CN113149677B - Nickel wire toughened silicon nitride-based ceramic with wood-like ring structure and preparation method and application thereof - Google Patents
Nickel wire toughened silicon nitride-based ceramic with wood-like ring structure and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure and a preparation method and application thereof, wherein the nickel wire is arranged in the silicon nitride-based ceramic during sintering; the nickel wire is in a spiral spring structure. The method specifically comprises the following steps: step 1, taking 90wt% -91 wt% of Si according to mass proportion 3 N 4 Powder and 9-10 wt% of Al 2 O 3 And Y 2 O 3 Uniformly mixing the powder and drying to obtain composite powder; taking a nickel wire with a spiral spring structure, wherein the mass of the nickel wire is 5-10% of that of the composite powder; step 2, fixing the nickel wire with the spiral spring structure in a die, and adding the composite powder obtained in the step 1 for prepressing; and 3, sintering the pre-pressed composite powder and the nickel wire under the protection of nitrogen atmosphere, wherein the sintering temperature is 1700-1800 ℃, the pressure is 30-50 MPa, and the heat preservation and pressure maintaining time is 30-60 min, so as to obtain the wood-like annual ring structure nickel wire toughened silicon nitride ceramic composite material. The material performance of the silicon nitride-based ceramic is improved through the bionic structure design, and the silicon nitride-based ceramic is prevented from brittle fracture.
Description
Technical Field
The invention belongs to the technical field of structural ceramic materials, and particularly belongs to a preparation method of nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure.
Background
With the development of science and technology, the performance requirements of structural ceramic materials, such as bearing balls, cutters on machine tools and the like, are higher and higher due to the traction of functional requirements, and people hope that the structural ceramic materials have good mechanical properties and tribological properties. The silicon nitride ceramic has high hardness, high melting point, corrosion resistance and self-lubricating capacity, and is excellent in tribological performance, but the brittleness of the silicon nitride ceramic enables the silicon nitride simple substance material to be easily subjected to brittle fracture, and the mechanical performance of the silicon nitride ceramic is greatly reduced, so that the application of the silicon nitride ceramic is influenced.
In conclusion, the ceramic material in the prior art has the problems of low toughness, easy brittle fracture and narrow application range.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure, and a preparation method and application thereof, so as to solve the problem of high brittleness of a silicon nitride ceramic material.
In order to achieve the purpose, the invention provides the following technical scheme:
a nickel wire toughened silicon nitride-based ceramic with a wood-like annual ring structure is provided, wherein a nickel wire is arranged inside the silicon nitride-based ceramic during sintering; the nickel wire is in a spiral spring structure.
Preferably, the number of turns of the nickel wire of the spiral spring structure is not less than 4.
A preparation method of a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure comprises the following steps:
step 1, taking 90wt% -91 wt% of Si according to mass proportion 3 N 4 Powder and 9-10 wt% of Al 2 O 3 And Y 2 O 3 Uniformly mixing the powder and drying to obtain composite powder; taking a nickel wire with a spiral spring structure, wherein the mass of the nickel wire is 5-10% of that of the composite powder;
and 3, sintering the pre-pressed composite powder and the nickel wire under the protection of nitrogen atmosphere, wherein the sintering temperature is 1700-1800 ℃, the pressure is 30-50 MPa, and the heat preservation and pressure maintaining time is 30-60 min, so as to obtain the wood-like annual ring structure nickel wire toughened silicon nitride ceramic composite material.
Preferably, in step 1, weighed Si is added 3 N 4 Powder of Al 2 O 3 And Y 2 O 3 Placing the powder in a ball milling tank, adding zirconium dioxide balls and alcohol, performing ball milling and mixing by using a planetary ball mill to form mixed slurry, and drying the mixed slurry to obtain composite powder;
the mass ratio of the zirconium dioxide balls to the powder is 10:1, the mass of the alcohol is 1/2 of that of the powder; the ball milling speed is 150 r/min-250 r/min, the ball milling time is 300 min-600min, 10-15 cycles are carried out, each cycle is stopped for 5 min-9 min, and the ball milling is carried out alternately in the forward direction and the reverse direction.
