CN209872799U - Device of low energy consumption hot pressing production boron nitride base pottery - Google Patents
Device of low energy consumption hot pressing production boron nitride base pottery Download PDFInfo
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Abstract
The utility model discloses a device of low energy consumption hot pressing production boron nitride base pottery, include: the sintering system is used for sintering the raw materials to obtain the boron nitride-based ceramic; the vacuumizing system is communicated with the sintering system and is used for vacuumizing the sintering system; inflation system, inflation system and sintering system are linked together for aerify the sintering system, the utility model discloses can practice thrift 10 ~ 50% power consumption, reduce the maintenance and the cost of maintenance of equipment, the preparation has the boron nitride base ceramic material of excellent performance.
Description
Technical Field
The utility model belongs to the technical field of hot pressing ceramic manufacture, particularly, the utility model relates to a low energy consumption hot pressing production boron nitride base pottery device.
Background
The boron nitride-based ceramic is an important engineering material, has the advantages of high thermal conductivity, small coefficient of thermal expansion, high thermal and vibration resistance, high temperature resistance, corrosion resistance and the like, and is widely applied to various industries. Because boron nitride is flaky, boron nitride-based ceramics are difficult to sinter, and hot-pressing sintering is generally adopted in the industry.
At present, in the hot pressing production process of boron nitride, the production is usually carried out in vacuum or in an atmosphere of circularly introducing protective gas at high temperature. Production in a vacuum environment generally maintains a certain vacuum degree in a furnace body in the whole production process, and the vacuum degree is generally required to be more than 10-2Pa; the production mode of filling protective gas is to pre-vacuumize the furnace body at low temperature and fill protective gas when the furnace body is kept in vacuum state and the temperature is raised to over 1000 ℃. At present, the two production modes have high energy consumption, and the vacuum pump continuously works and is quickly damaged, so that the electric energy consumption is increased, and the equipment maintenance cost is increased.
According to the above analysis, the conventional boron nitride hot-pressing production method has the following disadvantages:
the existing boron nitride hot-pressing production mode and device not only have high energy consumption, but also have the advantages that the vacuum pump continuously works and is fast in breakage, so that the electric energy consumption is increased, and the equipment maintenance cost is increased.
Disclosure of Invention
The utility model provides a device of low energy consumption hot pressing production boron nitride base pottery can solve the big technical problem with high maintenance cost of boron nitride hot pressing production mode power consumption among the prior art.
In order to solve the problems, the application provides a method for producing boron nitride-based ceramics by low-energy-consumption hot pressing, which adopts the following technical scheme:
a method for producing boron nitride-based ceramics by low-energy-consumption hot pressing sequentially comprises the following steps:
and (3) vacuumizing: vacuumizing the furnace body filled with the boron nitride-based ceramic raw material;
and (3) filling protective atmosphere: filling protective gas into the furnace body after vacuumizing;
heating and sintering: and heating and hot-pressing sintering the boron nitride-based ceramic raw material in the furnace body to obtain the boron nitride-based ceramic.
In the method for producing the boron nitride-based ceramic by hot pressing with low energy consumption, as a preferred mode, the furnace body is a hot pressing furnace body.
In the method for producing boron nitride-based ceramics by hot pressing with low energy consumption, as a preferable mode, in the step of vacuumizing, the furnace body is vacuumized until the vacuum degree in the furnace body is not lower than 10-2Pa。
In the method for producing boron nitride-based ceramic by low-energy-consumption hot pressing, as a preferred mode, in the step of vacuumizing, the boron nitride-based ceramic raw material is mixed powder of boron nitride and zirconium dioxide, and the boron nitride-based ceramic raw material is subjected to cold pressing treatment; the pressure of cold pressing is 3-10 MPa.
In the method for producing boron nitride-based ceramics by hot pressing with low energy consumption, as a preferable mode, in the step of filling the protective atmosphere, the protective gas is filled until the pressure in the furnace body reaches 20-50KPa, so that the inflow of external oxygen can be weakened, and the gas expansion when the temperature is raised due to too large pressure can not damage the furnace body.
In the method for producing boron nitride-based ceramics by hot pressing with low energy consumption, as a preferable mode, in the step of filling the protective atmosphere, the protective gas is an inert gas, and preferably, the inert gas is nitrogen.
In the method for producing boron nitride-based ceramic by low-energy-consumption hot pressing, as a preferred mode, in the temperature-rising sintering step, the temperature-rising rate is 5-10 ℃/min; the temperature of the hot-pressing sintering is 1800-2000 ℃, the pressure is 20-25MPa, the time is 0.5-1h, and then the temperature is reduced along with the furnace.
