CN104018019A - ZrB2/Cu composite material preparation method - Google Patents

ZrB2/Cu composite material preparation method Download PDF

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Publication number
CN104018019A
CN104018019A CN201410221818.6A CN201410221818A CN104018019A CN 104018019 A CN104018019 A CN 104018019A CN 201410221818 A CN201410221818 A CN 201410221818A CN 104018019 A CN104018019 A CN 104018019A
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zrb
powder
zrb2
matrix material
nickel plating
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CN104018019B (en
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王海龙
尚伟
李剑
赵笑统
邵刚
范冰冰
张锐
许红亮
卢红霞
陈德良
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Zhengzhou University
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Zhengzhou University
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Abstract

The invention belongs to the technical field of inorganic composite material preparation, and concretely relates to a ZrB2/Cu composite material preparation method. The method comprises the steps of nickeling ZrB2powder, mixing and grinding, performing hot pressing and sintering. According to the invention, active element Ni and ZrB2 have good wetability, Ni and Cu can form good solid solution, a layer of Ni is plated on the surface of the ZrB2 through a chemical nickeling technology, so that interface combination of ZrB2 and Cu can be effectively improved, then a hot pressing sintering process is employed, ZrB2 and Cu after nickeling can be taken as the raw materials, and thereby the ZrB2/Cu composite material with high density can be prepared under low temperature. The prepared ZrB2/Cu composite material has excellent comprehensive property, while using in preparation of an electrode for EDM processing, the ZrB2/Cu composite material can effectively reduce the electrode loss and replacing frequency, so that the ZrB2/Cu composite material has good social and economic benefit.