Further, in the step 1, the mixed slurry is placed in a drying oven for heating and drying, and is stirred while being evaporated until the alcohol is evaporated, so that the composite powder is formed.
Preferably, in the step 1, metallographic abrasive paper is used for uniformly polishing the surface of the nickel wire, and then the nickel wire is prepared into a spiral spring structure, wherein the number of turns of the nickel wire of the spiral spring structure is not less than 4.
Preferably, in step 2, before the composite powder is added into a mold for prepressing, the composite powder is ground and sieved, and the mesh number of the screen is 80-160 meshes.
Preferably, in the step 2, the graphite mold is coated with the cubic boron nitride solution, graphite paper is put into the graphite mold, the nickel wire with the spiral spring structure is fixed on a base of the graphite mold, and then the composite powder is put into the graphite mold.
Preferably, said Si 3 N 4 The purity of the powder is 99.99 percent, and the alpha phase>94% average particle size 0.3 μm, al 2 O 3 And Y 2 O 3 Purity of powder>99.5 percent, the average grain diameter is 1 mu m, the purity of the nickel wire is 99.9 percent, and the diameter is 0.4mm.
The application of the silicon nitride-based ceramic toughened by the nickel wires in the wood-like annual ring structure is applied to the field of mechanical manufacturing, and particularly applied to machine tool cutting tools, aircraft vortex engines and bearing balls.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the wood-like annual ring structure nickel wire toughened silicon nitride-based ceramic, the nickel wire with the spiral spring structure is added during firing of the silicon nitride-based ceramic to form a wood-like annual ring structure so as to increase the toughness of the silicon nitride-based ceramic, the material performance of the silicon nitride-based ceramic is improved through the bionic structure design, the silicon nitride-based ceramic is prevented from being subjected to brittle fracture, the structure is simple, and the application range of the silicon nitride-based ceramic is widened. The nickel wire and the silicon nitride ceramic have good interface bonding property, and show good wettability, and the toughening effect of the wood-like annual ring structure on the silicon nitride ceramic is highlighted only by the good interface bonding property. Physical mechanics tests show that the structure can effectively improve the fracture toughness, the bending strength, the density and the hardness of the silicon nitride ceramic.
Furthermore, a multi-layer annual ring structure is formed by arranging not less than 4 layers of nickel wires in a spiral spring structure, so that the mechanical property of the silicon nitride ceramic is further enhanced.
The invention relates to a preparation method of nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure, which adopts Si 3 N 4 And reinforcing phase metal Ni wire as raw material to prepare Si of wood-like annual ring structure 3 N 4 a/Ni ceramic composite material made of Al 2 O 3 And Y 2 O 3 The powder is used as a sintering aid, and is subjected to hot-pressing sintering under the condition of heat preservation and pressure maintaining in a nitrogen atmosphere to obtain the Ni-toughened silicon nitride-based ceramic composite material with better mechanical property, the density and hardness of the Ni-toughened silicon nitride-based ceramic composite material are improved compared with those of a simple substance silicon nitride block material, and the metal nickel and the ceramic matrix are good in combination behavior.
Drawings
FIG. 1 is a schematic diagram of a wood-like tree-shaped nickel wire in example 1 of the present invention;
FIG. 2 is a diagram illustrating the bonding between the metal nickel and the silicon nitride ceramic substrate in example 1 of the present invention;
fig. 3 is a microstructure view of the combination of metallic nickel and silicon nitride crystal grains in example 1 of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention relates to a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure, which is based on the design idea of 'simple composition and complex structure', integrates the idea of 'improving the material performance by bionic structure design', obtains design inspiration from high-toughness wood in nature, deeply analyzes the influence of the wood structure composition on the self-generation thereof, analyzes and speculates that the ring layer composite structure of the ring in the wood is one of the main reasons for high toughness, and starts the development and application from the ring structure of the tree to the preparation of the composite material.
