CN101318839B - Silicon carbide ceramic and method for manufacturing composite drawing mould of diamond - Google Patents
Silicon carbide ceramic and method for manufacturing composite drawing mould of diamond Download PDFInfo
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- CN101318839B CN101318839B CN2008100401389A CN200810040138A CN101318839B CN 101318839 B CN101318839 B CN 101318839B CN 2008100401389 A CN2008100401389 A CN 2008100401389A CN 200810040138 A CN200810040138 A CN 200810040138A CN 101318839 B CN101318839 B CN 101318839B
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Abstract
The invention relates to a preparation method for silicone carbide ceramics and diamond composite drawing die. The silicone carbide ceramics is taken as a substrate, and the process of conventional diamond coating deposition, plasma polishing, nano diamond coating deposition, and mechanical polishing is repeated for a plurality of times to remove original blister defects on the surface of an inner hole of a ceramic die. During the cycle of CVD diamond deposition and polishing, a conventional diamond coating is integrated with a nano diamond coating, the plasma polishing is integrated with the mechanical polishing, the plasma polishing is inserted between the conventional coating and the nano coating, and consequently the die becomes more adaptive to the mechanical polishing after the growth of the nano coating. The die which can replace a traditional hard alloy product not only can greatly prolong the service life of a traditional die and device, improve production efficiency, remarkably improve the quality of products concerned and effectively save raw material, but also has great significance for the great reduction of tungsten and cobalt consumption and effective solution to the resource crisis faced by the hard alloy industry.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of mold, specifically, relate to a kind of chemical vapour deposition (CVD) (being called for short CVD) silicon carbide ceramics and method for manufacturing composite drawing mould of diamond.
Background technology
Usually by the high-abrasive material preparation, comparatively ideal is diamond to drawing mould, secondly is carbide alloy, to improve the life-span of mould, guarantees the dimensional accuracy and the fineness of goods.Consider cost and technical factor; make at present drawing mould and mostly adopt carbide alloy in large aperture occasion (d 〉=5 millimeter); only just can adopt diamond (glomerocryst or monocrystalline) mould in small-bore occasion (d≤3 millimeter); yet; the wearing and tearing when drawing and twisted wire of tradition sintered-carbide die are very serious; working life is short; the correlated product precision is difficult to guarantee; surface quality is poor; mould consumption is big; especially waste of raw materials such as copper material is serious; cause production efficiency low; labor strength is big; seriously restricted the further raising of relevant industries benefit and product quality; on the other hand; the manufacturing of carbide alloy will consume a large amount of tungsten; the advantage that tungsten has been listed in important strategic metal and resource fades away; cemented carbide industry also will face crisis of resource, and tungsten resource safety has become development hard carbide industry bottleneck.
Characteristics such as high temperature resistant, wear-resistant, anti-oxidant, corrosion-resistant and good elevated temperature strength that engineering ceramic material has, just in many fields of in the past using carbide alloy, be applied at present, as cutter, wear resistant appliance, abrading-ball, bearing, nozzle, engine critical component etc.Along with the impact strength and the fracture toughness of advanced ceramics increases substantially, be hopeful most to develop into the desirable substitution material of Hardmetal materials of resource predicament, especially carborundum non-oxidized substance structural ceramics such as (SiC), there is not resource problem, the strong carbide that simultaneously is typical strong covalent bond combination again forms material, be similar to the diamond tetrahedral structural unit, on the SiC ceramic substrate, the CVD diamond nucleation density is big, with diamond coatings good associativity is arranged, compare with carbide alloy, the ceramic material thermal coefficient of expansion is less, and the graphitization of urging of not having Co again influences, therefore, on the SiC ceramic matrix material, obtain the diamond coatings that bond strength significantly improves than carbide alloy easily.
Yet, different with Hardmetal materials, ceramic material adopts solid-phase sintering more, crystalline ceramic exists a large amount of faults of construction, makes material not fine and close, and often there is more micropore inside, the grinding and polishing rear surface still is distributed with many tens of sand holes to 100 microns, the inherent shortcoming of ceramic material has very big influence to its physical and mechanical properties, especially to the friction and wear characteristic influence significantly, substitutes the serviceability of carbide alloy as high-abrasive material thereby directly influence it in tribological field.