Description

A kind of ZrB 2the preparation method of/Cu matrix material
Technical field
The invention belongs to inorganic composite materials preparing technical field, be specifically related to a kind of ZrB 2the preparation method of/Cu matrix material.
Background technology
Electrospark machining (Electrical Discharge Machining, be called for short EDM) be the physical process method of utilizing the galvanic action ablation electro-conductive material producing while being immersed in two interpolar impulsive discharge in working fluid, claim again electrodischarge machining(E.D.M.) or galvanic corrosion processing, because its unique processing mechanism has adapted to the needs of production development, thereby be developed rapidly.
In electrospark machining, the performance of tool-electrode material directly affects the EDM Performance of electrode, as processing speed, tool loss rate, workpiece surface quality etc.In prior art, Cu-base composites has high strength, electric-conductivity heat-conductivity high performance and good wear resistance and high temperature stability performance, be widely used in industries such as aerospace, electric apparatus, machinofacture, become one of study hotspot on Material Field.And institute's development research is at present mainly granule reinforced copper base composite material for the Cu-base composites of EDM electrode materials, it is by additional ceramic particle reinforced phase or spontaneous entering in fine copper matrix or copper alloy, obtains having concurrently the matrix material of high strength hardness, high-melting-point and the high-modulus performance of electrical and thermal conductivity performance that toughness that fine copper is good is moulding, high and enhanced granule.
ZrB 2it is a kind of hexagonal structure material, because covalent linkage, ionic linkage and metallic bond exist simultaneously, and possess a lot of premium propertiess: high-melting-point (3245 DEG C), high strength, high rigidity, good electrical and thermal conductivity performance and corrosion resistance etc., compound with Cu, can be in the situation that ensureing that EDM processing needs, give material high strength and high hardness and good wear resistance, as a kind of new E DM tool-electrode, can obviously reduce the tool loss in the course of processing.But in prior art, due to ZrB 2poor with the wettability of metal Cu, in sintering, both interfaces, in conjunction with poor, are difficult to reach the compactness extent of expectation, and material easily ruptures in both junctions, interface, thereby there is no a kind of ZrB preferably 2/the technology of preparing of Cu matrix material.
Summary of the invention
The object of the present invention is to provide a kind of ZrB 2the preparation method of/Cu matrix material, prepared ZrB 2/ Cu matrix material can be used as the candidate material application of EDM electrode materials, thereby it is serious to overcome existing electrode materials loss, needs the problem of often changing.
The technical solution used in the present invention is as follows:
A kind of ZrB 2the preparation method of/Cu matrix material, comprises the following steps:
(1) ZrB 2powder Nickel Plating Treatment: get ZrB 2powder, carries out pre-treatment according to the order of pickling, sensitization, activation, then carries out chemical nickel plating; ZrB after Nickel Plating Treatment 2powder is dry, for subsequent use under vacuum;
Described pickling adopts the HCl solution-treated that volume fraction is 37%;
Described sensitization adopts SnCl 2-HCl solution-treated, wherein SnCl 22H 2o concentration is 0.1 mol/L, and the addition of HCl is 30 ml/L;
It is the silver ammino solution processing of 0.02 mol/L that described activation adopts concentration;
In described chemical nickel plating plating solution used, taking nickel sulfate hexahydrate as main salt, sodium borohydride is as reductive agent, quadrol is complexing agent, and lead ion is stablizer; Wherein NiSO 46H 2o concentration is 15 g/L, NaBH 4concentration is 2 g/L, and quadrol concentration is 100 ml/L, Pb (NO 3) 2concentration is 10 mg/L.
Described chemical nickel plating is by ZrB 2powder is placed in chemical plating fluid, drips NaOH solution and regulates pH value>=10, is heated to more than 80 DEG C under alkaline environment, keeps 60 min, carries out nickel plating;
(2) mixed grinding: by the ZrB after Nickel Plating Treatment in step (1) 2powder and Cu powder proportionally, mix, and grind, dry;
Described ZrB 2powder and Cu powder are counted by volume, and the volume ratio of the interpolation of Cu powder is 50 ~ 70%;
Described grinding adopts ball mill grinding, adds zirconium oxide balls and dehydrated alcohol so that grind evenly when grinding, and after grinding, material adopts rotary evaporation mode to be dried;
(3) hot pressed sintering: step (2) material is incubated to 10 ~ 60 min under 700 ~ 1000 DEG C, 10 ~ 40 MPa pressure, 50 ~ 150 DEG C/min of sintering rate, hot pressed sintering, is prepared into ZrB 2/ Cu matrix material;
Described sintering carries out under vacuum.