The invention adopts Si 3 N 4 And reinforcing phase metal Ni wire as raw material to prepare Si imitating the structure of wood annual ring 3 N 4 a/Ni ceramic composite material made of Al 2 O 3 And Y 2 O 3 The powder is used as sintering aid, firstly Si 3 N 4 The powder and the sintering aid are subjected to ball milling, crushing and uniform mixing, drying and sieving, then metal Ni wires subjected to surface roughening treatment are made into 4 circles of spiral spring structures with different diameters and uniform intervals according to a wood annual ring structure, the metal Ni wires and the wood annual ring structure are placed into a graphite die, and the graphite die is subjected to heat preservation, pressure preservation and hot pressing sintering to obtain a Ni-toughened silicon nitride-based ceramic composite material with better mechanical property, the density and hardness of the material are improved compared with those of a simple substance silicon nitride block, the combination behavior between metal nickel and a ceramic matrix is good, the combination between the metal nickel and the silicon nitride ceramic matrix is shown in figures 2 and 3, and as shown in figure 2, no obvious gap exists between silicon nitride and the metal nickel at an interface combination position, and no shrinkage cracking phenomenon caused by the difference of thermal expansion coefficients is generated; from fig. 3, it can be seen that silicon nitride crystal grains are grown in a staggered manner in metallic nickel, and exhibit good wettability, so that the combination of the two is good.
The nickel wire toughened silicon nitride-based ceramic with the wood-like ring structure can be applied to the fields of aerospace military industry, mechanical engineering, superfine grinding, automobiles, machining and manufacturing and the like, and can be particularly used as an airplane vortex engine, a bearing ball, a mechanical sealing ring, a valve, a grinding ball, a diesel engine glow plug, a high-performance machine tool cutting tool and the like.
Example 1
A preparation method of a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure comprises the following steps:
step S1, batching: weighing silicon nitride, aluminum oxide and yttrium oxide (the total mass is 36 g), wherein the mass percentages are as follows: yttrium oxide and aluminum oxide total 9wt%, silicon nitride: 91wt%; in addition, weighing 5% of metal nickel wires relative to the mass of the powder to prepare the wood-like ring structure; wherein the parameter of the weighed raw materials is Si 3 N 4 Purity 99.99%, alpha phase>94 percent and the average grain diameter is 0.3 mu m; al (Al) 2 O 3 And Y 2 O 3 Purity of>99.5 percent and the average grain diameter is 1 mu m; the purity of the nickel wire is 99.9 percent, and the diameter of the nickel wire is 0.4mm.
S2, ball milling and mixing: putting the weighed powder into a ball milling tank, adding zirconium dioxide balls, pouring alcohol, adjusting the viscosity of fluid, and fully and uniformly mixing by using a planetary ball mill, wherein the ratio of the mass of the added zirconium dioxide balls to the mass of the powder is 10:1, adding the alcohol amount to be 1/2 of the material weight, setting the ball milling speed to be 150r/min, the ball milling time to be 300min, performing 10 cycles, stopping each cycle for 5min, and performing forward and reverse interactive ball milling.
Step S3, drying: and (3) putting the mixed slurry obtained in the step (S2) into an oven for heating and drying, setting the drying temperature to be 50 ℃ and the drying time to be 40min, and stirring by using a glass rod while evaporating.
Step S4, sieving: grinding the mixture obtained in the step S3, and sieving the mixture by using a 80-mesh sieve to obtain composite powder;
and S5, uniformly polishing the surface of the nickel wire weighed in the step S1 by using 240-mesh metallographic abrasive paper, and manufacturing 4 circles of spiral spring-shaped structures with different diameters by using the nickel wire according to the wood annual ring structure, wherein the diameters from inside to outside are phi 10, phi 20, phi 30 and phi 40 respectively.
Step S6, charging: and (5) loading the composite powder obtained in the step (S4) and the nickel wire annual ring structure obtained in the step (S5) into a graphite die for prepressing, brushing cubic boron nitride solution in the die, placing graphite paper, and then loading the composite powder and the nickel wires into the graphite die, wherein the specific loading sequence is as follows: fixing the spiral nickel wire on a base of a mold, and filling the prepared mixed powder into the mold.
