CN103938133B - A kind of take Zirconium oxide fibre as polycrystalline diamond of toughness reinforcing phase and preparation method thereof - Google Patents
A kind of take Zirconium oxide fibre as polycrystalline diamond of toughness reinforcing phase and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprise the steps: that (1) take basic zirconium chloride as raw material, continuous measurement method is adopted to add ammoniacal liquor or oxalic acid, continuously stirring heating forms transparent colloidal sol gradually, at microwave sintering kiln roasting after drying grinding, obtain nano zirconium oxide powder; (2) by blended to nano zirconium oxide powder obtained for step (1) and polyacrylonitrile resin, inorganic oxide zirconium fiber is obtained; (3) the inorganic oxide zirconium fiber obtained in step (2) is mixed with diadust, binding agent respectively as toughner, be pressed into test block; (4) test block of step (3) compression moulding and transmission medium are assembled into Synthetic block, obtain polycrystalline diamond by sintering.Compared with prior art, the standby polycrystalline diamond production technique of legal system of the present invention is more simple, and raw material is easy to get, and production cost is low.
Description
Technical field
The invention belongs to superhard material and manufacture field, being specifically related to a kind of take Zirconium oxide fibre as polycrystalline diamond of toughness reinforcing phase and preparation method thereof.
Background technology
Polycrystalline diamond PCD (Polycrystallinediamond) sinters at high temperature under high pressure with fine particle diamond and forms, this product tool has good wearability, thermostability, ultimate compression strength and toughness, is widely used in the fields such as geological prospecting, oil production, natural gemstone processing industry and mechanical workout dressing tool.
Along with the progress of Materials science, the hardness of polycrystalline diamond, wear resistance, toughness and intensity are had higher requirement, desirable polycrystalline diamond composite material should both have high hardness, wear resistance, be conducive to improving its working efficiency, the toughness simultaneously had again, makes it can bear large surging force.If poor toughness, easily occur " tipping " phenomenon in use procedure, not only can destroy workpiece to be machined, even occur the injury accident to equipment damage or operator, must stop the course of processing, the PCD goods more renewed, cause production cost obviously to increase.
Chinese patent 201110148812.7 discloses the preparation method that a kind of carbon nanotube strengthens diamond compact material, carbon nanotube and the disperse such as diadust and caking agent ground is made to mix the starting material becoming polycrystalline diamond layer equably through more than half wet mixing, the PDC of carbon nanotube enhancing is created by High Temperature High Pressure sintering process and suitable thermal treatment process, on the basis not reducing PDC wear resistance, significantly improve toughness and the stability of PDC material.Chinese patent 200910175257.X also discloses a kind of method that nanometer round onions head-carbon high-temp high pressure prepares polycrystalline diamond sintered body.The like product that its sintering temperature, pressure comparison do raw material with diamond particles obviously reduces, and thus makes it have high tenacity.Chinese patent 201110001815.8 by increasing transition layer between polycrystalline diamond layer and hard alloy layer, and transition layer can be individual layer also can be multilayer.According to different objects, the moiety of transition layer is also different.Owing to adding transition layer between polycrystalline diamond layer and hard alloy layer, the interface cohesion situation of polycrystalline diamond compacts (PDCs) can not only be improved, reduce interfacial stress, synchronously can also improve wear resistance and the toughness of polycrystalline diamond compacts (PDCs).These diverse ways enhance the toughness of polycrystalline diamond instrument all in various degree above, improve the work-ing life of polycrystalline diamond instrument.But above method also exists complex manufacturing or the higher problem of raw material production cost.Therefore, by more simple, that raw materials cost the is lower polycrystalline diamond material of the production technique of additive method development of new, there is realistic meaning.
Summary of the invention
For problems of the prior art, the invention provides a kind of take Zirconium oxide fibre as polycrystalline diamond of toughness reinforcing phase and preparation method thereof, this preparation method makes full use of the tensility of organic matrix, significantly improve Zirconium oxide fibre performance, fracture toughness property is good, shock resistance high to utilize it to have as polycrystalline diamond prepared by toughner, and production technique is simple, cost is lower.