The present invention utilizes active element Ni and ZrB 2have wettability well, simultaneously Ni can form with Cu the feature of good sosoloid, first by nickel chemical plating technology at ZrB 2powder surface plates layer of Ni, thereby effectively improves ZrB 2interface combination with Cu, adopts hot-pressing sintering technique afterwards, with the ZrB after nickel plating 2with Cu powder be raw material, at lower temperature, prepare the ZrB of high-compactness 2/cu matrix material.Detect the ZrB that adopts this method to prepare at 900 DEG C through actual 2/ Cu matrix material, with containing 60% Cu(volume content) ZrB 2/ Cu sample is example, its flexural strength can reach 452 MPa, hardness can reach 5.6 GPa, thermal conductivity is 251 W/ (mK), and resistivity is 2.8 μ Ω cm, in end face frictional wear experiment, before and after wearing and tearing, quality loss is lower, frictional coefficient is in 0.05 left and right, and wear surface is wear characteristic of adhesion, thereby high comprehensive performance.
In general, ZrB provided by the present invention 2the preparation method of/Cu matrix material, has solved second-phase ZrB preferably 2problem with being combined in the interface of body material Cu, makes ZrB 2be combined better with matrix Cu, improved the structure of material, improved the performance of material; Prepare material temperature required lower simultaneously, be easy to realize; Prepared ZrB 2/ Cu composite material combination property is good, while preparation, can effectively reduce loss and the replacement frequency of electrode, thereby have good social and economic effects for EDM processing with electrode.
Brief description of the drawings
Fig. 1 is ZrB in the present invention 2sEM figure before and after powder electroless nickel, before wherein a is nickel plating, after b is nickel plating;
Fig. 2 is embodiment 2 sintered sample ZrB 2/the section SEM figure of Cu matrix material;
Fig. 3 is embodiment 2 sintered sample ZrB 2the wear surface SEM figure of/Cu matrix material.
Embodiment
Below in conjunction with embodiment the present invention will be further explained explanation so that those skilled in the art can implement the present invention better.
embodiment 1
ZrB 2the preparation method of/Cu matrix material, comprises the following steps:
(1) ZrB 2powder Nickel Plating Treatment: get ZrB 2powder, carries out pre-treatment according to the order of pickling, sensitization, activation, then carries out chemical nickel plating; ZrB after Nickel Plating Treatment 2powder is dry, for subsequent use under vacuum;
Described pickling adopts HCl to process, by ZrB 2it is 37% HCl solution that powder is placed in volume fraction, and stirring at low speed 30 minutes, carries out pickling; Powder after pickling is placed in dehydrated alcohol ultrasonic cleaning 10 minutes, then vacuum-drying 4 hours;
Described sensitization adopts SnCl 2solution-treated, specifically refers to pickling, dried ZrB 2powder is placed in SnCl 2in-HCl solution, stirring at low speed is done sensitization processing for 30 minutes; Described sensitization SnCl 2snCl in-HCl solution-treated 22H 2o concentration is 0.1 mol/L, and the addition of HCl is 30 ml/L;
Described activation adopts silver ammino solution processing, specifically refers to sensitization is processed to rear ZrB 2powder cleaning is to neutral, and the concentration that is then placed in fresh configuration is that the silver ammino solution of 0.02 mol/L carries out activation treatment, and soak time is 45 minutes, and after processing, vacuum powder is dry;
In described chemical nickel plating plating solution used, taking nickel sulfate hexahydrate as main salt, sodium borohydride is as reductive agent, quadrol is complexing agent, and lead ion is stablizer; Wherein NiSO 46H 2o concentration is 15 g/L, NaBH 4concentration is 1 g/L, and quadrol concentration is 100 ml/L, Pb (NO 3) 2concentration is 10 mg/L;
Described chemical nickel plating is by ZrB 2powder is placed in chemical plating fluid, is heated to 80 DEG C under alkaline environment, drips NaOH solution and regulates pH value>=10, is heated to 80 DEG C under alkaline environment, keeps 60 min, carries out nickel plating;
(2) mixed grinding: by the ZrB after Nickel Plating Treatment in step (1) 2powder and Cu powder proportionally, mix, and grind, dry;
ZrB after nickel plating in material 2mix with Cu, the volume fraction of Cu is 50%, wherein ZrB after nickel plating 2grain weight amount is 25g, and Cu powder is 35g;
Described grinding adopts ball mill grinding, adds zirconium oxide balls and dehydrated alcohol so that grind evenly when grinding, and after grinding, material adopts rotary evaporation mode to be dried;
(3) hot pressed sintering: take the 3.3g material mixing in step (2), pack into and be of a size of 32 × 4.5 × 3 mm 3graphite grinding tool in carry out hot pressed sintering under vacuum atmosphere, pressure 10 MPa, are incubated 10 mins after rising to 900 DEG C with the temperature rise rate of 100 DEG C/min, obtain ZrB after naturally cooling 2/ Cu matrix material.
In preparation process, to ZrB 2before and after powder chemical nickel plating, carry out electron-microscope scanning, its SEM schemes as shown in Figure 1, as can be seen from Figure 1, and ZrB before chemical nickel plating 2powder surface is very smooth, after nickel plating, and ZrB 2powder surface has superscribed Ni coating equably.The ZrB that the present embodiment is prepared 2/ Cu matrix material, its hardness after measured, can reach 5.8 GPa.
embodiment 2
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, only ZrB in set-up procedure (2) 2with the volume ratio of Cu, the volume fraction of Cu is 60% to be, i.e. ZrB after nickel plating 2grain weight amount is 20g, and Cu powder is 40g; When the middle hot pressed sintering of set-up procedure (3), pressure is 20 MPa, and sintering temperature is 900 DEG C, and temperature rise rate is 100 DEG C/min, and soaking time is 30min.
