CN103334030B - Aluminium base self-lubricating composite of a kind of graphene-containing titanium and preparation method thereof - Google Patents
Aluminium base self-lubricating composite of a kind of graphene-containing titanium and preparation method thereof Download PDFInfo
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Abstract
The invention provides aluminium base self-lubricating composite of a kind of graphene-containing titanium and preparation method thereof.The method comprises the steps: 1) by mol ratio=1:1 ~ 1.5 of Ti:Al, choose Ti powder, Al powder; By the 1.5-4.5wt.% that the add-on of Graphene powder is Ti powder, Al powder total mass, choose Graphene powder; Then add Graphene powder in mixed powder above, prepared burden; 2) above-mentioned batching is carried out wet-milling, sieve, obtain after cleaning mixing suspension solution; 3), after above-mentioned mixing suspension solution being filtered removal filtrate, vacuum-drying, obtains the mixed powder that pre-treatment is good; 4) mixed powder that pre-treatment is good is placed in graphite jig, then takes discharge plasma sintering method under vacuum condition, namely sintering obtains the aluminium base self-lubricating composite of satisfactory graphene-containing titanium.Obtained matrix material crystal grain is tiny, density is high, excellent combination property, and has good tribological property.The present invention has that preparation cycle is short, cost is low, operating process is simple and be suitable for the features such as mass-producing batch production.
Description
Technical field
The present invention relates to metal-base composites technology of preparing, particularly relate to aluminium base self-lubricating composite of a kind of graphene-containing titanium and preparation method thereof.
Background technology
TiAl alloy has the excellent properties of metal and pottery concurrently; as high specific tenacity, specific modulus; good oxidation-resistance, creep resistance; excellent hot strength, rigidity and low density; these excellent performances become desirable lightweight structural material ([1] Feng Xudong, Yuan Qinglong, Cao Jingjing that the advanced career field such as aerospace field, high-temperature engine has wide application prospect; Su Zhi pretty .TiAl base alloy research progress [J]. Aerospace manufacturing technology, 2009(3): 35-38; [2] Qu Xuanhui, Huang Baiyun, Lv Haibo, waits .TiAl ordered alloy Review Study [J]. Rare Metals Materials and engineering, 1991, (4): 3-14.).
The development of the advanced industrial circle such as modern Aviation, space flight etc. makes the operating mode of structured material increasingly serious, causes friction, wearing and tearing and lubrication problem to become increasingly conspicuous, the therefore lubricant that adapts of an urgent demand development and self-lubricating material.Solid lubricant has obvious advantage compared with traditional lubricating oil, lubricating grease, therefore is a kind of effective way solving friction, lubrication problem at present by matrix material prepared by interpolation solid lubricant in the base.
Summary of the invention
The object of the present invention is to provide aluminium base self-lubricating composite of a kind of graphene-containing titanium and preparation method thereof, matrix material prepared by the method has excellent tribological property, and the method technique is simple, processing parameter is easy to control.
The present invention for solving the problems of the technologies described above taked technical scheme is:
The aluminium base self-lubricating composite of a kind of graphene-containing titanium, it is characterized in that, it is prepared from by Ti powder, Al powder and Graphene powder, wherein mol ratio=1:1 ~ 1.5 of Ti:Al, 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 graphene-containing titanium, is characterized in that it comprises the steps:
1) by mol ratio=1:1 ~ 1.5 of Ti:Al, Ti powder, Al powder is chosen; By the 1.5-4.5wt.% that the add-on of Graphene powder is Ti powder, Al powder total mass, choose Graphene powder;
By Ti powder, the mixing of Al powder, obtain mixed powder, then add Graphene powder in described mixed powder, prepared burden;
2) above-mentioned batching is carried out wet-milling, sieve, obtain after cleaning mixing suspension solution;
3), after above-mentioned mixing suspension solution being filtered removal filtrate, vacuum-drying, obtains the mixed powder that pre-treatment is good;
4) mixed powder that pre-treatment is good is placed in graphite jig, then takes discharge plasma sintering method under vacuum condition, namely sintering obtains the aluminium base self-lubricating composite of described graphene-containing titanium.
