CN113511913B - Bionic fiber monolithic structure boron nitride high-temperature self-lubricating material and preparation method thereof - Google Patents
Bionic fiber monolithic structure boron nitride high-temperature self-lubricating material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a boron nitride high-temperature self-lubricating material with a bionic fiber monolithic structure, which takes cBN (cBN-based composite material added with ceramic bonding agent) as a fiber cell body and hBN with the same different phases (hBN-based composite material added with ceramic bonding agent) as an interface layer, wherein the cBN is taken as the fiber cell body and is arranged in an orientation way and is separated into independent units by the interface layer. The cBN cellule body plays a role in high bearing, and the strength of the material is improved; the lubricating phase of the hBN weak interface has a lubricating effect, and simultaneously, the toughness and service reliability of the material are improved through external toughening mechanisms such as crack deflection induction, local high stress digestion, crack tip load redistribution and the like.
Description
Technical Field
The invention relates to a monolithic boron nitride high-temperature self-lubricating material, in particular to a bionic fiber monolithic boron nitride high-temperature self-lubricating material, and belongs to the field of composite materials and self-lubricating materials.
Background
The hexagonal boron nitride (hBN) is a typical two-dimensional material, the special lamellar structure of the hexagonal boron nitride (hBN) endows the material with excellent self-lubricating property, and the high-temperature chemical inertia and high-temperature oxidation resistance of the hexagonal boron nitride (hBN) enable the service temperature of the hexagonal boron nitride (hBN) in the air to reach more than 1000 ℃, so the hexagonal boron nitride (hBN) is a very ideal high-temperature solid lubricant. Furthermore, hBN was light and soft in texture and had a density of only 2.27g/cm 3 Has good machinability, can be widely used for sliding parts and lubrication sealing parts of mechanical equipment, and has high heat conductivity coefficient which can meet the friction heat of the sliding parts during high-speed operationHeat dissipation requirements.
The high-temperature self-lubricating composite ceramic is prepared, the high-temperature self-lubricating performance of the material is realized by utilizing the slippage of the lamella between the hBN, and meanwhile, the ceramic matrix can promote the sintering performance of the hBN. In the prior art (Journal of the European Ceramic Society, 27 (2007) 1425-1430), AlN is taken as a matrix, hBN powder with different contents is introduced, and the AlN-hBN Ceramic composite material is prepared by sintering at 1800 ℃, the relative density and the mechanical property of the AlN-hBN Ceramic composite material are obviously reduced along with the increase of the introduced hBN content, and when the introduced hBN content reaches 20 vol%, the relative density and the strength of the composite material are only 86.2 percent and 120 MPa. Reported in the literature (Tribology International, 154 (2021) 106748) on ZrO 2 In the self-lubricating ceramic composite material, 30vol% of hBN serving as a high-temperature solid lubricant and 10 vol% of SiC powder serving as an auxiliary agent are introduced, and the friction coefficient under the dry friction condition within the range of room temperature to 900 ℃ is 0.45. Due to the intrinsic brittleness of the ceramic and the poor sintering property of hBN, the ceramic serves as a defect in a matrix, the continuity of the ceramic matrix is damaged, the bearing capacity of the material is influenced, the composite material presents a catastrophic fracture characteristic once being damaged, and the mechanical property, the service reliability and the stability of the composite material are severely limited. Therefore, the development of the composite ceramic material with excellent mechanical properties and high-temperature self-lubricating properties is urgently needed, and the unification of high reliability, high wear resistance and excellent self-lubricating properties is realized, so as to meet the requirements of mechanical equipment high-speed operation rotary sealing parts on lubrication, sealing and high service reliability.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a boron nitride high-temperature self-lubricating material with a bionic fiber monolithic structure and excellent service reliability and a preparation method thereof.
The invention relates to a preparation method of a bionic fiber monolithic structure boron nitride high-temperature self-lubricating material, which takes cBN as a fiber cell body and hBN of the same different phase as an interface layer, wherein the cBN as the fiber cell body is arranged in an orientation way and is separated into independent units by the interface layer. The cBN cellule body plays a role in high bearing, and the strength of the material is improved; the lubricating phase of the hBN weak interface has a lubricating effect, and simultaneously, the toughness and service reliability of the material are improved through external toughening mechanisms such as crack deflection induction, local high stress digestion, crack tip load redistribution and the like.
