CN109719299B - Iron-based oil-retaining bearing material with controllable pore structure and preparation method thereof - Google Patents

Iron-based oil-retaining bearing material with controllable pore structure and preparation method thereof Download PDF

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CN109719299B
CN109719299B CN201811516789.0A CN201811516789A CN109719299B CN 109719299 B CN109719299 B CN 109719299B CN 201811516789 A CN201811516789 A CN 201811516789A CN 109719299 B CN109719299 B CN 109719299B
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pore
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CN109719299A (en
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尹延国
李蓉蓉
张开源
张国涛
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Hefei University of Technology
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Abstract

The invention relates to an iron-based oil-retaining bearing material with a controllable pore structure and a preparation method thereof. Mixing hair with titanium hydride powder as a composite pore-forming agent, and placing the mixture into an iron matrix blank. In the friction and wear process of the bearing material, oil in the pores flows to the surface to form a lubricating oil film, so that friction is reduced, and meanwhile, C60 nanoparticles in the oil can fill microscopic grooves on the surface of a friction pair to reduce the roughness of the friction pair, so that the friction reduction effect is achieved. The invention adopts a ball milling process to mechanically alloy the composite pore-forming agent and the iron powder, so that the shape of the pore-forming agent is regular, and the shape of the pore-forming agent has geometric heredity to the shape of pores, so that the sizes of the generated pores are also regular and are uniformly distributed in the iron base. The green body is sintered in inert gas, titanium hydride is dehydrogenated at high temperature in the sintering process to form open pores in the iron matrix, and the hairline is decomposed at high temperature to form a large number of micron-sized bridge pore passages which penetrate through the open pores formed by the titanium hydride, so that the connectivity of the pores is improved.

Description

Iron-based oil-retaining bearing material with controllable pore structure and preparation method thereof
Technical Field
The invention belongs to the technical field of bearing materials, and particularly relates to an iron-based oil-retaining bearing material with a controllable pore structure and a preparation method thereof.
Background
With the development of modern aerospace and aviation industries, the tribology of aerospace machinery is rapidly developed, and the iron-based self-lubricating iron-based material with low friction coefficient has inherent superiority due to the simplified mechanical structure design, and becomes a hot point of research in the field of tribology, and is successfully applied to the miniature iron-based bearing used in the outer space. The pore volume in the bearing is about l 0% -40%, and the pore volume can be used for storing the fluid lubricant to supply oil under the self-running state, so that the lubricating condition is improved.
In the aspect of preparing the iron-based oil-retaining bearing, the pore-forming agents which are prepared by adding ammonium bicarbonate, urea, stearic acid and the like into raw material powder in advance are taken as matrixes, but the pore-forming agents are easily decomposed or gasified at a lower temperature and are difficult to control in production management, and formed pores are easily closed in a late long sintering process to form closed pores which are not communicated with the outside, so that the effective porosity cannot reach the standard, and the oil storage capacity of the material is reduced. Meanwhile, urea decomposition product HCNO which is corrosive to the iron base has influence on the iron base when being discharged through the iron base, thereby influencing the performance and application of the material.
Disclosure of Invention
The invention uses titanium hydride powder (TiH)2) The invention provides an iron-based oil-retaining bearing material with a controllable pore structure, and simultaneously provides a preparation method of the iron-based oil-retaining bearing material with the controllable pore structure.
An iron-based oil-retaining bearing material with a controllable pore structure is prepared by mixing 81.5-98.5% of iron powder, 1.05-3.5% of composite pore-forming material and 0.1-2.5% of graphite powder according to mass percentage; the composite pore-forming material is 1-3% of titanium hydride powder (TiH)2) And 0.05% -0.5% of hair;
mixing and ball-milling the materials, pressing into a green body, carrying out gas shielded sintering, and carrying out vacuum oil immersion to obtain the iron-based oil-containing bearing material with a controllable pore structure;
the oil-containing iron base of the iron-based oil-containing bearing material has the hardness of 59HRB, the oil content of 16.13 percent and the density of 6.379g/cm3The friction coefficient is 0.12, and the depth of the grinding mark is 0.016 mm.
