CN104232961A - High-strength high-hardness Cu-Cr composite material as well as preparation method and application thereof - Google Patents
High-strength high-hardness Cu-Cr composite material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of metal-matrix composite material preparation and discloses a high-strength high-hardness Cu-Cr composite material as well as a preparation method and application thereof. The preparation method comprises the following steps: performing pre-ball-milling treatment on one of Cu powder and Cr powder used as raw materials in a high-energy planetary ball mill, adding another raw material and a grinding aid, mixing, performing ball-milling, drying the ball-milled powder, and performing sintering densification treatment in a discharge plasma sintering furnace to obtain the high-strength high-hardness Cu-Cr composite material. According to the preparation method, the high-strength high-hardness Cu-Cr composite material with high powder yield is obtained with relatively low enhanced-phase additive amount (the Cr content can be reduced to be 8at.%), is excellent in mechanical property, is kept good in plasticity, has the hardness of 250-330Hv, the compressive yield strength of 900-1,000MPa and the compression rate of 8%-25%, and has wide application prospects in the field of structures.
Description
Technical field
The invention belongs to metal-base composites preparing technical field, particularly hard Cu-Cr matrix material of the high-strength height of one and its preparation method and application.
Background technology
Metal-base composites, owing to comparing respective metal body material, has the plasticity that higher mechanical property keeps certain simultaneously, can be widely used in frictional wear, plastic making processing and other construction applications as structured material.In recent years, researchist prepares metal-base composites and expands large quantifier elimination at interpolation strengthening phase to improve metal material mechanics aspect of performance.Wherein, the wild phase added comprises the mixture of pure metals, carbide, oxide compound, boride and different sorts strengthening phase, and the preparation method adopted has powder metallurgy, extrusion casting, rapid solidification, arc melting, liquid metal infiltration and laser processing etc.
In order to obtain higher mechanical property, when preparing metal-base composites, usually to take some measures, such as add the wild phase (size is less than 100nm) of nanoscale, and add wild phase (volume fraction the is greater than 10%) (ChaS.I. of high level, KimK.T., ArshadS.N., MoC.B., HongS.H., Advanced Materials, 2005, 17 (11), 1377-1381.) (DaoushW.M., LimB.K., MoC.B., NamD.H., HongS.H., Materials Science and Engineering:A, 2009, 513-514, 247-253.).Nanometer reinforcing phase has higher strengthening efficiency, but its preparation cost is high, is unfavorable for large-scale commercial production.And the wild phase adding high level is while raising production cost, plasticity and other physicalies of material also can be worsened.Thus selecting economical and practical starting material, add the wild phase of small amount and utilize simple method efficiently to prepare good mechanical performance and can scale operation and the metal-base composites that is effectively applied in real life simultaneously, be the problem that the present invention is intended to solve.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art with not enough, primary and foremost purpose of the present invention is the preparation method providing the hard Cu-Cr matrix material of a kind of high-strength height, and this preparation method's process is easy to realize, and is suitable for commercial scale production.
Another object of the present invention is the hard Cu-Cr matrix material of high-strength height providing aforesaid method to prepare.The Cu-Cr matrix material of gained has excellent mechanical property, keeps higher plasticity simultaneously.
Still a further object of the present invention is to provide the application of the hard Cu-Cr matrix material of above-mentioned high-strength height in construction applications.
Object of the present invention is realized by following proposal:
The preparation method of the hard Cu-Cr matrix material of a kind of high-strength height, comprise the following steps: Cu powder and Cr powder are as starting material, to wherein be placed in high-energy planetary formula ball mill and carry out pre-ball-milling processing by a kind of starting material, add another kind of starting material again and grinding aid carries out mixing and ball milling process, in discharge plasma sintering stove, carry out sintering densification process after powder drying after ball milling, obtain the hard Cu-Cr matrix material of high-strength height.
In described starting material, the content of Cr is 8 ~ 10% of total amount atomic percent, is preferably 8at.%.Only need add in the present invention be low to moderate 8at.% Cr as wild phase, the matrix material of the hard excellent in mechanical performance of high-strength height can be obtained, and due to add wild phase content low, the toughness that matrix material is good can be kept again, make the matrix material obtained be more widely applicable for various fields.
Described grinding aid is preferably dehydrated alcohol.The amount of grinding aid used is 70 ~ 90% of raw material quality.