The cBN cellule is cBN base composite material, and Si can be introduced 3 N 4 、Al 2 O 3 、ZrO 2 、Y 2 O 3 And one or more of AlN and other ceramics are used as a bonding agent to reduce the sintering temperature in the preparation process and promote the compactness. The diameter of the cBN fibrocyte body is 400-800 mu m, and the size of cBN particles in the fibrocyte body is 5-10 mu m. The content of the adhesive is 30-60 wt%. As a preferred scheme, the formula of the cBN fibroid is as follows: 50wt% cBN + 22wt% Si 3 N 4 ＋10wt%Al 2 O 3 ＋4wt%Y 2 O 3 ＋14wt%AlN。
The hBN interface layer can also be made of hBN based composite material by adding ceramic phase such as SiO 2 、Si 3 N 4 、Al 2 O 3 And the like as an adhesive agent to improve the strength of itself and the bonding strength with the cellulosome. The hBN size in the hBN interface layer is 0.5-5 μm, and the thickness of the interface layer is 5-25 μm. The content of the adhesive is 2% -40%. As a preferred embodiment, the formulation of the hBN interfacial layer is 95 wt% hBN + 2.2wt% Si 3 N 4 ＋1.0wt%Al 2 O 3 ＋0.4wt%Y 2 O 3 ＋1.4wt%AlN。
The invention discloses a preparation method of a boron nitride high-temperature self-lubricating material with a bionic fiber monolithic structure, which comprises the following steps:
(1) cBN fibre cell precursor forming
The method comprises the steps of adding cBN powder and adhesive ceramic powder into a PVA (polyvinyl alcohol, the polymerization degree of 1750 +/-50 and used as an adhesive) aqueous solution (the mass concentration of the PVA aqueous solution is 1-2%, ball-milling and mixing are carried out uniformly to form ceramic mud (the mass percentage of the solid phase content of the mud is 30-50%), then forming a fiber cell precursor by the ceramic mud through an extrusion method, airing the extruded fiber cell precursor, and cutting the dried fiber cell precursor into a required length, wherein the diameter of the fiber cell precursor can be controlled within 400-800 mu m through the inner diameter of an extrusion opening.
The ceramic binder is Si 3 N 4 、Al 2 O 3 、ZrO 2 、Y 2 O 3 And one or more of ceramics such as AlN; the content of the adhesive is 30-60 wt%. As a preferred scheme, the formula of the cBN fibroid is as follows: 50wt% cBN + 22wt% Si 3 N 4 ＋10wt%Al 2 O 3 ＋4wt%Y 2 O 3 ＋14wt%AlN。
(2) Interfacial layer slurry preparation and coating
And (2) dispersing the hBN powder and the ceramic adhesive powder in ethanol, isopropanol or distilled water solution to form interface layer slurry with the concentration of 0.8-1.5 g/mL, coating the surface of the cBN cellule precursor with the interface layer slurry by a dipping or spraying method, and drying to form an interface separating layer. The thickness of the interface separation layer can be controlled to be 5-25 μm through the solid content of the interface layer slurry and the dipping times.
As a preferred embodiment, Al is used 2 O 3 When used as one of the interface layer adhesives, hydroxyl polyaluminum sol is used as Al 2 O 3 The precursor of (1). Mixing hBN powder with hydroxyl polymeric aluminum sol in corresponding proportion, ball-milling uniformly to form slurry with certain fluidity, and controlling the viscosity of the slurry and the Al in an interface layer by adjusting the concentration of the hydroxyl polymeric aluminum sol and the proportion of the hBN to the Al in the hydroxyl polymeric aluminum sol 2 O 3 Content of binder. The hydroxyl polymeric aluminum sol is dehydrated and decomposed in the sintering process, and finally reacts to form Al 2 O 3 . The concentration of Al in the hydroxyl polymeric aluminum sol is 2.5-3 mol/L. A certain amount of nano SiO can also be added during mixing 2 、SiO 2 、Si 3 N 4 The second phase binder thereby forms a multi-phase binder system that promotes densification of the interfacial layer.
(3) Forming a blank body: arranging the ceramic fiber cell bodies containing the interface separation layer in a steel mould according to one-dimensional orientation, pressurizing to 250-350 MPa for forming, and maintaining the pressure for 5-10 min; and demolding to obtain the ceramic body with the fiber monolithic structure.