Prepared ZrB 2the section SEM of/Cu matrix material schemes as shown in Figure 2, and as can be seen from the figure material sample compact structure, presents the fracture model that ductile rupture and brittle rupture combine.Fig. 3 is the ZrB of sintering 2the wear surface SEM figure of/Cu composite sample, can find out that sample surfaces presents bed separation, the feature of adhesive wear, and surface has slight groove to occur.
embodiment 3
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, only ZrB in set-up procedure (2) 2with the volume ratio of Cu, the volume fraction of Cu is 70%, i.e. ZrB after nickel plating 2grain weight amount is 15g, and Cu powder is 50g; When the middle hot pressed sintering of set-up procedure (3), pressure is 30 MPa, and sintering temperature is 900 DEG C, and temperature rise rate is 100 DEG C/min, and soaking time is 45min.
By ZrB prepared the present embodiment 2/ Cu matrix material carries out performance measurement, and its flexural strength is 475 MPa, and thermal diffusivity is 0.7781 m 2s, thermal conductivity is 270 W/ (mK), and resistivity is 2.1 μ Ω cm, and specific conductivity is 0.48 × 106 S/cm.
embodiment 4
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, and when the middle hot pressed sintering of set-up procedure (3), pressure is 40 MPa, and sintering temperature is 700 DEG C, and temperature rise rate is 50 DEG C/min, and soaking time is 60min.
embodiment 5
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, only ZrB in set-up procedure (2) 2with the volume ratio of Cu, the volume fraction of Cu is 60%, i.e. ZrB after nickel plating 2grain weight amount is 20g, and Cu powder is 40g; When the middle hot pressed sintering of set-up procedure (3), pressure is 20 MPa, and sintering temperature is 800 DEG C, and temperature rise rate is 100 DEG C/min, and soaking time is 40min.
embodiment 6
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, only ZrB in set-up procedure (2) 2with the volume ratio of Cu, the volume fraction of Cu is 70%, i.e. ZrB after nickel plating 2grain weight amount is 15g, and Cu powder is 50g; When the middle hot pressed sintering of set-up procedure (3), pressure is 30 MPa, and sintering temperature is 850 DEG C, and soaking time is 30min.
embodiment 7
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, only ZrB in set-up procedure (2) 2with the volume ratio of Cu, the volume fraction of Cu is 60%, i.e. ZrB after nickel plating 2grain weight amount is 20g, and Cu powder is 40g; When the middle hot pressed sintering of set-up procedure (3), pressure is 20 MPa, and sintering temperature is 850 DEG C, and temperature rise rate is 150 DEG C/min, and soaking time is 15min.
embodiment 8
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, only ZrB in set-up procedure (2) 2with the volume ratio of Cu, the volume fraction of Cu is 60%, i.e. ZrB after nickel plating 2grain weight amount is 20g, and Cu powder is 40g; When the middle hot pressed sintering of set-up procedure (3), pressure is 30 MPa, and sintering temperature is 950 DEG C, and temperature rise rate is 100 DEG C/min, and soaking time is 15min.
embodiment 9
The present embodiment is prepared ZrB 2when/Cu matrix material, step is with embodiment 1, only ZrB in set-up procedure (2) 2with the volume ratio of Cu, the volume fraction of Cu is 60%, i.e. ZrB after nickel plating 2grain weight amount is 20g, and Cu powder is 40g; When the middle hot pressed sintering of set-up procedure (3), pressure is 20 MPa, and sintering temperature is 950 DEG C, and temperature rise rate is 150 DEG C/min, and soaking time is 10min.
Electroless plating method is in one of common method of ceramic powder surface clad or compound coating, its essence is a kind of autocatalytic redox reaction process, metal ion in plating solution is reduced into metallics and is deposited on powder surface under katalysis, thereby obtains certain thickness metal plating.Due to compared with electroplating technology, it is even that electroless plating has thickness of coating, compact structure, and the advantage such as voidage is low, simple to operate, and environmental pollution is little, thereby the present invention utilizes Ni and ZrB 2there is the feature of good wettability, by adopting electroless plating method first active element Ni to be coated in to ZrB 2powder surface, then utilizes Ni can form with Cu the characteristic of unlimited solid solution, further adopts hot-pressing sintering method to prepare ZrB 2/ Cu matrix material.Due to the introducing of Ni element in composite system, improve ZrB 2with the interface binding power of Cu, thereby prepared ZrB 2/ Cu matrix material has comparatively good material property, is suitable for preparing EDM processing electrode, can effectively reduce loss and the replacement frequency of electrode, thereby has good social and economic effects.
It should be noted that; above-described embodiment is all preferred embodiments of the present invention; but embodiments of the present invention are not subject to the restriction of above-mentioned specific embodiment; the change such as concrete material proportion, sintering temperature parameter of doing on above-described embodiment basis, all should think within the claimed scope of the present invention.