Preferably, when selecting Cu powder to carry out pre-ball-milling processing, add grinding aid ball milling together.Preferably add the grinding aid of Cu opaque amount 70 ~ 90%, be more preferably 80wt%, and carry out subsequent disposal again carry out drying removing grinding aid after pre-ball milling after.
The time of described pre-ball-milling processing is preferably 15 ~ 25h.
The time of described mixing and ball milling process is preferably 90 ~ 110h.
Preferably, in above-mentioned preparation method, the diameter of ball milling abrading-ball used is respectively 15,10 and 6mm, and corresponding mass is than being 1:3:1, and ratio of grinding media to material is 10:1, and drum's speed of rotation is 226rpm.Ball grinder used and abrading-ball are preferably stainless steel.Pre-ball-milling processing of the present invention is identical with the processing parameter of mixing and ball milling process as mentioned above.
Preferably, the processing condition of described sintering densification process are sintering pressure is 30 ~ 40MPa, and sintering temperature is 650 ~ 800 DEG C, and soaking time is 6 ~ 10min.
In the invention described above preparation method process, described drying all preferred in vacuum drying oven dry 20 ~ 30h at 50 ~ 60 DEG C of temperature.
Preferably, the powder after described pre-ball-milling processing again drops in ball mill after can first carrying out above-mentioned drying again and carries out subsequent disposal with unclassified stores.
In order to realize the present invention better, the purity of raw materials Cu powder and Cr powder is all not less than 99%, and powder size is all not more than 75 μm.
In order to realize the present invention better, mechanical milling process preferably all carries out under protection of inert gas atmosphere, more preferably carries out under argon gas atmosphere protection.
Particularly, the preparation method of the hard Cu-Cr matrix material of high-strength height of the present invention, comprises the following steps:
Method one: take Cu powder (purity >=99%; powder size≤75 μm) and dehydrated alcohol grinding aid be placed in high-energy planetary formula ball mill; pre-ball-milling processing 15 ~ 25h under argon gas atmosphere protection; dry rear and Cr powder (purity >=99%; powder size≤75 μm) and the mixing of dehydrated alcohol grinding aid; add in high-energy planetary formula ball mill; and argon gas atmosphere protection under mixing and ball milling process 90 ~ 110h; obtain composite granule; in discharge plasma sintering stove, carry out sintering densification process after drying, obtain the hard Cu-Cr matrix material of high-strength height.
Wherein, ball grinder and Material quality of grinding balls are stainless steel, and ball radius used is respectively 15,10 and 6mm, and corresponding mass is than being 1:3:1, ratio of grinding media to material is 10:1, drum's speed of rotation is 226rpm, and dehydrated alcohol quality is 70 ~ 90%, Cr powder shared atomic percent in mixed powder of powder quality is 8%, described drying is dry 20 ~ 30h at 50 ~ 60 DEG C of temperature in vacuum drying oven all, sintering pressure is 30 ~ 40MPa, and sintering temperature is 650 ~ 800 DEG C, and soaking time is 6 ~ 10min.
Method two: take Cr powder (purity >=99%; powder size≤75 μm) be placed in high-energy planetary formula ball mill; pre-ball-milling processing 15 ~ 25h under argon gas atmosphere protection; then by the Cr powder of pre-ball milling and Cu powder (purity >=99%; powder size≤75 μm) and dehydrated alcohol grinding aid mixing after; add in high-energy planetary formula ball mill; mixing and ball milling process 90 ~ 110h under argon gas atmosphere protection; obtain composite granule; in discharge plasma sintering stove, carry out sintering densification process after drying, obtain the hard Cu-Cr matrix material of high-strength height.
Wherein, ball grinder and Material quality of grinding balls are stainless steel, and ball radius used is respectively 15,10 and 6mm, and corresponding mass is than being 1:3:1, ratio of grinding media to material is 10:1, drum's speed of rotation is 226rpm, and dehydrated alcohol quality is 70 ~ 90%, Cr powder shared atomic percent in mixed powder of powder quality is 8%, described drying is dry 20 ~ 30h at 50 ~ 60 DEG C of temperature in vacuum drying oven all, sintering pressure is 30 ~ 40MPa, and sintering temperature is 650 ~ 800 DEG C, and soaking time is 6 ~ 10min.
