CN108359824B - Graphene-reinforced Ti-18Mo-xSi composite material and preparation method thereof - Google Patents
Graphene-reinforced Ti-18Mo-xSi composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene-reinforced Ti-18Mo-xSi composite material and a preparation method thereof, wherein the composite material is prepared by compounding and sintering titanium powder, molybdenum powder, silicon powder and nano Graphene (GNP) powder; the components of the Ti-18Mo-xSi +0.5GNP composite powder are calculated by mass percent, wherein the titanium powder, the molybdenum powder and the silicon powder form matrix mixed powder; ti content (82-x) wt.%, Mo content 18wt.%, Si content x wt.%; the preparation method comprises the following steps: firstly, Ti powder, Mo powder, Si powder and nano GNP powder are uniformly mixed and then are subjected to high-energy ball milling to enable the Ti powder, the Mo powder, the Si powder and the nano GNP powder to be partially alloyed, then powder obtained by ball milling is sieved and dried, then the dried powder is prepared into briquettes through compression molding, and finally the briquettes are sintered in a vacuum and pressureless mode to enable the briquettes to be fully alloyed. The Ti-18Mo-xSi composite material provided by the invention has uniform components, improves the corrosion resistance and the like to a certain degree, and has wide application prospects in the fields of aerospace, military industry, navigation, automobiles and the like.
Description
Technical Field
The invention relates to a composite material technology, in particular to a graphene reinforced Ti-18Mo-xSi composite material for improving hardness and corrosion resistance and a preparation method thereof.
Background
Titanium and titanium alloy are very important metal structure materials, have the characteristics of high specific strength, excellent corrosion resistance and the like, and have wide application in the fields of aerospace, military industry, navigation, automobiles, petrochemical industry, biological medicine and the like. However, with the increasing demand for high-performance materials in the aerospace field, such as demand for lightweight high-strength materials for high-tech aerospace equipment such as hypersonic aircrafts, orbital aircrafts, and space shuttles, the titanium and titanium alloy materials have been difficult to meet the high-performance requirements, and therefore, the development of titanium and titanium alloys has gradually shifted to titanium-based composite materials (TMCs) and has been successfully applied to aerospace equipment parts with higher requirements. With decades of development, titanium-based composites have developed two major categories, namely continuous fiber reinforced titanium-based composites and discontinuous reinforced composites. The continuous fiber reinforced titanium-based composite material has the defects of high fiber price, anisotropy, complex preparation, difficult secondary processing and the like, so that the application range is greatly limited, and the non-continuous reinforced titanium-based composite material with isotropy and easy processing has the characteristics of large improvement range of mechanical properties, low cost and the like and has become an important research direction of the titanium-based composite material. The reinforcement with high specific strength and specific modulus added in the non-continuous reinforced titanium-based composite material can obviously improve the specific strength and specific modulus of the material, and simultaneously can endow the material with excellent mechanical properties, thereby meeting the requirements of aerospace high-tech equipment on the material.
The currently commonly used reinforcement is mainly B4C、TiB2、ZrB2TiC, TiB, SiC and the like, and in recent years, materials such as carbon nanotubes and GNP have been developed as reinforcements of titanium-based composites. Among these reinforcement materials, GNPs have a higher elastic modulus (1.0TPa), higher strength (130GPa), and a larger specific surface area, allowing a larger interface with the composite matrix. In addition, the SiC reinforcement can be generated in situ by adding GNP, and the comprehensive performance of the composite material is improved. Therefore, the GNP is selected as the reinforcement of the titanium-based composite material, and has high application value and wide research prospect.
Disclosure of Invention
The invention aims to solve the problem of low overall performance of the existing titanium alloy, and provides a nano-graphene reinforced Ti-18Mo-xSi composite material prepared by adopting a high-energy ball milling-compression molding-vacuum pressureless sintering process; the method is simple to operate and low in cost, and the obtained titanium-based composite material has high content of intermetallic compounds of titanium silicon and molybdenum silicon and good comprehensive performance.