Claims (5)

1. a ZrB 2the preparation method of/Cu matrix material, is characterized in that, the method comprises the following steps:
(1) ZrB 2powder Nickel Plating Treatment
Get ZrB 2powder, carries out pre-treatment according to the order of pickling, sensitization, activation, then carries out chemical nickel plating; ZrB after Nickel Plating Treatment 2powder is dry, for subsequent use under vacuum;
Described chemical nickel plating is by ZrB 2powder is placed in chemical plating fluid, drips NaOH solution and regulates pH value>=10, is heated to more than 80 DEG C under alkaline environment, more than keeping 60 min, carries out nickel plating;
(2) mixed grinding
By the ZrB after Nickel Plating Treatment in step (1) 2powder mixes with Cu powder, and the volume ratio of Cu powder is 50 ~ 70%, after powder mixes, grinds, dry;
(3) hot pressed sintering
Step (2) material is warming up to 700 ~ 1000 DEG C with the sintering rate of 50 ~ 150 DEG C/min, under 10 ~ 40 MPa pressure, insulation 10 ~ 60 min, hot pressed sintering is prepared into ZrB 2/ Cu matrix material.
2. ZrB as claimed in claim 1 2the preparation method of/Cu matrix material, is characterized in that, in step (1), described pickling adopts the HCl that volume fraction is 37% to process; Described sensitization adopts SnCl 2-HCl solution-treated, wherein SnCl 22H 2o concentration is 0.1 mol/L, and the addition of HCl is 30 ml/L; It is the silver ammino solution processing of 0.02 mol/L that described activation adopts concentration.
3. ZrB as claimed in claim 1 2the preparation method of/Cu matrix material, is characterized in that, in step (1), described chemical plating fluid is made up of main salt nickel sulfate hexahydrate, borane reducing agent sodium hydride, complexing agent quadrol, stablizer lead ion; Wherein NiSO 46H 2o concentration is 15 g/L, NaBH 4concentration is 2 g/L, and quadrol concentration is 100 ml/L, Pb 2+concentration is 10 mg/L.
4. ZrB as claimed in claim 1 2the preparation method of/Cu matrix material, is characterized in that, described in step (2), grinds and adopts ball mill grinding, adds zirconium oxide balls and dehydrated alcohol so that grind evenly when grinding; After grinding, material adopts rotary evaporation mode to be dried.
5. ZrB as claimed in claim 1 2the preparation method of/Cu matrix material, is characterized in that, described in step (3), sintering carries out under vacuum.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106424713A (en) * 2016-10-13 2017-02-22 中南大学 Copper-carbon composite material and preparing method thereof
CN108103340A (en) * 2017-12-21 2018-06-01 湖北工业大学 A kind of multistep processes in-situ synthesis of boride titanium-zirconium boride complex phase ceramic enhancing Cu-base composites and its preparation method and application
CN108118177A (en) * 2017-12-21 2018-06-05 湖北工业大学 A kind of in-situ synthesis of boride zirconium enhancing Cu-base composites and its preparation method and application
CN110512109A (en) * 2019-09-20 2019-11-29 西安稀有金属材料研究院有限公司 A kind of preparation method of graphene enhancing titanium composite material
CN110670051A (en) * 2019-09-27 2020-01-10 郑州大学 Preparation method of YSZ/Cu ceramic-based metal composite powder suitable for thermal spraying
CN115947602A (en) * 2022-10-10 2023-04-11 中南大学 ZrB 2 Metal ceramic inert anode and preparation method and application thereof

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106424713A (en) * 2016-10-13 2017-02-22 中南大学 Copper-carbon composite material and preparing method thereof
CN106424713B (en) * 2016-10-13 2019-01-22 中南大学 A kind of copper carbon composite and preparation method thereof
CN108103340A (en) * 2017-12-21 2018-06-01 湖北工业大学 A kind of multistep processes in-situ synthesis of boride titanium-zirconium boride complex phase ceramic enhancing Cu-base composites and its preparation method and application
CN108118177A (en) * 2017-12-21 2018-06-05 湖北工业大学 A kind of in-situ synthesis of boride zirconium enhancing Cu-base composites and its preparation method and application
CN108103340B (en) * 2017-12-21 2019-08-06 湖北工业大学 A kind of multistep processes in-situ synthesis of boride titanium-zirconium boride complex phase ceramic enhancing Cu-base composites and its preparation method and application
CN110512109A (en) * 2019-09-20 2019-11-29 西安稀有金属材料研究院有限公司 A kind of preparation method of graphene enhancing titanium composite material
CN110512109B (en) * 2019-09-20 2021-09-03 西安稀有金属材料研究院有限公司 Preparation method of graphene reinforced titanium-based composite material
CN110670051A (en) * 2019-09-27 2020-01-10 郑州大学 Preparation method of YSZ/Cu ceramic-based metal composite powder suitable for thermal spraying
CN110670051B (en) * 2019-09-27 2022-04-01 郑州大学 Preparation method of YSZ/Cu ceramic-based metal composite powder suitable for thermal spraying
CN115947602A (en) * 2022-10-10 2023-04-11 中南大学 ZrB 2 Metal ceramic inert anode and preparation method and application thereof
CN115947602B (en) * 2022-10-10 2023-11-07 中南大学 ZrB (ZrB) 2 Metal ceramic-based inert anode and preparation method and application thereof

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