CN103334030A - Graphene-containing titanium-aluminum-base self-lubricating composite material and preparation method thereof - Google Patents
Graphene-containing titanium-aluminum-base self-lubricating composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a graphene-containing titanium-aluminum-base self-lubricating composite material and a preparation method thereof. The method comprises the following steps: 1) selecting Ti powder and Al powder according to the Ti:Al mol ratio of 1:1-1:5; selecting graphene powder, wherein the graphene powder accounts for 1.5-4.5 wt.% of the Ti powder and Al powder; adding the graphene powder into the mixed powder to obtain a mixture; 2) carrying out wet milling on the mixture, screening, and cleaning to obtain a mixed suspensoid solution; 3) filtering the mixed suspensoid solution to remove the filtrate, and carrying out vacuum drying to obtain prtreated mixed powder; and 4) putting the pretreated mixed powder in a graphite jig, and sintering in a vacuum by a discharge plasma sintering process to obtain the satisfactory graphene-containing titanium-aluminum-base self-lubricating composite material. The prepared composite material has the advantages of fine crystal grains, high density, excellent comprehensive properties and favorable tribological properties. The invention has the characteristics of short preparation period, low cost, simple operational procedure and the like, and is suitable for large-scale mass production.
Description
Technical field
The present invention relates to the metal-base composites technology of preparing, relate in particular to aluminium base self-lubricating composite of a kind of graphitiferous alkene titanium and preparation method thereof.
Background technology
The TiAl alloy has the excellent properties of metal and pottery concurrently, as high specific tenacity, specific modulus, good oxidation-resistance, creep resistance, excellent high-temperature intensity, rigidity and low density, these good performances make it become desirable lightweight structural material ([1] Feng Xudong, Yuan Qinglong, Cao Jingjing that advanced career fields such as aerospace field, high-temperature engine have wide application prospect, Su Zhijun. TiAl base alloy research progress [J]. the space flight manufacturing technology, 2009(3): 35-38; [2] Qu Xuanhui, Huang Baiyun, Lv Haibo, etc. TiAl ordered alloy Review Study [J]. Rare Metals Materials and engineering, 1991, (4): 3-14.).
The development of advanced industrial circles such as modern Aeronautics and Astronautics etc. makes that the operating mode of structured material is increasingly serious, causes friction, wearing and tearing and lubrication problem to become increasingly conspicuous, so an urgent demand the development lubricant and the self-lubricating material that adapt.Solid lubricant is compared with traditional lubricating oil, lubricating grease has remarkable advantages, is a kind of effective way that solves the friction, lubrication problem at present so prepare matrix material by interpolation solid lubricant in matrix.
Summary of the invention
The object of the present invention is to provide aluminium base self-lubricating composite of a kind of graphitiferous alkene titanium and preparation method thereof, the matrix material of this method preparation has excellent tribological property, and this method technology is simple, processing parameter is easy to control.
The present invention solves the problems of the technologies described above the technical scheme of taking to be:
The aluminium base self-lubricating composite of a kind of graphitiferous alkene titanium is characterized in that it is prepared from by Ti powder, Al powder and Graphene powder, mol ratio=1:1 of Ti:Al～1.5 wherein, and Graphene powder add-on is the 1.5-4.5wt.% of Ti powder, Al powder total mass.
The preparation method of the aluminium base self-lubricating composite of above-mentioned graphitiferous alkene titanium is characterized in that it comprises the steps:
1) presses mol ratio=1:1～1.5 of Ti:Al, choose Ti powder, Al powder; Add-on by the Graphene powder is the 1.5-4.5wt.% of Ti powder, Al powder total mass, chooses the Graphene powder;
Ti powder, Al powder are mixed, obtain mixed powder, add the Graphene powder then in described mixed powder, obtain batching;
2) above-mentioned batching is carried out wet-milling, sieve, obtain mixing suspension solution after the cleaning;
3) with after the above-mentioned mixing suspension solution filtration removal filtrate, vacuum-drying obtains pretreated mixed powder;
4) pretreated mixed powder is placed graphite jig, take discharge plasma sintering method under the vacuum condition then, namely sintering obtains the aluminium base self-lubricating composite of described graphitiferous alkene titanium.
In the such scheme, described step 2) the wet-milling step in is that batching, alcohol and steel ball are placed in the stainless-steel vacuum ball grinder, wet-milling in ball mill, and the wet-milling time is 4-6 hour.