The invention is realized by the following technical scheme:
a graphene reinforced Ti-18Mo-xSi composite material is prepared by compounding and sintering titanium powder, molybdenum powder, silicon powder and nano Graphene (GNP) powder; the components of the Ti-18Mo-xSi +0.5GNP composite powder are calculated by mass percent, wherein the titanium powder, the molybdenum powder and the silicon powder form matrix mixed powder; ti content (82-x) wt.%, Mo content 18wt.%, Si content x wt.%; nano GNP powder was 0.5wt.% of matrix mix powder; the value range of x is 0-2.
Further, the value of x is 0, 0.5, 1 or 2.
The other technical scheme of the invention is as follows:
a preparation method of a graphene reinforced Ti-18Mo-xSi composite material comprises the following steps:
step one), high-energy ball milling and mixing powder: firstly, preparing Ti-18Mo-xSi mixed powder according to the components, putting the mixed powder into a ball milling tank, and ball milling the mixed powder in a ball mill according to certain ball milling parameters to partially alloy the Ti powder, the Mo powder and the Si powder; secondly, adding 0.5wt.% of nano GNP powder in the mass of the mixed powder based on the preparation of the matrix mixed powder, wet-grinding by adopting absolute ethyl alcohol to fully disperse the nano GNP powder, drying the mixed powder, then putting the dried mixed powder into a ball-milling tank for dry-milling to fully alloy the Ti, Mo, Si and nano GNP, sieving the mixed powder obtained after ball-milling by a 300-mesh sieve, and putting the powder into a vacuum drying oven for drying;
step two) conventional compression molding: pressing and molding the mixed powder prepared in the step one) to obtain a pressed block;
step three), vacuum pressureless sintering: and D) carrying out vacuum pressureless sintering on the pressed and molded pressing block in the step two), so that Ti, Mo, Si and nano GNP are further alloyed.
Further, in the high-energy ball-milling mixed powder in the step one), the dry milling process comprises the following steps: the ball-material ratio (8-12) is 1, the rotating speed is 300-500 r/min, the ball milling time is at least 48h, and the ball milling machine is stopped for 10min every 50 min; the wet milling process comprises the following steps: adding a proper amount of absolute ethyl alcohol to submerge the grinding balls, rotating at a speed of 300-500 r/min, ball-milling for at least 24h, and stopping for 10min every 50min of ball milling.
Further, placing the ball-milled composite powder in the step one) in a vacuum drying oven, heating to 60-80 ℃ along with the drying oven, preserving the heat for at least 4h, and sieving with a 300-mesh sieve.
Further, the press forming process in the step two) comprises the following steps: the working pressure adopted during pressing is 550-650 MPa, and the pressing block is a round block with phi of 30mm and thickness of 3-5 mm.
Further, the vacuum pressureless sintering process in the step three) comprises the following steps: vacuum-pumping to 1 × 10-1Pa, the heating rate is 4-5 ℃/min, the sintering process is 900 ℃ multiplied by 2h +1300 ℃ multiplied by 3h, and finally furnace cooling is carried out.
The invention has the beneficial effects that:
(1) the invention innovatively provides a novel powder metallurgy preparation process of high-energy ball milling-compression molding-vacuum pressureless sintering, wherein four kinds of powder of Ti, Mo, Si and nano GNP are partially alloyed through high-energy ball milling in a powder mixing stage, and the nano GNP is fully dispersed in a wet milling stage; during sintering, further alloying. Compared with the common powder metallurgy process, the process enables the alloying and compounding of the four kinds of powder to be more sufficient, and provides an industrial production preparation method for the titanium-based composite material.
(2) The graphene-reinforced Ti-18Mo-xSi composite material and the preparation method thereof provided by the invention are simple to operate, easy to realize and excellent in economy.
(3) Compared with the common Ti-18Mo-xSi alloy material, the graphene reinforced Ti-18Mo-xSi composite material prepared by the invention has the advantages that the hardness, the corrosion resistance and the like are improved to a certain degree.
(4) The difficult problem of the requirement on high-performance titanium alloy with light weight, high strength, corrosion resistance and the like is well solved.
