CN112645714B - Silicon nitride ceramic dehydration element and preparation method and application thereof - Google Patents
Silicon nitride ceramic dehydration element and preparation method and application thereof Download PDFInfo
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- CN112645714B CN112645714B CN202011577454.7A CN202011577454A CN112645714B CN 112645714 B CN112645714 B CN 112645714B CN 202011577454 A CN202011577454 A CN 202011577454A CN 112645714 B CN112645714 B CN 112645714B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 79
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 230000018044 dehydration Effects 0.000 title claims abstract description 51
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 75
- 239000007921 spray Substances 0.000 claims abstract description 41
- 239000011812 mixed powder Substances 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 28
- 238000005469 granulation Methods 0.000 claims abstract description 27
- 230000003179 granulation Effects 0.000 claims abstract description 27
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 18
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 11
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000005452 bending Methods 0.000 claims description 5
- 235000015895 biscuits Nutrition 0.000 abstract description 36
- 239000003292 glue Substances 0.000 abstract description 10
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 description 20
- 238000003756 stirring Methods 0.000 description 16
- 238000000227 grinding Methods 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of ceramic materials, and particularly relates to a silicon nitride ceramic dehydration element and a preparation method and application thereof. The preparation method of the silicon nitride ceramic dehydration element provided by the invention comprises the following steps: mixing silicon nitride powder, alumina powder, yttrium oxide powder, titanium oxide powder, polyethylene glycol and water to obtain slurry; and carrying out spray granulation on the slurry, and sequentially carrying out dry pressing forming, cold isostatic pressing, glue discharging and sintering on the obtained mixed powder to obtain the silicon nitride ceramic dehydration element. In the invention, the dry pressing is beneficial to accurately controlling the size of the ceramic biscuit, the ceramic biscuit bears uniform pressure in all directions under the condition of cold isostatic pressing, and the density and the uniformity of the internal structure of the ceramic biscuit are further improved on the premise of controllable size. Experimental results show that the silicon nitride ceramic dehydration element prepared by the preparation method provided by the invention has high volume density and excellent mechanical property.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a silicon nitride ceramic dehydration element and a preparation method and application thereof.
Background
The dewatering elements (dewatering sheet) are an important component of the paper machine, and the wear resistance and service life of the dewatering sheet directly affect the runnability and cost of the paper machine. In the field of dewatering elements, alumina is an economical ceramic material with wide application, but the alumina has poor thermal shock resistance and cannot meet the use requirements of high-speed paper machines. Compared with alumina, silicon nitride is harder and more wear-resistant, has small abrasion to a forming wire of a paper machine, has proper heat conductivity and excellent thermal shock resistance, and is suitable as a ceramic material of a high-speed paper machine dewatering element.
At present, the forming mode of the silicon nitride ceramic dehydration element comprises an injection forming process and a dry pressing forming process, wherein the feeding formula, mixing and mold development of the injection forming process are difficult, the quality of a formed blank body is directly influenced by the design of the mold and the mold filling flowing state of an injection melt, and the quality of the dehydration element is difficult to control. The dry pressing molding is to press ceramic powder into a green body with a certain shape, and has the characteristics of low cost and high material utilization rate in the production of high-rigidity flat-shaped right-prism-structure ceramic products such as dehydration elements and the like, but the density of a biscuit obtained by the dry pressing molding is layered along with the density in the pressing direction, so that the problems of sintering cracking and internal unevenness are caused, and the pressure loss in the green body is caused by the internal friction between the powder and the mold wall.
Isostatic pressing is also a common process for ceramic forming, but cold isostatic pressing is used singly, the size and the shape of a biscuit are not easy to be accurately controlled, and the biscuit of a dehydration element is difficult to be formed in a near-size mode.