In the such scheme, drum's speed of rotation is that 200-400 rev/min, ball material mass ratio are 10:1.
In the such scheme, vacuum tightness is 12-20Pa in the described stainless-steel vacuum ball grinder.
In the such scheme, described step 2) step of sieving in is to sieve by 300 order stainless steel sieves.
In the such scheme, the described vacuum drying vacuum tightness of described step 3) is 0.011-0.021MPa, and drying temperature is 60-70 ℃, and be 5-7 hour time of drying.
In the such scheme, the interior diameter of the graphite jig in the described step 4) is 20mm.
In the such scheme, described discharge plasma sintering process is: sintering temperature is that 950-1000 ℃, temperature rise rate are that 100-150 ℃/min, sintering pressure are that 30-50MPa, vacuum tightness are 1 * 10
-2-1 * 10
-1Pa, soaking time are 4-8min.
The invention has the beneficial effects as follows:
1, preparation is quick, feasibility is high: utilize SPS to carry out the sintering of material in the preparation process; reaction time is short; processing parameter is stable; can prepare this matrix material rapidly; and this matrix material purity height; have characteristics such as wide temperature range response, excellent comprehensive performances, and be applicable to the mass-producing batch process.
2, the preparation process processing step is few, and required equipment is simple: have the advantages that raw material sources are extensive, price is lower, technology is simple, control easily.
3, avoiding on the pollution of TiAl based composites particle surface and the problem of oxidation basis, adopt SPS to prepare the density height, graphitiferous alkene TiAl based composites with excellent over-all properties, can reduce sintering temperature, shorten sintering time, for example synthesis temperature is low 950-1000 ℃, the short 4-8min of generated time, save energy reduces synthetic cost.
4, the graphitiferous alkene titanium aluminum matrix composite of the present invention's preparation is a kind of novel self-lubricating matrix material.It is to be the high-performance self-lubricating composite that Graphene designs by TiAl matrix, wild phase and solid lubricant.
5, the aluminium base self-lubricating composite wood of graphitiferous alkene titanium of the present invention's preparation has good tribological property.
Description of drawings
Fig. 1 is preparation technology's schema of the present invention.
Fig. 2 is respectively the fracture FESEM photo (b) of the aluminium base self-lubricating composite of graphitiferous alkene titanium of Graphene powder (a) and embodiment 1 preparation.
Fig. 3 is that the aluminium base self-lubricating composite of graphitiferous alkene titanium that the embodiment of the invention 1 makes is the electronic probe photo of frictional abrasion surface under the 2N condition in load.
Fig. 4 is that the aluminium base self-lubricating composite of graphitiferous alkene titanium that the embodiment of the invention 1 makes is the electronic probe photo of frictional abrasion surface under the 4N condition in load.
Fig. 5 is that the aluminium base self-lubricating composite of graphitiferous alkene titanium that the embodiment of the invention 1 makes is the electronic probe photo of frictional abrasion surface under the 6N condition in load.
Fig. 6 is that the aluminium base self-lubricating composite of graphitiferous alkene titanium that the embodiment of the invention 1 makes is the electronic probe photo of frictional abrasion surface under the 8N condition in load.
Fig. 7 is that the aluminium base self-lubricating composite of graphitiferous alkene titanium that the embodiment of the invention 1 makes is the electronic probe photo of frictional abrasion surface under the 10N condition in load.
Fig. 8 is frictional coefficient and the wear rate curve of the aluminium base self-lubricating composite of the test embodiment of the invention 1 prepared graphitiferous alkene titanium, and test condition is: room temperature, sliding frequency 17.06Hz, time 40min, friction radius 2mm, load 2-10N.Adopt HT-1000 high temperature friction and wear experimental machine, according to USS ASTM G99-95, friction pair is the Si of diameter 6mm
3N
4Ball (HV 15GPa, Ra0.02 μ m).
Fig. 9 is the dynamic friction coefficient curve of the aluminium base self-lubricating composite of the test embodiment of the invention 2 prepared graphitiferous alkene titaniums, and test condition is: room temperature, sliding frequency 17.06Hz, time 40min, friction radius 2mm, load 10N.Adopt HT-1000 high temperature friction and wear experimental machine, according to USS ASTM G99-95, friction pair is the Si of diameter 6mm
3N
4Ball (HV 15GPa, Ra0.02 μ m).
