CN102268619B - Preparation method of carbon-nanotube-reinforced polycrystalline diamond compact (PDC) material - Google Patents
Preparation method of carbon-nanotube-reinforced polycrystalline diamond compact (PDC) material Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon-nanotube-reinforced polycrystalline diamond compact (PDC) material, and the preparation method comprises the following steps of: carrying out semi-wet mixing on carbon nanotubes, diamond micropowder, an adhesive and the like for dispersedly and uniformly mixing to obtain raw materials for a polycrystalline diamond layer; and carrying out a high-temperature high-pressure sintering process and an appropriate heat treatment process on the raw materials and a cemented carbide substrate to obtain the carbon-nanotube-reinforced PDC material which is a composite material with high impact toughness, high wear resistance and high heat stability. In the preparation method, the impact toughness and stability of the PDC material are greatly improved without reducing the wear resistance of the PDC material through researching and analyzing the impact damage and thermal injury of the PDC material, using a fiber-reinforcing theory, adding an appropriate amount of dispersed carbon nanotubes and utilizing a material heat treatment technology; and the impact toughness of the PDC material is improved by 100-1000%. The carbon-nanotube-reinforced PDC material can be used in the preparation of cutting tools or cutting edges for high-speed high-precision cutting of various non-ferrous metals.
Description
Technical field
The present invention relates to a kind of non-ferrous metal that forms through the HTHP sintering and cut the carbon nanotube enhanced diamond compact material of usefulness.It is the matrix material of highly anti-impact toughness, high-wearing feature, high thermal stability.
Background technology
Diamond compact (Polycrystalline Diamond Compacts; Abbreviate PDC as) be by wimet and man-made polycrystalline diamond process HTHP synthetic; The toughness and the weldability that had both had wimet; Have adamantine high-wearing feature again, be widely used in fields such as mechanical workout as the high-efficient cutting cutter.Along with non-ferrous metals such as duraluminum, titanium alloy being widely used on motor car engine and wheel box, the application of PDC cutter in the processing of high new equipments such as motor car engine and wheel box is also more and more.As a kind of novel super-hard cutter material, PDC has performance advantages such as high firmness, high-wearing feature, low-friction coefficient, high thermal conductivity, become cut aluminum alloy, the best cutter material of non-ferrous metal such as titanium alloy.The raising of single performance is paid attention in current PDC development.Actual effect shows that the wear resistance ratio of current PDC material can be near adamantine wear resistance ratio, and the impact fracture of diamond layer becomes the major cause that PDC lost efficacy.High-wearing feature requires PDC that very high intensity is arranged, and strong toughness then requires PDC to have deformability to a certain degree, and the two is conflicting.Therefore developing a kind of not only high abrasion but also strong shock proof high-precision and high-stability PDC material becomes the focus and the exigence of current PDC development.
The PDC material that the HTHP sintering forms has experienced the broken and processes such as diffusion infiltration migration in diamond layer such as recrystallize is grown up, cobalt of diamond.Be in the diamond gap location caking agent fragility with expand with heat and contract with cold and oxidation is the principal element of source and the thermostability decline of composite sheet impact fracture.Carbon nanotube is difficult to be transformed into diamond under HTHP, its tubular structure still can remain for 1450 ℃ in pressure 5～6GPa, temperature.The carbon nanotube that forms through the HTHP sintering strengthens the PDC material, existing fiber theoretical conventional crackle bridging, crack deflection, extracts mechanism such as effect, and its singularity is also arranged.(1) carbon nanotube is present in the diamond gap location of having grown up, and in the space, becomes three-dimensional net distribution, combines with caking agent, forms high-strength skeleton.(2) carbon nanotube is present in that each when cutter heats up, because carbon nanotube is close with adamantine thermal expansivity, thereby has reduced the formation of PDC internal heat segmentation crack at the interface in the polycrystalline diamond, makes its thermostability enhancing.
Summary of the invention
Technical problem to be solved by this invention provides a kind of carbon nanotube that makes the diamond compact material have highly anti-impact toughness, high-wearing feature, high thermal stability and strengthens the diamond compact preparation methods.