The high-strength height hard Cu-Cr matrix material purity that the invention described above method prepares is high, excellent in mechanical performance, keeps higher plasticity simultaneously, can be widely used in frictional wear, plastic making processing and other construction applications as structured material.
Preparation method of the present invention can prepare the matrix material that wild phase small and dispersed distributes, purity is high, and the utilization rate of raw materials of preparation method of the present invention is high, and technique is simple, easy to operate, can large-scale industrial production.
Mechanism of the present invention is:
The present invention is in conjunction with pure powder ball milling, mixed powder ball milling and discharge plasma sintering technique, this inventive method adopts cheap starting material, in conjunction with the pre-ball milling of pure powder, mixed powder ball milling and discharge plasma sintering technique, with lower wild phase addition, (Cr content can be low to moderate 8at.%, 8.14vol.%), namely obtain excellent in mechanical performance, keep the hard Cu-Cr matrix material of the high-strength height of good plasticity simultaneously.
The present invention, relative to prior art, has following advantage and beneficial effect:
1, a large amount of dehydrated alcohol is added in the inventive method preparation process as grinding aid; mixed powder is made to sentence wet-milling state; effectively slow down the reunion of powder in mechanical milling process and bonding phenomenon; and it is lower to the degree of powder pollution; in addition; compare dry grinding and only add the grinding aid of less content, wet-milling can also guarantee the powder obtaining high starch yield.
2, the present invention adopts high-energy-milling to prepare powder, and this technique to the impact several times of powder and grinding, makes powder experience repeatedly cold welding and fragmentation by abrading-ball, thus reaches the effect of refinement, Homogeneous phase mixing and alloying.High-energy ball milling is utilized first to carry out pre-ball-milling processing to wherein a kind of starting material powder, abrading-ball makes the defect concentrations such as the inner dislocation of powder increase to the continuous impact effect of powder, and promote the refinement of crystal grain, the hardening powder that grain-size is tiny can be obtained, in follow-up mixing and ball milling, be conducive to the powder obtaining less grain-size, realize wild phase small and dispersed simultaneously and be distributed in matrix, the better mechanical property of final acquisition.Adopt high-energy ball milling to prepare powder, do not need expensive equipment, technique is simple, easy and simple to handle, without the generation of waste water, waste gas and waste residue in preparation process, meets the requirement of environmental protection and energy saving.In addition, owing to have employed the vacuum tank of good airproof performance, pass into argon gas simultaneously and carry out atmosphere protection, thus effectively can prevent the oxidative phenomena of powder in mechanical milling process, thus guarantee powder process quality.
3, the present invention adopts discharge plasma sintering technique to carry out sintering densification process to composite granule, this technology is the gas of electric field clear powder resin particle surface oxide compound and the absorption utilizing applying pulse strong current to be formed, thus purification and activated material, and utilize strong current Short Time Heating powder to carry out densified sintering product at low pressures, high-quality sintered compact can be prepared with lower temperature and shorter time.Utilizing discharge plasma sintering process to sinter, be characterized in simple to operate, sintering temperature is low, heat-up rate is fast, sintering time is short, single-piece energy consumption is low, sintered compact density is high and crystal grain is tiny, is a kind of near-net-shape and Green synthesis technology.
4, the present invention adopts relatively inexpensive raw material to prepare metal-base composites, its excellent in mechanical performance, hardness reaches 250 ~ 330Hv, compression yield strength reaches 900 ~ 1000MPa, keep good plasticity simultaneously, rate of compression reaches 8 ~ 25%, and prepared matrix material is with a wide range of applications at construction applications.
Accompanying drawing explanation
Fig. 1 is the microstructure obtaining Cu-Cr matrix material in the embodiment of the present invention 1.
Fig. 2 is the microstructure (containing partial enlarged drawing) obtaining Cu-Cr matrix material in the embodiment of the present invention 2.
Fig. 3 is the microstructure sintering Cu-Cr matrix material in comparative example.
Fig. 4 is sample X ray diffracting spectrum in the embodiment of the present invention 1.
Fig. 5 is sample X ray diffracting spectrum in the embodiment of the present invention 2.
