CN102206771A - Pantograph slide composite material and preparation method thereof - Google Patents
Pantograph slide composite material and preparation method thereof Download PDFInfo
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- CN102206771A CN102206771A CN2011101366986A CN201110136698A CN102206771A CN 102206771 A CN102206771 A CN 102206771A CN 2011101366986 A CN2011101366986 A CN 2011101366986A CN 201110136698 A CN201110136698 A CN 201110136698A CN 102206771 A CN102206771 A CN 102206771A
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Abstract
A pantograph slide composite material and a preparation method thereof relate to a copper-based pantograph slide composite material and a preparation method thereof. The invention solves the problems of poor interfacial wettability and low interfacial bonding strength between a ceramic reinforced phase and coppor in existing copper-based pantograph slide composite materials. The composite material of the invention is prepared by copper powder and ceramic particles, wherein the surface of the ceramic particle has a chemical copper plate layer. A mixed material is obtained by mixing the ceramic particles with chemical copper plate layers on the surfaces and the copper powder, and then the mixed material is processed by a hot-pressing sintering process or a combined process of hot-pressing sintering and hot extrusion. The Ti3AlC2 ceramic particles inside the composite material have uniform distribution, high structure density, good interfacial bonding performance, and good mechanical properties; the density is up to 99.86%-100.79%; the hardness is up to 92.3-93.3 HB; the tensile strength is up to 230-300 MPa; and the friction coefficient is 0.15-0.4.
Description
Technical field
The present invention relates to a kind of copper-base pantograph slide plate matrix material and preparation method thereof.
Background technology
The trend of world today's transportation by railroad development is electrification and high speed.Along with the arriving in China Express Railway epoch, the electric railway of China also enters a temporary new period, and this just more requires novel, the appearance of the pantograph pan of high request.Present high performance pantograph pan requires to have good self-lubricating, Wear-resistant, electroconductibility, impelling strength, ultimate compression strength, bending strength.And China starts late owing to the research and development pantograph, insufficient investment, and high performance pantograph pan is mainly by import.Now the pantograph pan that uses mainly is divided into and soaks metal slider, pure carbon slide plate, powder metallurgy slide plate.But problem is separately arranged all.Soak metal slider anti-impact force deficiency, be prone to the piece phenomenon, use limited; Pure carbon slide plate physical strength is low, and toughness is poor, meets hard spot and falls piece, and pantograph and catenary fault is big, and uneven wear is serious; The powder metallurgy slide plate uses at most, but because material is approaching, and lubricated being difficult for, bigger to the wear resistance ratio of osculatory.
Utilize matrix material to make slide plate and have great advantage, especially the slide plate of Cu-base composites.Fine copper has lot of advantages, such as good electroconductibility, thermal conductivity, erosion resistance, connectivity, workability and moderate cost.But fine copper also has shortcoming, and is low such as intensity, wears no resistance etc.And add Ti in the fine copper the inside
3AlC
2When suitably improving comprehensive physical such as Cu-base composites intensity, hardness, wear resistance, guarantee the material excellent conducting performance, even more important have an excellent self-lubricating property, strengthens body materials with other of copper base and compare and have huge advantage, makes Ti
3AlC
2On the manufacturing pantograph pan, huge development potentiality is arranged.
Domestic also someone has carried out similar research work at present, and subject matter concentrates on Ti
3AlC
2And the interface junction between the Cu is closed, because the two, Ti
3AlC
2Be pottery, Cu is a metal, so there is the problem of wetting problem in interface and interface bond strength.
Summary of the invention
It is poor to the objective of the invention is in order to solve in the existing copper base pantograph slide plate matrix material interface wet ability between the ceramic enhancement phase and copper, and the problem that interface bond strength is low the invention provides a kind of pantograph pan matrix material and preparation method thereof.
Pantograph pan matrix material of the present invention is that by volume per-cent is made by 60%～90% copper powder and 10%～40% ceramic particle, and wherein ceramic grain surface has chemical plating copper layer.Wherein said ceramic particle is Ti
3AlC
2Ceramic particle, Ti
3SiC
2Ceramic particle or Ti
2The AlC ceramic particle.
The preparation method of pantograph pan matrix material of the present invention realizes by following steps: one, utilize chemical-copper-plating process to obtain chemical plating copper layer at ceramic grain surface; Two, ceramic particle that will be after step 1 is handled and copper powder mix mixture, ceramic particle after wherein by volume per-cent is handled by 10%～40% step 1 in the mixture and 60%～90% copper powder are formed; Three, hot pressed sintering: with the mixture of step 2 hot pressed sintering 0.5～1h under 800～900 ℃, 40～160MPa condition, obtain ceramic particle/Cu pantograph pan matrix material, finish the pantograph pan matrix material system each.
Copper powder granularity of the present invention is 150～250 orders, and the ceramic particle granularity is 150～250 orders.Ceramic particle is Ti in the step 1
3AlC
2Ceramic particle, Ti
3SiC
2Ceramic particle or Ti
2The AlC ceramic particle.
The preparation method of pantograph pan matrix material of the present invention realizes by following steps: one, utilize chemical-copper-plating process to obtain chemical plating copper layer at ceramic grain surface; Two, ceramic particle that will be after step 1 is handled and copper powder mix mixture, ceramic particle after wherein by volume per-cent is handled by 10%～40% step 1 in the mixture and 60%～90% copper powder are formed; Three, hot pressed sintering: with the mixture of step 2 hot pressed sintering 0.5～1h under 800～900 ℃, 40～160MPa condition, matrix material; Four, will carry out hot extrusion through the matrix material that the step 3 hot pressed sintering gets, hot extrusion technique is: extrusion cup, grinding tool temperature are 400～450 ℃, insulation 1h, composite temperature is 760～850 ℃, insulation 1h, obtain ceramic particle/Cu pantograph pan matrix material, finish the preparation of pantograph pan matrix material.