In such scheme, described step 2) in wet-milling step be that batching, alcohol and steel ball are placed in stainless-steel vacuum ball grinder, wet-milling in ball mill, the wet-milling time is 4-6 hour.
In such scheme, drum's speed of rotation is 200-400 rev/min, ball material mass ratio is 10:1.
In such scheme, in described stainless-steel vacuum ball grinder, vacuum tightness is 12-20Pa.
In such scheme, described step 2) in sifting step be by 300 order stainless steel sieve.
In such scheme, the vacuum drying vacuum tightness described in described step 3) is 0.011-0.021MPa, and drying temperature is 60-70 DEG C, and time of drying is 5-7 hour.
In such scheme, the interior diameter of the graphite jig in described step 4) is 20mm.
In such scheme, described discharge plasma sintering process is: sintering temperature is 950-1000 DEG C, temperature rise rate is 100-150 DEG C/min, sintering pressure is 30-50MPa, vacuum tightness is 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 preparation process; reaction time is short; processing parameter is stablized; this matrix material can be prepared rapidly; and this matrix material purity is high; there is the characteristics such as the response of wide temperature range, excellent over-all properties, and be applicable to mass-producing batch production.
2, preparation process processing step is few, and required equipment is simple: have raw material sources extensively, price is lower, technique is simple, hold manageable feature.
3, avoiding on the pollution of TiAl based composites particle surface and problem of oxidation basis, SPS is adopted to prepare density high, there is the graphene-containing TiAl based composites of Good All-around Property, sintering temperature can be reduced, shorten sintering time, the low 950-1000 DEG C of such as synthesis temperature, the short 4-8min of generated time, save energy, reduces synthesis cost.
4, the graphene-containing titanium-aluminium matrix composites that prepared by the present invention is a kind of novel self-lubricating matrix material.It is by TiAl matrix, wild phase and solid lubricant the high-performance self-lubricating matrix material that Graphene designs.
5, the graphene-containing titanium aluminium base self-lubricating composite wood that prepared by the present invention has good tribological property.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the present invention.
Fig. 2 is fracture FESEM photo (b) of the aluminium base self-lubricating composite of graphene-containing titanium prepared by Graphene powder (a) and embodiment 1 respectively.
Fig. 3 is the electronic probe photo of the aluminium base self-lubricating composite of graphene-containing titanium frictional abrasion surface under load is 2N condition that the embodiment of the present invention 1 obtains.
Fig. 4 is the electronic probe photo of the aluminium base self-lubricating composite of graphene-containing titanium frictional abrasion surface under load is 4N condition that the embodiment of the present invention 1 obtains.
Fig. 5 is the electronic probe photo of the aluminium base self-lubricating composite of graphene-containing titanium frictional abrasion surface under load is 6N condition that the embodiment of the present invention 1 obtains.
Fig. 6 is the electronic probe photo of the aluminium base self-lubricating composite of graphene-containing titanium frictional abrasion surface under load is 8N condition that the embodiment of the present invention 1 obtains.
Fig. 7 is the electronic probe photo of the aluminium base self-lubricating composite of graphene-containing titanium frictional abrasion surface under load is 10N condition that the embodiment of the present invention 1 obtains.
Fig. 8 is frictional coefficient and the wear rate curve of the graphene-containing titanium aluminium base self-lubricating composite of test obtained by the embodiment of the present invention 1, 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 ASTMG99-95, friction pair is the Si of diameter 6mm
3n
4ball (HV15GPa, Ra0.02 μm).
Fig. 9 is the dynamic friction coefficient curve of the graphene-containing titanium aluminium base self-lubricating composite of test obtained by the embodiment of the present invention 2, 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 ASTMG99-95, friction pair is the Si of diameter 6mm
3n
4ball (HV15GPa, Ra0.02 μm).