Figure 10 is that the aluminium base self-lubricating composite of graphitiferous alkene titanium that the embodiment of the invention 2 makes is the electronic probe photo of frictional abrasion surface under the 10N condition in load.
Figure 11 is the dynamic friction coefficient curve of the aluminium base self-lubricating composite of the test embodiment of the invention 3 prepared graphitiferous alkene titaniums, and test condition is: room temperature, sliding frequency 17.06Hz, time 40min, friction radius 2mm, load 10N.Adopt HT-1000 high temperature friction and wear experimental machine, according to USS ASTM G99-95, friction pair is the Si of diameter 6mm
3N
4Ball (HV 15GPa, Ra0.02 μ m).
Figure 12 is that the aluminium base self-lubricating composite of graphitiferous alkene titanium that the embodiment of the invention 3 makes is the electronic probe photo of frictional abrasion surface under the 10N condition in load.
Embodiment
Further the present invention will be described below in conjunction with drawings and Examples, but content of the present invention not only is confined to the following examples.
Embodiment 1:
As shown in Figure 1, the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium, it comprises the steps:
1) be matrix material with Ti powder, Al powder, the Graphene powder is solid lubricant and wild phase, mole by Ti:Al=1:1 matches well intermetallic compound TiAl matrix presintering powder, take by weighing 6.395 gram Ti powder, 3.605 gram Al powder, amount to 10g, add 0.15 gram Graphene powder then in above-mentioned mixed powder, obtain batching (admixtion);
2) above-mentioned batching and steel ball are placed in the vacuum steel ball grinder wet-milling 4 hours on planetary ball mill under the rough vacuum condition; Wet grinding media is alcohol; Wherein: drum's speed of rotation is that 200 rev/mins, ball material mass ratio are 10:1, vacuum tightness 12Pa;
3) with the mixed slurry that contains steel ball behind the ball milling by 300 order stainless steel sieves sieve clean after, obtain mixing suspension solution, mix suspension solution filter remove filtrate after, (vacuum tightness is 0.011MPa in vacuum-drying, temperature is 60 ℃, and the time is 7 hours), obtain pretreated mixed powder;
4) to place interior diameter be the graphite grinding tool of 20mm for powder that drying is good, carries out discharge plasma sintering then under the vacuum condition.Wherein sintering temperature is that 950 ℃, temperature rise rate are that 100 ℃/min, sintering pressure are that 30MPa, soaking time 4min, vacuum tightness are 1 * 10
-2Pa prepares the aluminium base self-lubricating composite of graphitiferous alkene titanium.
(a b) is the FESEM photo of the prepared aluminium base self-lubricating composite fracture of titanium (b) of Graphene powder (a) and embodiment 1 respectively to Fig. 2.Fig. 2 (a) illustrates that the Graphene surface exists a large amount of wrinkles and gauffer, and single-layer graphene thickness is about 5-8nm.Its transparency is very high; Fig. 2 (b) illustrates the matrix material density height that embodiment 1 prepares, and Graphene is distributed in matrix crystal boundary place or is embedded in the matrix, guarantees the excellent over-all properties of the aluminium base self-lubricating composite of graphitiferous alkene titanium.Adopting the hardness of the prepared aluminium base self-lubricating composite of graphitiferous alkene titanium of Vickers' hardness instrument test implementation example 1 is HV
1662.4 actual density and the theoretical density calculating relative density of testing this matrix material according to drainage are 96.8%.Fig. 3 to Fig. 7 makes the electronic probe photo that the aluminium base self-lubricating composite of graphitiferous alkene titanium corresponds respectively to the frictional abrasion surface under the condition that load is 2N, 4N, 6N, 8N, 10N for embodiment 1, Fig. 3 to Fig. 7 illustrates that this matrix material frictional abrasion surface is more smooth, guarantees that it has the excellent friction performance in load is the 2-10N interval.In addition, the wear rate of sample can pass through formula (1) ([11] M.Y. Niu, Q.L. Bi, J. Yang, W.M. Liu. Tribological performance of a Ni
31000 ℃ of Al matrix self-lubricating composite coating tested from 25 to. Surf Coat Technol, 2012,206(19-20): 3938-3943.) calculate:
In the formula: V represents wear volume, and P represents load, and L represents sliding distance, ρ
wRepresent density of material, M
wRepresent the lost material quality, the unit of W is mm
3(Nm)
-1
Fig. 8 is frictional coefficient and the wear rate curve of the aluminium base self-lubricating composite of the embodiment of the invention obtained graphitiferous alkene titanium, and Fig. 8 illustrates that this matrix material is that frictional coefficient and wear rate under the 2N condition is respectively 0.38 and 1.45 * 10 in load
-4Mm
3/ (Nm), the frictional coefficient of 4N and wear rate are respectively 0.37 and 1.68 * 10
-4Mm
3/ (Nm), the frictional coefficient of 6N and wear rate are respectively 0.35 and 2.03 * 10
-4Mm
3/ (Nm), the frictional coefficient of 8N and wear rate are respectively 0.34 and 2.33 * 10
-4Mm
3/ (Nm), the frictional coefficient of 10N and wear rate are respectively 0.33 and 2.46 * 10
-4Mm
3/ (Nm), all shown outstanding tribological property.