Chemical-copper-plating process is realized by following steps in the preparation method's of the pantograph pan matrix material of the present invention step 1: one, ceramic particle is carried out successively hydrophilization, alligatoring, sensitization, activation and reduction and handle, finish pre-treatment; Two, electroless copper: under 50～80 ℃ water bath condition, to add in the chemical plating fluid through the pretreated ceramic particle of step 1, then under whipped state, electroless copper 15～25min, promptly obtain chemical plating at ceramic grain surface, wherein chemical plating fluid is the CuSO of 15～25g/L by concentration
45H
2The Na of O, 22～26g/L
2The C of EDTA, 15～18g/L
4H
4KNa4H
2The α，α′-Lian Biding of the formaldehyde of O, 13～17mL/L, the sodium hydroxide of 8～15g/L and 30～50mg/L is formed, and control chemical plating fluid pH value is 12.5～13.Pretreated concrete operations wherein are as follows: a, hydrophilization: ceramic particle is boiled 15～25min in concentration is the sodium hydroxide solution of 8%～15% (quality); B, alligatoring: the ceramic particle after the hydrophilization is boiled 15～25min in concentration is the salpeter solution of 8%～15% (quality); C, sensitization: will add in the sensitizing solution through the ceramic particle after the step b roughening treatment, stirring reaction 15～25min under 35～45 ℃ water bath condition staticly settles 5～20min more then, filters and cleans, ceramic particle, the wherein SnCl of consisting of of sensitizing solution: 20g/L after the sensitization
2Mixed solution with the HCl of 10mL/L; D, activation: will after the steps d sensitization, add in the distilled water by ceramic particle, make the suspension liquid that the ceramic particle mass concentration is 6g/L～8g/L, again suspension liquid is joined in the activation solution, stirring reaction 15～25min under 35～45 ℃ water bath condition then, staticly settle 5～20min again, filter and clean, must activate back ceramic particle, the wherein AgNO of consisting of of activation solution: 4g/L
3Solution; E, reduction: will activating the back ceramic particle, to add concentration be that 3～5mL/L formaldehyde solution or ortho phosphorous acid are received in the solution, and stirring reaction 15～25min under 35～45 ℃ water bath condition filters also and cleans, and must reduce back Ti
3AlC
2Ceramic particle.
Utilize ball milling to mix powder craft in the preparation method's of the pantograph matrix material of the present invention step 2 and mix, ball milling mixes the powder parameter and is: ball material mass ratio 4: 1,150～300 rev/mins of rotating speeds (rpm), ball milling time 5～10h.
At first be warming up to 350～450 ℃ in the step 3 of the present invention, insulation 20～40min, and then be warming up to 800～900 ℃, and being forced into 40～160MPa in the time of intensification, heat-insulation pressure keeping 0.5～1h cools to room temperature again with the furnace and gets final product.Wherein, temperature rise rate is controlled at 10～30 ℃/min.
The present invention at first by chemical-copper-plating process at the ceramic grain surface electroless copper, then the mixture of itself and copper powder is obtained density height, interfacial combined function is good and mechanical property is good pantograph pan matrix material after hot pressed sintering (perhaps through hot pressed sintering and hot extrusion) is handled.
The present invention has dense structure's degree height through the pantograph pan matrix material of hot pressed sintering Processing of Preparation, the characteristics that interfacial combined function is good, and inner Ti
3AlC
2Ceramic particle is evenly distributed, and density reaches 99.86%, and hardness reaches 93.3HB, and mechanical property is good, tensile strength reaches 230MPa, and frictional coefficient is than higher, along with the increase of pressure, the variation of frictional coefficient is not obvious, and when pressure was 12.5MPa, frictional coefficient is minimum to be about 0.4.Density through the pantograph pan matrix material of hot extrusion Processing of Preparation reaches 100.79% again, and hardness reaches 92.3HB, and mechanical property is better, tensile strength reaches 300MPa, along with the increase of pressure, frictional coefficient diminishes gradually, and frictional coefficient only was 0.15 when pressure was 25MPa.
Description of drawings
Fig. 1 is the Ti of embodiment 40
3AlC
2Ceramic particle/Cu pantograph pan matrix material scanning electron photomicrograph; Fig. 2 is Ti
3AlC
2Ceramic particle/Cu pantograph pan composite material tensile strength graphic representation, curve A is the composite material tensile strength curve of embodiment 42 among the figure, curve B is the composite material tensile strength curve of embodiment 40, and curve C is the composite material tensile strength curve of embodiment 41; Fig. 3 is the Ti of embodiment 40
3AlC
2Frictional wear-the time plot of ceramic particle/Cu pantograph pan matrix material, " ■-" is frictional wear-time curve under the 5MPa pressure among the figure, and " zero-" under the 12.5MPa pressure, and " △-" under the 17.5MPa pressure,
For under the 25MPa pressure; Fig. 4 is the Ti of embodiment 41
3AlC
2Frictional wear-the time plot of ceramic particle/Cu pantograph pan matrix material, " ■-" is frictional wear-time curve under the 5MPa pressure among the figure, and " zero-" under the 12.5MPa pressure, and " △-" under the 17.5MPa pressure,
For under the 25MPa pressure.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment is the pantograph pan matrix material, and the pantograph pan matrix material is that by volume per-cent is made by 60%～90% copper powder and 10%～40% ceramic particle, and wherein ceramic grain surface has chemical plating copper layer.
