CN115896575A - Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material and preparation method thereof - Google Patents
Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material and a preparation method thereof, wherein the material is prepared by mixing and sintering Mo, si, B and Ag powder, the prepared material takes Mo-12Si-8.5B as a matrix, and Ag exists in a simple substance form. According to the invention, the high-temperature alloy Mo-12Si-8.5B is taken as a matrix, and the simple substance Ag is added, so that the wide-temperature-range self-lubricating property of the Mo-12Si-8.5B alloy from normal temperature to high temperature is effectively improved, and the continuous self-lubricating of the Mo-12Si-8.5B-Ag in service under the variable-temperature working condition is realized.
Description
Technical Field
The invention relates to the technical field of alloys, in particular to a Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material and a preparation method thereof.
Background
With the rapid development of modern industry and high and new technology, the service environment of moving mechanical parts is increasingly harsh, the service temperature of hot-end mechanical parts used for aerospace engines, gas turbines, automobile engines and the like is higher and higher, and a plurality of mechanical moving parts must endow friction pairs with continuous and stable wear-resistant lubricating functions in a wide temperature range. Therefore, the problems of lubrication and wear resistance of mechanical moving parts under the working condition of wide temperature range are the key to influence the reliability and service life of a mechanical system, the problems of long-acting lubrication, wear resistance, high-temperature protection and the like are increasingly prominent, and the development of a high-performance material with low friction, wear resistance and wear resistance under the working condition from normal temperature to high temperature is urgently needed.
At present, although the developed high-temperature alloy has a certain wide-temperature-range self-lubricating effect, the developed high-temperature alloy still has some defects: some alloys can generate lubricating films with self-lubricating performance at high temperature, and have certain antifriction and wear-resistant effects at high temperature, but the lubricating substances cannot be generated in low-temperature service, so that the alloys cannot have the self-lubricating function at low temperature, and the alloys are worn greatly in low-temperature service, and premature failure of the alloys is caused.
The phase composition of the high-temperature alloy Mo-12Si-8.5B is Mo ss +Mo 3 Si+Mo 5 SiB 2 (Mo ss Is a solid solution of Si and B in Mo), in the alloy, mo ss The intermetallic compound Mo provides better fracture toughness for the phase 3 Si and Mo 5 SiB 2 Provides good oxidation resistance and excellent mechanical property for the composite material. Therefore, the Mo-12Si-8.5B high-temperature alloy has better room-temperature fracture toughness, excellent high-temperature strength, high-temperature creep resistance and high-temperature oxidation resistance, the service temperature can exceed 1250 ℃, and the Mo-12Si-8.5B high-temperature alloy is considered to be one of candidate materials which are expected to replace nickel-based alloy and become next-generation high-temperature alloy. Mo-12Si-8.5B can form MoO having a lubricating function at a high temperature 3 、SiO 2 And B 2 O 3 And the like. It can be seen that the binder phase (Moss) and the reinforcing phase (Mo) are combined 3 Si，Mo 5 SiB 2 ) And autogenous lubricating phase (MoO) 3 ，SiO 2 ，B 2 O 3 ) The Mo-12Si-8.5B alloy is expected to be used as a novel high-temperature self-lubricating wear-resistant material. However, the research shows that Mo-12Si-8.5B is difficult to form a self-lubricating antifriction and wear-resistant layer below 600 ℃. Thus, the deviceOnly Mo-12Si-8.5B is used for oxidizing the self-generated lubricating phase, so that the Mo-12Si-8.5B is difficult to ensure the whole process of antifriction and wear resistance from normal temperature to high temperature.
Therefore, it is very important to develop an alloy having a self-lubricating function in a wide temperature range.
Disclosure of Invention
The invention aims to provide a Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material and a preparation method thereof, wherein a high-temperature alloy Mo-12Si-8.5B is used as a matrix, a simple substance Ag is added, the wide-temperature-range self-lubricating property of the Mo-12Si-8.5B alloy from normal temperature to high temperature is effectively improved, and the continuous self-lubricating of the Mo-12Si-8.5B-Ag in service under the variable-temperature working condition is realized.
The invention discloses a Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material which is prepared by mixing and sintering Mo, si, B and Ag powder, wherein the prepared material takes Mo-12Si-8.5B as a matrix, and Ag exists in a simple substance form.
Preferably, mo: si: the mass ratio of B is 94:4:1, the mass fraction of Ag is more than 0 and less than or equal to 15 percent. The mass fraction of Ag added is more preferably 5%, 10%, 15%.