An apparatus for producing a boron nitride-based ceramic by low-energy-consumption hot pressing, comprising:
the sintering system is used for sintering the raw materials to obtain the boron nitride-based ceramic;
the vacuumizing system is communicated with the sintering system and is used for vacuumizing the sintering system;
the gas charging system is communicated with the sintering system and is used for charging gas to the sintering system;
the sintering system comprises a furnace body and a mold, wherein a cavity-shaped heating body is arranged between the inside of the furnace body and the outer side of the mold and used for heating the raw materials in the mold; an outer heat insulation layer and a heat insulation layer are sequentially arranged on the outer surface of the heating body from inside to outside, and the heat insulation layer is positioned inside the furnace body; and lower heat-insulating layers are arranged at the lower parts of the heating body, the outer heat-insulating layer and the heat-insulating layer.
In the apparatus for producing boron nitride-based ceramic by hot pressing with low energy consumption, as a preferred mode, in the sintering system, an inductor is arranged on the outer surface of the heat insulation layer, and the inductor is a temperature inductor.
In the apparatus for producing boron nitride-based ceramics by low energy consumption hot pressing, as a preferred mode, in the sintering system, the mold is a graphite mold, and the mold is used for holding raw materials to be hot-pressed and sintered; preferably, the mold is a high-strength graphite mold; preferably, the mold comprises a male mold and a female mold, the female mold is positioned on the lower heat-insulating layer, and the male mold extends into the heating body from top to bottom; more preferably, the dimensional deviation of the male mold is-0.01 to-0.1 mm; and the tolerance size deviation of the female die is 0.01-0.1 mm.
In the apparatus for producing boron nitride-based ceramics by low-energy-consumption hot pressing, as a preferred mode, the vacuum pumping system comprises a vacuum pump, and preferably, a vacuum valve and a barometer for adjusting the vacuum pump are mounted on the vacuum pump.
In the apparatus for producing boron nitride-based ceramics by hot pressing with low energy consumption, the aeration system preferably comprises an aeration bottle for containing gas; preferably, the inflation bottle is provided with an inflation valve for opening and closing the inflation bottle and adjusting the flow of gas in the inflation bottle.
In the apparatus for producing boron nitride-based ceramics by low energy consumption hot pressing, as a preferred mode, the apparatus for producing boron nitride-based ceramics by low energy consumption hot pressing further comprises a hydraulic system, wherein the hydraulic system comprises a hydraulic station located below the sintering system, an upper oil press located above the sintering system, and a lower oil press located below the sintering system; preferably, a sealing corrugated pipe is arranged between the upper oil pressing machine and the die and used for adjusting a male die in the die to move up and down; preferably, a sealing corrugated pipe is arranged between the lower oil press and the lower bottom heat-insulating layer and used for adjusting the furnace body to move up and down.
The analysis can know, compare with prior art, the utility model discloses an advantage and beneficial effect lie in:
1) the traditional production mode needs the vacuum pump to keep working in most of time, and the method for producing the boron nitride-based ceramic through low-energy-consumption hot pressing only needs to start the vacuum pump to work for a period of time at room temperature, so that the power consumption can be reduced by about 10-50% during production, and the maintenance and repair cost of later equipment can be reduced due to the reduction of the use frequency of the vacuum pump.
2) The boron nitride-based ceramic material prepared by the utility model has excellent performance.
3) The device for producing the boron nitride-based ceramics by low energy consumption hot pressing is convenient, practical and good in heat preservation.
Drawings
FIG. 1 is a schematic structural diagram of the apparatus for producing boron nitride-based ceramics by low energy consumption hot pressing according to the present invention.
FIG. 2 is a cross-sectional view of the apparatus for producing boron nitride-based ceramics by low energy consumption hot pressing according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative work belong to the protection scope of the present invention.
Example 1
A method for producing boron nitride-based ceramics by low energy consumption hot pressing, referring to fig. 1, comprising the following steps:
the method comprises the following steps: and vacuumizing the furnace body.
The mixed powder of boron nitride and zirconia (the dosage relationship of boron nitride and zirconia is the conventional dosage relationship in the field) is put into a mould and then the mould is filled with the mixed powderPlacing the mold into a furnace body, adjusting pressure to make the mixed powder cold-pressed and molded under the pressure of 10MPa, sealing the hot-pressing furnace, closing an inflation valve, starting a vacuum-pumping system to vacuumize the interior of the furnace body, wherein the temperature is room temperature under a common working condition during vacuum-pumping, and the vacuum-pumping is carried out until the vacuum degree in the furnace body is not less than 10-2Pa。
Step two: and (4) filling protective gas into the furnace body after vacuumizing.
