation, the present invention obtains modified boron nitride composite it is also preferable to include pressure release and Temperature fall.
The present invention is not particularly limited the method for pressure release and Temperature fall, selects method well known to those skilled in the art.
The present invention is not particularly limited the type of mold, according to modified silicon nitride composite material can select
It selects.
The present invention also provides a kind of side seal board, the material of the side seal board be above-mentioned modified boron nitride composite or on
State the modification boron nitride composite that preparation method is prepared.
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
Raw material and its mass percentage
Ball milling 12 hours after the raw material of above-mentioned mass percentage is mixed, 200 meshes are crossed, mixture is obtained, it is then sharp
It is granulated with isostatic pressing machine and (is formed granularity≤5mm particle), then die-filling carry out Thermocompressed sintering and forming, Thermocompressed sintering and forming
Condition are as follows: rise to 900 DEG C from room temperature with 15 DEG C/min, then rise to 1400 DEG C with 5 DEG C/min, start to fill N2, with 5 DEG C/min liter
To 1600 DEG C and it is forced into 5MPa, heat-insulation pressure keeping 30min rises to 1700 DEG C with 4 DEG C/min, is forced into 8MPa, heat-insulation pressure keeping
60min rises to 1850 DEG C with 3 DEG C/min, and is forced into 14MPa, heat-insulation pressure keeping 60min, release Temperature fall, and depanning is changed
Property boron nitride composite.Modified boron nitride composite is tested, density 2.65g/cm3, using lee ' hardness
Measure lee ' hardness is 592, bending strength 165MPa is measured using three-point bending method, thermal expansion coefficient is 3.6 × 10-6/ K,
Thermal shock resistance is preferable, is heated to 1000 DEG C by room temperature, does not rupture for water cooling 40 times, tries out service life by client and does not jump a queue
The raising 50% or so of grand material.
Comparative example 1
O'-sialon is not added, it is other identical with embodiment 1, obtain common boron nitride composite.To common nitrogen
Change boron composite material to be tested for the property, as a result as follows: its density is 2.58g/cm3, using Leeb Hardness Tester to measure Richter scale hard
Degree is 522, measures bending strength 122MPa using three-point bending method, thermal expansion coefficient is 5.8 × 10-6/ K, is heated to by room temperature
1000 DEG C, there is slight crackle water cooling 32 times.
As embodiment 1 and comparative example 1 it is found that boron nitride composite density obtained in embodiment 1 is big, hardness is high, heat
The coefficient of expansion is low, and thermal shock resistance is good.
Embodiment 2
Raw material and its mass percentage
Ball milling 12 hours after the raw material of above-mentioned mass percentage is mixed, 200 meshes are crossed, mixture is obtained, it is then sharp
Be granulated with isostatic pressing machine, then die-filling carry out Thermocompressed sintering and forming, Thermocompressed sintering and forming condition are as follows: from room temperature with 10 DEG C/
Min rises to 800 DEG C, then rises to 1500 DEG C with 8 DEG C/min, starts to fill N2, 1550 DEG C are risen to 5 DEG C/min and are forced into
4MPa, heat-insulation pressure keeping 40min rise to 1750 DEG C with 4 DEG C/min, are forced into 10MPa, heat-insulation pressure keeping 70min, with 3 DEG C/min liter
To 1950 DEG C, and it is forced into 16MPa, heat-insulation pressure keeping 70min, release Temperature fall, depanning obtains modified boron nitride composite.
Modified boron nitride composite is tested, density 2.72g/cm3, use Leeb Hardness Tester measure lee ' hardness for
632, bending strength 182MPa is measured using three-point bending method, thermal expansion coefficient is 3.2 × 10-6/ K is heated to 1000 by room temperature
DEG C, it does not rupture for water cooling 40 times, tries out service life by client and do not jump a queue the raising 25% or so of grand material.