Disclosure of Invention
In view of the above, the present invention aims to provide a silicon nitride ceramic dehydration element and a preparation method thereof, and the silicon nitride ceramic dehydration element prepared by the preparation method provided by the present invention has characteristics of uniform density, accurate size, no microcrack, excellent mechanical properties, and capability of meeting use requirements of a paper machine dehydration element.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides a preparation method of a silicon nitride ceramic dehydration element, which comprises the following steps:
mixing silicon nitride powder, alumina powder, yttrium oxide powder, titanium oxide powder, polyethylene glycol and water to obtain slurry;
carrying out spray granulation on the slurry to obtain mixed powder;
and sequentially carrying out dry pressing forming, cold isostatic pressing, binder removal and sintering on the mixed powder to obtain the silicon nitride ceramic dehydration element.
Preferably, the mass ratio of the silicon nitride powder, the alumina powder, the yttrium oxide powder, the titanium oxide powder and the polyethylene glycol is (85-90): (4-8): (4-8): (0.5-2): (1-2).
Preferably, the solid content of the slurry is 35-60%.
Preferably, the conditions for spray granulation include: the pressure of the feeding pump is 800-1200 kPa, the pressure difference of the cyclone is 0.5-1 kPa, the inlet temperature of the spray tower is 180-200 ℃, and the outlet temperature of the spray tower is 90-100 ℃.
Preferably, the dry-pressing conditions include: the molding pressure is 2-5 MPa, and the pressure maintaining time is 1-10 s.
Preferably, the conditions of the cold isostatic pressing include: the vacuum degree is less than or equal to 1000Pa, the pressure is 150-250 Mpa, and the pressure maintaining time under the highest pressure is 50-400 s.
Preferably, the sintering heat preservation temperature is 1700-1800 ℃, and the heat preservation time is 1-2 h.
The invention also provides a silicon nitride ceramic dehydration element prepared by the preparation method in the technical scheme, wherein the crystal form of silicon nitride in the silicon nitride ceramic dehydration element is a beta phase;
the silicon nitride ceramic dehydration element contains a second phase of titanium nitride which is dispersed and distributed, and the size of the second phase of titanium nitride which is dispersed and distributed is less than or equal to 50 mu m.
Preferably, the volume density of the silicon nitride ceramic dehydration element is 3.2-3.3 g/cm3The Vickers hardness HV10 is 1380-1500, the bending strength is 600-1000 MPa, and the fracture toughness is 6-7 MPa.m-1/2And the metallurgical porosity rating is not lower than B06.
The invention also provides the application of the silicon nitride ceramic dewatering element in the technical scheme in a paper machine.
The invention provides a preparation method of a silicon nitride ceramic dehydration element, which comprises the following steps: mixing silicon nitride powder, alumina powder, yttrium oxide powder, titanium oxide powder, polyethylene glycol and water to obtain slurry; carrying out spray granulation on the slurry to obtain mixed powder; and sequentially carrying out dry pressing forming, cold isostatic pressing, binder removal and sintering on the mixed powder to obtain the silicon nitride ceramic dehydration element. In the invention, the alumina powder, the yttrium oxide powder and the titanium oxide powder are beneficial to obtaining the mixed powder containing columnar crystal grain beta-phase silicon nitride, and when the ceramic material cracks, the columnar crystal grains and the high-elasticity-modulus titanium nitride (formed by nitriding the titanium oxide) in dispersion promote the cracks to deflect and branch, consume the fracture energy and improve the mechanical property of the ceramic material; the dry pressing is favorable for accurately controlling the size of the ceramic biscuit, then under the condition of cold isostatic pressing, the ceramic biscuit bears uniform pressure in all directions, and shrinks in equal proportion, so that the density of the ceramic biscuit and the uniformity of an internal structure are further improved under the premise of controllable size, the uniformity degree and the size accuracy degree of the ceramic density are favorably improved, and the occurrence of cracking and deformation is reduced. In addition, the sintering process is directly carried out without cooling and running after rubber discharging, so that the risk of material damage in the cooling and running processes is reduced, and the production efficiency is improved.
Experimental results show that the bulk density of the silicon nitride ceramic dehydration element prepared by the preparation method provided by the invention is 3.2-3.25 g/cm3The Vickers hardness HV10 is 1380-1500, the bending strength is 600-800 MPa, and the fracture toughness is 6-7 MPa.m-1/2And the metallurgical porosity rating is not lower than B06.