It is raw material that present embodiment adopts the ceramic particle that has chemical plating copper layer on the surface, and with dense structure's degree height of the mixed pantograph pan matrix material that gets of copper powder, interfacial combined function is good, and inner Ti
3AlC
2Ceramic particle is evenly distributed, and density reaches 99.86%～100.79%, and hardness reaches 92.3HB～93.3HB, and mechanical property is good, and tensile strength reaches 230～300MPa, and frictional coefficient is 0.15～0.4.
Than higher, along with the increase of pressure, the variation of frictional coefficient is not obvious, when pressure is 12.5MPa, frictional coefficient is minimum be about.Density through the pantograph pan matrix material of hot extrusion Processing of Preparation reaches 100.79% again, and hardness reaches 92.3HB, and mechanical property is better, tensile strength reaches 300Mpa, along with the increase of pressure, frictional coefficient diminishes gradually, and frictional coefficient only was 0.15 when pressure was 25MPa.
Embodiment two: what present embodiment and embodiment one were different is that described ceramic particle is Ti
3AlC
2Ceramic particle, Ti
3SiC
2Ceramic particle or Ti
2The AlC ceramic particle.Other parameter is identical with embodiment one.
Embodiment three: present embodiment is different with embodiment one or two is that the pantograph pan matrix material is that by volume per-cent is made by 70% copper powder and 30% ceramic particle.Other parameter is identical with embodiment one or two.
Embodiment four: present embodiment is different with embodiment one or two is that the pantograph pan matrix material is that by volume per-cent is made by 80% copper powder and 20% ceramic particle.Other parameter is identical with embodiment one or two.
Embodiment five: what present embodiment was different with one of embodiment one to four is that the copper powder granularity is 150～250 orders, and the ceramic particle granularity is 150～250 orders.Other parameter is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different with one of embodiment one to four is that the copper powder granularity is 200 orders, and the ceramic particle granularity is 200 orders.Other parameter is identical with one of embodiment one to four.
Embodiment seven: present embodiment is the preparation method of embodiment one described pantograph pan matrix material, and the preparation method of pantograph pan matrix material realizes by following steps: one, utilize chemical-copper-plating process to obtain chemical plating copper layer at ceramic grain surface; Two, ceramic particle that will be after step 1 is handled and copper powder mix mixture, ceramic particle after wherein by volume per-cent is handled by 10%～40% step 1 in the mixture and 60%～90% copper powder are formed; Three, hot pressed sintering: with the mixture of step 2 hot pressed sintering 0.5～1h under 800～900 ℃, 40～160MPa condition, obtain ceramic particle/Cu pantograph pan matrix material, finish the preparation of pantograph pan matrix material.
Preparation method's technology of present embodiment is simple, and cost is low.
Present embodiment at first by chemical-copper-plating process at the ceramic grain surface electroless copper, obtain density height, interfacial combined function is good and mechanical property is good pantograph pan matrix material after then the mixture of itself and copper powder being handled hot pressed sintering successively.
Present embodiment has dense structure's degree height through the pantograph pan matrix material of hot pressed sintering Processing of Preparation, the characteristics that interfacial combined function is good, and inner Ti
3AlC
2Ceramic particle is evenly distributed, and density reaches 99.86%, and hardness reaches 93.3HB, and mechanical property is good, tensile strength reaches 230MPa, and frictional coefficient is than higher, along with the increase of pressure, the variation of frictional coefficient is not obvious, and when pressure was 12.5MPa, frictional coefficient is minimum to be about 0.4.
Embodiment eight: what present embodiment and embodiment seven were different is that chemical-copper-plating process is realized by following steps in the step 1: one, ceramic particle is carried out successively hydrophilization, alligatoring, sensitization, activation and reduction and handle, finish pre-treatment; Two, electroless copper: under 50～80 ℃ water bath condition, to add in the chemical plating fluid through the pretreated ceramic particle of step 1, then under whipped state, electroless copper 15～25min, promptly obtain chemical plating at ceramic grain surface, wherein chemical plating fluid is the CuSO of 15～25g/L by concentration
45H
2The Na of O, 22～26g/L
2The C of EDTA, 15～18g/L
4H
4KNa4H
2The α，α′-Lian Biding of the formaldehyde of O, 13～17mL/L, the sodium hydroxide of 8～15g/L and 30～50mg/L is formed, and control chemical plating fluid pH value is 12.5～13.Other step and parameter are identical with embodiment seven.
Embodiment nine: what present embodiment and embodiment eight were different is that hydrophilicity-imparting treatment is as follows: ceramic particle is boiled 15～25min in concentration is the sodium hydroxide solution of 8%～15% (quality).Other step and parameter are identical with embodiment eight.
Embodiment ten: what present embodiment and embodiment eight were different is that roughening treatment is as follows: the ceramic particle after the hydrophilization is boiled 15～25min in concentration is the salpeter solution of 8%～15% (quality).Other step and parameter are identical with embodiment eight.
Embodiment 11: what present embodiment and embodiment eight were different is that sensitization is handled as follows: the ceramic particle after roughening treatment is added in the sensitizing solution, stirring reaction 15～25min under 35～45 ℃ water bath condition then, staticly settle 5～20min again, filter and clean, ceramic particle, the wherein SnCl of consisting of of sensitizing solution: 20g/L after the sensitization
2Mixed solution with the HCl of 10mL/L.Other step and parameter are identical with embodiment eight.
Embodiment 12: what present embodiment and embodiment eight were different is that activation treatment is as follows: will add in the distilled water by ceramic particle after sensitization, make the suspension liquid that the ceramic particle mass concentration is 6g/L～8g/L, again suspension liquid is joined in the activation solution, stirring reaction 15～25min under 35～45 ℃ water bath condition then, staticly settle 5～20min again, filter and clean, must activate back ceramic particle, the wherein AgNO of consisting of of activation solution: 4g/L
3Solution.Other step and parameter are identical with embodiment eight.