Drawings
FIG. 1 is a macroscopic view of a Ti-18Mo alloy before and after sintering in a comparative example of the present invention;
FIG. 2 is a macroscopic view of a Ti-18Mo +0.5GNP composite material before and after sintering according to an embodiment of the present invention;
FIG. 3 is an XRD diffractogram of the sintered Ti-18Mo-0.5Si alloy of the comparative example of the present invention;
FIG. 4 is an XRD diffractogram of the sintered Ti-18Mo-0.5Si +0.5GNP composite material in the examples of the present invention;
FIG. 5 is a graph of the corrosion kinetics of the Ti-18Mo-1Si alloy and the Ti-18Mo-1Si +0.5GNP composite material of the comparative example and the example of the present invention.
Detailed Description
The following detailed description of the present invention will be made with reference to the accompanying drawings and examples, but the present invention is not limited to the examples.
Example 1
A graphene reinforced Ti-18Mo-xSi composite material, Ti-18Mo +0.5GNP, is prepared by the following method: firstly, preparing 30g of mixed powder of Ti powder, Si powder and Mo powder, wherein the mass of the Ti powder is 82 wt.% (24.6g), the mass of the Mo powder is 18wt.% (5.4g), and placing the mixed powder in a beaker for uniformly stirring; secondly, 240g of agate balls are weighed according to the ball-to-material ratio of 8:1 and placed in a 500ml nylon ball milling tank, then the mixed powder is placed in the nylon ball milling tank, and the nylon ball milling tank is covered and sealed; then, mounting the ball milling tank on a planetary ball mill, starting ball milling, setting ball milling parameters to be 500r/min, stopping the ball milling for 50min for 10min, and taking out powder in the ball milling tank after ball milling for 48 h; on the basis of preparing matrix mixed powder, adding 0.5wt.% of nano GNP powder (0.15g) in the mass of the mixed powder, wet-grinding by adopting absolute ethyl alcohol, setting ball-milling parameters to be 500r/min, stopping the ball-milling for 10min after 50min, and after 24h of ball-milling, placing the ball-milled powder in a drying oven for vacuum drying at 60-80 ℃ for at least 4 h; cooling the mixed powder, then carrying out dry milling, setting ball milling parameters to be 500r/min, stopping the ball milling for 50min for 10min, and taking out the powder in the ball milling tank after ball milling for 24 h; sieving the taken mixed powder with a 300-mesh sieve to obtain powder with uniform granularity, and then placing the powder in a vacuum drying oven for vacuum drying for at least 4 hours at the temperature of 60-80 ℃ to obtain the required powder; then, the obtained powder is pressed and formed by adopting a powder compact forming method of unidirectional pressurization of a die, the inner diameter of the die is phi 30mm, the working pressure is 550MPa, and round blocks with the phi 30mm and the thickness of 3-5 mm are prepared; finally, the obtained pressed block is placed in a tubular vacuum sintering furnace for vacuum pressureless sintering, the furnace is firstly vacuumized to 1 multiplied by 10-1Pa, the heating rate is 4 ℃/min, the sintering process is 900 ℃ multiplied by 2h +1300 ℃ multiplied by 3h, and finally furnace cooling is carried out.
Comparative example
Preparation method of Ti-18Mo alloy
FIG. 1 is a macroscopic view of a Ti-18Mo alloy before and after sintering in an embodiment of the invention, and the sintering shrinkage of the alloy is 10.5%; hardness of Ti-18Mo alloy628.14Hv, and the weight loss after 100 hours of corrosion in 1mol/L HCl solution is 4.51mg cm-2。
FIG. 2 is a macroscopic view of the Ti-18Mo +0.5GNP composite material before and after sintering in the embodiment of the invention, and the sintering shrinkage of the composite material is improved by 60.9% (16.9% VS 10.5%) compared with that of the alloy, which shows that the nano GNP improves the sintering quality. Comparing example 1 with the comparative example, it was found that the Ti-18Mo +0.5GNP composite material obtained after adding nano GNP powder is more excellent in overall performance, wherein the hardness of the Ti-18Mo +0.5GNP composite material is increased by 22.5% (719.13HvVS628.14Hv) compared with the Ti-18Mo alloy, and the weight loss after 100h corrosion in 1mol/L HCl solution is reduced by 60.8% (1.77mg cm) compared with the Ti-18Mo alloy-2VS 4.51mg·cm-2)。
Example 2
A graphene reinforced Ti-18Mo-xSi composite: the Ti-18Mo-0.5Si +0.5GNP is prepared by the following method: this example is similar to example 1 except that the mass fraction of the Si powder was increased from 0 wt.% (0g) to 0.5wt.% (0.15g) and correspondingly the mass fraction of the Ti powder was decreased from 82 wt.% (24.6g) to 81.5 wt.% (24.45 g).