Find through literature search prior art, it is substrate that Chinese patent " method for preparing wire drawing mold with diamond compoiste coating " (patent No. ZL01113027.X) proposes with the large aperture sintered-carbide die, with chemical gas-phase method conventional diamond of hole surface deposition one deck and Nano diamond composite coating within it, make the diamond coatings mould, can improve working life 5-10 doubly, it is WC-Co cemented carbide substrate material that but substrate is adopted in this invention, by tungsten carbide particle and adhesive (cobalt, nickel etc.) sintering forms, because Co urges graphitizing and influence factors such as carbide alloy and diamond thin thermal expansion coefficient difference, make and exist bigger thermal stress in the diamond coatings, cause between diamond thin and the matrix material bond strength to be still waiting to improve, coating product performance discreteness is bigger, limited the further raising of diamond composite coating die life, because substrate remains carbide alloy, exists tungsten equally, the pressure that cobalt resource consumption and manufacturing cost improve constantly.Further in the retrieval, do not find silicon carbide ceramics and diamond coatings composite die as yet.
Summary of the invention
The objective of the invention is to existing problems at prior art, a kind of silicon carbide ceramics and method for manufacturing composite drawing mould of diamond are provided, with silicon carbide ceramics as the mould substrate, adopt the method for diamond coatings through repeatedly depositing, polishing, overcome the ceramic surface defective, obtain silicon carbide ceramics and diamond coatings composite die.
The present invention is achieved by the following technical solutions:
The present invention is substrate with the silicon carbide ceramics, carry out repeatedly " conventional diamond coatings deposition → plasma polishing → nano diamond coating deposition → machine glazed finish " process, make the disappearances such as (pits) of the original bore area defective of ceramic die sand holes, not only improved the fineness of mould bore area, and since the reinforcement of diamond coatings increase service life more than 10 times.At the CVD diamond deposition---the polishing cyclic process, adopt conventional diamond coatings to combine with nano diamond coating, plasma polishing combines with machine glazed finish, inserts plasma polishing between deposition conventional coating and nano coating, more adapts to machine glazed finish after making the growing nano coating.
The inventive method may further comprise the steps:
After the first step, silicon carbide ceramics mould pass through nitric acid, hydrofluoric acid mixed solution preliminary treatment, with diadust the nib surface is rotated grinding, in the ultrasonic clean rearmounted heated filament CVD reative cell, adopt the vertical pulling tantalum wire to pass nib, stretching with high temperature resistant spring, and heated filament and nib axis are matched.
Described nitric acid, hydrofluoric acid mixed solution preliminary treatment are meant: place nitric acid, hydrofluoric acid mixed solution, wherein HNO
3: HF is 1: 3, to remove the SiO of outer surface
2With free Si.
Second step, feeding hydrogen and acetone deposit conventional diamond coatings at the mould bore area, and crystal grain is thick and inhomogeneous, and the surface is rough and uneven in surface.
The conventional diamond coatings of described deposition, its sedimentation time 4 hours, THICKNESS CONTROL is at 7 μ m-9 μ m.
The 3rd step, original position are carried out plasma polishing, add argon gas (Ar/H
2Be 1.0, volume ratio), because mould endoporus diamond thin has negative electron affinity, applies a Dc bias that has Alternating Component between filament and mould, the cation stream that forms directed movement is bombarded the wedge angle of removing the coating surface coarse grain.
Described plasma polishing, its concrete parameter is pressure 100Pa, voltage 200V, bias current 0.5A, the time is 0.5 hour.
The 4th step, original position continue the depositing nano diamond coatings.
Described depositing nano diamond coatings, its technological parameter is: pressure 1KPa, acetone and hydrogen are 4%-6% (volume ratio), add Ar gas, Ar and H
2Be 1.0 (volume ratios), 1 and a half hours time, THICKNESS CONTROL is at 2 μ m-4 μ m;
The 5th step, the nib surface is rotated grinding machinery polishing with diadust.