Figure 10 is the electronic probe photo of the aluminium base self-lubricating composite of graphene-containing titanium frictional abrasion surface under load is 10N condition that the embodiment of the present invention 2 obtains.
Figure 11 is the dynamic friction coefficient curve of the graphene-containing titanium aluminium base self-lubricating composite of test obtained by the embodiment of the present invention 3, 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 ASTMG99-95, friction pair is the Si of diameter 6mm
3n
4ball (HV15GPa, Ra0.02 μm).
Figure 12 is the electronic probe photo of the aluminium base self-lubricating composite of graphene-containing titanium frictional abrasion surface under load is 10N condition that the embodiment of the present invention 3 obtains.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described further, but content of the present invention is not only confined to the following examples.
embodiment 1:
As shown in Figure 1, the preparation method of the aluminium base self-lubricating composite of graphene-containing titanium, it comprises the steps:
1) with Ti powder, Al powder for matrix material, Graphene powder is solid lubricant and wild phase, mole intermetallic compound TiAl matrix presintering powder is matched well by Ti:Al=1:1, take 6.395 grams of Ti powder, 3.605 grams of Al powder, amount to 10g, then add 0.15 gram of Graphene powder in above-mentioned mixed powder, obtain preparing burden (admixtion);
2) above-mentioned batching and steel ball are placed in vacuum steel ball grinder, wet-milling 4 hours on planetary ball mill under rough vacuum condition; Wet grinding media is alcohol; Wherein: drum's speed of rotation is 200 revs/min, ball material mass ratio is 10:1, vacuum tightness 12Pa;
3) mixed slurry of steel ball will be contained after ball milling by after 300 order stainless steel sieve cleanings, obtain mixing suspension solution, after mixing suspension solution filters and removes filtrate, (vacuum tightness is 0.011MPa in vacuum-drying, temperature is 60 DEG C, time is 7 hours), obtain the mixed powder that pre-treatment is good;
4) dried powder is placed in the graphite grinding tool that interior diameter is 20mm, then carries out discharge plasma sintering under vacuum condition.Wherein sintering temperature is 950 DEG C, temperature rise rate is 100 DEG C/min, sintering pressure is 30MPa, soaking time 4min, vacuum tightness is 1 × 10
-2pa, prepares the aluminium base self-lubricating composite of graphene-containing titanium.
Fig. 2 (a, b) is the FESEM photo of Graphene powder (a) and aluminium base self-lubricating composite fracture (b) of titanium prepared by embodiment 1 respectively.Fig. 2 (a) illustrates that graphenic surface also exists a large amount of wrinkle and gauffer, and single-layer graphene thickness is about 5-8nm.Its transparency is very high; Fig. 2 (b) illustrates that the matrix material density that embodiment 1 is prepared is high, and Graphene is distributed in matrix grain boundaries or embeds in the base, ensures the Good All-around Property of the aluminium base self-lubricating composite of graphene-containing titanium.The hardness adopting the aluminium base self-lubricating composite of graphene-containing titanium prepared by Vickers' hardness instrument testing example 1 is HV
1662.4, testing the actual density of this matrix material and theoretical density according to drainage, to calculate relative density be 96.8%.Fig. 3 to Fig. 7 is that embodiment 1 obtains the aluminium base self-lubricating composite of graphene-containing titanium and corresponds respectively to the electronic probe photo that load is the frictional abrasion surface under the condition of 2N, 4N, 6N, 8N, 10N, Fig. 3 to Fig. 7 illustrates that this matrix material frictional abrasion surface is more smooth, ensures that it is have excellent tribological property in 2-10N interval in load.In addition, the wear rate of sample is by formula (1) ([11] M.Y.Niu, Q.L.Bi, J.Yang, W.M.Liu.TribologicalperformanceofaNi
3almatrixself-lubricatingcompositecoatingtestedfrom25to10 00 DEG C of .SurfCoatTechnol, 2012,206(19-20): 3938-3943.) calculate:
(1)
In formula: V represents wear volume, P represents load, and L represents sliding distance, ρ
wrepresent density of material, M
wrepresent 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 graphene-containing titanium obtained by the embodiment of the present invention, and Fig. 8 illustrates that the frictional coefficient of this matrix material under load is 2N condition and wear rate are respectively 0.38 and 1.45 × 10
-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 shows outstanding tribological property.