Comparative example
Preparation method of Ti-18Mo-0.5Si alloy
FIG. 3 is an XRD pattern of the sintered Ti-18Mo-0.5Si alloy; analyzed to contain Ti5Si4TiSi and Mo5Si3The compounds, Ti5Si4Diffraction peak intensity ratio of Mo5Si3The diffraction peak intensity of (A) is slightly higher; the Ti-18Mo-0.5Si alloy has a hardness of 674.62Hv and a weight loss of 3.93mg cm after etching in 1mol/L HCl solution for 100 hours-2. FIG. 4 is an XRD pattern of a Ti-18Mo-0.5Si +0.5GNP composite material, similar to FIG. 3, analyzed to contain Ti5Si4、TiSi、Mo5Si3And compounds of SiC and the like, Mo5Si3Diffraction peak intensity ratio of Ti5Si4The diffraction peak intensity of the nano GNP is slightly higher, which indicates that the nano GNP can promote the conversion between compounds; the Ti-18Mo-0.5Si +0.5GNP composite material prepared after the nano GNP powder is added has more excellent comprehensive performance than the Ti-18Mo-0.5Si, wherein the Ti-18Mo-0.The hardness of the 5Si +0.5GNP composite material is improved by 22.5 percent (782.4Hv VS 674.62Hv) compared with that of the Ti-18Mo-0.5Si alloy, and the weight loss after the composite material is corroded in 1mol/L HCl solution for 100 hours is reduced by 35.9 percent (2.52mg cm) compared with that of the Ti-18Mo-0.5Si alloy-2VS 3.93mg·cm-2)。
Example 3
A graphene reinforced Ti-18Mo-xSi composite: the Ti-18Mo-1Si +0.5GNP is prepared by the following method: firstly, preparing 30g of mixed powder of Ti powder, Si powder and Mo powder, wherein the mass of the Ti powder is 81 wt.% (24.3g), the mass of the Mo powder is 18wt.% (5.4g) and the mass of the Si powder is 1 wt.% (0.3g), and placing the mixed powder in a beaker for uniformly stirring;
secondly, weighing 240g of agate balls in a ball-to-material ratio of 8:1, placing the agate balls in a 500ml nylon ball milling tank, placing the uniformly mixed powder in the nylon ball milling tank, and covering and sealing the tank;
then, mounting the ball milling tank on a planetary ball mill, starting ball milling, setting ball milling parameters to be 500r/min, stopping the ball milling for 50min for 10min, and taking out powder in the ball milling tank after ball milling for 48 h;
on the basis of preparing matrix mixed powder, adding 0.5wt.% of nano GNP (0.15g) powder in the mass of the mixed powder, wet-grinding by adopting absolute ethyl alcohol, setting ball-milling parameters to be 500r/min, stopping the ball-milling for 10min after 50min, placing the ball-milled powder in a drying oven for vacuum drying at 60-80 ℃ for at least 4h after 24h of ball-milling;
carrying out dry grinding on the cooled mixed powder, setting ball milling parameters to be 500r/min, stopping the ball milling for 50min for 10min, and taking out the powder in the ball milling tank after ball milling for 24 h;
sieving the taken mixed powder with a 300-mesh sieve to obtain powder with uniform granularity, and then placing the powder in a vacuum drying oven for vacuum drying for at least 4 hours at the temperature of 60-80 ℃ to obtain the required powder;
then, the obtained powder is pressed and formed by adopting a powder compact forming method of unidirectional pressurization of a die, the inner diameter of the die is phi 30mm, the working pressure is 550MPa, and round blocks with the phi 30mm and the thickness of 3-5 mm are prepared;
finally, the obtained pressed block is placed in a tubular vacuum sintering furnace for vacuum pressureless sintering, the furnace is firstly vacuumized to 1 multiplied by 10-1Pa, the heating rate is 4 ℃/min, the sintering process is 900 ℃ multiplied by 2h +1300 ℃ multiplied by 3h, and finally furnace cooling is carried out.