Step S7, hot-pressing sintering: sintering under the protection of nitrogen atmosphere, wherein the sintering temperature is 1700 ℃, the pressure is 30MPa, and the heat preservation and pressure maintaining time is 30min, so as to obtain the wood-like annual ring structure nickel wire toughened silicon nitride ceramic composite material.
The fracture toughness of the simple substance silicon nitride block material measured by the unilateral notched beam method is 6.25 MPa.m 1/2, and the same test method is used for measuring the Si prepared in the embodiment 1 of the invention 3 N 4 The fracture toughness of the/Ni ceramic composite material is 8.12 MPa.m 1/2, which shows that the preparation method can improve the fracture toughness of the silicon nitride ceramic. The density and porosity of the elemental silicon nitride block material are respectively 3.18 g-cm measured by an Archimedes method -3 0.84%, the same test method was used to test Si prepared in example 1 of the present invention 3 N 4 The density and porosity of the/Ni ceramic composite material are respectively 3.22 g-cm -3 And 0.431 percent, which shows that the preparation method leads the silicon nitride ceramic to be more compact. The bending strength of the simple substance silicon nitride ceramic is measured to be 812MPa by adopting a three-point bending method, and the Si prepared in the embodiment 1 of the invention is measured by using the same test method 3 N 4 The bending strength of the/Ni ceramic composite material is 989MPa, which shows that the bending strength of the silicon nitride ceramic is improved by the preparation method. The Vickers hardness of the elemental silicon nitride block material is measured to be 14.88GPa by adopting a Huayin HV-1000A microscopic Vickers hardness meter, and the Si prepared in the embodiment 1 of the invention is measured by the same testing method 3 N 4 The Vickers hardness of the/Ni ceramic composite material is 18.23GPa, which shows that the preparation method can improve the hardness of the silicon nitride ceramic. In addition, the process selects the metal Ni wire as the toughening phase material, so that the manufacturing cost is low, and the raw material cost is saved.
Example 2
A preparation method of a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure comprises the following steps:
step S1, batching: weighing silicon nitride, aluminum oxide and yttrium oxide (the total mass is 36 g), wherein the mass percentages are as follows: yttrium oxide and aluminum oxide total 9.2wt%, silicon nitride: 90.8wt%; in addition, weighing metal nickel wires accounting for 6 percent of the mass of the powder to prepare the wood-like ring structure; wherein the weighed raw material parameter is Si 3 N 4 Purity 99.99%, alpha phase>94 percent and the average grain diameter is 0.3 mu m; al (Al) 2 O 3 And Y 2 O 3 Purity of>99.5%, average grain size 1 μm; the purity of the nickel wire is 99.9 percent, and the diameter of the nickel wire is 0.4mm.
Step S2, ball milling and mixing: putting the weighed powder into a ball milling tank, adding zirconium dioxide balls, pouring alcohol, adjusting the viscosity of fluid, and fully and uniformly mixing by using a planetary ball mill, wherein the ratio of the mass of the added zirconium dioxide balls to the mass of the powder is 10:1, adding alcohol amount of 1/2 of the material weight, setting ball milling speed of 180r/min, ball milling time of 400min,12 cycles, stopping each cycle for 6min, and performing forward and reverse interactive ball milling.
Step S3, drying: and (3) putting the mixed slurry obtained in the step (S2) into an oven, heating and drying, setting the drying temperature to be 55 ℃, setting the drying time to be 45min, and stirring by using a glass rod while evaporating.
Step S4, sieving: grinding the mixture obtained in the step S3, and sieving the mixture by using a 100-mesh sieve to obtain composite powder;
and S5, uniformly polishing the surface of the nickel wire weighed in the step S1 by using 320-mesh metallographic abrasive paper, and manufacturing 4 circles of spiral spring-shaped structures with different diameters by using the nickel wire according to the wood annual ring structure, wherein the diameters from inside to outside are phi 10, phi 20, phi 30 and phi 40 respectively.