In order to solve the problems of the technologies described above, carbon nanotube provided by the invention strengthens the diamond compact preparation methods, and step is following:
(1) purifying of carbon nanotube and dispersion treatment:
The carbon nanotube of many walls or single wall adopts the acetone soaking and washing, and purifying process such as conventional method are positioned over carbon nanotube then and carry out the ultra-sonic oscillation dispersion in the mixing solutions, put into drying in oven at last;
(2) synthesis material is prepared:
The synthesis material prescription: massfraction 0.5～5% dispersed carbon nanotubes, caking agent are 18～22%, and surplus is the diadust of particle size range 5 μ m～20 μ m, hard alloy substrate; Diadust carries out surface cleaning processing and preparatory greying before using, and hard alloy substrate and caking agent carry out surface cleaning to be handled; Other subsidiary material that use carry out corresponding cleaning to be handled; Agalmatolite piece, agalmatolite ring before the assembling must be removed moisture; With diadust, caking agent and carbon nanotube compound, use earlier the absolute ethyl alcohol wet mixing, the oven dry back is done to mix and is processed mixing raw material;
(3) close caked vacuum heat treatment and preservation:
Adopt briquetting to set up the vacuum heat treatment process method, earlier mixing raw material and hard alloy substrate, molybdenum cup, molybdenum sheet, carbon pipe are processed synthetic piece, will synthesize piece then and vacuumize thermal treatment together, temperature is 620～680 ℃, and the time is 0.5～1.5h; After vacuum-treat finishes, with synthetic piece be placed on temperature be preserve in 80～100 ℃ the baking oven subsequent use;
(4) ultra-high voltage is synthetic:
To synthesize piece and be positioned in the agalmatolite piece mould, and add at mould and load onto agalmatolite ring, conducting steel ring and catalyst sheet, in six-plane piercer, carry out the high pressure high temperature compound experiment; Synthesis technologic parameter is: 1450～1600 ℃ of sintering temperatures, and sintering pressure 5～6GPa, the heat-insulation pressure keeping time is 3～5 minutes;
(5) unrelieved stress is eliminated:
To synthesize the back product and carry out vacuum aging annealing.
Described mixing solutions is in 200ml absolute ethyl alcohol+0.1～1.0g sodium lauryl sulphate mixing solutions.
Described six-plane piercer is the hinge type six-plane piercer, the synthetic middle liquid phase pressure transmission mode that adopts.
The surface cleaning of described hard alloy substrate and caking agent is handled and is meant: at first mating surface is carried out sanding and polishing and handle; Erase the zone of oxidation and the hole of mating surface; Until exposing unsalted surface; Deoil then, washing, ultrasonic cleaning, infrared oven dry, subsequent use in the clean vessel of packing at last.
Described caking agent is cobalt sheet and titanium sheet.
Above-mentioned steps (3) is closed caked vacuum heat treatment and preservation: after vacuum-treat finishes, will synthesize piece and be placed in the baking oven and to preserve subsequent usely, oven temperature is 80～100 ℃.
Adopt the carbon nanotube of technique scheme to strengthen the diamond compact preparation methods; Make disperse ground such as carbon nanotube and diadust and caking agent mix the starting material that become polycrystalline diamond layer equably through more than half wet mixings; With it and hard alloy substrate; Create carbon nanotube enhanced PDC through HTHP sintering process and suitable thermal treatment process, this material is the matrix material with highly anti-impact toughness, high-wearing feature, high thermal stability.Through research and analysis for PDC impact fracture and thermal damage; Utilize fiber reinforcement theoretical; Through adding an amount of dispersed carbon nano tube and material heat treatment technology, on the basis that does not reduce the PDC wear resistance, significantly improve the toughness and the stability of PDC material.Toughness increase rate 100%～1000%.This carbon nanotube strengthens diamond compact material and is applied to prepare in the cutting tool or cutting edge that high-speed, high precision cuts various non-ferrous metals.The effect of molybdenum cup, molybdenum sheet and carbon pipe is typing.
Advantage of the present invention and beneficial effect are: routine in the PDC material that the HTHP sintering forms, the formed reticulated structure of caking agent make to have occurred D-M-D combining form in the material, and the bonding strength of D-M-D is far below the bonding strength with D-D; On the other hand, there are three kinds of distribution forms in caking agent in the PDC cutter, is respectively that the caking agent of spherical particle, " Co island " and vein shape between diamond distributes, and wherein has the greatest impact with the caking agent of the vein shape distribution thermostability to the PDC cutter; The heat crack crackle that caking agent expands with heat and contract with cold and oxidation is produced, the reduction of the PDC tool mechanical performance that is caused is the principal element that PDC cutter thermostability descends.Owing to above reason, the toughness of conventional composite sheet is difficult to basic raising, and stability is low in the working angles, is prone to defectives such as little tipping.Material use of the present invention carbon nanotube strengthen toughening effect and unrelieved stress control techniques etc.; The solid netted distribution that makes on the one hand the carbon nanotube that is present in the diamond gap location of having grown up form high-strength tubular armature in the space has improved the intensity and the toughness of polycrystalline diamond layer, and the distribution form of having controlled caking agent in the diamond gap makes it the vein shape not occur to distribute; Partly eliminated the PDC internal residual stress that the HTHP sintering is caused on the other hand, thus improved effectively cutter material toughness, strengthened the stability of working angles, prolonged the cutter material life-span, reduced production cost.
