CN107803507A - A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer - Google Patents

A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer Download PDF

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Publication number
CN107803507A
CN107803507A CN201710899004.1A CN201710899004A CN107803507A CN 107803507 A CN107803507 A CN 107803507A CN 201710899004 A CN201710899004 A CN 201710899004A CN 107803507 A CN107803507 A CN 107803507A
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pressurize
diamond compact
pressure value
passed
compressed air
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CN201710899004.1A
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CN107803507B (en
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花波波
陈强
张钲
王恒
李富玲
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Henan Yalong Diamond Products Ltd By Share Ltd
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Henan Yalong Diamond Products Ltd By Share Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/241Chemical after-treatment on the surface
    • B22F2003/244Leaching

Abstract

The invention discloses a kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, concretely comprise the following steps:Diamond compact is put into the closed container for filling acid solution system, is passed through compressed air, the 2h of pressurize 1, then it vacuumized, the 2h of pressurize 1;Compressed air, the 2h of pressurize 1 are passed through again, then it is vacuumized, the 2h of pressurize 1;..., pulse cycle successively, diamond compact is taken out after 20 30h and is rinsed well with water.Beneficial effects of the present invention are:Method by adding nonionic surfactant and positive-negative voltage pulse, increase acid solution and the deep layer of PDC glomerocryst layers is infiltrated, can realize that deep layer takes off cobalt, greatly improves production efficiency in a short time.