Embodiment 3
Raw material and its mass percentage
Ball milling 12 hours after the raw material of above-mentioned mass percentage is mixed, 200 meshes are crossed, mixture is obtained, it is then sharp
Be granulated with isostatic pressing machine, then die-filling carry out Thermocompressed sintering and forming, Thermocompressed sintering and forming condition are as follows: from room temperature with 20 DEG C/
Min rises to 1000 DEG C, then rises to 1650 DEG C with 10 DEG C/min, starts to fill N2, 1800 DEG C are risen to 8 DEG C/min and are forced into
3MPa, heat-insulation pressure keeping 20min rise to 1800 DEG C with 4 DEG C/min, are forced into 12MPa, heat-insulation pressure keeping 50min, with 3 DEG C/min liter
To 1950 DEG C, and it is forced into 20MPa, heat-insulation pressure keeping 50min, release Temperature fall, depanning obtains modified boron nitride composite.
Modified boron nitride composite is tested, density 2.32g/cm3, use Leeb Hardness Tester measure lee ' hardness for
512, bending strength 122MPa is measured using three-point bending method, thermal expansion coefficient is 4.1 × 10-6/ K, thermal shock resistance is preferable, by room
Temperature is heated to 1000 DEG C, does not rupture for water cooling 40 times, tries out service life by client and does not jump a queue the raising 15% of grand material
Left and right.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of modified boron nitride composite is prepared by the raw material for including following mass percentage:
2. modified boron nitride composite according to claim 1, which is characterized in that by including following mass percentage
Raw material be prepared:
3. modified boron nitride composite according to claim 1 or 2, which is characterized in that the Sialon be β-sialon,
α-sialon or O '-sialon.
4. modified boron nitride composite according to claim 1 or 2, which is characterized in that the additive includes oxidation
One of aluminium, magnesia and oxidation hundred million are a variety of.
5. the preparation method of modification boron nitride composite described in Claims 1 to 4 any one, comprising the following steps:
Boron nitride, zirconium oxide, Sialon, silicon carbide and additive are subjected to ground and mixed, obtain mixed powder；
By the mixed powder Thermocompressed sintering and forming, modified boron nitride composite is obtained.
6. preparation method according to claim 5, which is characterized in that the partial size of powder obtained by after the ground and mixed≤
200 mesh.
7. preparation method according to claim 5, which is characterized in that the Thermocompressed sintering and forming the following steps are included:
The mixed powder is fitted into mold, from room temperature the first heating to the first holding temperature, carries out the first heat preservation；Described
The temperature of one heat preservation is 1550~1650 DEG C, and the time of first heat preservation is 20~40min, and the pressure of first heat preservation is
3~5MPa；
Mixed powder second after first heat preservation is warming up to the second holding temperature, carries out the second heat preservation；Second heat preservation
Temperature be 1700~1800 DEG C, it is described second heat preservation time be 50~70min, it is described second heat preservation pressure be 8~
12MPa；
Mixed powder third after second heat preservation is warming up to third holding temperature, carries out third heat preservation；The third heat preservation
Temperature is 1850~1950 DEG C, and the time of third heat preservation is 50~70min, the pressure of the third heat preservation is 14~
20MPa。
8. preparation method according to claim 7, which is characterized in that the first heating be from room temperature with 10~20 DEG C/
Min is warming up to 800~1000 DEG C, is then warming up to 1500~1600 DEG C with 5~10 DEG C/min, then with 5~10 DEG C/min liter
Temperature is to the first holding temperature；
Second heating is to be warming up to the second holding temperature from the first holding temperature with 3~5 DEG C/min；
The third heating is to be warming up to third holding temperature from the second holding temperature with 3~5 DEG C/min.
9. a kind of side seal board, which is characterized in that the material of the side seal board is modification described in Claims 1 to 4 any one
The modification boron nitride composite wood that preparation method described in boron nitride composite or claim 5~8 any one is prepared
Material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113683411A (en) * | 2021-08-12 | 2021-11-23 | 山东鹏程陶瓷新材料科技有限公司 | Ceramic side sealing plate for twin-roll thin-strip continuous casting and preparation method thereof |
-
2019
- 2019-01-29 CN CN201910086738.7A patent/CN109704779A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113683411A (en) * | 2021-08-12 | 2021-11-23 | 山东鹏程陶瓷新材料科技有限公司 | Ceramic side sealing plate for twin-roll thin-strip continuous casting and preparation method thereof |
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Application publication date: 20190503 |
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