The technical scheme for further limiting is as follows:
the titanium hydride powder (TiH)2) Titanium hydride powder (TiH) of 300 mesh2)。
The hair is 0.5-1.5 mm in length and 30-100 um in diameter.
The graphite powder is scaly 80-mesh graphite powder.
The operation steps for preparing the iron-based oil-retaining bearing material with the controllable pore structure are as follows:
(1) ball-milling powder: mixing titanium hydride powder (TiH)2) Adding the graphite powder, the hair, and the process control agent into a grinding tank for ball milling to obtain uniformly mixed powder;
(2) pressing a green blank: putting the powder into a pressing die, and preparing a green body under unidirectional pressure;
(3) and (3) protective gas sintering: putting the pressed blank into a mesh belt type sintering furnace, and introducing decomposed ammonia gas for protection;
(4) oil immersion in vacuum: placing the sintered material intoContaining nano C60And (4) carrying out vacuum oil immersion in oil liquid.
The technical scheme of the preparation method is further limited as follows:
in the step (1), when the powder is prepared by ball milling, the mass ratio of the milling balls to the mixed material to be milled is 10: 1-60: 1, the rotating speed is 100-400 r/min, and the ball milling time is 1-30 h.
In the step (1), the process control agent is one of ethanol, stearic acid and zinc stearate, and the mass of the process control agent is 0.5-1.5% of that of the mixed material to be ground.
In the step (2), the pressure of the pressed green body is 650-750 MPa.
In the step (3), the sintering conditions are as follows: the sintering temperature is 1050-1200 ℃, and the heat preservation time is 4 h.
In the step (4), the sintering material is completely immersed in the nano-C60In the oil, nano C60The content in the oil liquid is 0.25g/L, the oil immersion time is 3 hours, the vacuum pressure value is not more than 7KPa, and the oil temperature is 70-100 ℃.
Compared with the prior art, the beneficial technical effects of the invention are embodied in the following aspects:
1. titanium hydride powder (TiH) in contrast to ammonium bicarbonate2) The decomposition temperature is higher, the defect that partial pores are closed at a higher temperature after the traditional pore-forming agent is used for pore-forming is avoided, and the mechanical property of the material is improved due to the hard phase TiC generated after sintering.
2. The hair is abundant in source and easy to obtain. The hair of 0.5 mm-1.5 mm can not be easily deformed in the ball milling process. The bridge pore passage obtained after sintering can be connected with a plurality of pores in series, so that the connectivity of the pores in the material is improved, the aperture ratio is improved, and the oil storage performance of the material is enhanced. Compared with urea, the decomposition products after the hair is sintered have no corrosion effect on the iron matrix.
3. The invention is based on a powder metallurgy method, adopts a ball milling process to mechanically alloy the composite pore-forming agent and the iron powder, and ensures that the shape of the pore-forming agent is regular, and the shape of the pore-forming agent has geometric heredity to the shape of pores, so that the sizes of the generated pores are the same and regular, and the pores are uniformly distributed in the iron base. Sintering the green body in inert gasTitanium hydride (TiH)2) Dehydrogenating at high temperature to form open pores in the iron matrix, and decomposing the hair at high temperature to form a great amount of micron-sized bridge pores penetrating through titanium hydride (TiH)2) The connectivity of the pores is improved among the open pores, and the pores are uniformly distributed in the iron-based bearing material.
4. When oil is immersed in vacuum, C60 nano material is added into the oil. In the process of friction and wear of the material, the nano material in the pores can be separated out from oil to fill the microscopic grooves on the surface of the friction pair so as to reduce the roughness of the material, a lubricating oil film is formed on the surface, and the friction reduction effect is further achieved on the basis of oil lubrication.
Detailed Description
The technical solution of the present invention will be described in detail by examples.
Example 1
The operation steps for preparing the iron-based oil-retaining bearing material with the controllable pore structure are as follows:
step 1, weighing 116.58g (97.15%) of iron powder and titanium hydride powder (TiH) according to mass percentage2) 2.4g (2%), graphite powder 0.78g (0.65%), hair 0.24g (0.2%), 120g in total; 0.6g (0.5% of the total mass) of zinc stearate was added.