embodiment 2:
1) with Ti powder, Al powder for matrix material, Graphene powder is solid lubricant and wild phase, mole intermetallic compound TiAl matrix presintering powder is matched well by Ti:Al=1:1.3, take 5.771 grams of Ti powder, 4.229 grams of Al powder, amount to 10g, then add 0.30 gram of Graphene powder in above-mentioned mixed powder, obtain preparing burden (admixtion);
2) above-mentioned batching and steel ball are placed in Stainless Steel Vacuum ball grinder, wet-milling 5 hours on planetary ball mill under rough vacuum condition; Wet grinding media is alcohol; Wherein: drum's speed of rotation is 300 revs/min, ball material mass ratio is 10:1, vacuum tightness 16Pa;
3) ball milling ball is sieved cleaning after obtain mixed slurry by 300 order stainless steel sieve cleaning after, obtain mixing suspension solution, after mixing suspension solution filters and removes filtrate, (vacuum tightness is 0.016MPa in vacuum-drying, temperature is 65 DEG C, time is 6 hours), obtain the mixed powder that pre-treatment is good;
4) dried powder is placed in the graphite grinding tool that interior diameter is 20mm, then carries out discharge plasma sintering under vacuum condition.Wherein sintering temperature is 980 DEG C, temperature rise rate is 120 DEG C/min, sintering pressure is 40MPa, soaking time 6min, vacuum tightness is 1 × 10
-1pa, prepares the aluminium base self-lubricating composite of graphene-containing titanium.
The hardness adopting the aluminium base self-lubricating composite of graphene-containing titanium prepared by Vickers' hardness instrument testing example 2 is HV
1685.8, testing the actual density of this matrix material and theoretical density according to drainage, to calculate relative density be 97.3%.Fig. 9 is that embodiment 2 obtains the aluminium base self-lubricating composite of graphene-containing titanium dynamic friction coefficient curve under load is 10N condition, and 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 calculating according to formula (1) this matrix material that embodiment 2 is prepared is 2.74 × 10
-4mm
3/ (Nm).Therefore the aluminium base self-lubricating composite of graphene-containing titanium shows outstanding tribological property.The electronic probe photo of graphene-containing titanium aluminium base self-lubricating composite load be 10N part under the frictional abrasion surface of Figure 10 obtained by embodiment 2, Figure 10 illustrates that this matrix material frictional abrasion surface is more smooth, ensures that it has excellent tribological property.
embodiment 3:
1) with Ti powder, Al powder for matrix material, Graphene powder is solid lubricant and wild phase, mole intermetallic compound TiAl matrix presintering powder is matched well by Ti:Al=1:1.5, take 5.418 grams of Ti powder, 4.582 grams of Al powder, amount to 10g, then add 0.45 gram of Graphene powder in above-mentioned mixed powder, obtain preparing burden (admixtion);
2) above-mentioned batching and steel ball are placed in vacuum steel ball grinder, wet-milling 6 hours on planetary ball mill under rough vacuum condition; Wet grinding media is alcohol; Wherein: drum's speed of rotation is 400 revs/min, ball material mass ratio is 10:1, vacuum tightness 20Pa;
3) mixed slurry of steel ball will be contained after ball milling by after 300 order stainless steel sieve cleanings, obtain mixing suspension solution, after mixing suspension solution filters and removes filtrate, (vacuum tightness is 0.021MPa in vacuum-drying, temperature is 70 DEG C, time is 5 hours), obtain the mixed powder that pre-treatment is good;
4) dried powder is placed in the graphite grinding tool that interior diameter is 20mm, then carries out discharge plasma sintering (SPS) under vacuum condition.Wherein sintering temperature is 1000 DEG C, temperature rise rate is 150 DEG C/min, sintering pressure is 50MPa, soaking time 8min, vacuum tightness is 8 × 10
-2pa, prepares the aluminium base self-lubricating composite of graphene-containing titanium.