For achieving the above object, the present invention is by the following technical solutions:
A kind of take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprise the steps: that (1) take basic zirconium chloride as raw material, continuous measurement method is adopted to add ammoniacal liquor or oxalic acid, continuously stirring heating forms transparent colloidal sol gradually, then extremely use Silver Nitrate reagent test without chlorion by water and washing with alcohol successively, at microwave sintering kiln roasting after drying grinding, obtain nano zirconium oxide powder; (2) by nano zirconium oxide powder obtained for step (1) and polyacrylonitrile resin blended, then prepare organic inorganic hybridization fiber through solvent spinning, then through thermostabilization, charing, obtain inorganic oxide zirconium fiber; (3) the inorganic oxide zirconium fiber obtained in step (2) is mixed with diadust, binding agent respectively as toughner, be pressed into test block; (4) test block of step (3) compression moulding and transmission medium are assembled into Synthetic block, obtain polycrystalline diamond by sintering.
In described step (1), the mol ratio of basic zirconium chloride and ammoniacal liquor or oxalic acid is 1:0.5 ~ 2.0, the temperature of stirring heating is 60 ~ 99 DEG C, maturing temperature is 700 ~ 1500 DEG C, and roasting soaking time is 0.5 ~ 2.0h, and the particle diameter of gained nano zirconium oxide powder is 10 ~ 190nm.
Thermostabilization in described step (2) and charing will be carried out stage by stage, carry out during described organic inorganic hybridization fiber thermostabilization in the air of drying, are that 10 DEG C/h is warming up to 210 ~ 320 DEG C of insulation 0.5-2h according to temperature rise rate; Then carbonize, be warming up to 1200 ~ 1800 DEG C according to the temperature rise rate of 20 ~ 40 DEG C/h, roasting 1 ~ 4h obtains inorganic oxide zirconium fiber.
The particle diameter of diadust has three kinds of distributions in described step (3), and massfraction proportioning is: particle diameter 2-8 μm scope account for 5% ~ 30%, particle diameter 15-25 μm scope account for 35% ~ 70%, particle diameter 35-45 μm scope account for 15% ~ 45%; During the mixing of diadust, inorganic oxide zirconium fiber and binder phase, massfraction is respectively diadust 55% ~ 95%, toughner 0.5% ~ 15%, binding agent 2% ~ 35%.
Binding agent in described step (3) is at least one in silica flour, boron powder, nickel powder or cobalt powder, and its purity is all greater than 99%, and particle diameter is not more than 10 microns.
Be the test block of compression moulding put in the molybdenum cup of salt tube shield layer isolation in described step (4), then put the molybdenum cup installed into graphite jig, finally load agalmatolite cavity, end socket, is assembled into Synthetic block; Sintering adopts cubic pressure machine equipment to synthesize, and pressure is 4.5 ~ 7.5GPa, and temperature is 1250 ~ 1500
oc, generated time is 5 ~ 30 minutes.
The microhardness of polycrystalline diamond obtained is according to the method described above HV4150-8620, and impelling strength is 426-890 time.
Compared with prior art, the present invention has following advantage: the method 1. adopting preparing zirconium oxide fibers through inorganic hybridization of organic polymer, makes full use of the tensility of organic matrix, significantly improves Zirconium oxide fibre performance; 2. fracture toughness property is good, shock resistance high to utilize Zirconium oxide fibre to have as polycrystalline diamond prepared by toughner, can greatly avoid tipping phenomenon, extend work-ing life; 3. the polycrystalline diamond production technique prepared of the method is more simple, and raw material is easy to get, and production cost is low.