(4) And (3) glue discharging and sintering: and (3) placing the fiber monolithic structure ceramic blank in a vacuum furnace, removing glue for 1-3 h at 200-500 ℃, sintering by adopting SPS (spark plasma sintering), cooling and demolding to obtain the bionic fiber monolithic structure boron nitride high-temperature self-lubricating material. And (3) SPS sintering process: the pressure is 25-40 MPa; the sintering temperature is 1500-1700 ℃, and the sintering time is 5-10 min.
The boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure prepared by the invention presents a typical external toughening mechanism and has a friction coefficient.
FIG. 1 is a photograph of a cross section of a boron nitride high-temperature self-lubricating material with a bionic fiber monolithic structure prepared by the method. Therefore, the cross section of the material presents a typical net structure, the fibrocyte body is wrapped by the interface layer, and the interface is uniformly distributed in the whole material to form a continuous interface lubricating phase, so that the sufficient supply of the interface lubricant in the friction process can be ensured.
Fig. 2 and 3 respectively show the crack resistance curve and the crack propagation path of the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure prepared by the invention. It can be seen from the figure that the resistance of the crack in the process of propagation is continuously increased (fig. 2), which is mainly benefited by the existence of external toughening mechanisms such as crack deflection, crack delamination and fiber extraction (fig. 3), and the external toughening mechanisms greatly counteract local high stress and dissipate fracture energy, thus achieving excellent toughening effect.
FIG. 4 is a high-temperature crack resistance curve of the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure at 1000 ℃. In the process of the material breaking at 1000 ℃, the resistance of the crack is continuously increased, and the material shows higher structural reliability, good damage resistance and obvious plastic fracture characteristics.
The tribology performance of a sample is tested by adopting a ball-disk type high-temperature frictional wear tester (HT-1000), the load is 5-10N, the frequency is 3-5 Hz, and the dual is Si 3 N 4 A ball or a peg. FIG. 5 is a high-temperature friction coefficient curve of the boron nitride high-temperature self-lubricating material with a bionic fiber monolithic structure at 1000 ℃. It can be seen that the material has a coefficient of friction of about 0.3 at 1000 c.
In summary, the present invention has the following advantages over the prior art:
1. different phases of the same material are adopted to respectively form a fibrocyte body and a cell interface layer, the bearing effect of the cBN fibrocyte body and the induction and high-temperature lubrication effect of the hBN weak interface layer on cracks are utilized, and simultaneously, the toughness and service reliability of the material are improved through external toughening mechanisms such as crack deflection induction, local high stress digestion, crack tip load redistribution and the like, the unification of mechanical property and high-temperature lubrication property is realized, and the problem of material defects caused by cubic boron nitride phase change in the sintering process is avoided;
2. by using the hydroxyl polymeric aluminum sol as a binder precursor, the problems of agglomeration or non-uniformity and difficult sintering of hBN in the traditional dry mixing or wet mixing can be avoided, and the densification of an hBN interface layer is promoted;
3. the compactness of the fiber cell body and the adhesive in the interface layer are regulated and controlled, so that the comprehensive performance of the material is regulated.
Drawings
FIG. 1 is a photograph of a cross section of a boron nitride high-temperature self-lubricating material with a bionic fiber monolithic structure prepared by the method.
FIG. 2 shows the crack resistance curve of the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure.
FIG. 3 shows the crack propagation path of the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure prepared by the invention.
FIG. 4 is a high-temperature crack resistance curve of the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure prepared by the invention.
FIG. 5 is a high-temperature friction coefficient curve of the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure prepared by the invention.
Detailed Description
Example 1
With addition of ZrO 2 (3Y) powder and alpha-Al 2 O 3 cBN powder of 5-10 μm in mass ratio of cBN: ZrO as raw material of celluloid body 2 (3Y):Al 2 O 3 =50:5: 45. Adding the cellucosome raw material powder into an absolute ethyl alcohol solution, ball-milling for 20 hours at the ball-milling speed of 150 r/min, drying the cellucosome raw material powder into powder in a drying oven at 70 ℃,sieving with 0.1 mm sieve; adding 2wt% of PVA adhesive into the prepared cBN cellulosome raw material powder, wherein the mass ratio of the solid phase of the adhesive to the powder is 1:32 to obtain fiber precursor slurry, and preparing the slurry into the cBN cellulosome by adopting an extrusion molding method, wherein the diameter of the cBN cellulosome is 0.6 mm;
taking hydroxyl polyaluminum sol as an interface additive precursor, and ball-milling and mixing the precursor with 1 mu m hBN powder for 10 hours to obtain uniform interface slurry, wherein the concentration of Al in the hydroxyl polyaluminum sol is 2.5mol/L, and the mass ratio of hBN to Al is 77: 1;
dipping the cBN fiber matrix into the interface slurry in a pulling and dipping mode, drying the interface slurry, and then performing dry pressing forming at 320 MPa in a single axial arrangement mode to prepare a blank body;
the high-temperature self-lubricating boron nitride ceramic material with the highly reliable bionic fiber monolithic structure is sintered by adopting a Spark Plasma Sintering (SPS) technology and preserving the heat for 10 min at 1500 ℃ and 30 MPa. Through detection, the strength of the material is about 200 MPa, and the crack propagation resistance is about 5-15 MPa.m 1/2 The coefficient of friction at 1000 ℃ is about 0.35.