Detailed Description
The invention provides a preparation method of a silicon nitride ceramic dehydration element, which comprises the following steps:
mixing silicon nitride powder, alumina powder, yttrium oxide powder, titanium oxide powder, polyethylene glycol and water to obtain slurry;
carrying out spray granulation on the slurry to obtain mixed powder;
and sequentially carrying out dry pressing forming, cold isostatic pressing, binder removal and sintering on the mixed powder to obtain the silicon nitride ceramic dehydration element.
In the present invention, the components are commercially available products well known to those skilled in the art, unless otherwise specified.
The method comprises the step of mixing silicon nitride powder, alumina powder, yttrium oxide powder, titanium oxide powder, polyethylene glycol and water to obtain slurry.
In the present invention, the median particle diameter of the silicon nitride powder is preferably not more than 1 μm, more preferably not more than 0.9. mu.m. In the invention, the content of alpha phase in the silicon nitride powder is preferably more than or equal to 90%. In the present invention, the median particle diameter of the alumina powder is preferably not more than 1 μm, more preferably not more than 0.8. mu.m. In the present invention, the yttrium oxide powder preferably has a median particle diameter of 1 μm or less, more preferably 0.8 μm or less. In the present invention, the median particle diameter of the titanium oxide powder is preferably not more than 1 μm, more preferably not more than 0.5. mu.m. In the invention, the mass ratio of the silicon nitride powder, the alumina powder, the yttrium oxide powder, the titanium oxide powder and the polyethylene glycol is preferably (85-90): (4-8): (4-8): (0.5-2): (1-2), more preferably (85.5-89.5): (4.5-7.5): (4.5-7.5): (0.7-1.7): (1.2-1.8). In the invention, the alumina powder, the yttrium oxide powder and the titanium oxide powder are beneficial to obtaining the mixed powder containing the columnar crystal grain beta-phase silicon nitride, and the columnar crystal grains and the high-elasticity-modulus titanium nitride which is dispersed and distributed are beneficial to promoting the deflection and the bifurcation of cracks when the ceramic material has the cracks, consuming the fracture energy and improving the mechanical property of the ceramic dehydration element.
In the present invention, the water is preferably deionized water. In the invention, the solid content of the slurry is preferably 35-60%, and more preferably 40-55%.
In the invention, the mixing of the silicon nitride powder, the alumina powder, the yttrium oxide powder, the titanium oxide powder, the polyethylene glycol and the water is preferably a stirring mill. In the present invention, the material of the grinding medium in the stirring mill is preferably silicon nitride. In the invention, the stirring speed of the stirring mill is preferably 180-230 rpm, more preferably 190-220 rpm; the time is preferably 10 to 20 hours, and more preferably 12 to 18 hours. In the invention, the stirring mill is beneficial to improving the uniform mixing degree of all the components of the slurry.
After the slurry is obtained, the slurry is subjected to spray granulation to obtain mixed powder.
In the present invention, the conditions for spray granulation include: the pressure of the feeding pump is preferably 800-1200 kPa, and more preferably 850-1150 kPa; the cyclone pressure difference is preferably 0.5-1 kPa, and more preferably 0.5-0.9 kPa; the inlet temperature of the spray tower is preferably 180-200 ℃, and more preferably 180-195 ℃; the outlet temperature of the spray tower is preferably 90-100 ℃, and more preferably 90-95 ℃. In the present invention, the spray granulation apparatus is preferably a spray granulation tower, and more preferably a pressure type spray granulation tower. The invention preferably introduces the slurry into the pressure spray granulation tower by means of a feed pump.
In the spray granulation process, the invention preferably stirs the slurry which is not introduced into the spray granulation equipment at low speed to prevent the slurry from precipitating and layering; the stirring speed of the low-speed stirring is preferably 5-20 rpm, and more preferably 10-15 rpm.