And 2, adding the mixed powder into a grinding tank for ball milling, wherein 250g of large balls and 350g of small balls are filled in the grinding tank, vacuumizing, filling high-purity argon, rotating at 300r/min, carrying out ball milling for 10 hours, stopping the ball milling machine for 15 minutes every 60 minutes, facilitating heat dissipation in the ball milling process, and naturally cooling for 5 hours after ball milling is finished to obtain uniformly mixed powder.
And 3, putting the powder into a pressing die, and preparing a green body under unidirectional pressure, wherein the pressure for pressing the green body is 650-750 MPa.
And 4, putting the pressed blank into a mesh belt type sintering furnace, introducing decomposed ammonia gas for protection, wherein the sintering temperature is 1050-1200 ℃, and the heat preservation time is 4 hours of sintering.
Step 5, putting the sintering material into the sintering furnace and doping the nano C60The oil liquid of the material is immersed in the oil in vacuum. Completely immersing the sintered material in the solution containing the nano-C60In the oil, nano C60The content of the C60 nano material in the oil liquid is 0.25g/L, the oil immersion time is 3 hours, the vacuum pressure value is not more than 7KPa, the oil temperature is 70-100 ℃, and the C60 nano material accounts for 0.25g/L in the oil liquid.
And 6, respectively carrying out mechanical property detection and frictional wear performance detection on the test sample under a dry friction working condition. The obtained oil-containing iron matrix has hardness of 59HRB, oil content of 16.13%, and density of 6.379g/cm3The friction coefficient is 0.10, and the depth of grinding mark is 0.013 mm.
Example 2
The operation steps for preparing the iron-based oil-retaining bearing material are as follows:
1. according to the mass percent, 116.58g (97.15 percent) of iron powder and titanium hydride powder (TiH) are weighed2) 2.4g (2%), graphite powder 0.78g (0.65%), hair 0.24g (0.2%), 120g in total; 0.6g of zinc stearate (0.5 percent of the total mass) is additionally added;
2. step 2 as in example 1;
3. same as example 1, step 3;
4. same as example 1, step 4;
5. and putting the sintering material into common oil liquid for vacuum oil immersion. The oil quantity is more than the quantity of the immersed sample, the oil immersion time is 3 hours, the vacuum pressure value is not more than 7KPa, and the oil temperature is 70-100 ℃;
6. and respectively carrying out mechanical property detection and frictional wear performance detection on the test sample under a dry friction working condition. The obtained oil-containing iron matrix has hardness of 59HRB, oil content of 16.13%, and density of 6.379g/cm3The friction coefficient is 0.12, and the depth of the grinding mark is 0.016 mm.
Example 3
The operation steps for preparing the iron-based oil-retaining bearing material are as follows:
1. according to the mass percent, 116.58g (97.15 percent) of iron powder and titanium hydride powder (TiH) are weighed2) 2.4g (2%), graphite powder 0.78g (0.65%), hair 0.24g (0.2%), 120g in total; 0.6g (0.5% of the total mass) of zinc stearate was added
2. And putting the powder into a pressing die, and preparing a green body under unidirectional pressure, wherein the pressure for pressing the green body is 650-750 MPa.
3. And (3) putting the pressed blank into a mesh belt type sintering furnace, introducing decomposed ammonia gas for protection, wherein the sintering temperature is 1050-1200 ℃, and the heat preservation time is 4 hours.
4. And putting the sintering material into common oil liquid for vacuum oil immersion. The oil amount is more than the immersed sample amount, the oil immersion time is 3 hours, the vacuum pressure value is not more than 7KPa, and the oil temperature is 70-100 ℃.
5. And respectively carrying out mechanical property detection and frictional wear performance detection on the test sample under a dry friction working condition. The Rockwell hardness of the test specimens was measured using an HBRVU-187.5 optical Brookfield hardness tester, and the coefficient of friction was measured on an HDM-10 type end face friction wear tester. The obtained oil-containing iron matrix has hardness of 63HRB, oil content of 14.31%, and density of 6.401g/cm3The friction coefficient is 0.15, and the depth of the grinding mark is 0.018 mm.