Embodiment 2:
1) be matrix material with Ti powder, Al powder, the Graphene powder is solid lubricant and wild phase, mole by Ti:Al=1:1.3 matches well intermetallic compound TiAl matrix presintering powder, take by weighing 5.771 gram Ti powder, 4.229 gram Al powder, amount to 10g, add 0.30 gram Graphene powder then in above-mentioned mixed powder, obtain batching (admixtion);
2) above-mentioned batching and steel ball are placed in the Stainless Steel Vacuum ball grinder wet-milling 5 hours on planetary ball mill under the rough vacuum condition; Wet grinding media is alcohol; Wherein: drum's speed of rotation is that 300 rev/mins, ball material mass ratio are 10:1, vacuum tightness 16Pa;
3) the ball milling ball is sieved obtain after cleaning mixed slurry by 300 order stainless steel sieves sieve clean after, obtain mixing suspension solution, after mixing suspension solution filtration removal filtrate, (vacuum tightness is 0.016MPa in vacuum-drying, temperature is 65 ℃, time is 6 hours), obtain pretreated mixed powder;
4) to place interior diameter be the graphite grinding tool of 20mm for powder that drying is good, carries out discharge plasma sintering then under the vacuum condition.Wherein sintering temperature is that 980 ℃, temperature rise rate are that 120 ℃/min, sintering pressure are that 40MPa, soaking time 6min, vacuum tightness are 1 * 10
-1Pa prepares the aluminium base self-lubricating composite of graphitiferous alkene titanium.
Adopting the hardness of the prepared aluminium base self-lubricating composite of graphitiferous alkene titanium of Vickers' hardness instrument test implementation example 2 is HV
1685.8 actual density and the theoretical density calculating relative density of testing this matrix material according to drainage are 97.3%.Fig. 9 be embodiment 2 to make the aluminium base self-lubricating composite of graphitiferous alkene titanium be dynamic friction coefficient curve under the 10N condition in load, Fig. 9 illustrates that the frictional coefficient fluctuating range of this matrix material is little, mean value is about 0.35.In addition, the wear rate that calculates this matrix material that embodiment 2 prepares according to formula (1) is 2.74 * 10
-4Mm
3/ (Nm).So the aluminium base self-lubricating composite of graphitiferous alkene titanium has shown outstanding tribological property.Figure 10 is the electronic probe photo of frictional abrasion surface under the 10N spare for the aluminium base self-lubricating composite of embodiment 2 prepared graphitiferous alkene titaniums in load, and Figure 10 illustrates that this matrix material frictional abrasion surface is more smooth, guarantees that it has the excellent friction performance.
Embodiment 3:
1) be matrix material with Ti powder, Al powder, the Graphene powder is solid lubricant and wild phase, mole by Ti:Al=1:1.5 matches well intermetallic compound TiAl matrix presintering powder, take by weighing 5.418 gram Ti powder, 4.582 gram Al powder, amount to 10g, add 0.45 gram Graphene powder then in above-mentioned mixed powder, obtain batching (admixtion);
2) above-mentioned batching and steel ball are placed in the vacuum steel ball grinder wet-milling 6 hours on planetary ball mill under the rough vacuum condition; Wet grinding media is alcohol; Wherein: drum's speed of rotation is that 400 rev/mins, ball material mass ratio are 10:1, vacuum tightness 20Pa;
3) with the mixed slurry that contains steel ball behind the ball milling by 300 order stainless steel sieves sieve clean after, obtain mixing suspension solution, mix suspension solution filter remove filtrate after, (vacuum tightness is 0.021MPa in vacuum-drying, temperature is 70 ℃, and the time is 5 hours), obtain pretreated mixed powder;
4) to place interior diameter be the graphite grinding tool of 20mm for powder that drying is good, carries out discharge plasma sintering (SPS) then under the vacuum condition.Wherein sintering temperature is that 1000 ℃, temperature rise rate are that 150 ℃/min, sintering pressure are that 50MPa, soaking time 8min, vacuum tightness are 8 * 10
-2Pa prepares the aluminium base self-lubricating composite of graphitiferous alkene titanium.