Step S6, charging: and (3) putting the composite powder obtained in the step (S4) and the nickel wire annual ring structure obtained in the step (S5) into a graphite die for prepressing, brushing a cubic boron nitride solution in the die, putting graphite paper, and then putting the composite powder and the nickel wire into the graphite die, wherein the specific filling sequence is as follows: fixing the spiral nickel wire on a base of a mould, and filling the prepared mixed powder into the mould.
Step S7, hot-pressing sintering: and sintering under the protection of nitrogen atmosphere, wherein the sintering temperature is 1720 ℃, the pressure is 35MPa, and the heat preservation and pressure maintaining time is 35min, so that the wood-like ring structure nickel wire toughened silicon nitride ceramic composite material is obtained.
Example 3
A preparation method of a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure comprises the following steps:
step S1, batching: weighing silicon nitride, aluminum oxide and yttrium oxide (the total mass is 36 g), wherein the mass percentages are as follows: yttrium oxide and aluminum oxide total 9.5wt%, silicon nitride: 90.5wt%; in addition, weighing metal nickel wires accounting for 8 percent of the mass of the powder to prepare the wood-like ring structure; wherein the weighed raw material parameter is Si 3 N 4 Purity 99.99%, alpha phase>94 percent and the average grain diameter is 0.3 mu m; al (Al) 2 O 3 And Y 2 O 3 Purity of>99.5%, average grain size 1 μm; the purity of the nickel wire is 99.9 percent, and the diameter of the nickel wire is 0.4mm.
Step S2, ball milling and mixing: putting the weighed powder into a ball milling tank, adding zirconium dioxide balls, pouring alcohol, adjusting the viscosity of fluid, and fully and uniformly mixing by using a planetary ball mill, wherein the ratio of the mass of the added zirconium dioxide balls to the mass of the powder is 10:1, adding alcohol amount of 1/2 of the material weight, setting ball milling speed at 200r/min, ball milling time at 450min, ball milling time at 13 cycles, stopping each cycle for 7min, and performing forward and reverse interactive ball milling.
Step S3, drying: and (3) putting the mixed slurry obtained in the step (S2) into an oven for heating and drying, setting the drying temperature to be 65 ℃ and the drying time to be 50min, and stirring by using a glass rod while evaporating.
Step S4, sieving: grinding the mixture obtained in the step S3, and sieving the mixture by using a 120-mesh sieve to obtain composite powder;
and S5, uniformly polishing the surface of the nickel wire weighed in the step S1 by using 400-mesh metallographic abrasive paper, and manufacturing 4 circles of spiral spring-shaped structures with different diameters by using the nickel wire according to the wood annual ring structure, wherein the diameters from inside to outside are phi 10, phi 20, phi 30 and phi 40 respectively.
Step S6, charging: and (5) putting the composite powder obtained in the step (S4) and the nickel wire annual ring structure obtained in the step (S5) into a graphite die for prepressing, brushing a cubic boron nitride solution in the die, putting graphite paper, and then putting the composite powder and the nickel wire into the graphite die, wherein the specific filling sequence is as follows: fixing the spiral nickel wire on a base of a mould, and filling the prepared mixed powder into the mould.
Step S7, hot-pressing sintering: sintering under the protection of nitrogen atmosphere, wherein the sintering temperature is 1750 ℃, the pressure is 40MPa, and the heat preservation and pressure maintaining time is 45min, so that the wood-like annual ring structure nickel wire toughened silicon nitride ceramic composite material is obtained.
Example 4
A preparation method of a nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure comprises the following steps:
step S1, batching: weighing silicon nitride, aluminum oxide and yttrium oxide (the total mass is 36 g), wherein the mass percentages are as follows: yttrium oxide and aluminum oxide total 9.7wt%, silicon nitride: 90.3wt%; in addition, weighing 9% of metal nickel wires relative to the mass of the powder to prepare the wood-like ring structure; wherein the parameter of the weighed raw materials is Si 3 N 4 Purity 99.99%, alpha phase>94 percent and the average grain diameter is 0.3 mu m; al (Al) 2 O 3 And Y 2 O 3 Purity of>99.5%, average grain size 1 μm; the purity of the nickel wire is 99.9 percent, and the diameter of the nickel wire is 0.4mm.