Stopping vacuumizing, closing the vacuum valve and the vacuumizing system, opening the inflation valve and the inflation system, and inflating nitrogen. When the air pressure reaches 30KPa, the inflation valve and the inflation system are closed.
Step three: and heating the furnace body filled with the protective gas to sinter the raw materials in the furnace body.
Heating to 1800 ℃ according to the heating rate of 10 ℃/min, and then carrying out hot-pressing sintering for 1 hour, wherein the hot-pressing pressure is 25MPa, so as to obtain the boron nitride-based ceramic.
The whole process of the invention consumes about 20 degrees.
The performance results of the obtained boron nitride-based ceramics are as follows: the average value of the hardness of the steel is 452HL, and the density is 2.55g/cm3。
The density test adopts a standard drainage method, and the method for testing the hardness of the steel plate comprises the following steps: the surface of the sample is printed with 1 hardness value in each area of 3cm multiplied by 3cm, and the 10 hardness values are printed in total, and then the 10 hardness values are averaged to obtain the average value which is taken as the Richter hardness value of the sample.
Example 2
A low energy consumption hot pressing method for producing boron nitride-based ceramics, comprising:
the method comprises the following steps: same as in example 1.
Step two: the same procedure as in example 1 was repeated except that the pressure of nitrogen gas was changed to 40 KPa.
Step three: the same applies to example 1.
The performance results of the obtained boron nitride-based ceramics are as follows: the average value of the hardness is 450HL, and the density is 2.56g/cm3。
Example 3
A low energy consumption hot pressing method for producing boron nitride-based ceramics, comprising:
the method comprises the following steps: same as in example 1.
Step two: same as in example 1.
Step three: the same procedure as in example 1 was repeated, except that the temperature increase rate was 5 ℃ C/min and the temperature of the mixture was changed to example 1.
The obtained boron nitride-based ceramic had the property results that the average value of the hardness in Rich was 463HL and the density was 2.58g/cm3。
Example 4
A low energy consumption hot pressing method for producing boron nitride-based ceramics, comprising:
the method comprises the following steps: same as in example 1.
Step two: same as in example 1.
Step three: the same as example 1 except that the sintering temperature was 2000 ℃ and the sintering temperature was different from example 1.
The performance results of the obtained boron nitride-based ceramics are as follows: the average value of the hardness of the alloy is 523HL, and the density is 2.7g/cm3。
Example 5
A low energy consumption hot pressing method for producing boron nitride-based ceramics, comprising:
the method comprises the following steps: same as in example 1.
Step two: same as in example 1.
Step three: the same as example 1 except that the sintering temperature was 1900 ℃ and the sintering temperature was different from example 1.
The performance results of the obtained boron nitride-based ceramics are as follows: the average value of the hardness is 505HL, and the density is 2.65g/cm3。
Example 6
A low energy consumption hot pressing method for producing boron nitride-based ceramics, comprising:
the method comprises the following steps: same as in example 1.
Step two: same as in example 1.
Step three: the process was the same as in example 1 except that the sintering time was 0.5 hours and the sintering time was different from that of example 1.
The obtained boron nitride-based ceramicsThe performance results of the porcelain were: the average value of the hardness is 456HL, and the density is 2.52g/cm3。
Example 7
A low energy consumption hot pressing method for producing boron nitride-based ceramics, comprising:
the method comprises the following steps: same as in example 1.
Step two: same as in example 1.
Step three: the same as example 1 except that the hot-pressing pressure was 20MPa, and the same as example 1.
The performance results of the obtained boron nitride-based ceramics are as follows: the average value of the hardness is 456HL, and the density is 2.55g/cm3。
Comparative example 1
A conventional method for producing a boron nitride-based ceramic by hot pressing, comprising:
the method comprises the following steps: and vacuumizing the furnace body.
Loading boron nitride and zirconia (the dosage relation of the two is the same as that of the embodiment 1) into a mould 1, carrying out cold press molding under the pressure of 10MPa, then loading the mould into a furnace body 4, sealing the furnace body 4, closing an inflation system 3 and an inflation valve 6, opening a vacuum pumping system 2 and a vacuum valve 5 to carry out vacuum pumping on the furnace body of the hot pressing furnace, wherein the temperature is room temperature under the common working condition during vacuum pumping, and carrying out vacuum pumping until the vacuum degree in the furnace body of the hot pressing furnace is not lower than 10-2Pa。
Step two: sintering under vacuum
And continuously vacuumizing, heating the furnace body 4 to 1800 ℃ at the heating rate of 10 ℃/min in a vacuum state, and then carrying out hot-pressing sintering for 1 hour, wherein the hot-pressing pressure is 25MPa, so as to obtain the boron nitride-based ceramic.