In the invention, the flow time of the mixed powder is preferably 60-80 s, and the judgment standard of the flow time is GB/T1482-2010. In the present invention, the bulk density of the mixture powder is preferably 0.6 to 1.0g/cm3The judgment standard of the loose packing density is GB/T1479-.
After the mixed powder is obtained, the mixed powder is sequentially subjected to dry pressing forming, cold isostatic pressing, binder removal and sintering to obtain the silicon nitride ceramic dehydration element.
After the mixed powder is obtained, the mixed powder is subjected to dry pressing forming to obtain a primary ceramic biscuit.
In the present invention, the dry press molding conditions include: the molding pressure is preferably 2-5 MPa, and more preferably 2.5-5 MPa; the dwell time is preferably 1 to 10s, and more preferably 2 to 5 s. In the present invention, the dry-pressing apparatus is preferably a dry powder press. In the present invention, the cross-sectional longest dimension of the primary ceramic biscuit is preferably 60mm or less and the height is preferably 65mm or less. In the present invention, the dry pressing is advantageous for improving the dimensional accuracy of the primary ceramic biscuit.
After the primary ceramic biscuit is obtained, the primary ceramic biscuit is subjected to cold isostatic pressing to obtain a secondary ceramic biscuit.
In the present invention, the conditions of the cold isostatic pressing include: the vacuum degree is preferably less than or equal to 1000Pa, and more preferably less than or equal to 900 Pa; the pressure intensity is preferably 150-250 MPa, and more preferably 150-230 MPa; the dwell time under the highest pressure condition is preferably 50-400 s, and more preferably 70-380 s. In the present invention, the cold isostatic pressing equipment is preferably a cold isostatic press. In the invention, the cold isostatic pressing is preferably carried out by placing the primary ceramic biscuit in a vacuum bag, vacuumizing, and then placing the primary ceramic biscuit in a cold isostatic pressing machine for cold isostatic pressing. In the invention, in the cold isostatic pressing, the primary ceramic biscuit bears uniform pressure in all directions, and shrinks in equal proportion, so that the density and the internal structure uniformity of the ceramic biscuit are further improved under the premise of controllable size, the density uniformity and the size accuracy of the ceramic are improved, and the cracking and deformation are reduced.
After the secondary ceramic biscuit is obtained, the secondary ceramic biscuit is subjected to glue removal and sintering to obtain the silicon nitride ceramic dehydration element.
In the invention, the heat preservation temperature of the binder removal is preferably 450-600 ℃, and more preferably 450-580 ℃; the heat preservation time is preferably 1-4 h, and more preferably 1.5-3.5 h. In the invention, the heat preservation temperature of the binder removal is preferably obtained by raising the temperature at room temperature; the heating rate is preferably 2-10 ℃/min, and more preferably 2-5 ℃/min. The invention discharges organic matters in the secondary ceramic biscuit by glue discharging.
In the invention, the sintering heat preservation temperature is preferably 1700-1800 ℃, and more preferably 1720-1780 ℃; the heat preservation time is preferably 1-2 h, and more preferably 1.2-1.8 h. In the invention, the sintering heat preservation temperature is preferably obtained by raising the temperature of the heat preservation temperature of the discharged glue; the heating rate is preferably 3-10 ℃/min, and more preferably 3-5 ℃/min. In the invention, the equipment for discharging and sintering glue is preferably a pneumatic furnace. In the invention, the equipment for discharging the glue and sintering is the same air pressure furnace, and temperature reduction and transportation are not needed.
After sintering, the invention preferably cools the product obtained by sintering; the cooling is not particularly limited in the present invention, and may be any cooling known to those skilled in the art, specifically, natural cooling.
The invention also provides the silicon nitride ceramic dehydration element prepared by the preparation method of the technical scheme. In the invention, the crystal form of silicon nitride in the silicon nitride ceramic dehydration element is beta phase. In the invention, the silicon nitride ceramic dehydration element contains a second phase of titanium nitride which is dispersed and distributed, and the size of the second phase of titanium nitride which is dispersed and distributed is less than or equal to 50 mu m.