Preferably, in an environment with oxygen of more than 600 ℃, ag and Mo in the surface layer of Mo-12Si-8.5B are oxidized to generate Ag with a self-lubricating effect 2 MoO 4 And Ag 2 Mo 4 O 11 。
The invention also discloses a preparation method of the Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material, which comprises the following steps:
the method comprises the following steps: powder preparation: taking Mo, si, B and Ag powder as raw materials, putting the four kinds of powder into a ball milling tank in inert protective atmosphere, and performing high-energy ball milling by adopting a ball mill to uniformly mix the four kinds of powder;
step two: sintering preparation: and (2) putting the mixed powder into a graphite die, sintering by a two-step method by adopting a plasma discharge sintering technology (SPS), firstly sintering at 900 ℃, then heating to 1400 ℃, sintering, and finally cooling along with a furnace.
Preferably, the inert protective gas is argon.
Preferably, the ball mill adopts an all-directional planetary ball mill, the ball-material ratio is 10-20, the ball milling time is 10-40 h, and the ball milling speed is 300-500 r/min.
Preferably, the plasma discharge sintering is performed in a vacuum of 10 degrees of vacuum -2 Pa, the heating rate is 150 ℃/min when sintering at 900 ℃, the pressure is 40-60 MPa, the heat preservation time is 5-10 min, the heating rate is 150 ℃/min when sintering at 1400 ℃, the pressure is 30-45 MPa, and the heat preservation time is 5-10 min.
The invention has the beneficial effects that:
1. the invention prepares the material which takes Mo-12Si-8.5B as a matrix and Ag exists in a simple substance form by mixing and sintering Mo, si, B and Ag powder, wherein the simple substance Ag is a solid lubricant within the range of normal temperature (25 ℃) to 600 ℃ on one hand, and on the other hand, mo and Ag in the surface layer of the Mo-12Si-8.5B are oxidized in the air to generate Ag in the friction process of an environment with oxygen of more than 600 ℃ on the other hand 2 MoO 4 And Ag 2 Mo 4 O 11 Oxide film, and MoO formed on alloy surface 3 、SiO 2 And B 2 O 3 The composite oxide films have excellent self-lubricating effect at the temperature of more than 600 ℃ and also have good anti-oxidation effect, so that the whole process of self-lubricating of the alloy from room temperature to high temperature is realized.
2. The Mo-12Si-8.5B-Ag prepared by the invention has excellent wide-temperature-range self-lubricating antifriction and wear-resistant properties on the premise of ensuring that the Mo-12Si-8.5B alloy has excellent high-temperature strength, oxidation resistance and corrosion resistance, widens the application field of Mo-12Si-8.5B alloy materials, and has very important significance for ensuring long-term safe and stable operation of mechanical equipment and parts thereof.
3. The Mo-12Si-8.5B-Ag prepared by the method can be used as a block alloy material, and can also be used for constructing self-lubricating antifriction and wear-resistant coatings on the surfaces of other moving parts, so that the equipment parts can be ensured to have excellent mechanical strength, and the moving parts can be endowed with excellent self-lubricating wear-resistant performance.
Drawings
FIG. 1 is a flow chart of the preparation of the Mo-12Si-8.5B-Ag alloy of the invention.
FIG. 2 shows the friction coefficients at 25 ℃ and 600 ℃ for Mo-12Si-8.5B-Ag alloys with different Ag contents.
FIG. 3 is a graph showing the change of the friction coefficient with time at 25 ℃ and 600 ℃ of the Mo-12Si-8.5B alloy in comparative example 1.
FIG. 4 is a graph showing the change with time of friction coefficients at 25 ℃ and 600 ℃ of Mo-12Si-8.5B-5wt% Ag alloy in example 1.
FIG. 5 is a graph showing the time-dependent change of friction coefficients at 25 ℃ and 600 ℃ of Mo-12Si-8.5B-10wt% Ag alloy in example 2.
FIG. 6 is a graph showing the change with time in friction coefficients at 25 ℃ and 600 ℃ of Mo-12Si-8.5B-15wt% Ag alloy in example 3.
FIG. 7 is an XRD diffraction pattern of Mo-12Si-8.5B-10wt% Ag in example 2 after SPS sintering.
FIG. 8 is an XRD diffraction pattern of Mo-12Si-8.5B-10wt% Ag in example 2 after oxidation at 600 ℃.
FIG. 9 is an SEM morphology of the surface of Mo-12Si-8.5B in comparative example 1 after oxidation at 600 ℃.
FIG. 10 is an SEM morphology of the surface of Mo-12Si-8.5B-10wt% Ag after oxidation at 600 ℃ in example 2.