Adopting the hardness of the prepared aluminium base self-lubricating composite of graphitiferous alkene titanium of Vickers' hardness instrument test implementation example 3 is HV
1723.5 actual density and the theoretical density calculating relative density of testing this matrix material according to drainage are 97.6%.Figure 11 be embodiment 3 to make the aluminium base self-lubricating composite of graphitiferous alkene titanium be dynamic friction coefficient curve under the 10N condition in load, Figure 11 illustrates that the frictional coefficient fluctuating range of this matrix material is little, mean value is about 0.33.In addition, the wear rate that calculates this matrix material that embodiment 3 prepares according to formula (1) is 3.01 * 10
-4Mm
3/ (Nm).So the aluminium base self-lubricating composite of titanium has shown outstanding tribological property.Figure 12 is the electronic probe photo of frictional abrasion surface under the 10N condition for the aluminium base self-lubricating composite of embodiment 3 prepared graphitiferous alkene titaniums in load, and Figure 12 illustrates that this matrix material frictional abrasion surface is smooth, guarantees that it has the excellent friction performance.
Each cited raw material of the present invention can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention, bound value and the interval value of processing parameter of the present invention (as temperature, time, vacuum tightness etc.) can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (9)
1. the aluminium base self-lubricating composite of graphitiferous alkene titanium is characterized in that it is prepared from by Ti powder, Al powder and Graphene powder, mol ratio=1:1 of Ti:Al～1.5 wherein, and Graphene powder add-on is the 1.5-4.5wt.% of Ti powder, Al powder total mass.
2. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 1 is characterized in that it comprises the steps:
1) presses mol ratio=1:1～1.5 of Ti:Al, choose Ti powder, Al powder; Add-on by the Graphene powder is the 1.5-4.5wt.% of Ti powder, Al powder total mass, chooses the Graphene powder;
Ti powder, Al powder are mixed, obtain mixed powder, add the Graphene powder then in described mixed powder, obtain batching;
2) above-mentioned batching is carried out wet-milling, sieve, obtain mixing suspension solution after the cleaning;
3) with after the above-mentioned mixing suspension solution filtration removal filtrate, vacuum-drying obtains pretreated mixed powder;
4) pretreated mixed powder is placed graphite jig, take discharge plasma sintering method under the vacuum condition then, namely sintering obtains the aluminium base self-lubricating composite of described graphitiferous alkene titanium.
3. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 2, it is characterized in that, described step 2) the wet-milling step in is that batching, alcohol and steel ball are placed in the stainless-steel vacuum ball grinder, wet-milling in ball mill, and the wet-milling time is 4-6 hour.
4. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 3 is characterized in that, drum's speed of rotation is that 200-400 rev/min, ball material mass ratio are 10:1.
5. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 3 is characterized in that, vacuum tightness is 12-20Pa in the described stainless-steel vacuum ball grinder.
6. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 2 is characterized in that described step 2) in the step of sieving be to sieve by 300 order stainless steel sieves.
7. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 2 is characterized in that, the described vacuum drying vacuum tightness of described step 3) is 0.011-0.021MPa, and drying temperature is 60-70 ℃, and be 5-7 hour time of drying.
8. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 2 is characterized in that, the interior diameter of the graphite jig in the described step 4) is 20mm.
9. the preparation method of the aluminium base self-lubricating composite of graphitiferous alkene titanium as claimed in claim 2, it is characterized in that described discharge plasma sintering process is: sintering temperature is that 950-1000 ℃, temperature rise rate are that 100-150 ℃/min, sintering pressure are that 30-50MPa, vacuum tightness are 1 * 10
-2-1 * 10
-1Pa, soaking time are 4-8min.
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