Fig. 6 is the room temperature stress under compression strain curve sintering Cu-Cr matrix material in the embodiment of the present invention 1 ~ 4 and comparative example, and wherein 1 ~ 4 corresponding embodiment 1 ~ 4,5 is comparative example.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
Step one: pre-ball milling Cu powder
Precise Cu powder (purity >=99%, powder size≤75 μm) 500g, dehydrated alcohol 400g; be placed in 4L stainless steel jar mill; and adding stainless steel abrading-ball, ratio of grinding media to material is 10:1, and ball radius is respectively 15,10 and 6mm; corresponding mass is than being 1:3:1; after ball grinder is sealed, first vacuumize, more logical argon gas; and repetitive operation twice continuously, mechanical milling process is in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 20h.After completing ball milling, shut down cooling ball grinding jar, and take out Cu powder, be placed in vacuum drying oven, vacuumize, set temperature is 50 DEG C, keeps 24h, obtains dry pre-ball-milling processing Cu powder.
Step 2: mixing and ball milling Cu powder and Cr powder
Precise pre-ball milling Cu powder 466.8g, Cr powder (purity >=99%, powder size≤75 μm) 33.2g; dehydrated alcohol 400g, is placed in 4L stainless steel jar mill, and adds stainless steel abrading-ball; ratio of grinding media to material is 10:1; ball radius is respectively 15,10 and 6mm, and corresponding mass ratio is 1:3:1, after being sealed by ball grinder; first vacuumize; logical argon gas again, and repetitive operation twice continuously, make mechanical milling process be in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 100h.After completing ball milling, shut down cooling ball grinding jar, and take out mixed powder, be placed in vacuum drying oven, vacuumize, set temperature is 50 DEG C, keeps 24h, obtains dry composite granule.
Step 3: sintered combined powder
Precise composite granule 16.7g is placed in the graphite jig that internal diameter is 20.4mm, wherein pads the thick graphite paper of one deck 0.2mm between powder and mould inner wall, so that the demoulding.Subsequently mould is put graphite insulation ring, and be placed in discharge plasma sintering stove, after vacuumizing 30min, start sintering.Temperature in 3min is set and rises to 100 DEG C, heat up with the speed of 100 DEG C/min subsequently, rise to 700 DEG C, then in 3min, temperature is risen to 750 DEG C, and being incubated 8min at such a temperature, omnidistance maintenance pressure is 30MPa, and after insulation 8min, stove is chilled to room temperature, and take out sample, obtain the hard Cu-Cr matrix material of high-strength height.
Embodiment 2
Step one: pre-ball milling Cr powder
Precise Cr powder (purity >=99%; powder size≤75 μm) 500g, be placed in 4L stainless steel jar mill, and add stainless steel abrading-ball; ratio of grinding media to material is 10:1; ball radius is respectively 15,10 and 6mm, and corresponding mass ratio is 1:3:1, after being sealed by ball grinder; first vacuumize; logical argon gas again, and repetitive operation twice continuously, make mechanical milling process be in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 20h.After completing ball milling, shut down cooling ball grinding jar, obtain pre-ball-milling processing Cr powder.
Step 2: mixing and ball milling Cu powder and Cr powder
Precise Cu powder (purity >=99%, powder size≤75 μm) 466.8g, pre-ball milling Cr powder 33.2g; dehydrated alcohol 400g, is placed in 4L stainless steel jar mill, and adds stainless steel abrading-ball; ratio of grinding media to material is 10:1; ball radius is respectively 15,10 and 6mm, and corresponding mass ratio is 1:3:1, after being sealed by ball grinder; first vacuumize; logical argon gas again, and repetitive operation twice continuously, make mechanical milling process be in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 100h.After completing ball milling, shut down cooling ball grinding jar, and take out mixed powder, be placed in vacuum drying oven, vacuumize, set temperature is 50 DEG C, keeps 24h, obtains dry composite granule.
Step 3: sintered combined powder
Precise composite granule 16.7g is placed in the graphite jig that internal diameter is 20.4mm, wherein pads the thick graphite paper of one deck 0.2mm between powder and mould inner wall, so that the demoulding.Subsequently mould is put graphite insulation ring, and be placed in discharge plasma sintering stove, after vacuumizing 30min, start sintering.Temperature in 3min is set and rises to 100 DEG C, heat up with the speed of 100 DEG C/min subsequently, rise to 700 DEG C, then in 3min, temperature is risen to 750 DEG C, and being incubated 8min at such a temperature, omnidistance maintenance pressure is 30MPa, and after insulation 8min, stove is chilled to room temperature, and take out sample, obtain the Cu-Cr matrix material that high-strength height is hard.