Embodiment
Embodiment 1
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprises the steps: that (1) takes basic zirconium chloride 300g, and continuous measurement adds the ammoniacal liquor 100g that mass concentration is 25%, 75
oc continuously stirring heats, and forms transparent colloidal sol gradually, then respectively with water and washing with alcohol to Silver Nitrate reagent test without chlorion, drying and grinding, in microwave agglomerating furnace 1000
oc roasting insulation 1h, obtain nano zirconium oxide powder, median size is at 92 ± 21nm; (2) by the nano zirconium oxide powder of deionization and polyacrylonitrile resin blended, organic inorganic hybridization fiber is prepared again through solvent spinning, the organic inorganic hybridization fiber prepared through thermostabilization, charing, thermostabilization temperature is at 210 DEG C, and temperature rise rate is at 10 DEG C/h.The roasting at maturing temperature 1200 DEG C of fiber after thermostabilization, temperature rise rate controls at 30 DEG C/h, and soaking time is 2h, obtains inorganic oxide zirconium fiber; (3) select three kinds of adamantine admixed finepowders of particle diameter, the massfraction ratio in each comfortable admixed finepowder of diamond of different-grain diameter is: the mass percent of 2-8 μm of scope be 20%, 15-25 μm of scope be 50%, 35-45 μm of scope be 30%; Wherein diadust accounts for the massfraction ratio of raw material micro mist is 80%, Zirconium oxide fibre toughner 3%, the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 7% and 10%, above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block; (4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, put the salt pipe installed into graphite jig again, finally load agalmatolite cavity, end socket, is assembled into Synthetic block, dry in baking oven, polycrystalline diamond is obtained again by high pressure high temperature sintering, the actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.5GPa, and temperature is 1450
oc, generated time is 7 minutes.
The polycrystalline diamond material microhardness prepared according to the method described above is HV7650, and impelling strength is 691 times.
Embodiment 2
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprises the steps: that (1) takes basic zirconium chloride 150g, and continuous measurement adds the oxalic acid solution 750g that mass concentration is 10%, 80
oc continuously stirring heats, and forms transparent colloidal sol gradually, then respectively with water and washing with alcohol to Silver Nitrate reagent test without chlorion, drying and grinding, in microwave agglomerating furnace 1000
oc roasting insulation 1h, obtain nano zirconium oxide powder, median size is at 68 ± 20nm; (2) by the nano zirconium oxide powder of deionization and polyacrylonitrile resin blended, then prepare organic inorganic hybridization fiber through solvent spinning.The organic inorganic hybridization fiber prepared through thermostabilization, charing, thermostabilization temperature is 250
oc, temperature rise rate is 10
oc/h, the fiber after thermostabilization is at maturing temperature 1300
otemperature rise rate under C during roasting controls 20
oc/h, soaking time is 2h, obtains inorganic oxide zirconium fiber; (3) three kinds of adamantine admixed finepowders of particle diameter are selected, massfraction ratio in each comfortable admixed finepowder of diamond of different-grain diameter is: the mass percent of 2-8 μm of scope is 20%, 15-25 μm of scope be 50%, 35-45 μm of scope be 30%, the massfraction ratio that diadust accounts for raw material micro mist is 82%, Zirconium oxide fibre toughner 2%, the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 6% and 10%, above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block; (4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, put the salt pipe installed into graphite jig again, finally load agalmatolite cavity, end socket, is assembled into Synthetic block, dry in baking oven, polycrystalline diamond is obtained again by high pressure high temperature sintering, the actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.6GPa, temperature 1400
oc, generated time 9 minutes.
The polycrystalline diamond material microhardness prepared according to the method described above is HV7750, and impelling strength is 703 times.
Embodiment 3
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprises the steps: that (1) takes basic zirconium chloride 300g, and continuous measurement adds the ammoniacal liquor 100g that concentration is 25%, 85
oc continuously stirring heats, and forms transparent colloidal sol gradually, then respectively with water and washing with alcohol to Silver Nitrate reagent test without chlorion, drying and grinding, in microwave agglomerating furnace 900
oc roasting insulation 1.5h, obtain nano zirconium oxide powder, median size is at 92 ± 21nm; (2) by the nano zirconium oxide powder of deionization and polyacrylonitrile resin blended, then prepare organic inorganic hybridization fiber through solvent spinning.The organic inorganic hybridization fiber prepared through thermostabilization, charing, thermostabilization temperature is 280
oc, temperature rise rate is 10
oc/h, the fiber after thermostabilization is at maturing temperature 1350
otemperature rise rate under C during roasting controls 40
oc/h, soaking time is 2.5h, obtains inorganic oxide zirconium fiber; (3) three kinds of adamantine admixed finepowders of particle diameter are selected, massfraction ratio in each comfortable admixed finepowder of diamond of different-grain diameter is: the mass percent of 2-8 μm of scope is 20%, 15-25 μm of scope be 50%, 35-45 μm of scope be 30%, the massfraction ratio that diadust accounts for raw material micro mist is 80%, Zirconium oxide fibre toughner 3%, the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 9% and 8%, above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block; (4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, put the salt pipe installed into graphite jig again, finally load agalmatolite cavity, end socket, is assembled into Synthetic block, dry in baking oven, polycrystalline diamond is obtained again by high pressure high temperature sintering, the actual conditions wherein sintered adopts cubic pressure machine equipment to synthesize, and pressure is 5.4GPa, temperature 1430
oc, generated time 8 minutes.