Detailed Description
The present invention will be further described with reference to the structures or terms used herein. The description is given for the sake of example only, and is not intended to limit the invention in any way.
Comparative example 1
The comparative example is the preparation of Mo-12Si-8.5B material, no simple substance Ag is added into Mo-12Si-8.5B, and the preparation method is as follows:
the method comprises the following steps: preparing powder: taking Mo: si: b is 94:4:1, preparing Mo-12Si-8.5B powder, wherein the total mass of the powder is 35g, then putting the powder into a ball milling tank, weighing steel balls according to the ball material ratio of 15: the ball milling time is 30h, and the ball milling rotating speed is 300r/min, so that the materials are uniformly mixed.
Step two: taking powder: and (3) sticking the powder obtained in the step one on the grinding ball and the wall of the tank, adding a proper amount of alcohol into the ball milling tank, carrying out ball milling on the ball milling tank again for 10min, then putting the ball milling tank into a drying box, drying for 10h at the temperature of 120 ℃, and filtering the dried powder by using a 400-mesh sieve to obtain the finished product powder.
Step three: sintering of Mo-12Si-8.5B powder: putting the powder obtained in the step two into a graphite die, and sintering in a plasma discharge sintering furnace, wherein the sintering process comprises the following steps: the plasma discharge sintering is carried out in vacuum with a vacuum degree of 10 -2 Pa, the sintering temperature is 1400 ℃, the sintering pressure is 45MPa, the heat preservation time is 6min, and finally, the sample is obtained after furnace cooling.
The performance was tested as follows:
the Mo-12Si-8.5B sample prepared in comparative example 1 was polished to a mirror surface state, and the sample was set in a pin-and-disk type frictional wear tester and tested with Al in an environment of room temperature (25 ℃ C.) and 600 ℃ C 2 O 3 Coefficient of friction and wear rate for the mill. FIG. 3 shows the curves of the change of the friction coefficient of the Mo-12Si-8.5B alloy at 25 ℃ and 600 ℃ along with time, and the graphs show that the friction coefficient at 25 ℃ is 0.59 and the friction coefficient at 600 ℃ is 0.38, which shows that the Mo-12Si-8.5B alloy has different self-lubricating properties at different temperatures, and the friction coefficient at 25 ℃ is larger and the self-lubricating property is poorer.
FIG. 9 is an SEM image of the surface of the Mo-12Si-8.5B alloy after oxidation at 600 deg.C, from which it can be seen that the Mo-12Si-8.5B comparative sample has only SiO generated on the surface 2 -B 2 O 3 And MoO 3 。
FIG. 1 is a flow chart of the preparation of Mo-12Si-8.5B-Ag wide temperature range lubricating materials of examples 1-3.
Example 1
A preparation method of a Mo-12Si-8.5B-Ag wide-temperature-range lubricating material comprises the following specific steps:
the method comprises the following steps: preparing powder: taking Mo: si: b is 94:4:1, preparing Mo-12Si-8.5B powder with the total mass of 33.25g, then adding 1.75g of Ag powder with the total mass of 35g, then placing the powder into a ball milling tank, weighing steel balls according to the ball material ratio of 15: the ball milling time is 30h, and the ball milling rotating speed is 300r/min, so that the materials are uniformly mixed.
Step two: taking powder: and (3) sticking the powder obtained in the step one on the grinding ball and the wall of the tank, adding a proper amount of alcohol into the ball milling tank, carrying out ball milling on the ball milling tank again for 10min, then putting the ball milling tank into a drying box, drying for 10h at the temperature of 120 ℃, and filtering the dried powder by using a 400-mesh sieve to obtain the finished product powder.
Step three: mo-12Si-8.5B-5wt% sintering of Ag powder: putting the powder obtained in the step two into a graphite die, and sintering in a plasma discharge sintering furnace, wherein the sintering process comprises the following steps: the plasma discharge sintering is carried out in vacuum with a vacuum degree of 10 - 2 Pa, the heating rate is 150 ℃/min when sintering at 900 ℃, the pressure is 45MPa, the heat preservation time is 6min, then the heating rate is 150 ℃/min when sintering at 1400 ℃, the pressure is 45MPa, the heat preservation time is 6min, and finally the sample is obtained after furnace cooling.