The hardness adopting the aluminium base self-lubricating composite of graphene-containing titanium prepared by Vickers' hardness instrument testing example 3 is HV
1723.5, testing the actual density of this matrix material and theoretical density according to drainage, to calculate relative density be 97.6%.Figure 11 is that embodiment 3 obtains the aluminium base self-lubricating composite of graphene-containing titanium dynamic friction coefficient curve under load is 10N condition, and 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 calculating according to formula (1) this matrix material that embodiment 3 is prepared is 3.01 × 10
-4mm
3/ (Nm).Therefore the aluminium base self-lubricating composite of titanium shows outstanding tribological property.The electronic probe photo of graphene-containing titanium aluminium base self-lubricating composite load be 10N condition under the frictional abrasion surface of Figure 12 obtained by embodiment 3, Figure 12 illustrates that this matrix material frictional abrasion surface is smooth, ensures that it has excellent tribological property.
Each raw material cited by the present invention can realize the present invention, and the bound value of each raw material, interval value can realize the present invention, bound value and the interval value of processing parameter of the present invention (as temperature, time, vacuum tightness etc.) can realize the present invention, do not enumerate embodiment at this.
Claims (7)
1. a preparation method for the aluminium base self-lubricating composite of graphene-containing titanium, is characterized in that it comprises the steps:
1) by mol ratio=1:1 ~ 1.5 of Ti:Al, Ti powder, Al powder is chosen; By the 1.5-4.5wt.% that the add-on of Graphene powder is Ti powder, Al powder total mass, choose Graphene powder;
By Ti powder, the mixing of Al powder, obtain mixed powder, then add Graphene powder in described mixed powder, prepared burden;
2) above-mentioned batching is carried out wet-milling, sieve, obtain after cleaning mixing suspension solution;
3), after above-mentioned mixing suspension solution being filtered removal filtrate, vacuum-drying, obtains the mixed powder that pre-treatment is good;
4) mixed powder that pre-treatment is good is placed in graphite jig, then discharge plasma sintering method is taked under vacuum condition, namely sintering obtains the aluminium base self-lubricating composite of described graphene-containing titanium, and sintering temperature is 950-1000 DEG C, temperature rise rate is 100-150 DEG C/min, sintering pressure is 30-50MPa, vacuum tightness is 1 × 10
-2-1 × 10
-1pa, soaking time are 4-8min.
2. the preparation method of the aluminium base self-lubricating composite of graphene-containing titanium as claimed in claim 1, it is characterized in that, described step 2) in wet-milling step be that batching, alcohol and steel ball are placed in stainless-steel vacuum ball grinder, wet-milling in ball mill, the wet-milling time is 4-6 hour.
3. the preparation method of the aluminium base self-lubricating composite of graphene-containing titanium as claimed in claim 2, is characterized in that, drum's speed of rotation is 200-400 rev/min, ball material mass ratio is 10:1.
4. the preparation method of the aluminium base self-lubricating composite of graphene-containing titanium as claimed in claim 2, it is characterized in that, in described stainless-steel vacuum ball grinder, vacuum tightness is 12-20Pa.
5. the preparation method of the aluminium base self-lubricating composite of graphene-containing titanium as claimed in claim 1, is characterized in that, described step 2) in sifting step be by 300 order stainless steel sieve.
6. the preparation method of the aluminium base self-lubricating composite of graphene-containing titanium as claimed in claim 1, it is characterized in that, the vacuum drying vacuum tightness described in described step 3) is 0.011-0.021MPa, and drying temperature is 60-70 DEG C, and time of drying is 5-7 hour.
7. the preparation method of the aluminium base self-lubricating composite of graphene-containing titanium as claimed in claim 1, it is characterized in that, the interior diameter of the graphite jig in described step 4) is 20mm.
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