The polycrystalline diamond material microhardness prepared according to the method described above is HV7460, and impelling strength is 658 times.
Embodiment 4
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprises the steps: that (1) takes basic zirconium chloride 150g, and continuous measurement adds the oxalic acid solution 750g that concentration is 10%, 80
oc continuously stirring heats, and forms transparent colloidal sol gradually, then respectively with water and washing with alcohol to Silver Nitrate reagent test without chlorion, drying and grinding, in microwave agglomerating furnace 1100
oc roasting insulation 1h, obtain nano zirconium oxide powder, median size is at 68 ± 20nm; (2) by the nano zirconium oxide powder of deionization and polyacrylonitrile resin blended, then prepare organic inorganic hybridization fiber through solvent spinning.The organic inorganic hybridization fiber prepared through thermostabilization, charing, thermostabilization temperature is 300
oc, temperature rise rate is 10
oc/h, the fiber after thermostabilization is at maturing temperature 1400
otemperature rise rate under C during roasting controls 40
oc/h, soaking time is 2h, obtains inorganic oxide zirconium fiber; (3) select three kinds of adamantine admixed finepowders of particle diameter, the massfraction ratio in each comfortable admixed finepowder of diamond of different-grain diameter is: the mass percent of 2-8 μm of scope be 20%, 15-25 μm of scope be 50%, 35-45 μm of scope be 30%.The massfraction ratio that diadust accounts for raw material micro mist is 82%, Zirconium oxide fibre toughner 3%, and the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 10% and 6%, above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block; (4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, put the salt pipe installed into graphite jig again, finally load agalmatolite cavity, end socket, is assembled into Synthetic block, dry in baking oven, polycrystalline diamond is obtained again by high pressure high temperature sintering, the actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.6GPa, temperature 1440
oc, generated time 10 minutes.
The polycrystalline diamond material microhardness prepared according to the method described above is HV7790, and impelling strength is 641 times.
Embodiment 5
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprises the steps: that (1) takes basic zirconium chloride 150g, and continuous measurement adds the oxalic acid solution 750g that concentration is 10%, 82
oc continuously stirring heats, and forms transparent colloidal sol gradually, then extremely uses Silver Nitrate reagent test without chlorion by water and washing with alcohol respectively, drying and grinding, 900 DEG C of roasting insulation 2h in microwave agglomerating furnace, obtain nano zirconium oxide powder, median size is at 68 ± 20nm; (2) by the nano zirconium oxide powder of deionization and polyacrylonitrile resin blended, then prepare organic inorganic hybridization fiber through solvent spinning, the organic inorganic hybridization fiber prepared through thermostabilization, charing, thermostabilization temperature is 320
oc, temperature rise rate is 10
oc/h.Fiber after thermostabilization is at maturing temperature 1500
otemperature rise rate under C during roasting controls 40
oc/h, soaking time is 3h, obtains inorganic oxide zirconium fiber; (3) select three kinds of adamantine admixed finepowders of particle diameter, the massfraction ratio in each comfortable admixed finepowder of diamond of different-grain diameter is: the mass percent of 2-8 μm of scope be 20%, 15-25 μm of scope be 50%, 35-45 μm of scope be 30%.The massfraction ratio that diadust accounts for raw material micro mist is 70%, Zirconium oxide fibre toughner 10%, and the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 10% and 10%, above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block; (4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then put the salt pipe installed into graphite jig, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, then obtain polycrystalline diamond by high pressure high temperature sintering.The actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.7GPa, temperature 1430
oc, generated time 5 minutes.