The performance test was as follows:
mo-12Si-8.5B-5wt% Ag sample prepared in example 1 was polished to a mirror surface state, the sample was set in a pin-and-disk type frictional wear tester, and it was tested with Al at ordinary temperature and 600 ℃ environment 2 O 3 Coefficient of friction and wear rate for the mill. FIG. 4 shows the curves of the friction coefficients of Mo-12Si-8.5B-5wt% Ag alloy at 25 ℃ and 600 ℃ as a function of time, and it can be seen that the friction coefficient at 25 ℃ is 0.29 and the friction coefficient at 600 ℃ is 0.30, indicating that the self-lubricating properties of the Mo-12Si-8.5B-5wt% Ag alloy at different temperatures are not significantly different, and the friction coefficients at 25 ℃ and 600 ℃ are smaller and the self-lubricating properties are better.
Example 2
A preparation method of a Mo-12Si-8.5B-Ag wide-temperature-range lubricating material comprises the following specific steps:
the method comprises the following steps: preparing powder: and the ratio of Mo: si: b is 94:4:1, preparing Mo-12Si-8.5B powder with the total mass of 31.5g, then adding 3.5g of Ag powder with the total mass of 35g, then placing the powder into a ball milling tank, weighing steel balls according to a ball material ratio of 15: the ball milling time is 30h, and the ball milling rotating speed is 300r/min, so that the materials are uniformly mixed.
Step two: taking powder: and (3) sticking the powder obtained in the step one on the grinding ball and the wall of the tank, adding a proper amount of alcohol into the ball milling tank, carrying out ball milling on the ball milling tank again for 10min, then putting the ball milling tank into a drying box, drying for 10h at the temperature of 120 ℃, and filtering the dried powder by using a 400-mesh sieve to obtain the finished product powder.
Step three: mo-12Si-8.5B-10wt% sintering of Ag powder: putting the powder obtained in the step two into a graphite die, and sintering in a plasma discharge sintering furnace, wherein the sintering process comprises the following steps: the plasma discharge sintering is carried out in vacuum with a vacuum degree of 10 -2 Pa, the heating rate is 150 ℃/min when sintering at 900 ℃, the pressure is 45MPa, the heat preservation time is 6min, then the heating rate is 150 ℃/min when sintering at 1400 ℃, the pressure is 45MPa, the heat preservation time is 6min, and finally furnace cooling is carried out to obtain the sample.
The performance test was as follows:
mo-12Si-8.5B-10wt% Ag specimen prepared in example 2 was polished to a mirror surface state, the specimen was set in a pin-and-disk type frictional wear tester, and it was tested with Al in an environment of room temperature and 600 deg.C 2 O 3 Coefficient of friction and wear rate for the mill. FIG. 5 shows the time-dependent change of the friction coefficients at 25 ℃ and 600 ℃ of the Mo-12Si-8.5B-10wt% Ag alloy, from which it can be seen that the friction coefficient at 25 ℃ is 0.30 and the friction coefficient at 600 ℃ is 0.31, indicating that the difference in the self-lubricating properties at different temperatures is not significant between the Mo-12Si-8.5B-10wt% Ag alloy, and that the friction coefficients at 25 ℃ and 600 ℃ are small and the self-lubricating properties are good.
FIG. 7 is an XRD diffraction pattern of Mo-12Si-8.5B-10wt% Ag after SPS sintering, and the results show that Mo-12Si-8.5B-10wt% Ag exists in the form of simple substance. FIG. 8 is an XRD diffraction pattern of Mo-12Si-8.5B-10wt% after oxidation of Ag at 600 ℃ showing that Mo-12Si-8.5B-10wt% generates Ag on the surface 2 MoO 4 、Ag 2 Mo 4 O 11 、MoO 3 、SiO 2 、B 2 O 3 A series of oxides. FIG. 10 shows Mo-12Si-8.5B-10wSEM morphology of surface after oxidation of t% Ag at 600 deg.C, results showed that Mo-12Si-8.5B-10wt% of Ag surface oxidation produced a silico-boron glass phase with self-lubricating function, ag 2 MoO 4 、Ag 2 Mo 4 O 11 。
Example 3
A preparation method of a Mo-12Si-8.5B-Ag wide-temperature-range lubricating material comprises the following specific steps:
the method comprises the following steps: preparing powder: taking Mo: si: b is 94:4:1, preparing Mo-12Si-8.5B powder with the total mass of 29.75g, then adding 5.25g of Ag powder with the total mass of 35g, then placing the powder into a ball milling tank, weighing steel balls according to the ball material ratio of 15: the ball milling time is 30h, and the ball milling rotating speed is 300r/min, so that the materials are uniformly mixed.