Embodiment 13: what present embodiment and embodiment eight were different is that reduction is handled as follows: will activate back ceramic particle adding concentration and be 3～5mL/L formaldehyde solution or ortho phosphorous acid and receive in the solution, stirring reaction 15～25min under 35～45 ℃ water bath condition, filter and clean reduction back Ti
3AlC
2Ceramic particle.Other step and parameter are identical with embodiment eight.
Embodiment 14: what present embodiment was different with one of embodiment seven to 13 is that ceramic particle is Ti in the step 1
3AlC
2Ceramic particle, Ti
3SiC
2Ceramic particle or Ti
2The AlC ceramic particle.Other step and parameter are identical with one of embodiment seven to 13.
Embodiment 15: present embodiment is different with one of embodiment seven to 14 is that the granularity of ceramic particle in the step 1 is 150～250 orders, and the granularity of copper powder is 150～250 orders in the step 2.Other step and parameter are identical with one of embodiment seven to 14.
Embodiment 16: present embodiment is different with one of embodiment seven to 14 is that the granularity of ceramic particle in the step 1 is 200 orders, and the granularity of copper powder is 200 orders in the step 2.Other step and parameter are identical with one of embodiment seven to 14.
Embodiment 17: present embodiment is different with one of embodiment seven to 16 is that ceramic particle after by volume per-cent is handled by 20% step 1 in the mixture in the step 2 and 80% copper powder are formed.Other step and parameter are identical with one of embodiment seven to 16.
Embodiment 18: present embodiment is different with one of embodiment seven to 16 is that ceramic particle after by volume per-cent is handled by 30% step 1 in the mixture in the step 2 and 70% copper powder are formed.Other step and parameter are identical with one of embodiment seven to 16.
Embodiment 19: what present embodiment was different with one of embodiment seven to 18 is to utilize ball milling to mix powder craft in the step 2 to mix, ball milling mixes the powder parameter: ball material mass ratio 4: 1,150～300 rev/mins of rotating speeds (rpm), ball milling time 5～10h.Other step and parameter are identical with one of embodiment seven to 18.
Embodiment 20: what present embodiment was different with one of embodiment seven to 19 is at first to be warming up to 350～450 ℃ in the step 3, insulation 20～40min, and then be warming up to 800～900 ℃, be forced into 40～160MPa when heating up, heat-insulation pressure keeping 0.5～1h cools to room temperature again with the furnace and gets final product.Other step and parameter are identical with one of embodiment seven to 19.
Embodiment 21: what present embodiment and embodiment 20 were different is that temperature rise rate is controlled at 10～30 ℃/min.Other step and parameter are identical with embodiment 20.
Embodiment 22: what present embodiment was different with embodiment 20 or 21 is to begin pressurization when being warming up to 700～780 ℃, is forced into 40～160MPa when being warming up to 800～900 ℃.Other step and parameter are identical with embodiment 20 or 21.
Embodiment 23: present embodiment is the preparation method as embodiment one described pantograph pan matrix material, and it is realized by following steps: one, utilize chemical-copper-plating process to obtain chemical plating copper layer at ceramic grain surface; Two, ceramic particle that will be after step 1 is handled and copper powder mix mixture, ceramic particle after wherein by volume per-cent is handled by 10%～40% step 1 in the mixture and 60%～90% copper powder are formed; Three, hot pressed sintering: with the mixture of step 2 hot pressed sintering 0.5～1h under 800～900 ℃, 40～160MPa condition, matrix material; Four, will carry out hot extrusion through the matrix material that the step 3 hot pressed sintering gets, hot extrusion technique is: extrusion cup, grinding tool temperature are 400～450 ℃, insulation 1h, composite temperature is 760～850 ℃, insulation 1h, obtain ceramic particle/Cu pantograph pan matrix material, finish the preparation of pantograph pan matrix material.
Present embodiment at first by chemical-copper-plating process at the ceramic grain surface electroless copper, then the mixture of itself and copper powder is obtained successively density height, interfacial combined function is good and mechanical property is good pantograph pan matrix material after hot pressed sintering and hot extrusion are handled.
Present embodiment has dense structure's degree height through the pantograph pan matrix material of hot pressed sintering and hot extrusion Processing of Preparation, the characteristics that interfacial combined function is good, and inner Ti
3AlC
2Ceramic particle is evenly distributed, and density reaches 100.79%, and hardness reaches 92.3HB, and mechanical property is better, and tensile strength reaches 300MPa, and along with the increase of pressure, frictional coefficient diminishes gradually, and frictional coefficient only was 0.15 when pressure was 25MPa.
Embodiment 24: what present embodiment and embodiment 23 were different is that chemical-copper-plating process is realized by following steps in the step 1: one, ceramic particle is carried out successively hydrophilization, alligatoring, sensitization, activation and reduction and handle, finish pre-treatment; Two, electroless copper: under 50～80 ℃ water bath condition, to add in the chemical plating fluid through the pretreated ceramic particle of step 1, then under whipped state, electroless copper 15～25min, promptly obtain chemical plating at ceramic grain surface, wherein chemical plating fluid is the CuSO of 15～25g/L by concentration
45H
2The Na of O, 22～26g/L
2The C of EDTA, 15～18g/L
4H
4KNa4H
2The α，α′-Lian Biding of the formaldehyde of O, 13～17mL/L, the sodium hydroxide of 8～15g/L and 30～50mg/L is formed, and control chemical plating fluid pH value is 12.5～13.Other step and parameter are identical with embodiment 23.