In the invention, the longest dimension of the cross section of the silicon nitride ceramic dehydration element is preferably less than or equal to 45mm, and the height is preferably less than or equal to 50 mm.
In the invention, the bulk density of the silicon nitride ceramic dehydration element is preferably 3.2-3.3 g/cm3More preferably 3.2E3.25g/cm3(ii) a The Vickers hardness HV10 is preferably 1380-1500, more preferably 1400-1500; the bending strength is preferably 600-1000 MPa, and more preferably 600-800 MPa; the fracture toughness is preferably 6-7 MPa m-1/2(ii) a And the metallurgical porosity rating is not lower than B06.
The invention also provides the application of the silicon nitride ceramic dewatering element in the technical scheme in a paper machine. In the present invention, the paper machine is preferably a high-speed paper machine or a low-speed paper machine. The concrete installation method of the silicon nitride ceramic dewatering element in the paper machine is not limited in the invention, and the installation method of the dewatering element well known to those skilled in the art can be adopted.
In order to further illustrate the present invention, the following examples are provided to describe the silicon nitride ceramic dehydration component and the preparation method and application thereof in detail, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents used in the examples are all commercially available.
Example 1
Putting 89 parts of silicon nitride powder (the median particle size is less than or equal to 0.9 mu m), 4 parts of alumina powder (the median particle size is less than or equal to 0.8 mu m), 4 parts of yttrium oxide powder (the median particle size is less than or equal to 0.8 mu m), 1 part of titanium oxide powder (the median particle size is less than or equal to 0.5 mu m), 2 parts of polyethylene glycol and water into a stirring mill, and stirring and grinding for 15 hours at the rotating speed of 195rpm by taking a silicon nitride grinding ball as a grinding medium to obtain slurry with the solid content of 40%;
and (3) introducing the slurry into a pressure type spray granulation tower by using a feed pump for spray granulation, wherein the spray granulation conditions are as follows: the pressure of the feed pump was 850kPa, the cyclone pressure difference was 0.5kPa, the inlet temperature of the spray tower was 180 ℃ and the outlet temperature of the spray tower was 90 ℃ to obtain a mixed powder, the flow time of the obtained mixed powder was 62 seconds, and the apparent density was 0.8g/cm3；
Introducing the mixed powder into a dry powder press, designing the longest dimension of the section of a primary ceramic biscuit to be 25mm and the height to be 50mm, maintaining the pressure for 2s under the pressure of 3MPa for dry pressing and forming, placing the obtained primary ceramic biscuit in a vacuum bag, vacuumizing to be less than 1000Pa, placing the primary ceramic biscuit in a cold isostatic press, performing cold isostatic pressing for 120s under the pressure of 150MPa, placing the obtained secondary ceramic biscuit in a pressure furnace, heating to 450 ℃ at the speed of 4 ℃/min, preserving the heat for 2h for glue discharge, heating to 1700 ℃ at the speed of 6 ℃/min, preserving the heat for 2h, and cooling to obtain the silicon nitride ceramic dehydration element, wherein the longest dimension of the section of the obtained silicon nitride ceramic dehydration element is 20mm and the height is 40 mm.