Embodiment 3
Step one: pre-ball milling Cr powder
Precise Cr powder (purity >=99%; powder size≤75 μm) 500g, be placed in 4L stainless steel jar mill, and add stainless steel abrading-ball; ratio of grinding media to material is 10:1; ball radius is respectively 15,10 and 6mm, and corresponding mass ratio is 1:3:1, after being sealed by ball grinder; first vacuumize; logical argon gas again, and repetitive operation twice continuously, make mechanical milling process be in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 20h.After completing ball milling, shut down cooling ball grinding jar, obtain pre-ball-milling processing Cr powder.
Step 2: mixing and ball milling Cu powder and Cr powder
Precise Cu powder (purity >=99%, powder size≤75 μm) 466.8g, pre-ball milling Cr powder 33.2g; dehydrated alcohol 400g, is placed in 4L stainless steel jar mill, and adds stainless steel abrading-ball; ratio of grinding media to material is 10:1; ball radius is respectively 15,10 and 6mm, and corresponding mass ratio is 1:3:1, after being sealed by ball grinder; first vacuumize; logical argon gas again, and repetitive operation twice continuously, make mechanical milling process be in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 100h.After completing ball milling, shut down cooling ball grinding jar, and take out mixed powder, be placed in vacuum drying oven, vacuumize, set temperature is 50 DEG C, keeps 24h, obtains dry composite granule.
Step 3: sintered combined powder
Precise composite granule 16.7g is placed in the graphite jig that internal diameter is 20.4mm, wherein pads the thick graphite paper of one deck 0.2mm between powder and mould inner wall, so that the demoulding.Subsequently mould is put graphite insulation ring, and be placed in discharge plasma sintering stove, after vacuumizing 30min, start sintering.Temperature in 3min is set and rises to 100 DEG C, heat up with the speed of 100 DEG C/min subsequently, rise to 600 DEG C, then in 3min, temperature is risen to 650 DEG C, and being incubated 8min at such a temperature, omnidistance maintenance pressure is 30MPa, and after insulation 8min, stove is chilled to room temperature, and take out sample, obtain the hard Cu-Cr matrix material of high-strength height.
Embodiment 4
Step one: pre-ball milling Cr powder
Precise Cr powder (purity >=99%; powder size≤75 μm) 500g, be placed in 4L stainless steel jar mill, and add stainless steel abrading-ball; ratio of grinding media to material is 10:1; ball radius is respectively 15,10 and 6mm, and corresponding mass ratio is 1:3:1, after being sealed by ball grinder; first vacuumize; logical argon gas again, and repetitive operation twice continuously, make mechanical milling process be in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 20h.After completing ball milling, shut down cooling ball grinding jar, obtain pre-ball-milling processing Cr powder.
Step 2: mixing and ball milling Cu powder and Cr powder
Precise Cu powder (purity >=99%, powder size≤75 μm) 466.8g, pre-ball milling Cr powder 33.2g; dehydrated alcohol 400g, is placed in 4L stainless steel jar mill, and adds stainless steel abrading-ball; ratio of grinding media to material is 10:1; ball radius is respectively 15,10 and 6mm, and corresponding mass ratio is 1:3:1, after being sealed by ball grinder; first vacuumize; logical argon gas again, and repetitive operation twice continuously, make mechanical milling process be in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 100h.After completing ball milling, shut down cooling ball grinding jar, and take out mixed powder, be placed in vacuum drying oven, vacuumize, set temperature is 50 DEG C, keeps 24h, obtains dry composite granule.
Step 3: sintered combined powder
Precise composite granule 16.7g is placed in the graphite jig that internal diameter is 20.4mm, wherein pads the thick graphite paper of one deck 0.2mm between powder and mould inner wall, so that the demoulding.Subsequently mould is put graphite insulation ring, and be placed in discharge plasma sintering stove, after vacuumizing 30min, start sintering.Temperature in 3min is set and rises to 60 DEG C, heat up with the speed of 100 DEG C/min subsequently, rise to 760 DEG C, then in 3min, temperature is risen to 800 DEG C, and being incubated 8min at such a temperature, omnidistance maintenance pressure is 40MPa, and after insulation 8min, stove is chilled to room temperature, and take out sample, obtain high hard high hard Cu-Cr matrix material.