Description

A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer
Technical field
The invention belongs to remove the technical field of kish method, and in particular to a kind of quick removal diamond compact The method that cobalt is remained in glomerocryst layer.
Background technology
Diamond compact(Abbreviation PDC)It is by diadust, hard alloy substrate and a certain amount of metal solvent (Metal Co, Ni etc.)As raw material, under high pressure high temperature under the conditions of a kind of composite superhard material for sintering.In view of its is excellent Different performance, the ideal material of manufacture drilling bit, cutting tool and other wear resistant tools is turned at present.
Although the addition of metal solvent reduces synthesis condition early stage, promote the formation of diamond-diamond key, but Metal residual after sintering in polycrystalline diamond also generates detrimental effect for the use of later product.When in PDC uses by During to high temperature, on the one hand the metal solvent of residual can promote diamond to change to graphite, aggravate PDC graphitization or oxidation;Separately On the one hand, the thermal expansion coefficient difference between metal and diamond, expansion of metal can be made to cause generation inside polycrystalline diamond micro- The appearance of crackle, thermal stress and micro-crack exacerbates PDC hydraulic performance declines.In order to reduce the adverse effect of kish catalyst, I Need to be removed it.
At present, it is also more both at home and abroad that the residual of the cobalt in polycrystalline diamond layer is removed using infusion method, tradition soak in Acid and the propulsion of metallochemistry reaction, the kish cobalt at glomerocryst layer shallow-layer is gradually dissolved by acid solution, and forms a series of Intricate microcosmic air vent channel, but carried out along with reaction, the impurity with acid reaction is not easy inside glomerocryst layer(Diamond with The interphase of metal generation, SiC etc.)Continuous peeling, accumulation, plug these air vent channels, hinder deep layer and take off cobalt and OK.Take off that cobalt efficiency is too low, and deep layer takes off cobalt if thinking which results in traditional method(De- more than cobalt depth 0.25mm), often More than hundreds of hours are needed, are extremely not suitable for mass production.
Therefore, the quick removal of kish in diamond compact glomerocryst layer how is realized, turns into this area and urgently solves Technical problem certainly.
The content of the invention
For problems of the prior art, the present invention provides residual in a kind of quick removal diamond compact glomerocryst layer The method for staying cobalt.The present invention is simple to operate, high in machining efficiency, can realize that the deep layer of cobalt residual removes within a short period of time, Yi Shi Existing mass.
The purpose of the present invention is realized in the following manner:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air, pressurize 1-2h are passed through, then it is vacuumized, pressurize 1-2h;Again Compressed air, pressurize 1-2h are passed through, then it is vacuumized, pressurize 1-2h;..., circulate successively, diamond is taken out after 20-30h Composite sheet is rinsed well with water.
The acid solution system is made up of chloroazotic acid, hydrogen peroxide and nonionic surfactant.
The acid solution system is made up of the raw material of following parts by weight:Chloroazotic acid 7-8 parts, hydrogen peroxide 1.5-2 parts, it is non-from Sub- surfactant 0.5-1 parts.
The nonionic surfactant is PE6200.
Pressure value when being passed through pressurize after compressed air is 10~20KPa, pressure value when vacuumizing rear pressurize for- 10~-20KPa.
Vacuumizing in the pressure value and any one circulation when being passed through pressurize after compressed air in any one circulation The absolute value of pressure value during pressurize is equal afterwards, dwell time being passed through after compressed air in any one circulation and any One circulation in vacuumize after dwell time it is also equal.
Relative to prior art, nonionic surfactant act as in the present invention:For reducing the surface of acid solution Tension force, infiltration of the increase acid solution to PDC glomerocryst layers, to promote de- cobalt.Nonionic surfactant has scattered, breast simultaneously The performances such as change, foam, wetting, by these features, it can promote to be taken off impurity in cobalt region or be mingled with etc. and excluded in time, from And deep layer is promoted to take off cobalt.
Positive and negative air-pressure pulse is act as:Change PDC glomerocrysts layer in acid solution by changing the pressure in closed container The pressure born, to promote infiltration of the acid solution to PDC glomerocryst layers, so as to promote to remain the removal of cobalt.Meanwhile underbalance pulse When can also discharge gas caused by acid mist and interior reaction in container in time, can reduce what diamond compact substrate was corroded indirectly Probability.
Beneficial effects of the present invention are:Method by adding nonionic surfactant and positive-negative voltage pulse, is increased Acid solution infiltrates to the deep layer of PDC glomerocryst layers, can realize that deep layer takes off cobalt, greatly improves production efficiency in a short time.
Brief description of the drawings
Fig. 1 is the polycrystalline diamond layer before the de- cobalt of electron microscope shooting.
Fig. 2 is the polycrystalline diamond layer after the de- cobalt of electron microscope shooting.
Embodiment
20Kpa or -20Kpa in the present invention are the gauge pressure shown by pressure gauge, that is, " relative pressure ", gauge pressure be with On the basis of atmospheric pressure, malleation=atmospheric pressure+gauge pressure, vacuum(Negative pressure)=atmospheric pressure-gauge pressure.
Nonionic surfactant PE6200 is purchased from Yangtze petrochemical industry-BASF Co., Ltd.
Embodiment 1:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air, pressurize 1-2h are passed through, then it is vacuumized, pressurize 1-2h;Again Compressed air, pressurize 1-2h are passed through, then it is vacuumized, pressurize 1-2h;..., circulate successively, diamond is taken out after 20-30h Composite sheet is rinsed well with water.
That is, a circulation is:Compressed air, pressurize 1-2h are passed through, then it is vacuumized, pressurize 1-2h.Altogether N number of such circulation is carried out, 5≤N≤15, N are integer, and dwell time sum is 20-30h.
The acid solution system is made up of chloroazotic acid, hydrogen peroxide and nonionic surfactant.
The acid solution system is made up of the raw material of following parts by weight:Chloroazotic acid 7-8 parts, hydrogen peroxide 1.5-2 parts, it is non-from Sub- surfactant 0.5-1 parts.
The nonionic surfactant is PE6200.
Pressure value when being passed through pressurize after compressed air is 10~20KPa, pressure value when vacuumizing rear pressurize for- 10~-20KPa.
Vacuumizing in the pressure value and any one circulation when being passed through pressurize after compressed air in any one circulation The absolute value of pressure value during pressurize is equal afterwards, dwell time being passed through after compressed air in any one circulation and any One circulation in vacuumize after dwell time it is also equal.