Step S2, ball milling and mixing: putting the weighed powder into a ball milling tank, adding zirconium dioxide balls, pouring alcohol, adjusting the viscosity of fluid, and fully and uniformly mixing by using a planetary ball mill, wherein the ratio of the mass of the added zirconium dioxide balls to the mass of the powder is 10:1, adding alcohol amount of 1/2 of the material weight, setting ball milling speed at 230r/min, ball milling time at 500min,14 cycles, stopping each cycle for 8min, and performing forward and reverse interactive ball milling.
Step S3, drying: and (3) putting the mixed slurry obtained in the step (S2) into an oven, heating and drying, setting the drying temperature to be 75 ℃, setting the drying time to be 55min, and stirring by using a glass rod while evaporating.
Step S4, sieving: grinding the mixture obtained in the step S3, and sieving the mixture by using a 140-mesh sieve to obtain composite powder;
and S5, uniformly polishing the surface of the nickel wire weighed in the step S1 by using 600-mesh metallographic abrasive paper, and manufacturing 4 circles of spiral spring-shaped structures with different diameters by using the nickel wire according to the wood annual ring structure, wherein the diameters from inside to outside are phi 10, phi 20, phi 30 and phi 40 respectively.
Step S6, charging: filling the composite powder obtained in the step S4 and the nickel wire annual ring structure obtained in the step S5 into a graphite die
And (2) medium prepressing, namely brushing cubic boron nitride solution in the mould, putting graphite paper, and then filling the composite powder and nickel wires into the graphite mould, wherein the specific filling sequence is as follows: fixing the spiral nickel wire on a base of a mould, and filling the prepared mixed powder into the mould.
Step S7, hot-pressing sintering: sintering under the protection of nitrogen atmosphere, wherein the sintering temperature is 1780 ℃, the pressure is 45MPa, and the heat preservation and pressure maintaining time is 55min, so as to obtain the wood-like annual ring structure nickel wire toughened silicon nitride ceramic composite material.
Example 5
A preparation method of nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure comprises the following steps:
step S1, batching: weighing silicon nitride, aluminum oxide and yttrium oxide (the total mass is 36 g), wherein the mass percentages are as follows: yttrium oxide and aluminum oxide, total 10wt%, silicon nitride: 90wt%; in addition, weighing 10% of metal nickel wires relative to the mass of the powder to prepare a wood-like ring structure; wherein the weighed raw material parameter is Si 3 N 4 Purity 99.99%, alpha phase>94 percent and the average grain diameter is 0.3 mu m; al (Al) 2 O 3 And Y 2 O 3 Purity of>99.5%, average grain size 1 μm; the purity of the nickel wire is 99.9 percent, and the diameter of the nickel wire is 0.4mm.
S2, ball milling and mixing: putting the weighed powder into a ball milling tank, adding zirconium dioxide balls, pouring alcohol, adjusting the viscosity of fluid, and fully and uniformly mixing by using a planetary ball mill, wherein the ratio of the mass of the added zirconium dioxide balls to the mass of the powder is 10:1, adding the alcohol amount to be 1/2 of the material weight, setting the ball milling speed to be 250r/min, the ball milling time to be 600min,15 cycles, stopping each cycle for 9min, and performing forward and reverse interactive ball milling.
Step S3, drying: and (3) putting the mixed slurry obtained in the step (S2) into an oven, heating and drying, setting the drying temperature to be 80 ℃, setting the drying time to be 60min, and stirring by using a glass rod while evaporating.
Step S4, sieving: grinding the mixture obtained in the step S3, and sieving the mixture by using a 160-mesh sieve to obtain composite powder;
and S5, uniformly polishing the surface of the nickel wire weighed in the step S1 by using 800-mesh metallographic abrasive paper, and manufacturing 4 circles of spiral spring-shaped structures with different diameters by using the nickel wire according to a wood annual ring structure, wherein the diameters of the spiral spring-shaped structures are phi 10, phi 20, phi 30 and phi 40 from inside to outside respectively.