Example 2
Putting 86 parts of silicon nitride powder (the median particle size is less than or equal to 0.9 mu m), 5 parts of alumina powder (the median particle size is less than or equal to 0.8 mu m), 5 parts of yttrium oxide powder (the median particle size is less than or equal to 0.8 mu m), 2 parts of titanium oxide powder (the median particle size is less than or equal to 0.5 mu m), 2 parts of polyethylene glycol and water in a stirring mill, taking a silicon nitride grinding ball as a grinding medium, and stirring and grinding for 20 hours at the rotating speed of 195rpm to obtain slurry with the solid content of 45%;
and (3) introducing the slurry into a pressure type spray granulation tower by using a feed pump for spray granulation, wherein the spray granulation conditions are as follows: the pressure of the feed pump was 900kPa, the cyclone pressure difference was 0.5kPa, the inlet temperature of the spray tower was 185 ℃ and the outlet temperature of the spray tower was 90 ℃ to obtain a mixed powder, the flow time of the obtained mixed powder was 63s, and the apparent density was 0.9g/cm3；
Introducing the mixed powder into a dry powder press, designing the longest dimension of the section of a primary ceramic biscuit to be 25mm and the height to be 50mm, keeping the pressure for 2s under the pressure of 5MPa for dry pressing and forming, placing the obtained primary ceramic biscuit in a vacuum bag, vacuumizing to be less than 1000Pa, placing the primary ceramic biscuit in a cold isostatic press, carrying out cold isostatic pressing for 120s under the pressure of 150MPa, placing the obtained secondary ceramic biscuit in a pressure furnace, heating to 450 ℃ at the speed of 4 ℃/min, preserving the heat for 2h for glue discharge, heating to 1700 ℃ at the speed of 6 ℃/min, preserving the heat for 1h, and cooling to obtain the silicon nitride ceramic dehydration element, wherein the longest dimension of the section of the obtained silicon nitride ceramic dehydration element is 20mm and the height is 40 mm.
Example 3
Putting 88 parts of silicon nitride powder (the median particle size is less than or equal to 0.9 mu m), 6 parts of alumina powder (the median particle size is less than or equal to 0.8 mu m), 2 parts of yttrium oxide powder (the median particle size is less than or equal to 0.8 mu m), 2 parts of titanium oxide powder (the median particle size is less than or equal to 0.5 mu m), 2 parts of polyethylene glycol and water in a stirring mill, taking a silicon nitride grinding ball as a grinding medium, and stirring and grinding for 20 hours at the rotating speed of 195rpm to obtain slurry with the solid content of 45%;
and (3) introducing the slurry into a pressure type spray granulation tower by using a feed pump for spray granulation, wherein the spray granulation conditions are as follows: the pressure of the feed pump was 900kPa, the cyclone pressure difference was 0.5kPa, the inlet temperature of the spray tower was 185 ℃ and the outlet temperature of the spray tower was 90 ℃ to obtain a mixed powder, the flow time of the obtained mixed powder was 63s, and the apparent density was 0.9g/cm3；
Introducing the mixed powder into a dry powder press, designing the longest dimension of the section of a primary ceramic biscuit to be 25mm and the height to be 50mm, keeping the pressure for 2s under the pressure of 5MPa for dry pressing and forming, placing the obtained primary ceramic biscuit in a vacuum bag, vacuumizing to be less than 1000Pa, placing the primary ceramic biscuit in a cold isostatic press, carrying out cold isostatic pressing for 120s under the pressure of 200MPa, placing the obtained secondary ceramic biscuit in a pressure furnace, heating to 450 ℃ at the speed of 4 ℃/min, preserving the heat for 2h for glue discharge, heating to 1700 ℃ at the speed of 6 ℃/min, preserving the heat for 1h, and cooling to obtain the silicon nitride ceramic dehydration element, wherein the longest dimension of the section of the obtained silicon nitride ceramic dehydration element is 20mm and the height is 40 mm.
Comparative example 1
Putting 89 parts of silicon nitride powder (the median particle size is less than or equal to 0.9 mu m), 4 parts of alumina powder (the median particle size is less than or equal to 0.8 mu m), 4 parts of yttrium oxide powder (the median particle size is less than or equal to 0.8 mu m), 1 part of titanium oxide powder (the median particle size is less than or equal to 0.5 mu m), 2 parts of polyethylene glycol and water into a stirring mill, and stirring and grinding for 15 hours at the rotating speed of 195rpm by taking a silicon nitride grinding ball as a grinding medium to obtain slurry with the solid content of 40%;
and (3) introducing the slurry into a pressure type spray granulation tower by using a feed pump for spray granulation, wherein the spray granulation conditions are as follows: the pressure of a feeding pump is 850kPa, the cyclone pressure difference is 0.5kPa, the inlet temperature of a spray tower is 180 ℃, and the outlet temperature of the spray tower is 90 ℃, so that the mixed powder is obtainedThe flow time of the obtained mixed powder is 62s, and the apparent density is 0.8g/cm3；
And introducing the mixed powder into a dry powder press, designing the section size of a primary ceramic biscuit to be 20mm and the height to be 50mm, keeping the pressure for 2s under the pressure of 3MPa for dry pressing and forming, placing the obtained primary ceramic biscuit in a pressure furnace, heating to 450 ℃ at the speed of 4 ℃/min, preserving the temperature for 2h for removing glue, heating to 1700 ℃ at the speed of 6 ℃/min, preserving the temperature for 2h, and cooling to obtain the silicon nitride ceramic dehydration element.