Embodiment 2:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 10KPa, pressurize 1h, then to it Vacuumize, when pressure value reaches -10KPa, pressurize 1h;Compressed air is passed through again, when pressure value reaches 10KPa, pressurize 1h, It is vacuumized again, when pressure value reaches -10KPa, pressurize 1h;..., periodic cycle successively, diamond is taken out after 20h Composite sheet is rinsed well with water, and it is 0.402mm to measure de- cobalt depth.
Acid solution system is mixed by chloroazotic acid 7kg, hydrogen peroxide 1.5kg, PE6200 0.5kg.
Embodiment 3:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 12KPa, pressurize 1.2h, then it is right It is vacuumized, when pressure value reaches -12KPa, pressurize 1.2h;Compressed air is passed through again, when pressure value reaches 12KPa, is protected 1.2h is pressed, then it is vacuumized, when pressure value reaches -12KPa, pressurize 1.2h;..., periodic cycle successively, after 21.6h Take out diamond compact to be rinsed well with water, it is 0.457mm to measure de- cobalt depth.
Acid solution system is mixed by chloroazotic acid 7.2kg, hydrogen peroxide 1.6kg, PE6200 0.6kg.
Embodiment 4:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 14KPa, pressurize 1.4h, then it is right It is vacuumized, when pressure value reaches -14KPa, pressurize 1.4h;Compressed air is passed through again, when pressure value reaches 14KPa, is protected 1.4h is pressed, then it is vacuumized, when pressure value reaches -14KPa, pressurize 1.4h;..., periodic cycle successively, after 22.4h Take out diamond compact to be rinsed well with water, it is 0.470mm to measure de- cobalt depth.
Acid solution system is mixed by chloroazotic acid 7.4kg, hydrogen peroxide 1.7kg, PE6200 0.7kg.
Embodiment 5:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 15KPa, pressurize 1.5h, then it is right It is vacuumized, when pressure value reaches -15KPa, pressurize 1.5h;Compressed air is passed through again, when pressure value reaches 15KPa, is protected 1.5h is pressed, then it is vacuumized, when pressure value reaches -15KPa, pressurize 1.5h;..., periodic cycle successively, take after 24h Go out diamond compact to be rinsed well with water, it is 0.483mm to measure de- cobalt depth.The de- cobalt of electron microscope shooting is forward and backward As shown in Figure 1-2, silver color part in the left side is hard alloy to polycrystalline diamond layer in Fig. 2, and the right black portions are polycrystalline diamond Layer, it is evident that polycrystalline diamond layer shows two parts, color deeper portion is de- cobalt rear region, and color is omited superficial part and is divided into Cobalt region is not taken off.
Acid solution system is mixed by chloroazotic acid 7.5kg, hydrogen peroxide 1.75kg, PE6200 0.75kg.
Embodiment 6:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 16KPa, pressurize 1.6h, then it is right It is vacuumized, when pressure value reaches -16KPa, pressurize 1.6h;Compressed air is passed through again, when pressure value reaches 16KPa, is protected 1.6h is pressed, then it is vacuumized, when pressure value reaches -16KPa, pressurize 1.6h;..., periodic cycle successively, after 25.6h Take out diamond compact to be rinsed well with water, it is 0.465mm to measure de- cobalt depth.
Acid solution system is mixed by chloroazotic acid 7.6kg, hydrogen peroxide 1.8kg, PE6200 0.8kg.
Embodiment 7:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 18KPa, pressurize 1.8h, then it is right It is vacuumized, when pressure value reaches -18KPa, pressurize 1.8h;Compressed air is passed through again, when pressure value reaches 18KPa, is protected 1.8h is pressed, then it is vacuumized, when pressure value reaches -18KPa, pressurize 1.8h;..., periodic cycle successively, after 28.8h Take out diamond compact to be rinsed well with water, it is 0.446mm to measure de- cobalt depth.
Acid solution system is mixed by chloroazotic acid 7.8kg, hydrogen peroxide 1.9kg, PE6200 0.9kg.
Embodiment 8:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 20KPa, pressurize 1h, then to it Vacuumize, when pressure value reaches -20KPa, pressurize 1h;Compressed air is passed through again, when pressure value reaches 20KPa, pressurize 1h, It is vacuumized again, when pressure value reaches -20KPa, pressurize 1h;..., periodic cycle successively, diamond is taken out after 30h Composite sheet is rinsed well with water, and it is 0.367mm to measure de- cobalt depth.
Acid solution system is mixed by chloroazotic acid 8kg, hydrogen peroxide 2kg, PE6200 1.0kg.
Embodiment 9:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 20KPa, pressurize 2h, then to it Vacuumize, when pressure value reaches -20KPa, pressurize 2h;Compressed air is passed through again, when pressure value reaches 20KPa, pressurize 2h, It is vacuumized again, when pressure value reaches -20KPa, pressurize 2h;..., periodic cycle successively, diamond is taken out after 28h Composite sheet is rinsed well with water, and it is 0.379mm to measure de- cobalt depth.
Acid solution system is mixed by chloroazotic acid 8kg, hydrogen peroxide 2kg, PE6200 1.0kg.
Embodiment 10:
A kind of quick method for removing residual cobalt in diamond compact glomerocryst layer, is concretely comprised the following steps:Diamond compact is put In the closed container for entering to fill acid solution system, compressed air is passed through, when pressure value reaches 12KPa, pressurize 1.8h, then it is right It is vacuumized, when pressure value reaches -10KPa, pressurize 1.6h;Compressed air is passed through again, when pressure value reaches 15KPa, is protected 1.5h is pressed, then it is vacuumized, when pressure value reaches -18KPa, pressurize 1.2h;Compressed air is passed through again, when pressure value reaches During 11KPa, pressurize 1.9h, then it is vacuumized, when pressure value reaches -14KPa, pressurize 1.6h;Compressed air is passed through again, when When pressure value reaches 15KPa, pressurize 1.5h, then it is vacuumized, when pressure value reaches -17KPa, pressurize 1.3h;It is passed through again Compressed air, when pressure value reaches 13KPa, pressurize 1.7h, then it is vacuumized, when pressure value reaches -12KPa, pressurize 1.8h;Be passed through compressed air again, when pressure value reaches 14KPa, pressurize 1.6h, then vacuumized to it, when pressure value reaches- During 18KPa, pressurize 1.6h;Compressed air is passed through again, when pressure value reaches 13KPa, pressurize 1.4h, then it is vacuumized, when When pressure value reaches -17KPa, pressurize 1.2h;Compressed air is passed through again, when pressure value reaches 15KPa, pressurize 1.2h, then it is right It is vacuumized, when pressure value reaches -16KPa, pressurize 1.6h;Take out diamond compact to be rinsed well with water, measure de- cobalt Depth is 0.418mm.
Acid solution system is mixed by chloroazotic acid 7.2kg, hydrogen peroxide 1.6kg, PE6200 0.6kg.
Above-described is only the preferred embodiment of the present invention, it is noted that for those skilled in the art, Under the premise of general idea of the present invention is not departed from, some changes and improvements can also be made, these should also be considered as the present invention's Protection domain.