In sum, the present invention is that a kind of carbon nanotube that makes the diamond compact material have highly anti-impact toughness, high-wearing feature, high thermal stability strengthens the diamond compact preparation methods.
Description of drawings
Fig. 1 is that embodiment 1 carbon nanotube strengthens diamond compact material impact fracture microscopic appearance figure.
Fig. 2 is that embodiment 2 carbon nanotubes strengthen diamond compact material impact fracture microscopic appearance figure.
Fig. 3 is that embodiment 3 carbon nanotubes strengthen diamond compact material impact fracture microscopic appearance figure.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1:
Carbon nanotube strengthens the diamond compact preparation methods, and step is following:
(1) purifying of carbon nanotube and dispersion treatment
The carbon nanotube of many walls or single wall adopts the acetone soaking and washing; Purifying process such as conventional method; Then carbon nanotube is positioned in 200ml absolute ethyl alcohol+0.5g sodium lauryl sulphate mixing solutions, carries out ultra-sonic oscillation and disperse, put into drying in oven at last;
(2) synthesis material is prepared
The synthesis material prescription: massfraction 0.5% dispersed carbon nanotubes, the diadust of particle size range 5～10 μ m, caking agent are 22%, hard alloy substrate; Diadust must carry out surface cleaning processing and preparatory greying before using; Hard alloy substrate, cobalt sheet, titanium sheet raw and auxiliary material; At first mating surface is carried out sanding and polishing and handle, erase the zone of oxidation and the hole of mating surface, until exposing unsalted surface; Deoil then, washing, ultrasonic cleaning, infrared oven dry, subsequent use in the clean vessel of packing at last; Other subsidiary material that use also should carry out corresponding cleaning to be handled; Agalmatolite piece, agalmatolite ring before the assembling must carry out calcination process earlier, to remove the moisture in the agalmatolite; With diadust, caking agent and carbon nanotube compound, use earlier the absolute ethyl alcohol wet mixing, the oven dry back is done and is mixed, and preserves mixing raw material;
(3) close caked vacuum heat treatment and preservation
Adopt briquetting to set up the vacuum heat treatment process method, earlier mixing raw material and wimet substrate, cobalt sheet, titanium sheet, molybdenum cup, molybdenum sheet, carbon pipe are processed synthetic piece, will synthesize piece then and vacuumize thermal treatment together; The vacuum heat treatment condition is the vacuum of 10KPa for the perfect vacuum degree, 620, and time 1.5h after vacuum-treat finishes, will synthesize piece and be placed in the baking oven and to preserve subsequent usely, and oven temperature is 80 ℃;
(4) ultra-high voltage is synthetic
To synthesize piece and be positioned over, and add at mould and load onto agalmatolite ring, conducting steel ring and catalyst sheet, in the hinge type six-plane piercer, carry out the high pressure high temperature compound experiment by in the agalmatolite piece mould; Adopt liquid phase pressure transmission mode in synthetic, synthesis technologic parameter is: sintering temperature 1450, and sintering pressure 5GPa, the heat-insulation pressure keeping time is 3 minutes;
(5) unrelieved stress is eliminated
To synthesize the back product and carry out vacuum aging annealing.
The sample effect: the wear resistance ratio that utilizes PDC grinding silicon carbide grinding wheel method to measure PDC is about 2.70461 * 10
5Utilize the toughness of tension weight churning method test PDC, single strike work 1.4J, it is 4 times that carbon-free nanoscale pipe sample average impacts number of times, it is 13 times that the sample average impact number of times of carbon nanotube is arranged.Fig. 1 is that carbon nanotube strengthens diamond compact material impact fracture microscopic appearance figure.