Step two: taking powder: and (3) sticking the powder obtained in the step one on the grinding ball and the wall of the tank, adding a proper amount of alcohol into the ball milling tank, carrying out ball milling on the ball milling tank again for 10min, then putting the ball milling tank into a drying box, drying for 10h at the temperature of 120 ℃, and filtering the dried powder by using a 400-mesh sieve to obtain the finished product powder.
Step three: mo-12Si-8.5B-15wt% sintering of Ag powder: putting the powder obtained in the step two into a graphite die, and sintering in a plasma discharge sintering furnace, wherein the sintering process comprises the following steps: plasma discharge sintering was carried out in vacuum at a vacuum of 10 deg.C -2 Pa, sintering at 900 ℃ with the heating rate of 150 ℃/min, the pressure of 45MPa and the heat preservation time of 6min; and then sintering at 1400 ℃, wherein the heating rate is 150 ℃/min, the pressure is 45MPa, the heat preservation time is 6min, and finally, furnace cooling is carried out to obtain the sample.
The performance was tested as follows:
mo-12Si-8.5B-15wt% Ag sample prepared in example 3 was ground to a mirror surface state, the sample was set in a pin-and-disc frictional wear tester, and it was tested with Al at ordinary temperature and 600 ℃ environment 2 O 3 Coefficient of friction and wear rate to the mill. FIG. 6 shows the friction coefficient versus time curves for Mo-12Si-8.5B-15wt% Ag alloy at 25 ℃ and 600 ℃As can be seen from the figure, the coefficient of friction at 25 ℃ was 0.28 and the coefficient of friction at 600 ℃ was 0.32, indicating that the difference in self-lubricating properties between Mo-12Si-8.5B-15wt% Ag alloy at different temperatures was not significant, and that the coefficients of friction at 25 ℃ and 600 ℃ were small and the self-lubricating properties were good.
FIG. 2 shows the friction coefficients of the alloys of comparative example 1 and examples 1-3 at 25 ℃ and 600 ℃, and FIG. 2 intuitively illustrates that the Mo-12Si-8.5B-Ag alloy has good self-lubricating effect from normal temperature to high temperature and has excellent wide-temperature-range self-lubricating antifriction and wear-resistant properties.
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 amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (7)
1. A Mo-12Si-8.5B-Ag wide temperature range self-lubricating material is characterized in that: the material is prepared by mixing and sintering Mo, si, B and Ag powder, the prepared material takes Mo-12Si-8.5B as a matrix, and Ag exists in a simple substance form.
2. The Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material of claim 1, wherein: mo: si: the mass ratio of B is 94:4:1, the mass fraction of Ag is more than 0 and less than or equal to 15 percent.
3. The Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material of claim 1, wherein: in the environment with oxygen above 600 ℃, ag and Mo in the surface layer of Mo-12Si-8.5B can be oxidized to generate Ag with self-lubricating effect 2 MoO 4 And Ag 2 Mo 4 O 11 。
4. A method for preparing a Mo-12Si-8.5B-Ag wide temperature range self-lubricating material according to any one of claims 1 to 3, comprising the steps of:
the method comprises the following steps: powder preparation: taking Mo, si, B and Ag powder as raw materials, filling the four kinds of powder into a ball milling tank in inert protective atmosphere, and performing high-energy ball milling by adopting a ball mill to uniformly mix the powder;
step two: sintering preparation: and (2) putting the mixed powder into a graphite die, sintering by adopting a two-step method by adopting a plasma discharge sintering technology, firstly sintering at 900 ℃, then heating to 1400 ℃, and finally cooling along with a furnace.
5. The method for preparing a Mo-12Si-8.5B-Ag wide temperature range self-lubricating material as claimed in claim 4, wherein: the inert protective gas is argon.
6. The method for preparing a Mo-12Si-8.5B-Ag wide temperature range self-lubricating material as claimed in claim 4, wherein: the ball mill adopts an omnibearing planetary ball mill, the ball-material ratio is 10-20, the ball milling time is 10-40 h, and the ball milling rotating speed is 300-500 r/min.
7. The method for preparing a Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material according to claim 4, wherein the Mo-12Si-8.5B-Ag wide-temperature-range self-lubricating material comprises the following steps: the plasma discharge sintering is carried out in vacuum with a vacuum degree of 10 -2 Pa, the heating rate is 150 ℃/min when sintering at 900 ℃, the pressure is 40-60 MPa, the heat preservation time is 5-10 min, the heating rate is 150 ℃/min when sintering at 1400 ℃, the pressure is 30-45 MPa, and the heat preservation time is 5-10 min.
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