Claims (6)

  1. A kind of 1. quick method for removing residual cobalt in diamond compact glomerocryst layer, it is characterised in that:Concretely comprise the following steps:By gold Hard rock composite sheet is put into the closed container for filling acid solution system, is passed through compressed air, pressurize 1-2h, then it is taken out very Sky, pressurize 1-2h;Compressed air, pressurize 1-2h are passed through again, then it is vacuumized, pressurize 1-2h;..., circulate successively, 20- Diamond compact is taken out after 30h to be rinsed well with water.
  2. 2. the quick method for removing residual cobalt in diamond compact glomerocryst layer according to claim 1, it is characterised in that: The acid solution system is made up of chloroazotic acid, hydrogen peroxide and nonionic surfactant.
  3. 3. the quick method for removing residual cobalt in diamond compact glomerocryst layer according to claim 2, it is characterised in that: The acid solution system is made up of the raw material of following parts by weight:Chloroazotic acid 7-8 parts, hydrogen peroxide 1.5-2 parts, non-ionic surface are lived Property agent 0.5-1 parts.
  4. 4. the quick method for removing residual cobalt in diamond compact glomerocryst layer according to claim 2, it is characterised in that: The nonionic surfactant is PE6200.
  5. 5. the quick method for removing residual cobalt in diamond compact glomerocryst layer according to claim 1, it is characterised in that: Pressure value when being passed through pressurize after compressed air is 10~20KPa, pressure value when vacuumizing rear pressurize for -10~- 20KPa。
  6. 6. the quick method for removing residual cobalt in diamond compact glomerocryst layer according to claim 1, it is characterised in that: In the pressure value and any one circulation when being passed through pressurize after compressed air in any one circulation when vacuumizing rear pressurize Pressure value absolute value it is equal, the dwell time being passed through after compressed air and any one circulation in any one circulation In vacuumize after dwell time it is also equal.
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