The 6th step, repetition second go on foot the 52 to 3 time, the alternating deposit and the polishing of routine and nano diamond coating, thick about 20-30 micron prepares silicon carbide ceramics and composite drawing mould of diamond, the remarkable minimizing of the defective on ceramic substrate surface (sand holes etc.).
Compared with prior art, it is substrate that the present invention substitutes carbide alloy with silicon carbide ceramics, carry out repeatedly chemical gas-phase method (being called for short the CVD method) diamond deposition and polishing cyclic process, one side ceramic die bore area native defect, disappeared as sand holes (pit), surface smoothness significantly improves, and has satisfied the drawing mould instructions for use; Strengthened ceramic surface with diamond coatings on the other hand, die life prolongs more than 10 times.Characteristics of the present invention are that conventional diamond coatings combines with nano diamond coating; plasma polishing and machine glazed finish combine; between conventional coating of deposition and nano coating, insert the plasma glossing; more adapt to machine glazed finish after making the growing nano coating; plasma polishing can original position carry out in heated filament CVD depositing diamond equipment; pottery/the composite drawing mould of diamond of the present invention's preparation can be widely used in the drawing of metal wire rod and tubing; the conductor wire core strand is made and is pressed; metal pipe-wall butt welding and drawing; the welding rod powder coating mould; nozzle; sliding bearing; occasions such as wear-resisting valve seat; the diamond coated film coating of ceramic material working surface; be applied to substitute traditional hart metal product (tool and mould and wear resistant appliance) occasion; can not only prolong the service life of traditional moulds and device significantly; enhance productivity; significantly improve the quality of Related product; effectively save material; and for reducing tungsten significantly; the consumption of cobalt resource, effectively solving cemented carbide industry, to face crisis of resource significant.
Description of drawings
Fig. 1 is a die surface sand holes disappearance process schematic diagram;
Fig. 2 diamond coatings deposition polishing process schematic diagram;
Wherein: figure Fig. 2 a plasma polishing, Fig. 2 .b removes the coating surface wedge angle, Fig. 2 c depositing nano diamond coatings, Fig. 2 d obtains the smooth diamond coatings of one deck.
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment
As shown in Figure 1, wherein a is the initial surface of pottery, presents sand holes (pit); B. be to adopt the CVD method through a deposition of diamond thin films, and the surface after polishing.The sand holes size significantly reduces, and this is the result that the very fast and outer surface of diamond film speed polishes the attenuate double action in the pit.C is that the sand holes size further significantly reduces through the surface after CVD diamond deposition, the polishing for the second time.D is for almost to have disappeared through the sand holes after depositing for the third time, polishing.So just reached two purposes: (1) sand holes defective fades away, and surface smoothness significantly improves, and has satisfied the instructions for use of mould; (2) diamond surface has substituted ceramic surface, and because of diamond is the hardest in the world material, its hardness is than pottery (SiC, Si
3N
4, Al
2O
3Deng) high many, therefore the surface has obtained very desirable reinforcement.Adopt this pottery/diamond composite die, not only saved strategic resource tungsten, and die life prolong more than 10 times, Related product dimensional accuracy and fineness have also all obtained significantly improving, and will become the desirable upgraded product of carbide alloy diamond coatings drawing mould.
The preparation process of present embodiment is on carborundum SiC ceramic substrate, adopts chemical gas-phase method uniform deposition diamond coatings, forms smooth diamond surface, has obtained desirable pottery/diamond composite die.Wherein the technology of most critical is the alternating deposit and the polishing of diamond coatings.In general, because diamond has very big surface energy, the diamond coatings surface is uneven, and extreme hardness, is difficult to coating is polished.To this, solution as shown in Figure 2, D: conventional diamond coatings, ND: nano diamond coating.Aperture preliminary treatment in the pottery, usefulness chemical gas-phase method (CVD method) are carried out plasma polishing (Fig. 2 .a, Ar after depositing the thick conventional diamond coatings of the about 7-9 μ of one deck m
+, H
+Ion beam polishing),, change the process conditions of CVD then, the nano diamond coating (Fig. 2 .c) about deposition one deck 3-5 μ m to remove coating surface wedge angle (Fig. 2 .b).After machine glazed finish (diamond dust is made abrasive material), just can obtain the smooth diamond coatings of one deck (Fig. 2 .d), " conventional diamond coatings deposition → plasma polishing → nano diamond coating deposition → machine glazed finish " cyclic process that present embodiment proposes, it is mutually compound with nano diamond coating to can be understood as conventional diamond, a kind of method that plasma polishing combines with machine glazed finish.