Embodiment 25: what present embodiment and embodiment 24 were different is that hydrophilicity-imparting treatment is as follows: ceramic particle is boiled 15～25min in concentration is the sodium hydroxide solution of 8%～15% (quality).Other step and parameter are identical with embodiment 24.
Embodiment 26: what present embodiment and embodiment 24 were different is that roughening treatment is as follows: the ceramic particle after the hydrophilization is boiled 15～25min in concentration is the salpeter solution of 8%～15% (quality).Other step and parameter are identical with embodiment 24.
Embodiment 27: what present embodiment and embodiment 24 were different is that sensitization is handled as follows: the ceramic particle after roughening treatment is added in the sensitizing solution, stirring reaction 15～25min under 35～45 ℃ water bath condition then, staticly settle 5～20min again, filter and clean, ceramic particle, the wherein SnCl of consisting of of sensitizing solution: 20g/L after the sensitization
2Mixed solution with the HCl of 10mL/L.Other step and parameter are identical with embodiment 24.
Embodiment 28: what present embodiment and embodiment 24 were different is that activation treatment is as follows: will add in the distilled water by ceramic particle after sensitization, make the suspension liquid that the ceramic particle mass concentration is 6g/L～8g/L, again suspension liquid is joined in the activation solution, stirring reaction 15～25min under 35～45 ℃ water bath condition then, staticly settle 5～20min again, filter and clean, must activate back ceramic particle, the wherein AgNO of consisting of of activation solution: 4g/L
3Solution.Other step and parameter are identical with embodiment 24.
Embodiment 29: what present embodiment and embodiment 24 were different is that reduction is handled as follows: will activate back ceramic particle adding concentration and be 3～5mL/L formaldehyde solution or ortho phosphorous acid and receive in the solution, stirring reaction 15～25min under 35～45 ℃ water bath condition, filter and clean reduction back Ti
3AlC
2Ceramic particle.Other step and parameter are identical with embodiment 24.
Embodiment 30: what present embodiment was different with one of embodiment 23 to 29 is that ceramic particle is Ti in the step 1
3AlC
2Ceramic particle, Ti
3SiC
2Ceramic particle or Ti
2The AlC ceramic particle.Other step and parameter are identical with one of embodiment 23 to 29.
The embodiment hentriaconta-: present embodiment is different with one of embodiment 23 to 30 is that the granularity of ceramic particle in the step 1 is 150～250 orders, and the granularity of copper powder is 150～250 orders in the step 2.Other step and parameter are identical with one of embodiment 23 to 30.
Embodiment 32: present embodiment is different with one of embodiment 23 to 30 is that the granularity of ceramic particle in the step 1 is 200 orders, and the granularity of copper powder is 200 orders in the step 2.Other step and parameter are identical with one of embodiment 23 to 30.
Embodiment 33: present embodiment is different with one of embodiment 23 to 32 is that ceramic particle after by volume per-cent is handled by 20% step 1 in the mixture in the step 2 and 80% copper powder are formed.Other step and parameter are identical with one of embodiment 23 to 32.
Embodiment 34: present embodiment is different with one of embodiment 23 to 32 is that ceramic particle after by volume per-cent is handled by 30% step 1 in the mixture in the step 2 and 70% copper powder are formed.Other step and parameter are identical with one of embodiment 23 to 32.
Embodiment 35: what present embodiment was different with one of embodiment 23 to 34 is to utilize ball milling to mix powder craft in the step 2 to mix, ball milling mixes the powder parameter: ball material mass ratio 4: 1,150～300 rev/mins of rotating speeds (rpm), ball milling time 5～10h.Other step and parameter are identical with one of embodiment 23 to 34.
Embodiment 36: what present embodiment was different with one of embodiment 23 to 35 is at first to be warming up to 350～450 ℃ in the step 3, insulation 20～40min, and then be warming up to 800～900 ℃, be forced into 40～160MPa when heating up, heat-insulation pressure keeping 0.5～1h cools to room temperature again with the furnace and gets final product.Other step and parameter are identical with one of embodiment 23 to 35.
Embodiment 37: what present embodiment and embodiment 36 were different is that temperature rise rate is controlled at 10～30 ℃/min.Other step and parameter are identical with embodiment 36.
Embodiment 38: what present embodiment was different with embodiment 36 or 37 is to begin pressurization when being warming up to 700～780 ℃, is forced into 40～160MPa when being warming up to 800～900 ℃.Other step and parameter are identical with embodiment 36 or 37.
Embodiment 39: what present embodiment was different with one of embodiment 23 to 38 is that hot extrusion technique is in the step 4: extrusion cup, grinding tool temperature are 420 ℃, insulation 1h, and composite temperature is 780 ℃, insulation 1h.Other step and parameter are identical with one of embodiment 23 to 38.