The silicon nitride ceramic dehydration components obtained in examples 1 to 3 and in the same ratio 1 were tested, and the test standards and test results are shown in table 1.
TABLE 1 test results of silicon nitride ceramic dehydration elements obtained in examples 1 to 3 and in equal proportion 1
As shown in Table 1, the bulk density of the silicon nitride ceramic dehydration element obtained by the preparation method provided by the invention is 3.21-3.25 g/cm3Higher bulk density; bending strength of 600-800 MPa, and fracture toughness of 6-7 MPa.m-1/2The material has higher mechanical property; the metallographic porosity rating is B02-B06, and the metallographic porosity is excellent. In addition, the preparation method provided by the invention reasonably controls the machining allowance, and the silicon nitride ceramic dehydration element obtained by dry pressing and matching with cold isostatic pressing is consistent with the design size, which shows that the preparation method provided by the invention can obviously improve the size precision of the silicon nitride ceramic dehydration element.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A preparation method of a silicon nitride ceramic dehydration element is characterized by comprising the following steps:
mixing silicon nitride powder, alumina powder, yttrium oxide powder, titanium oxide powder, polyethylene glycol and water to obtain slurry;
carrying out spray granulation on the slurry to obtain mixed powder;
sequentially carrying out dry pressing forming, cold isostatic pressing, binder removal and sintering on the mixed powder to obtain the silicon nitride ceramic dehydration element;
the mass ratio of the silicon nitride powder, the alumina powder, the yttrium oxide powder, the titanium oxide powder and the polyethylene glycol is (85-90): (4-8): (4-8): (0.5-2): (1-2);
the dry-pressing molding conditions include: the molding pressure is 2-5 MPa, and the pressure maintaining time is 1-10 s;
the conditions of the cold isostatic pressing include: the vacuum degree is less than or equal to 1000Pa, the pressure is 150-250 MPa, and the pressure maintaining time under the highest pressure is 50-400 s;
the sintering heat preservation temperature is 1700-1800 ℃, and the heat preservation time is 1-2 h.
2. The method according to claim 1, wherein the slurry has a solid content of 35 to 60%.
3. The method of claim 1, wherein the conditions of the spray granulation include: the pressure of the feeding pump is 800-1200 kPa, the pressure difference of the cyclone is 0.5-1 kPa, the inlet temperature of the spray tower is 180-200 ℃, and the outlet temperature of the spray tower is 90-100 ℃.
4. The silicon nitride ceramic dehydration component prepared by the preparation method of any one of claims 1 to 3, wherein the crystal form of silicon nitride in the silicon nitride ceramic dehydration component is beta phase;
the silicon nitride ceramic dehydration element contains a second phase of titanium nitride which is dispersed and distributed, and the size of the second phase of titanium nitride which is dispersed and distributed is less than or equal to 50 mu m.
5. The silicon nitride ceramic dewatering element according to claim 4, wherein the silicon nitride ceramic dewatering element has a bulk density of 3.2-3.3 g/cm3The Vickers hardness HV10 is 1380-1500, the bending strength is 600-1000 MPa, and the fracture toughness is 6-7 MPa.m-1/2And the metallurgical porosity rating is not lower than B06.
6. Use of a silicon nitride ceramic dewatering element according to claim 4 or 5 in a paper machine.
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