Embodiment 2:
Carbon nanotube strengthens the diamond compact preparation methods, and step is following:
(1) purifying of carbon nanotube and dispersion treatment
The carbon nanotube of many walls or single wall adopts the acetone soaking and washing; Purifying process such as conventional method; Then carbon nanotube is positioned in 200ml absolute ethyl alcohol+0.1g sodium lauryl sulphate mixing solutions, carries out ultra-sonic oscillation and disperse, put into drying in oven at last;
(2) synthesis material is prepared
The synthesis material prescription: massfraction 1% dispersed carbon nanotubes, the diadust of particle size range 15～20 μ m, caking agent are 20%, hard alloy substrate; Diadust must carry out surface cleaning processing and preparatory greying before using; Hard alloy substrate, cobalt sheet, titanium sheet raw and auxiliary material; At first mating surface is carried out sanding and polishing and handle, erase the zone of oxidation and the hole of mating surface, until exposing unsalted surface; Deoil then, washing, ultrasonic cleaning, infrared oven dry, subsequent use in the clean vessel of packing at last; Other subsidiary material that use also should carry out corresponding cleaning to be handled; Agalmatolite piece, agalmatolite ring before the assembling must carry out calcination process earlier, to remove the moisture in the agalmatolite; With diadust, caking agent and carbon nanotube compound, use earlier the absolute ethyl alcohol wet mixing, the oven dry back is done and is mixed, and preserves mixing raw material;
(3) close caked vacuum heat treatment and preservation
Adopt briquetting to set up the vacuum heat treatment process method, earlier mixing raw material and wimet substrate, cobalt sheet, titanium sheet, molybdenum cup, molybdenum sheet, carbon pipe are processed synthetic piece, will synthesize piece then and vacuumize thermal treatment together; The vacuum heat treatment condition is the vacuum of 20KPa for the perfect vacuum degree, and 650 ℃, time 1h after vacuum-treat finishes, will synthesize piece and be placed in the baking oven and to preserve subsequent usely, and oven temperature is 90 ℃;
(4) ultra-high voltage is synthetic
To synthesize piece and be positioned over, and add at mould and load onto agalmatolite ring, conducting steel ring and catalyst sheet, in the hinge type six-plane piercer, carry out the high pressure high temperature compound experiment by in the agalmatolite piece mould; Adopt liquid phase pressure transmission mode in synthetic, synthesis technologic parameter is: 1500 ℃ of sintering temperatures, and sintering pressure 5.5GPa, the heat-insulation pressure keeping time is 5 minutes;
(5) unrelieved stress is eliminated
To synthesize the back product and carry out vacuum aging annealing.
The sample effect: the wear resistance ratio that utilizes PDC grinding silicon carbide grinding wheel method to measure PDC is about 2.70461 * 10
5Utilize the toughness of tension weight churning method test PDC, single strike work 1.4J, it is 4 times that carbon-free nanoscale pipe sample average impacts number of times, it is 14 times that the sample average impact number of times of carbon nanotube is arranged.Fig. 2 is that carbon nanotube strengthens diamond compact material impact fracture microscopic appearance figure.
Embodiment 3:
Carbon nanotube strengthens the diamond compact preparation methods, and step is following:
(1) purifying of carbon nanotube and dispersion treatment
The carbon nanotube of many walls or single wall adopts the acetone soaking and washing; Purifying process such as conventional method; Then carbon nanotube is positioned in 200ml absolute ethyl alcohol+1.0g sodium lauryl sulphate mixing solutions, carries out ultra-sonic oscillation and disperse, put into drying in oven at last;
(2) synthesis material is prepared
The synthesis material prescription: massfraction 5% dispersed carbon nanotubes, the diadust of particle size range 10～20 μ m, caking agent are 18%, hard alloy substrate; Diadust must carry out surface cleaning processing and preparatory greying before using; Hard alloy substrate, cobalt sheet, titanium sheet raw and auxiliary material; At first mating surface is carried out sanding and polishing and handle, erase the zone of oxidation and the hole of mating surface, until exposing unsalted surface; Deoil then, washing, ultrasonic cleaning, infrared oven dry, subsequent use in the clean vessel of packing at last; Other subsidiary material that use also should carry out corresponding cleaning to be handled; Agalmatolite piece, agalmatolite ring before the assembling must carry out calcination process earlier, to remove the moisture in the agalmatolite; With diadust, caking agent and carbon nanotube compound, use earlier the absolute ethyl alcohol wet mixing, the oven dry back is done and is mixed, and preserves mixing raw material;
(3) close caked vacuum heat treatment and preservation
Adopt briquetting to set up the vacuum heat treatment process method, earlier mixing raw material and wimet substrate, cobalt sheet, titanium sheet, molybdenum cup, molybdenum sheet, carbon pipe are processed synthetic piece, will synthesize piece then and vacuumize thermal treatment together; The vacuum heat treatment condition is about the vacuum of 30KPa for the perfect vacuum degree, and 680 ℃, 0.5h after vacuum-treat finishes, will synthesize piece and be placed on and preserve subsequent usely in the baking oven, and oven temperature is 100 ℃;
(4) ultra-high voltage is synthetic
To synthesize piece and be positioned over, and add at mould and load onto agalmatolite ring, conducting steel ring and catalyst sheet, in the hinge type six-plane piercer, carry out the high pressure high temperature compound experiment by in the agalmatolite piece mould; Adopt liquid phase pressure transmission mode in synthetic, synthesis technologic parameter is: 1550 ℃ of sintering temperatures, and sintering pressure 6GPa, the heat-insulation pressure keeping time is 4 minutes;
(5) unrelieved stress is eliminated
To synthesize the back product and carry out vacuum aging annealing.