The whole process consumes about 60 degrees.
The average value of the hardness in Rich and the density of the boron nitride-based ceramics obtained by this comparative example are substantially the same as those of example 1.
Comparative example 2
A conventional method for producing a boron nitride-based ceramic by hot pressing, comprising:
the method comprises the following steps: and vacuumizing the furnace body.
Loading boron nitride and zirconia (the dosage relation of the two is the same as that of the embodiment 1) into a mould 1, carrying out cold press molding under the pressure of 10MPa, then loading the mould 1 into a furnace body of a furnace body 4, sealing the furnace body 4, closing an inflation system 3 and an inflation valve 6, opening a vacuumizing system 2 and a vacuum valve 5 to vacuumize the furnace body, wherein the temperature is room temperature under the common working condition during vacuumizing, and vacuumizing is carried out until the vacuum degree in the furnace body is not lower than 10-2Pa。
Step two: preliminary temperature rise under vacuum
And continuously vacuumizing, and heating the furnace body 4 to 1000 ℃ in a vacuum state according to the heating rate of 10 ℃/min.
Step three: filling protective gas, and hot-pressing sintering
And (3) filling nitrogen into the furnace body of the hot pressing furnace until the pressure in the furnace body of the hot pressing furnace is 30KPa, then heating the hot pressing furnace 4 to 1800 ℃ according to the heating rate of 10 ℃/min, and then carrying out hot pressing sintering for 1 hour, wherein the hot pressing pressure is 25MPa, so as to obtain the boron nitride-based ceramic.
The whole process consumes about 60 degrees.
The average value of the hardness in Rich and the density of the boron nitride-based ceramics obtained by this comparative example are substantially the same as those of example 1.
Example 8
An apparatus for producing a boron nitride-based ceramic by low-energy-consumption hot pressing, comprising:
the sintering system is used for sintering the raw materials to obtain the boron nitride-based ceramic; the vacuumizing system is communicated with the sintering system and is used for vacuumizing the sintering system; the gas charging system is communicated with the sintering system and is used for charging gas to the sintering system; and a hydraulic system connected to the sintering system.
The sintering system comprises a furnace body 1 and a graphite mold 2 for bearing raw materials to be hot-pressed and sintered, wherein a cavity-shaped heating body 3 is arranged between the inside of the furnace body 1 and the outer side of the mold 2 and used for heating the raw materials in the mold; an outer heat-insulating layer 4 and a heat-insulating layer 5 are sequentially arranged on the outer surface of the heating body 3 from inside to outside; the lower parts of the heating body 3, the outer heat-insulating layer 4 and the heat-insulating layer 5 are provided with a lower heat-insulating layer 7. The outer surface of the heat insulation layer 5 is provided with a temperature sensor 6. The die 2 comprises a male die and a female die, the female die is positioned on the lower heat-insulating layer 7, and the male die extends into the heating body 3 from top to bottom.
The vacuum pumping system comprises a vacuum pump 8, and a vacuum valve 17 and an air pressure gauge are arranged on the vacuum pump 8; the vacuum valve is used to open, close and regulate the vacuum pump 8.
The inflation system comprises an inflation bottle 15 for containing gas and an inflation valve 16 arranged on the inflation bottle 15; the charging valve 16 is used for adjusting the flow of the gas flowing into the furnace body 1 in the charging bottle 15.
The hydraulic system comprises a hydraulic station 11, an upper oil press 9 positioned above the sintering system and a lower oil press 13 positioned below the sintering system; an upper oil pressing cylinder 12 is arranged on the upper oil pressing machine 9; a sealing corrugated pipe 10 is arranged between the upper oil pressing machine 9 and the die 2 and is used for adjusting the male die in the die 2 to move up and down.
A lower oil press 13 is provided with a lower oil cylinder 14; a sealing corrugated pipe is arranged between the lower oil press 13 and the lower bottom heat-insulating layer 7 and is used for adjusting the furnace body 1 to move up and down.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of the invention or which are equivalent to the scope of the invention are embraced by the invention.