Embodiment 40: present embodiment is the preparation method of pantograph pan matrix material, and the preparation method of pantograph pan matrix material realizes by following steps:
One, utilize chemical-copper-plating process at Ti
3AlC
2Ceramic grain surface obtains chemical plating copper layer: (one) pre-treatment: a, hydrophilization: with Ti
3AlC
2Ceramic particle boils 20min in concentration is the sodium hydroxide solution of 10% (quality); B, alligatoring: with the Ti after the hydrophilization
3AlC
2Ceramic particle boils 20min in concentration is the salpeter solution of 10% (quality); C, sensitization: will be through the Ti after the step b roughening treatment
3AlC
2Ceramic particle adds in the sensitizing solution, and stirring reaction 20min under 40 ℃ water bath condition staticly settles 15min more then, filter also and clean, Ti after the sensitization
3AlC
2Ceramic particle, the wherein SnCl of consisting of of sensitizing solution: 20g/L
2Mixed solution with the HCl of 10mL/L; D, activation: will be after the steps d sensitization Ti
3AlC
2Ceramic particle adds in the distilled water, makes the suspension liquid that the ceramic particle mass concentration is 6g/L～8g/L, suspension liquid is joined in the activation solution again, stirring reaction 20min under 40 ℃ water bath condition then, staticly settle 20min again, filter and clean, must activate back Ti
3AlC
2Ceramic particle, the wherein AgNO of consisting of of activation solution: 4g/L
3Solution; E, reduction: will activate back Ti
3AlC
2It is that 3～5mL/L formaldehyde solution or ortho phosphorous acid are received in the solution that ceramic particle adds concentration, stirring reaction 15～25min under 35～45 ℃ water bath condition, filter reduction back Ti
3AlC
2Ceramic particle; (2) electroless copper: under 60 ℃ water bath condition, will be through the pretreated Ti of step ()
3AlC
2Ceramic particle adds in the chemical plating fluid, and under whipped state, electroless copper 20min promptly obtains chemical plating at ceramic grain surface then, and wherein chemical plating fluid is the CuSO of 20g/L by concentration
45H
2The Na of O, 24g/L
2The C of EDTA, 15g/L
4H
4KNa4H
2The α，α′-Lian Biding of 37% (quality) formaldehyde of O, 15mL/L, the sodium hydroxide of 8g/L and 30mg/L is formed, and control chemical plating fluid pH value is 12.5～13;
Two, Ti that will be after step 1 is handled
3AlC
2Ceramic particle and copper powder mix mixture, the Ti after wherein by volume per-cent is handled by 10% step 1 in the mixture
3AlC
2Ceramic particle and 90% copper powder are formed;
Three, hot pressed sintering: the mixture of step 2 is packed in the graphite jig, again graphite jig is put into vacuum hotpressing stove, being evacuated to vacuum tightness is 0.01～0.03Pa, be warming up to 350～450 ℃ then, insulation 20～40min, and then be warming up to 800 ℃, and be forced into 40MPa, hot pressed sintering 1h under 800 ℃, 40MPa condition obtains Ti
3AlC
2Ceramic particle/Cu pantograph pan matrix material is finished the preparation of pantograph pan matrix material.
Preparation method's technology of present embodiment is simple, and cost is low.Ti in the step 1
3AlC
2The granularity of ceramic particle is 200 orders, and the granularity of copper powder is 200 orders in the step 2.
The pantograph pan matrix material that present embodiment prepares be by volume per-cent by 90% copper powder and 10% Ti
3AlC
2Ceramic particle makes, and wherein ceramic grain surface has chemical plating copper layer.
Present embodiment adopts the Archimeds drainage to measure Ti
3AlC
2The density of ceramic particle/Cu pantograph pan matrix material, its calculation formula is:
Wherein, m
AirThe aerial quality of-sample (g);
m
CuThe quality (g) of-auxiliary copper wire
ρ
H2ODensity (the g/cm of distilled water under the-mensuration temperature
3).
With ρ and the Ti that calculates
3AlC
2The theoretical density ρ of the mixed powder of ceramic particle and Cu powder
TheoreticalRatio promptly obtain density.
The model that adopts Laizhou, Shandong test apparatus factory to produce is the Brinell tester tested for hardness of HB-3000B, and load is 250kg, and protecting the lotus time is 30s.
Adopt Instron-5569 electronic universal tester tested for tensile strength, the tensile strength curve that records is shown in curve B among Fig. 2.
The frictional wear machine that present embodiment adopts Harbin Institute of Technology advanced coating laboratory to make, the friction-wear test condition is: with the sweep velocity of 0.05m/s, under 5MPa, 12.5MPa, 17.5MPa and 25MPa pressure, carry out the friction and wear behavior test respectively, frictional wear-the time plot that records is shown in 3, " ■-" is frictional wear-time curve under the 5MPa pressure among the figure, " zero-" under the 12.5MPa pressure, " △-" under the 17.5MPa pressure
For under the 25MPa pressure.
Present embodiment is through the Ti of hot pressed sintering Processing of Preparation
3AlC
2The electron scanning micrograph of ceramic particle/Cu pantograph pan matrix material as shown in Figure 1, as seen from Figure 1, Ti
3AlC
2Ceramic particle/Cu pantograph pan composite inner Ti
3AlC
2Ceramic particle is evenly distributed, dense structure's degree height, and interfacial combined function is good.
The Ti of present embodiment
3AlC
2The density of ceramic particle/Cu pantograph pan matrix material reaches 98.28%, hardness reaches 84.9HB, mechanical property is good, tensile strength reaches 230MPa (among Fig. 2 shown in the curve B), frictional coefficient is than higher, and along with the increase of pressure, the variation of frictional coefficient is not obvious, when pressure was 12.5MPa, frictional coefficient is minimum to be about 0.4 (as shown in Figure 3).