Step S6, charging: and (5) putting the composite powder obtained in the step (S4) and the nickel wire annual ring structure obtained in the step (S5) into a graphite die for prepressing, brushing a cubic boron nitride solution in the die, putting graphite paper, and then putting the composite powder and the nickel wire into the graphite die, wherein the specific filling sequence is as follows: fixing the spiral nickel wire on a base of a mold, and filling the prepared mixed powder into the mold.
Step S7, hot-pressing sintering: sintering under the protection of nitrogen atmosphere, wherein the sintering temperature is 1800 ℃, the pressure is 50MPa, and the heat preservation and pressure maintaining time is 60min, so as to obtain the wood-like annual ring structure nickel wire toughened silicon nitride ceramic composite material.
Claims (4)
1. A preparation method of nickel wire toughened silicon nitride-based ceramic with a wood-like ring structure is characterized by comprising the following steps:
step 1, taking 90wt% -91 wt% of Si according to mass proportion 3 N 4 Powder and 9-10 wt% of Al 2 O 3 And Y 2 O 3 Uniformly mixing the powder and drying to obtain composite powder; taking a nickel wire with a spiral spring structure, wherein the mass of the nickel wire is 5-10% of that of the composite powder; firstly, uniformly polishing the surface of a nickel wire by using metallographic abrasive paper, and then manufacturing the nickel wire into 4 circles of spiral spring structures with different diameters and uniform intervals according to a wood annual ring structure;
weighing Si 3 N 4 Powder of Al 2 O 3 And Y 2 O 3 Placing the powder in a ball milling tank, adding zirconium dioxide balls and alcohol, performing ball milling and mixing by using a planetary ball mill to form mixed slurry, and drying the mixed slurry to obtain composite powder;
the mass ratio of the zirconium dioxide balls to the powder is 10:1, the mass of the alcohol is 1/2 of the mass of the powder; the ball milling speed is 150 r/min-250 r/min, the ball milling time is 300 min-600min, 10-15 cycles are carried out, each cycle is stopped for 5 min-9 min, and the ball milling is carried out alternately in the forward direction and the reverse direction; said Si 3 N 4 The purity of the powder is 99.99 percent and the alpha phase>94% average particle size 0.3 μm, al 2 O 3 And Y 2 O 3 Purity of powder>99.5 percent, the average grain diameter is 1 mu m, the purity of the nickel wire is 99.9 percent, and the diameter is 0.4mm;
step 2, fixing the nickel wire with the spiral spring structure in a die, and adding the composite powder obtained in the step 1 for prepressing;
and 3, sintering the pre-pressed composite powder and the nickel wire under the protection of nitrogen atmosphere, wherein the sintering temperature is 1700-1800 ℃, the pressure is 30-50 MPa, and the heat preservation and pressure maintaining time is 30-60 min, so as to obtain the wood-like annual ring structure nickel wire toughened silicon nitride ceramic composite material.
2. The method for preparing the wood-like ring structure nickel wire toughened silicon nitride-based ceramic according to claim 1, wherein in step 1, the mixed slurry is placed in an oven for heating and drying, and is stirred while being evaporated until the alcohol is evaporated, so as to form composite powder.
3. The method for preparing the wood-like ring structure nickel wire toughened silicon nitride-based ceramic according to claim 1, wherein in step 2, the composite powder is ground and sieved before being added into a mold for prepressing, and the mesh number of the screen is 80-160 meshes.
4. The method for preparing the nickel wire toughened silicon nitride-based ceramic in the wood-like ring structure according to claim 1, wherein in the step 2, a cubic boron nitride solution is coated in a graphite mold, graphite paper is put in the graphite mold, the nickel wire in the spiral spring structure is fixed on a base of the graphite mold, and then the composite powder is filled in the graphite mold.
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