Comparative example
Step one: mixing and ball milling Cu powder and Cr powder
Precise Cu powder (purity >=99%, powder size≤75 μm) 466.8g, Cr powder (purity >=99%; powder size≤75 μm) 33.2g, dehydrated alcohol 400g, be placed in 4L stainless steel jar mill; and adding stainless steel abrading-ball, ratio of grinding media to material is 10:1, and ball radius is respectively 15,10 and 6mm; corresponding mass is than being 1:3:1; after ball grinder is sealed, first vacuumize, more logical argon gas; and repetitive operation twice continuously, mechanical milling process is in argon atmosphere.Arranging drum's speed of rotation is 226rpm.In order to prevent temperature in mechanical milling process too high, arranging ball mill and rotating forward hesitation 30min after 30min, rotating backward 30min subsequently, so hocket, every ball milling 5h dead halt cooling, until ball milling 100h.After completing ball milling, shut down cooling ball grinding jar, and take out mixed powder, be placed in vacuum drying oven, vacuumize, set temperature is 50 DEG C, keeps 24h, obtains dry composite granule.
Step 2: sintered combined powder
Precise composite granule 16.7g is placed in the graphite jig that internal diameter is 20.4mm, wherein pads the thick graphite paper of one deck 0.2mm between powder and mould inner wall, so that the demoulding.Subsequently mould is put graphite insulation ring, and be placed in discharge plasma sintering stove, after vacuumizing 30min, start sintering.Arrange temperature in 3min and rise to 100 DEG C, heat up subsequently, rise to 700 DEG C with the speed of 100 DEG C/min, then in 3min, temperature is risen to 750 DEG C, and be incubated 8min at such a temperature, omnidistance maintenance pressure is 30MPa.After insulation 8min, stove is chilled to room temperature, and takes out sample, obtains Cu-Cr matrix material.
Following detection sign has been carried out to sample topography, phase and mechanical property that embodiment 1 ~ 4 and comparative example prepare:
(1) sample surface morphology: use scanning electron microscope to carry out morphology observation (see Fig. 1 ~ 3) to sintered sample surface, can find out that in the Cu-Cr matrix material that the present invention prepares, Cr wild phase Dispersed precipitate is in Cu matrix; And there is the Cr wild phase of large-size in the matrix material of comparative example in Cu matrix, and this wild phase skewness.
(2) sample facies analysis: adopt X-ray diffractometer to carry out phase composition sign (see Fig. 4,5) to sample, do not find to there is other assorted peaks, therefore prepared Cu-Cr matrix material purity is higher.
(3) mechanical property: adopt Vickers hardness tester to carry out hardness sign to sample, test force is 2.94N, and test result is the mean value of 10 different zones test values, and each test value deviation is all no more than 5% of mean value; Use compression testing machine to carry out room temperature compression testing to sintered sample, adopt wire cutting method to obtain the sample being of a size of Φ 3 × 4.5mm, compressive strain speed is 1 × 10
-3s
-1, obtain room temperature stress under compression strain curve (see Fig. 6).The mechanical property of measured sample is in table 1.From table 1, the hard Cu-Cr matrix material of the high-strength height that the present invention prepares has excellent mechanical property, keeps good plasticity simultaneously; And under identical sintering condition, the obvious composite property more of the present invention of composite materials property that comparative example does not prepare through pre-ball milling powder body is poor.
(4) flour extraction rate: to ball milling and dried powder weigh on electronic scales (pre-ball milling Cr powder for dry grinding, without the need to drying, take out from ball grinder after ball milling and directly weigh), the mass ratio of adding powder used in ball grinder after ball milling before the quality of powder and ball milling to is the flour extraction rate of this powder.For example 1, pre-ball milling Cu powder flour extraction rate is 96.1%, and after mixing and ball milling, flour extraction rate is 92.7%, for example 2 ~ 4, pre-grinding Cr powder flour extraction rate is 95.9%, and after mixing and ball milling, flour extraction rate is 93.1%, for comparative example, after mixing and ball milling, flour extraction rate is 92.1%.The dehydrated alcohol of visible employing high level carries out ball-milling processing, higher flour extraction rate can be obtained (for the pre-ball milling of Cr powder, because the hardness of Cr own is higher, compare Cu, not easily there is slimeball and wall sticking phenomenon, therefore carry out ball-milling processing without the need to adding grinding aid), as can be seen here, under this experiment condition, utilization rate of raw materials is higher.