Example 2
To add Si 3 N 4 Powder, AlN powder, alpha-Al 2 O 3 Powder and Y 2 O 3 cBN powder of 5-10 μm in mass ratio of cBN to Si as a binder as a raw material for a fibroblast 3 N 4 :AlN:Al 2 O 3 :Y 2 O 3 =50:22:14:10: 4. Adding the cellucosome raw material powder into an absolute ethyl alcohol solution, carrying out ball milling for 20 hours at the ball milling speed of 150 r/min, drying the mixture into powder in a drying oven at the temperature of 60 ℃ after finishing ball milling, and sieving the powder by using a 0.1 mm sieve. Adding 2wt% of PVA adhesive into the prepared cBN cellulosome raw material powder, wherein the mass ratio of the solid phase of the adhesive to the powder is 1:33, obtaining fiber precursor slurry, and preparing the slurry into the cBN cellulosome by adopting an extrusion molding method, wherein the diameter of the cBN cellulosome is 0.8 mm;
mixing Si 3 N 4 Powder, AlN powder, alpha-Al 2 O 3 Powder and Y 2 O 3 The powder is added into 3 μm hBN powder as adhesive, and the mass ratio of hBN to Si is 3 N 4 :AlN:Al 2 O 3 :Y 2 O 3 =95:2.2:1.4:1.0:0.4, and configured as interfacial slurry with a concentration of 0.1 g/mL;
dipping the cBN cellulosome into the interface slurry by adopting a pulling and dipping mode, drying the interface slurry, and then carrying out dry pressing forming under 300 MPa by adopting a single axial arrangement mode to prepare a blank;
the high-temperature self-lubricating boron nitride ceramic material with the highly reliable bionic fiber monolithic structure is sintered by adopting a Spark Plasma Sintering (SPS) technology at 1600 ℃ and 40 MPa for 10 min. The detection shows that the strength of the material is about 250 MPa, and the crack propagation resistance at room temperature is about 4.7-20 MPa.m 1/2 The friction coefficient at 1000 ℃ is about 0.35, and the friction coefficient is stable during the friction process.
Example 3
To add Si 3 N 4 Powder, AlN powder, alpha-Al 2 O 3 Powder and Y 2 O 3 cBN powder of 5-10 μm in mass ratio of cBN to Si as a binder as a raw material for a fibroblast 3 N 4 :AlN:Al 2 O 3 :Y 2 O 3 =50:22:14:10: 4; adding the cellucosome raw material powder into an absolute ethyl alcohol solution, carrying out ball milling for 20 hours at the ball milling speed of 200 r/min, drying the mixture into powder in a drying oven at 70 ℃ after finishing ball milling, and sieving the powder by using a 0.1 mm sieve; adding 2wt% of PVA adhesive into the prepared cBN cellulosome raw material powder, wherein the mass ratio of the solid phase of the adhesive to the powder is 1:32 to obtain fiber precursor slurry, and preparing the fiber cellulosome with the diameter of 0.6mm by adopting an extrusion molding method;
with 1 μm hBN powder as interface, SiC powder, alpha-Al 2 O 3 Powder and Y 2 O 3 The powder is interface adhesive, and the mass ratio of the powder is hBN to Si 3 N 4 : Al 2 O 3 :Y 2 O 3 Adding absolute ethyl alcohol to prepare interface slurry of 0.1 g/mL, wherein the ratio of the absolute ethyl alcohol to the interface slurry is not less than 66:25:5: 4;
dipping the cBN fibrocyte body with interface layer slurry in a pulling and dipping mode, drying the interface layer slurry, and then performing dry pressing forming under 250 MPa in a single axial arrangement mode to prepare a blank body;
the high-temperature self-lubricating boron nitride ceramic material with the highly reliable bionic fiber monolithic structure is sintered by adopting a Spark Plasma Sintering (SPS) technology at 1700 ℃ and 35 MPa for 8 min. The detection proves that the strength of the material is about 230MPa, and the crack propagation resistance at 1000 ℃ is about 5-16 MPa.m 1/2 The friction coefficient at 1000 ℃ is about 0.30, and the friction coefficient is stable during the friction process.