Claims (10)
1. An apparatus for producing boron nitride-based ceramics by low energy consumption hot pressing, comprising:
the sintering system is used for sintering the raw materials to obtain the boron nitride-based ceramic;
the vacuumizing system is communicated with the sintering system and is used for vacuumizing the sintering system;
the gas charging system is communicated with the sintering system and is used for charging gas to the sintering system;
the sintering system comprises a furnace body and a mold, wherein a cavity-shaped heating body is arranged between the inside of the furnace body and the outer side of the mold and used for heating the raw materials in the mold; an outer heat insulation layer and a heat insulation layer are sequentially arranged on the outer surface of the heating body from inside to outside; and lower heat-insulating layers are arranged at the lower parts of the heating body, the outer heat-insulating layer and the heat-insulating layer.
2. The apparatus for low-energy-consumption hot-pressing production of boron nitride-based ceramics according to claim 1, wherein in the sintering system, the outer surface of the thermal insulation layer is provided with an inductor, and the inductor is a temperature inductor.
3. The apparatus for low-energy-consumption hot-pressing production of boron nitride-based ceramics according to claim 1, wherein in the sintering system, the mold is a high-strength graphite mold for holding a raw material to be hot-pressed and sintered.
4. The apparatus for low-energy-consumption hot-pressing production of a boron nitride-based ceramic according to claim 1, wherein in the sintering system, the mold comprises a male mold and a female mold, the female mold is positioned on the lower heat-insulating layer, and the male mold extends into the interior of the heating body from top to bottom.
5. The apparatus for low-energy-consumption hot-pressing production of a boron nitride-based ceramic according to claim 4, wherein in the sintering system, the male die dimensional deviation is-0.01 to-0.1 mm; and the tolerance size deviation of the female die is 0.01-0.1 mm.
6. The apparatus for low-energy-consumption hot-pressing production of a boron nitride-based ceramic according to claim 1, wherein the evacuation system comprises a vacuum pump on which a vacuum valve and a barometer for adjusting the vacuum pump are mounted.
7. The apparatus for low energy consumption hot pressing production of boron nitride based ceramics according to claim 1, wherein the inflation system comprises an inflation bottle for holding gas, the inflation bottle is equipped with an inflation valve for opening and closing the inflation bottle and adjusting the flow of gas in the inflation bottle.
8. The apparatus for low energy consumption hot pressing production of boron nitride based ceramics according to claim 1, wherein the apparatus for low energy consumption hot pressing production of boron nitride based ceramics further comprises a hydraulic system comprising a hydraulic station located below the sintering system, an upper oil press located above the sintering system, and a lower oil press located below the sintering system.
9. The apparatus for producing boron nitride-based ceramics according to claim 8, wherein a sealing bellows is provided between the upper oil press and the mold for adjusting the up-and-down movement of the male mold in the mold.
10. The apparatus for producing boron nitride-based ceramics according to claim 8, wherein a sealing bellows is provided between the lower hydraulic press and the lower bottom insulating layer for regulating the up-and-down movement of the furnace body.
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| EP1701121A3 (en) * | 2005-03-10 | 2007-07-25 | Edison Hard | Thermal treatment furnace |
| CN1300056C (en) * | 2005-07-19 | 2007-02-14 | 武汉理工大学 | Fast preparation of high-purity hexagonal boron nitride ceramic material under low-temperature |
| CN2844815Y (en) * | 2005-10-21 | 2006-12-06 | 北京时创真空工业炉有限责任公司 | The vacuum hydrogen sintering furnace |
| CN101655310B (en) * | 2009-09-18 | 2012-07-04 | 沈阳恒进真空科技有限公司 | Protective atmosphere vacuum sintering furnace with high temperature of 1800 DEG C |
| CN203908307U (en) * | 2014-06-18 | 2014-10-29 | 上海福乃斯电炉科技有限公司 | Integrated high-temperature vacuum hot pressing sintering furnace |
| CN106278284A (en) * | 2016-08-04 | 2017-01-04 | 长兴鑫宇耐火材料有限公司 | A kind of method utilizing ring-shaped graphite mould step sintering to prepare boron nitride ceramic material |
| CN107869909B (en) * | 2016-09-26 | 2019-06-28 | 宁波江丰电子材料股份有限公司 | Vacuum hotpressing stove |
| CN207842264U (en) * | 2017-12-15 | 2018-09-11 | 郑州机械研究所有限公司 | A kind of silver-bearing copper composite band vacuum hot pressing device |
| CN109824368A (en) * | 2018-12-14 | 2019-05-31 | 安泰天龙钨钼科技有限公司 | A kind of method and apparatus of low energy consumption hot pressing production boron nitride-base ceramic |
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