The mechanical property parameters of table 1Cu-Cr matrix material
| Sample | Hardness (Hv) | Compression yield strength (MPa) | Rate of compression (%) |
| Example 1 | 303 | 934 | 21 |
| Example 2 | 327 | 970 | 13.7 |
| Example 3 | 257 | 926 | 8.7 |
| Example 4 | 303 | 947 | 11.8 |
| Comparative example | 246 | 757 | 34.1 |
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the preparation method of the hard Cu-Cr matrix material of high-strength height, it is characterized in that comprising the following steps: Cu powder and Cr powder are as starting material, to wherein be placed in high-energy planetary formula ball mill and carry out pre-ball-milling processing by a kind of starting material, add another kind of starting material again and grinding aid carries out mixing and ball milling process, in discharge plasma sintering stove, carry out sintering densification process after powder drying after ball milling, obtain the hard Cu-Cr matrix material of high-strength height.
2. the preparation method of the hard Cu-Cr matrix material of high-strength height according to claim 1, is characterized in that: in described starting material, and the content of Cr is 8 ~ 10% of total amount atomic percent.
3. the preparation method of the hard Cu-Cr matrix material of high-strength height according to claim 1, is characterized in that: in described ball milling, the diameter of abrading-ball used is respectively 15,10 and 6mm, and corresponding mass is than being 1:3:1, and ratio of grinding media to material is 10:1, and drum's speed of rotation is 226rpm.
4. the preparation method of the hard Cu-Cr matrix material of high-strength height according to claim 1, is characterized in that: described grinding aid is dehydrated alcohol.
5. the preparation method of the hard Cu-Cr matrix material of high-strength height according to claim 1, is characterized in that: the amount of grinding aid used is 70 ~ 90% of raw material quality.
6. the preparation method of the hard Cu-Cr matrix material of high-strength height according to claim 1, is characterized in that: the time of described pre-ball-milling processing is 15 ~ 25h; The time of described mixing and ball milling process is 90 ~ 110h.
7. the preparation method of the hard Cu-Cr matrix material of high-strength height according to claim 1, is characterized in that: the processing condition of described sintering densification process are sintering pressure is 30 ~ 40MPa, and sintering temperature is 650 ~ 800 DEG C, and soaking time is 6 ~ 10min; Described drying to refer in vacuum drying oven dry 20 ~ 30h at 50 ~ 60 DEG C of temperature.
8. the preparation method of the hard Cu-Cr matrix material of high-strength height according to claim 1, is characterized in that: when selecting Cu powder to carry out described pre-ball-milling processing, adds grinding aid ball milling together.
9. the hard Cu-Cr matrix material of high-strength height, is characterized in that the preparation method of the hard Cu-Cr matrix material of high-strength height according to any one of claim 1 ~ 8 obtains.
10. the application of the hard Cu-Cr matrix material of high-strength height according to claim 9 in construction applications.
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Cited By (4)
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| CN105945293A (en) * | 2016-04-26 | 2016-09-21 | 武汉大学 | High-hardness high-conductivity CuCr25 contact material and preparation method and application thereof |
| CN106591610A (en) * | 2015-10-16 | 2017-04-26 | 中南大学 | Method for preparation of high strength and high conductivity copper alloy by spark plasma sintering |
| CN107345280A (en) * | 2016-05-06 | 2017-11-14 | 华为技术有限公司 | A kind of method for preparing Cu alloy material, Cu alloy material and equipment |
| CN110282717A (en) * | 2019-07-03 | 2019-09-27 | 中国海洋大学 | A kind of method of mechanical ball mill activation zeroth order aluminium removal water pollutant |
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| CN106591610A (en) * | 2015-10-16 | 2017-04-26 | 中南大学 | Method for preparation of high strength and high conductivity copper alloy by spark plasma sintering |
| CN105945293A (en) * | 2016-04-26 | 2016-09-21 | 武汉大学 | High-hardness high-conductivity CuCr25 contact material and preparation method and application thereof |
| CN107345280A (en) * | 2016-05-06 | 2017-11-14 | 华为技术有限公司 | A kind of method for preparing Cu alloy material, Cu alloy material and equipment |
| CN110282717A (en) * | 2019-07-03 | 2019-09-27 | 中国海洋大学 | A kind of method of mechanical ball mill activation zeroth order aluminium removal water pollutant |
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| CN104232961B (en) | 2016-09-21 |
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