Claims (8)
1. A bionic fiber monolithic structure boron nitride high-temperature self-lubricating material is characterized in that cBN is used as a cellule body, hBN of the same phase and different phase is used as an interface layer, and the cBN cellule bodies are arranged in an oriented mode and are divided into independent units by the interface layer; the cBN fibrocyte body is cBN-based composite material with bonding agent introduced into cBN, wherein the bonding agent is Si 3 N 4 、Al 2 O 3 、ZrO 2 、Y 2 O 3 At least one of AlN, the content of the adhesive is 30-60 wt%; the hBN interface layer is an hBN-based composite material formed by adding a ceramic phase adhesive into hBN; the ceramic phase adhesive is SiO 2 、Si 3 N 4 、Al 2 O 3 At least one of; the content of the ceramic phase adhesive is 2% -40%.
2. The boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure as claimed in claim 1, wherein: the diameter of the cBN cellule body is 400-800 mu m, and the size of cBN particles in the cellule body is 5-10 mu m.
3. The boron nitride high-temperature self-lubricating material with a bionic fiber monolithic structure as claimed in claim 1, characterized in that: the thickness of the hBN interface layer is 5-25 mu m, and the hBN size in the hBN interface layer is 0.5-5 mu m.
4. The boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure as claimed in claim 1, wherein: the cBN fibrocyte body is: 50wt% cBN + 22wt% Si 3 N 4 ＋10wt%Al 2 O 3 ＋4wt%Y 2 O 3 ＋14wt%AlN。
5. The boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure as claimed in claim 1, wherein: the hBN interfacial layer is 95 wt% hBN + 2.2wt% Si 3 N 4 ＋1.0wt%Al 2 O 3 ＋0.4wt%Y 2 O 3 ＋1.4wt%AlN。
6. The preparation method of the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure as claimed in claim 1, comprises the following steps:
(1) and (3) forming a cBN fiber cell precursor: adding cBN powder and adhesive ceramic powder into a polyvinyl alcohol aqueous solution, performing ball milling and mixing uniformly to form ceramic pug, then forming a fibrocyte precursor by the ceramic pug through an extrusion method, and cutting the extruded fibrocyte precursor after drying in the air;
(2) preparing and coating interface layer slurry: dispersing the hBN powder and the ceramic adhesive powder in ethanol, isopropanol or distilled water solution to form interface layer slurry with the concentration of 0.8-1.5 g/mL, coating the surface of a cBN cellule precursor with the interface layer slurry by a dipping or spraying method, and drying to form an interface separating layer;
(3) forming a blank body: arranging the ceramic fibrocyte bodies containing the interface separation layer in a steel mould according to one-dimensional orientation, pressurizing to 250-350 MPa for forming, and maintaining the pressure for 5-10 min; demoulding to obtain a ceramic blank body with a fiber monolithic structure;
(4) glue discharging and sintering: and (3) placing the ceramic blank with the fiber monolithic structure in a vacuum furnace, discharging glue at 200-500 ℃ for 1-3 h, sintering by adopting discharge plasma, cooling and demolding to obtain the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure.
7. The method for preparing the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure according to claim 6, wherein the method comprises the following steps: in the step (1), the polymerization degree of the polyvinyl alcohol is 1750 +/-50, and the mass concentration of the polyvinyl alcohol in the aqueous solution is 1-2%; the solid phase content of the ceramic mud material is 30-50% by mass.
8. The method for preparing the boron nitride high-temperature self-lubricating material with the bionic fiber monolithic structure according to claim 6, wherein the method comprises the following steps: in the step (4), the spark plasma sintering process comprises the following steps: the pressure is 25-40 MPa; the sintering temperature is 1500-1700 ℃, and the sintering time is 5-10 min.
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