Example 4
The operation steps for preparing the iron-based oil-retaining bearing material are as follows:
1. according to the mass percent, 116.82g (97.35%) of iron powder and titanium hydride powder (TiH) are weighed2) 2.4g (2%), graphite powder 0.78g (0.65%), and 120g in total. 0.6g of zinc stearate (0.5 percent of the total mass) is additionally added;
2. step 2 as in example 3;
3. step 3 as in example 3;
4. step 4 as in example 3;
5. and respectively carrying out mechanical property detection and frictional wear performance detection on the test sample under a dry friction working condition. The obtained oil-containing iron matrix has hardness of 64HRB, oil content of 12.15%, and density of 6.401g/cm3The friction coefficient is 0.22, and the depth of grinding mark is 0.021 mm.
Example 5
The operation steps for preparing the iron-based oil-retaining bearing material are as follows:
1. weighing 119.22g (99.35%) of iron powder, 0.78g (0.65%) of graphite powder and 120g in total according to the mass percentage, and adding 0.6g (0.5% of total mass) of zinc stearate;
2. step 2 as in example 3;
3. step 3 as in example 3;
4. step 4 as in example 3;
5. and respectively carrying out mechanical property detection and frictional wear performance detection on the test sample under a dry friction working condition. The obtained oil-containing iron matrix has hardness of 46HRB, oil content of 11.56%, and density of 6.428g/cm3The friction coefficient is 0.27, and the depth of the grinding mark is 0.040 mm.
Table 1 is obtained by combining the comparative examples of the above examples
Figure DEST_PATH_IMAGE001
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (6)

1. An iron-based oil-retaining bearing material with a controllable pore structure is characterized in that: mixing 81.5-98.5% of iron powder, 1.05-3.5% of composite pore-forming material and 0.1-2.5% of graphite powder according to mass percentage; the composite pore-forming material is 1-3% of titanium hydride powder (TiH)2) And 0.05% -0.5% of hair; mixing and ball-milling the materials, pressing into a green body, carrying out gas shielded sintering, and carrying out vacuum oil immersion to obtain the iron-based oil-containing bearing material with a controllable pore structure;
the titanium hydride powder (TiH)2) Titanium hydride powder (TiH) of 300 mesh2);
The hair is 0.5-1.5 mm in length and 30-100 microns in diameter;
the graphite powder is scaly 80-mesh graphite powder;
the oil-containing iron base of the iron-based oil-containing bearing material has the hardness of 59HRB, the oil content of 16.13 percent and the density of 6.379g/cm3The friction coefficient is 0.11, and the depth of the grinding mark is 0.013 mm;
the iron-based oil-retaining bearing material is prepared by the following specific preparation operation steps:
(1) ball-milling powder: mix TiH2Adding the powder, graphite powder, hair, and process control agent into a grinding tank, and ball-milling to obtain uniformly mixed powder;
(2) pressing a green blank: putting the powder into a pressing die, and preparing a green body under unidirectional pressure;
(3) and (3) protective gas sintering: putting the pressed blank into a mesh belt type sintering furnace, and introducing decomposed ammonia gas for protection;
(4) oil immersion in vacuum: placing the sintered material into a container containing nano C60And (4) carrying out vacuum oil immersion in oil liquid.
2. The pore structure controllable iron-based oil-impregnated bearing material according to claim 1, wherein: in the step (1), when the powder is prepared by ball milling, the mass ratio of the milling balls to the mixed material to be milled is 10: 1-60: 1, the rotating speed is 100-400 r/min, and the ball milling time is 1-30 h.
3. The pore structure controllable iron-based oil-impregnated bearing material according to claim 1, wherein: in the step (1), the process control agent is one of ethanol and zinc stearate, and the mass of the process control agent is 0.5-1.5% of that of the mixed material to be ground.
4. The pore structure controllable iron-based oil-impregnated bearing material according to claim 1, wherein: in the step (2), the pressure of the pressed green body is 650-750 MPa.
5. The pore structure controllable iron-based oil-impregnated bearing material according to claim 1, wherein: in the step (3), the sintering conditions are as follows: the sintering temperature is 1050-1200 ℃, and the heat preservation time is 4 h.
6. The pore structure controllable iron-based oil-impregnated bearing material according to claim 1, wherein: in the step (4), the sintering material is completely immersed in the nano-C60In the oil, nano C60The content in the oil liquid is 0.25g/L, the oil immersion time is 3 hours, the vacuum pressure value is not more than 7KPa, and the oil temperature is 70-100 ℃.
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