Comparative example
Preparation method of Ti-18Mo-1Si alloy
The Ti-18Mo-1Si alloy has a hardness of 698.79Hv and a weight loss of 3.62mg cm after being etched in 1mol/L HCl solution for 100 hours-2。
FIG. 5 shows the corrosion kinetics curves of Ti-18Mo-1Si alloy and Ti-18Mo-1Si +0.5GNP composite material, and comparing example 3 with the comparative example, it was found that the Ti-18Mo-1Si +0.5GNP composite material prepared after adding nano GNP powder has better combination properties than Ti-18Mo-1Si, wherein the hardness of Ti-18Mo-1Si +0.5GNP composite material is improved by 22.5% (817.37Hv VS 698.79Hv) than that of Ti-18Mo-1Si alloy, and the weight loss after 100h corrosion in 1mol/L HCl solution is reduced by 72.4% (1.0 mg. cm. Si alloy)-2VS 3.62mg·cm-2)。
Example 4
A graphene reinforced Ti-18Mo-xSi composite: the Ti-18Mo-2Si +0.5GNP is prepared by the following method: firstly, preparing 30g of mixed powder of Ti powder, Si powder and Zr powder, wherein the mass of the Ti powder is 80 wt.% (24g), the mass of the Mo powder is 18wt.% (5.4g) and the mass of the Si powder is 2 wt.% (0.6g), and placing the mixed powder in a beaker for uniformly stirring; secondly, weighing 240g of agate balls in a ball-to-material ratio of 8:1, placing the agate balls in a 500ml nylon ball milling tank, placing the weighed and uniformly mixed powder in the nylon ball milling tank, and covering and sealing the nylon ball milling tank; then, mounting the ball milling tank on a planetary ball mill, starting ball milling, setting ball milling parameters to be 500r/min, stopping the ball milling for 1h for 15min, and taking out powder in the ball milling tank after ball milling for 48 h; on the basis of preparing matrix mixed powder, adding 0.5wt.% of nano GNP (0.15g) powder in the mass of the mixed powder, wet-grinding by adopting absolute ethyl alcohol, setting ball-milling parameters to be 500r/min, stopping the ball-milling for 10min after 50min, placing the ball-milled powder in a drying oven for vacuum drying at 60-80 ℃ for at least 4h after 24h of ball-milling; carrying out final dry grinding on the cooled mixed powder, setting ball milling parameters to be 500r/min, stopping the ball milling for 50min for 10min, and taking out the powder in the ball milling tank after ball milling for 24 h; sieving the mixed powder with 300 mesh sieve to obtain the product with uniform granularityAfter the powder is put into a vacuum drying oven, vacuum drying is carried out for at least 4 hours at the temperature of 60-80 ℃ to obtain the required powder; then, the obtained powder is pressed and formed by adopting a powder compact forming method of unidirectional pressurization of a die, the inner diameter of the die is phi 30mm, the working pressure is 550MPa, and round blocks with the phi 30mm and the thickness of 3-5 mm are prepared; finally, the obtained pressed block is placed in a tubular vacuum sintering furnace for vacuum pressureless sintering, the furnace is firstly vacuumized to 1 multiplied by 10-1Pa, the heating rate is 4 ℃/min, the sintering process is 900 ℃ multiplied by 2h +1300 ℃ multiplied by 3h, and finally furnace cooling is carried out.