Embodiment 41: present embodiment is the preparation method of pantograph pan matrix material, and the preparation method of pantograph pan matrix material realizes by following steps:
One, utilize chemical-copper-plating process at Ti
3AlC
2Ceramic grain surface obtains chemical plating copper layer: (one) pre-treatment: a, hydrophilization: with Ti
3AlC
2Ceramic particle boils 20min in concentration is the sodium hydroxide solution of 10% (quality); B, alligatoring: with the Ti after the hydrophilization
3AlC
2Ceramic particle boils 20min in concentration is the salpeter solution of 10% (quality); C, sensitization: will be through the Ti after the step b roughening treatment
3AlC
2Ceramic particle adds in the sensitizing solution, and stirring reaction 20min under 40 ℃ water bath condition staticly settles 15min more then, filter also and clean, Ti after the sensitization
3AlC
2Ceramic particle, the wherein SnCl of consisting of of sensitizing solution: 20g/L
2Mixed solution with the HCl of 10mL/L; D, activation: will be after the steps d sensitization Ti
3AlC
2Ceramic particle adds in the distilled water, makes the suspension liquid that the ceramic particle mass concentration is 6g/L～8g/L, suspension liquid is joined in the activation solution again, stirring reaction 20min under 40 ℃ water bath condition then, staticly settle 20min again, filter and clean, must activate back Ti
3AlC
2Ceramic particle, the wherein AgNO of consisting of of activation solution: 4g/L
3Solution; E, reduction: will activate back Ti
3AlC
2It is that 3～5mL/L formaldehyde solution or ortho phosphorous acid are received in the solution that ceramic particle adds concentration, stirring reaction 15～25min under 35～45 ℃ water bath condition, filter reduction back Ti
3AlC
2Ceramic particle; (2) electroless copper: under 60 ℃ water bath condition, will be through the pretreated Ti of step ()
3AlC
2Ceramic particle adds in the chemical plating fluid, and under whipped state, electroless copper 20min promptly obtains chemical plating at ceramic grain surface then, and wherein chemical plating fluid is the CuSO of 20g/L by concentration
45H
2The Na of O, 24g/L
2The C of EDTA, 15g/L
4H
4KNa4H
2The α，α′-Lian Biding of 37% (quality) formaldehyde of O, 15mL/L, the sodium hydroxide of 8g/L and 30mg/L is formed, and control chemical plating fluid pH value is 12.5～13;
Two, Ti that will be after step 1 is handled
3AlC
2Ceramic particle and copper powder mix mixture, the Ti after wherein by volume per-cent is handled by 10% step 1 in the mixture
3AlC
2Ceramic particle and 90% copper powder are formed;
Three, hot pressed sintering: the mixture of step 2 is packed in the graphite jig, again graphite jig is put into vacuum hotpressing stove, being evacuated to vacuum tightness is 0.01～0.03Pa, be warming up to 350～450 ℃ then, insulation 20～40min, and then be warming up to 800 ℃, and be forced into 40MPa, hot pressed sintering 1h under 800 ℃, 40MPa condition obtains matrix material;
Four, will carry out hot extrusion through the matrix material that the step 3 hot pressed sintering gets, hot extrusion technique is: extrusion cup, grinding tool temperature are 420 ℃, insulation 1h, and composite temperature is 780 ℃, insulation 1h obtains Ti
3AlC
2Ceramic particle/Cu pantograph pan matrix material is finished the preparation of pantograph pan matrix material.
Preparation method's technology of present embodiment is simple, and cost is low.Ti in the step 1
3AlC
2The granularity of ceramic particle is 200 orders, and the granularity of copper powder is 200 orders in the step 2.
The pantograph pan matrix material that present embodiment prepares be by volume per-cent by 90% copper powder and 10% Ti
3AlC
2Ceramic particle makes, and wherein ceramic grain surface has chemical plating copper layer.
Adopt with embodiment 40 in the identical means of testing put down in writing test, record present embodiment Ti
3AlC
2The density of ceramic particle/Cu pantograph pan matrix material reaches 100.79%, hardness reaches 92.3HB, mechanical property is better, tensile strength reaches 300MPa (among Fig. 2 shown in the curve C), increase along with pressure, frictional coefficient diminishes gradually, and frictional coefficient only was 0.15 (as shown in Figure 4) when pressure was 25MPa.Fig. 4 is the Ti of present embodiment
3AlC
2Frictional wear-the time plot of ceramic particle/Cu pantograph pan matrix material, " ■-" is frictional wear-time curve under the 5MPa pressure among the figure, and " zero-" under the 12.5MPa pressure, and " △-" under the 17.5MPa pressure,
For under the 25MPa pressure.
Embodiment 42: present embodiment be the contrast experiment, the preparation method of common pantograph pan matrix material realizes by following steps: one, with Ti
3AlC
2Ceramic particle and copper powder mix mixture, the Ti after wherein by volume per-cent is handled by 10% step 1 in the mixture
3AlC
2Ceramic particle and 90% copper powder are formed;
Two, hot pressed sintering:, obtain matrix material with the mixture of step 1 hot pressed sintering 1h under 800 ℃, 40MPa condition;
Three, will carry out hot extrusion through the matrix material that the step 2 hot pressed sintering gets, hot extrusion technique is: extrusion cup, grinding tool temperature are 420 ℃, and composite temperature is 780 ℃, is incubated 1h respectively, and pressure adopts 10 tons, obtains general T i
3AlC
2Ceramic particle/Cu pantograph pan matrix material is finished the preparation of pantograph pan matrix material.
Ti in the present embodiment step 1
3AlC
2The granularity of ceramic particle is 200 orders, and the granularity of copper powder is 200 orders.
Adopt with embodiment 40 in the identical means of testing put down in writing test, record present embodiment general T i
3AlC
2The density of ceramic particle/Cu pantograph pan matrix material reaches 95.86%, and hardness reaches 73.3HB, and mechanical property is better, and tensile strength reaches 162MPa (among Fig. 2 shown in the curve A).
As seen, the ceramic particle that adopts the surface to have chemical plating copper layer is a raw material, the Ti that the mixture of itself and copper powder is obtained through hot-pressing sintering technique (embodiment 40) and hot pressed sintering and hot extrusion combined process (embodiment 41)
3AlC
2The dense structure of ceramic particle/Cu pantograph pan matrix material, interfacial combined function is good.