The present embodiment substrate is a pressureless sintering SiC pottery, and appearance and size is 50 * 25 millimeters of φ, and the aperture is 18.2 millimeters of φ, and the mould bore area grinds through finishing and places nitric acid, hydrofluoric acid mixed solution (HNO
3: HF is 1: 3), to remove the SiO of outer surface
2With free Si, neutralization is carried out milled processed, supersound washing with diadust to the nib surface after cleaning, and cleans in the rearmounted heated filament CVD reative cell.Hot filament adopts the tantalum wire of 1.0 millimeters of φ, and this heated filament links to each other with filament electrode after passing nib, and is stretching with high temperature resistant spring, and heated filament and nib axis are matched.
Reative cell vacuumizes the back and feeds reacting gas (hydrogen and acetone), begin the CVD deposition of diamond coatings after adjusting chamber pressure, technological parameter is pressure 5KPa, total gas flow rate 700 ml/min, acetone/hydrogen are 2% (volume ratio), about 2200 ℃ of hot filament temperature, DC bias current is 4A, and the nib surface deposition obtains the conventional diamond coatings about 8 microns after depositing through 4 hours.
Original position is carried out plasma polishing on this basis, adds argon gas (Ar/H
2Be 1.0, volume ratio) between filament and mould, apply a Dc bias (not filtering after the full-wave rectification) that has Alternating Component, make Ar
+And H
+The bombardment substrate, to remove the wedge angle on diamond coatings surface, coating layer thickness also slightly reduces, and concrete parameter is pressure 100Pa, voltage 200V, bias current 0.5A, the time is 0.5 hour.
Then adjust parameter, original position continues the depositing nano diamond coatings, and process conditions become: pressure 1KPa, the volume ratio of acetone and hydrogen is 4%, 5%, 6%, adds Ar gas, Ar and H
2Volume ratio be 1.0, after 1 and a half hours, about about 3 microns nano diamond coating of getting back.
From reative cell, take out mould, carry out machine glazed finish, can obtain the thick smooth diamond composite coating in the 8 μ m left and right sides.
Repeat the said process secondary again, just obtained pottery and diamond composite die, the significantly minimizing of the defective on ceramic substrate surface (sand holes or pit), the thick about 20-30 micron of the diamond coatings of this mould, surface smoothness Ra≤0.05 μ m.The sand holes that ceramic substrate originally presented also disappear, and this mould is used for 240 millimeters
2The strand system of the power cable conductor wire core in cross section is pressed, and its working life can be brought up to (about 20 times) more than the 600km from the 30km of original sintered-carbide die, and the surface quality of core and dimensional accuracy have also obtained very big improvement.Pottery/diamond composite coating can be widely used in wire, bar, pipe drawing, conductor wire core strand system and press, tube wall butt welding and shaping, welding rod powder coating mould, nozzle etc., also can be applied to occasions such as sliding bearing, wear-resisting valve seat, it is little to have coefficient of friction, anti-all soda acids, service life is long especially, advantages such as No Assets consumption problem.
The foregoing description before the growing nano diamond coatings, inserts plasma polishing technology behind the conventional diamond coatings of deposition, to remove the wedge angle of conventional coating surface, improve the coating flatness, make behind the growing nano diamond coatings, be more prone to adapt to machine glazed finish.Plasma polishing can carry out on the ion beam etching machine, also can original position carry out in heated filament CVD depositing device.Because in the deposition of diamond thin films process, the substrate surface temperature can reach 800-900 ℃, and under high like this temperature, silicon carbide ceramics and diamond coatings have all become conductor from original insulator, it can be used as electrode.If between filament and ceramic substrate, apply a direct current or alternating voltage, or the alternating voltage of band bias voltage, under certain air pressure, just can produce plasma, just can reach the purpose of plasma polishing.The distinguishing feature of the foregoing description is that plasma polishing can original position carry out, and has effectively simplified the CVD technical process.