The sample effect: the wear resistance ratio that utilizes PDC grinding silicon carbide grinding wheel method to measure PDC is about 2.70461 * 10
5Utilize the toughness of tension weight churning method test PDC, single strike work 1.4J, it is 4 times that carbon-free nanoscale pipe sample average impacts number of times, it is 34 times that the sample average impact number of times of carbon nanotube is arranged.Fig. 3 is that carbon nanotube strengthens diamond compact material impact fracture microscopic appearance figure.
This carbon nanotube strengthens the PDC material and is applied to prepare in the cutting tool or cutting edge that high-speed, high precision cuts various non-ferrous metals.
Claims (6)
1. a carbon nanotube strengthens the diamond compact preparation methods, and it is characterized in that: step is following:
(1) purifying of carbon nanotube and dispersion treatment:
The carbon nanotube of many walls or single wall adopts the acetone soaking and washing, and purifying process adopts ordinary method, carbon nanotube is positioned over carries out the ultra-sonic oscillation dispersion in the mixing solutions then, puts into drying in oven at last;
(2) synthesis material is prepared:
The synthesis material prescription: massfraction 0.5～5% dispersed carbon nanotubes, caking agent are 18～22%, and surplus is the diadust of particle size range 5 μ m～20 μ m, hard alloy substrate; Diadust carries out surface cleaning processing and preparatory greying before using, and hard alloy substrate and caking agent carry out surface cleaning to be handled; Other subsidiary material that use carry out corresponding cleaning to be handled; Agalmatolite piece, agalmatolite ring before the assembling must be removed moisture; With diadust, caking agent and carbon nanotube compound, use earlier the absolute ethyl alcohol wet mixing, the oven dry back is done to mix and is processed mixing raw material;
(3) close caked vacuum heat treatment and preservation:
Adopt briquetting to set up the vacuum heat treatment process method, earlier mixing raw material and hard alloy substrate, molybdenum cup, molybdenum sheet, carbon pipe are processed synthetic piece, will synthesize piece then and vacuumize thermal treatment together, temperature is 620～680 ℃, and the time is 0.5～1.5h; After vacuum-treat finishes, with synthetic piece be placed on temperature be preserve in 80～100 ℃ the baking oven subsequent use;
(4) ultra-high voltage is synthetic:
To synthesize piece and be positioned in the agalmatolite piece mould, and add at mould and load onto agalmatolite ring, conducting steel ring and catalyst sheet, in six-plane piercer, carry out the high pressure high temperature compound experiment; Synthesis technologic parameter is: 1450～1600 ℃ of sintering temperatures, and sintering pressure 5～6GPa, the heat-insulation pressure keeping time is 3～5 minutes;
(5) unrelieved stress is eliminated:
To synthesize the back product and carry out vacuum aging annealing.
2. carbon nanotube according to claim 1 strengthens the diamond compact preparation methods, and it is characterized in that: described mixing solutions is 200ml absolute ethyl alcohol+0.1～1.0g sodium lauryl sulphate mixing solutions.
3. carbon nanotube according to claim 1 strengthens the diamond compact preparation methods, and it is characterized in that: described six-plane piercer is the hinge type six-plane piercer, the synthetic middle liquid phase pressure transmission mode that adopts.
4. carbon nanotube according to claim 1 and 2 strengthens the diamond compact preparation methods; It is characterized in that: the surface cleaning of described hard alloy substrate and caking agent is handled and is meant: at first mating surface is carried out sanding and polishing and handle; Erase the zone of oxidation and the hole of mating surface; Until exposing unsalted surface, deoil then, washing, ultrasonic cleaning, infrared oven dry, subsequent use in the clean vessel of packing at last.
5. carbon nanotube according to claim 1 strengthens the diamond compact preparation methods, and it is characterized in that: described caking agent is cobalt sheet and titanium sheet.
6. carbon nanotube according to claim 1 strengthens the diamond compact preparation methods, it is characterized in that: closing caked vacuum heat treatment in the above-mentioned steps (3) is the vacuum of 10～30KPa for the perfect vacuum degree with preserving the vacuum heat treatment condition.
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