Comparative example
Preparation method of Ti-18Mo-2Si alloy
The Ti-18Mo-2Si alloy has the hardness of 934.28Hv, and the weight loss after being corroded in 1mol/L HCl solution for 100 hours is 4.51 mg-cm-2。
Comparative example 4 and comparative example it was found that the Ti-18Mo-2Si +0.5GNP composite material obtained after addition of nano GNP powder has an overall better performance than Ti-18Mo-2Si, wherein the hardness of the Ti-18Mo-2Si +0.5GNP composite material is increased by 22.5% (1047.13Hv VS 934.28Hv) compared to the Ti-18Mo-2Si alloy, and the weight loss after 100h corrosion in 1mol/L HCl solution is reduced by 94.0% (0.27mg cm. multidot.cm) compared to the Ti-18Mo-2Si alloy-2VS 4.51mg·cm-2)。
The parts not involved in the present invention are the same as or can be implemented using the prior art.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (7)
1. A preparation method of a graphene reinforced Ti-18Mo-xSi composite material is characterized by comprising the following steps: the components of the Ti-18Mo-xSi +0.5GNP composite powder are calculated by mass percent, wherein the titanium powder, the molybdenum powder and the silicon powder form matrix mixed powder; ti content (82-x) wt.%, Mo content 18wt.%, Si content x wt.%; nano GNP powder was 0.5wt.% of matrix mix powder; the value range of x is 0-2;
the preparation method specifically comprises the following steps:
step one), high-energy ball milling and mixing powder: firstly, preparing Ti-18Mo-xSi mixed powder according to the components, putting the mixed powder into a ball milling tank, and ball milling the mixed powder in a ball mill according to certain ball milling parameters to partially alloy Ti, Mo and Si powder; secondly, adding 0.5wt.% of nano GNP powder in the mass of the mixed powder based on the preparation of the matrix mixed powder, wet-grinding by adopting absolute ethyl alcohol to fully disperse the nano GNP powder, drying the mixed powder, then putting the dried mixed powder into a ball-milling tank for dry-milling to fully alloy the Ti, Mo, Si and nano GNP, sieving the mixed powder obtained after ball-milling by a 300-mesh sieve, and putting the powder into a vacuum drying oven for drying;
step two) conventional compression molding: pressing and molding the mixed powder prepared in the step one) to obtain a pressed block;
step three), vacuum pressureless sintering: and D) carrying out vacuum pressureless sintering on the pressed and molded pressing block in the step two), so that Ti, Mo, Si and nano GNP are further alloyed.
2. The method of preparing a graphene-reinforced Ti-18Mo-xSi composite material according to claim 1, wherein: in the high-energy ball-milling mixed powder in the step one), a dry milling process comprises the following steps: the ball-material ratio (8-12) is 1, the rotating speed is 300-500 r/min, the ball milling time is at least 48h, and the ball milling machine is stopped for 10min every 50 min; the wet milling process comprises the following steps: adding a proper amount of absolute ethyl alcohol to submerge the grinding balls, rotating at a speed of 300-500 r/min, ball-milling for at least 24h, and stopping for 10min every 50min of ball milling.
3. The method of preparing a graphene-reinforced Ti-18Mo-xSi composite material according to claim 1, wherein: placing the mixed powder subjected to wet grinding in the step one) in a vacuum drying oven, heating to 60-80 ℃ along with the drying oven, preserving heat for at least 4h, and sieving with a 300-mesh sieve.
4. The method for preparing the graphene-reinforced Ti-18Mo-xSi composite material according to claim 1, wherein the press-molding in the second step) comprises: the working pressure adopted during pressing is 550-650 MPa, and the pressing block is a round block with phi of 30mm and thickness of 3-5 mm.
5. The method for preparing a graphene-reinforced Ti-18Mo-xSi composite material according to claim 1, wherein the process of vacuum pressureless sintering in step three) is: vacuum-pumping to 1 × 10-1Pa, the heating rate is 4-5 ℃/min, the sintering process is 900 ℃ multiplied by 2h +1300 ℃ multiplied by 3h, and finally furnace cooling is carried out.
6. A composite material prepared by the method for preparing a graphene-reinforced Ti-18Mo-xSi composite material according to any one of claims 1 to 5.
7. The composite material of claim 6, wherein x has a value of 0 or 0.5 or 1 or 2.
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