Claims (6)
1. silicon carbide ceramics and method for manufacturing composite drawing mould of diamond is characterized in that, may further comprise the steps:
After the first step, silicon carbide ceramics mould pass through nitric acid, hydrofluoric acid mixed solution preliminary treatment, with diadust the nib surface is rotated grinding, in the ultrasonic clean rearmounted heated filament CVD reative cell, adopt the vertical pulling tantalum wire to pass nib, stretching with high temperature resistant spring, and heated filament and nib axis are matched;
Second step, feeding hydrogen and acetone deposit conventional diamond coatings at the mould bore area;
The 3rd step, original position are carried out plasma polishing, add argon gas, mould endoporus diamond thin has negative electron affinity, between filament and mould, apply a Dc bias that has Alternating Component, the cation stream that forms directed movement is bombarded the wedge angle of removing the coating surface coarse grain;
The 4th step, original position continue the depositing nano diamond coatings;
The 5th step, the nib surface is rotated grinding machinery polishing with diadust;
The 6th step, repetition second go on foot the 5th and go on foot 2 to 3 times, and conventional diamond coatings and nano diamond coating alternating deposit and polishing prepare silicon carbide ceramics and composite drawing mould of diamond.
2. silicon carbide ceramics according to claim 1 and method for manufacturing composite drawing mould of diamond is characterized in that, in second step, and the conventional diamond coatings of described deposition, 4 hours its time, THICKNESS CONTROL is at 7 μ m-9 μ m.
3. silicon carbide ceramics according to claim 1 and method for manufacturing composite drawing mould of diamond is characterized in that, in the 3rd step, the argon gas of interpolation is 1.0 with the hydrogen volume ratio.
4. according to claim 1 or 3 described silicon carbide ceramics and method for manufacturing composite drawing mould of diamond, it is characterized in that, in the 3rd step, described original position is carried out plasma polishing, and its concrete parameter is pressure 100Pa, voltage 200V, bias current 0.5A, the time is 0.5 hour.
5. silicon carbide ceramics according to claim 1 and method for manufacturing composite drawing mould of diamond is characterized in that, in the 4th step, described depositing nano diamond coatings, its technological parameter is: pressure 1KPa, the volume ratio of acetone and hydrogen is 4%-6%, add Ar gas, Ar gas and H
2Volume ratio be 1.0,1 and a half hours time, THICKNESS CONTROL is at 2 μ m-4 μ m.
6. silicon carbide ceramics according to claim 1 and method for manufacturing composite drawing mould of diamond is characterized in that, in the 6th step, the total thickness of described conventional diamond coatings and nano diamond coating is the 20-30 micron.
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| CN102140627B (en) * | 2011-01-27 | 2013-01-02 | 上海交通大学 | Preparation method of planarized coating layer for diamond with ultra-large-aperture inner holes |
| CN105200391B (en) * | 2014-05-29 | 2018-12-18 | 上海交友钻石涂层有限公司 | Diamond coatings drawing mould preparation method suitable for water lubrication |
| CN107983787B (en) * | 2017-11-16 | 2019-06-21 | 中国航空工业集团公司洛阳电光设备研究所 | It produces Copper-Aluminum compound row and uses thyrite drawing mould and manufacturing method |
| CN109226299A (en) * | 2018-11-09 | 2019-01-18 | 东南大学 | A kind of lamination self-lubrication ceramic wire-drawing die and preparation method thereof |
| CN111775381A (en) * | 2019-04-04 | 2020-10-16 | 苏州卡利肯新光讯科技有限公司 | Processing technology of mold for car lamp reflector |
| CN110802453A (en) * | 2019-11-13 | 2020-02-18 | 久钻科技(成都)有限公司 | Polishing method for inner hole coating of wire drawing die |
| CN113096964B (en) * | 2021-03-11 | 2021-12-28 | 西安交通大学 | Electrode preparation method for realizing adhesive fibrosis based on expansion micro stress |
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| US5152917A (en) * | 1991-02-06 | 1992-10-06 | Minnesota Mining And Manufacturing Company | Structured abrasive article |
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