Claims (10)
1. pantograph pan matrix material is characterized in that the pantograph pan matrix material is that by volume per-cent is made by 60%～90% copper powder and 10%～40% ceramic particle, and wherein ceramic grain surface has chemical plating copper layer.
2. a kind of pantograph pan matrix material according to claim 1 is characterized in that ceramic particle is Ti
3AlC
2Ceramic particle, Ti
3SiC
2Ceramic particle or Ti
2The AlC ceramic particle.
3. a kind of pantograph pan matrix material according to claim 1 is characterized in that the copper powder granularity is 150～250 orders, and the ceramic particle granularity is 150～250 orders.
4. the preparation method of pantograph pan matrix material as claimed in claim 1 is characterized in that the preparation method of pantograph pan matrix material realizes by following steps: one, utilize chemical-copper-plating process to obtain chemical plating copper layer at ceramic grain surface; Two, ceramic particle that will be after step 1 is handled and copper powder mix mixture, ceramic particle after wherein by volume per-cent is handled by 10%～40% step 1 in the mixture and 60%～90% copper powder are formed; Three, with the mixture of step 2 hot pressed sintering 0.5～1h under 800～900 ℃, 40～160MPa condition, obtain ceramic particle/Cu pantograph pan matrix material, finish the preparation of pantograph pan matrix material.
5. the preparation method of pantograph pan matrix material according to claim 4 is characterized in that ceramic particle is Ti in the step 1
3AlC
2Ceramic particle, Ti
3SiC
2Ceramic particle or Ti
2The AlC ceramic particle.
6. the preparation method of pantograph pan matrix material according to claim 4, it is characterized in that chemical-copper-plating process is realized by following steps in the step 1: one, ceramic particle is carried out successively hydrophilization, alligatoring, sensitization, activation and reduction and handle, finish pre-treatment; Two, electroless copper: under 50～80 ℃ water bath condition, to add in the chemical plating fluid through the pretreated ceramic particle of step 1, then under whipped state, electroless copper 15～25min, promptly obtain chemical plating at ceramic grain surface, wherein chemical plating fluid is the CuSO of 15～25g/L by concentration
45H
2The Na of O, 22～26g/L
2The C of EDTA, 15～18g/L
4H
4KNa4H
2The α，α′-Lian Biding of the formaldehyde of O, 13～17mL/L, the sodium hydroxide of 8～15g/L and 30～50mg/L is formed, and control chemical plating fluid pH value is 12.5～13.
7. the preparation method of pantograph pan matrix material according to claim 6 is characterized in that pretreated concrete operations are as follows: a, hydrophilization: ceramic particle is boiled 15～25min in concentration is the sodium hydroxide solution of 8%～15% (quality); B, alligatoring: the ceramic particle after the hydrophilization is boiled 15～25min in concentration is the salpeter solution of 8%～15% (quality); C, sensitization: will add in the sensitizing solution through the ceramic particle after the step b roughening treatment, stirring reaction 15～25min under 35～45 ℃ water bath condition staticly settles 5～20min more then, filters and cleans, ceramic particle, the wherein SnCl of consisting of of sensitizing solution: 20g/L after the sensitization
2Mixed solution with the HCl of 10mL/L; D, activation: will after the steps d sensitization, add in the distilled water by ceramic particle, make the suspension liquid that the ceramic particle mass concentration is 6g/L～8g/L, again suspension liquid is joined in the activation solution, stirring reaction 15～25min under 35～45 ℃ water bath condition then, staticly settle 5～20min again, filter and clean, must activate back ceramic particle, the wherein AgNO of consisting of of activation solution: 4g/L
3Solution; E, reduction: will activating the back ceramic particle, to add concentration be that 3～5mL/L formaldehyde solution or ortho phosphorous acid are received in the solution, stirring reaction 15～25min under 35～45 ℃ water bath condition, filter reduction back Ti
3AlC
2Ceramic particle.
8. according to the preparation method of claim 4,5,6 or 7 described pantograph pan matrix materials, it is characterized in that at first being warming up to 350～450 ℃ in the step 3, insulation 20～40min, and then be warming up to 800～900 ℃, be forced into 40～160MPa when heating up, heat-insulation pressure keeping 0.5～1h cools to room temperature again with the furnace and gets final product.Wherein, temperature rise rate is controlled at 10～30 ℃/min.
9. the preparation method of pantograph pan matrix material as claimed in claim 1 is characterized in that the preparation method of pantograph pan matrix material realizes by following steps: one, utilize chemical-copper-plating process to obtain chemical plating copper layer at ceramic grain surface; Two, ceramic particle that will be after step 1 is handled and copper powder mix mixture, ceramic particle after wherein by volume per-cent is handled by 10%～40% step 1 in the mixture and 60%～90% copper powder are formed; Three, hot pressed sintering: with the mixture of step 2 hot pressed sintering 0.5～1h under 800～900 ℃, 40～160MPa condition, matrix material; Four, will carry out hot extrusion through the matrix material that the step 3 hot pressed sintering gets, hot extrusion technique is: extrusion cup, grinding tool temperature are 400～450 ℃, insulation 1h, composite temperature is 760～850 ℃, insulation 1h, obtain ceramic particle/Cu pantograph pan matrix material, finish the preparation of pantograph pan matrix material.
10. the preparation method of pantograph pan matrix material according to claim 9 is characterized in that hot extrusion technique is in the step 4: extrusion cup, grinding tool temperature are 420 ℃, insulation 1h, and composite temperature is 780 ℃, insulation 1h.
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Application publication date: 20111005 |