The polycrystalline diamond material microhardness prepared according to the method described above is HV6736, and impelling strength is 610 times.
embodiment 6
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprise the steps: that (1) takes basic zirconium chloride 322.25g, continuous measurement method is adopted to add the ammoniacal liquor 87.62g that mass concentration is 20%, at 60 DEG C, continuously stirring heating forms transparent colloidal sol gradually, then extremely use Silver Nitrate reagent test without chlorion by water and washing with alcohol successively, after drying grinding, in microwave agglomerating furnace, 700 DEG C of roastings are incubated 0.5h, obtain the Zirconium powder that particle diameter is 10 nanometers; (2) by nano zirconium oxide powder obtained for step (1) and polyacrylonitrile resin blended, organic inorganic hybridization fiber is prepared again through solvent spinning, the organic inorganic hybridization fiber prepared is carried out thermostabilization in the air of drying, is that 10 DEG C/h is warming up to 210 DEG C of insulation 0.5h according to temperature rise rate; Then carbonize, the roasting at maturing temperature 1200 DEG C of the fiber after thermostabilization, temperature rise rate is 20 DEG C/h, and roasting 1h obtains inorganic oxide zirconium fiber; (3) the inorganic oxide zirconium fiber obtained in step (2) is mixed as toughner respectively with diadust, binding agent, wherein the particle diameter of diadust has three kinds of distributions, massfraction proportioning is: particle diameter 2-8 μm account for 5%, particle diameter 15-25 μm account for 50%, particle diameter 35-45 μm account for 45%; The massfraction ratio that diadust accounts for raw material micro mist is 95%, and Zirconium oxide fibre toughner is 0.5%, and the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 2% and 2.5%, mixes, and be pressed into test block according to aforementioned proportion; (4) test block of step (3) compression moulding is put in the molybdenum cup of salt tube shield layer isolation, put the salt pipe installed into graphite jig again, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, adopt cubic pressure machine equipment to synthesize, pressure is 4.5GPa, temperature 1250
oc, generated time 5 minutes, obtained polycrystalline diamond.
The microhardness of the polycrystalline diamond prepared according to the method described above is HV8620, and impelling strength is 426 times.
embodiment 7
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprise the steps: that (1) takes basic zirconium chloride 322.25g, continuous measurement method is adopted to add the oxalic acid 600g that mass concentration is 15%, at 85 DEG C, continuously stirring heating forms transparent colloidal sol gradually, then extremely use Silver Nitrate reagent test without chlorion by water and washing with alcohol successively, after drying grinding, in microwave agglomerating furnace, 1200 DEG C of roastings are incubated 1h, obtain the Zirconium powder that particle diameter is 120 nanometers; (2) by nano zirconium oxide powder obtained for step (1) and polyacrylonitrile resin blended, organic inorganic hybridization fiber is prepared again through solvent spinning, the organic inorganic hybridization fiber prepared is carried out thermostabilization in the air of drying, is that 10 DEG C/h is warming up to 280 DEG C of insulation 1.5h according to temperature rise rate; Then carbonize, the roasting at maturing temperature 1500 DEG C of the fiber after thermostabilization, temperature rise rate is 30 DEG C/h, and roasting 2h obtains inorganic oxide zirconium fiber; (3) the inorganic oxide zirconium fiber obtained in step (2) is mixed as toughner respectively with diadust, binding agent, wherein the particle diameter of diadust has three kinds of distributions, massfraction proportioning is: particle diameter 2-8 μm account for 30%, particle diameter 15-25 μm account for 55%, particle diameter 35-45 μm account for 15%; The massfraction ratio that diadust accounts for raw material micro mist is 55%, Zirconium oxide fibre toughner 15%, and the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 14% and 16%, mixes, and be pressed into test block according to aforementioned proportion; (4) test block of step (3) compression moulding is put in the molybdenum cup of salt tube shield layer isolation, put the salt pipe installed into graphite jig again, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, adopt cubic pressure machine equipment to synthesize, pressure is 5.6GPa, temperature 1300
oc, generated time 20 minutes, obtained polycrystalline diamond.
The microhardness of the polycrystalline diamond prepared according to the method described above is HV4150, and impelling strength is 863 times.
embodiment 8
The present embodiment take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, comprise the steps: that (1) takes basic zirconium chloride 322.25g, continuous measurement method is adopted to add the ammoniacal liquor 233.6g that mass concentration is 30%, at 99 DEG C, continuously stirring heating forms transparent colloidal sol gradually, then extremely use Silver Nitrate reagent test without chlorion by water and washing with alcohol successively, after drying grinding, in microwave agglomerating furnace, 1500 DEG C of roastings are incubated 2h, obtain the Zirconium powder that particle diameter is 190 nanometers; (2) by nano zirconium oxide powder obtained for step (1) and polyacrylonitrile resin blended, organic inorganic hybridization fiber is prepared again through solvent spinning, the organic inorganic hybridization fiber prepared is carried out thermostabilization in the air of drying, is that 10 DEG C/h is warming up to 320 DEG C of insulation 2h according to temperature rise rate; Then carbonize, the roasting at maturing temperature 1800 DEG C of the fiber after thermostabilization, temperature rise rate is 40 DEG C/h, and roasting 4h obtains inorganic oxide zirconium fiber; (3) the inorganic oxide zirconium fiber obtained in step (2) is mixed as toughner respectively with diadust, binding agent, wherein the particle diameter of diadust has three kinds of distributions, massfraction proportioning is: particle diameter 2-8 μm account for 10%, particle diameter 15-25 μm account for 60%, particle diameter 35-45 μm account for 30%; The massfraction ratio that diadust accounts for raw material micro mist is 55%, Zirconium oxide fibre toughner 10%, the massfraction ratio that binding agent silica flour and nickel powder account for raw material micro mist is respectively 19% and 16%, and above-mentioned raw materials micro mist is mixed in setting ratio, mix according to aforementioned proportion, and be pressed into test block; (4) test block of step (3) compression moulding is put in the molybdenum cup of salt tube shield layer isolation, put the salt pipe installed into graphite jig again, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, adopt cubic pressure machine equipment to synthesize, pressure is 7.5GPa, temperature 1500
oc, generated time 30 minutes, obtained polycrystalline diamond.
The microhardness of the polycrystalline diamond prepared according to the method described above is HV4340, and impelling strength is 890 times.
Claims (4)
1. one kind take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, it is characterized in that, comprise the steps: that (1) take basic zirconium chloride as raw material, continuous measurement method is adopted to add ammoniacal liquor or oxalic acid, continuously stirring heating forms transparent colloidal sol gradually, then extremely use Silver Nitrate reagent test without chlorion by water and washing with alcohol successively, at microwave sintering kiln roasting after drying grinding, obtain nano zirconium oxide powder; (2) by nano zirconium oxide powder obtained for step (1) and polyacrylonitrile resin blended, then prepare organic inorganic hybridization fiber through solvent spinning, then through thermostabilization, charing, obtain inorganic oxide zirconium fiber; (3) the inorganic oxide zirconium fiber obtained in step (2) is mixed with diadust, binding agent respectively as toughner, be pressed into test block; (4) test block of step (3) compression moulding and transmission medium are assembled into Synthetic block, obtain polycrystalline diamond by sintering;
In described step (1), the mol ratio of basic zirconium chloride and ammoniacal liquor or oxalic acid is 1:0.5 ~ 2.0, the temperature of stirring heating is 60 ~ 99 DEG C, maturing temperature is 700 ~ 1500 DEG C, and roasting soaking time is 0.5 ~ 2.0h, and the particle diameter of gained nano zirconium oxide powder is 10 ~ 190nm;
Thermostabilization in described step (2) and charing will be carried out stage by stage, carry out during described organic inorganic hybridization fiber thermostabilization in the air of drying, are that 10 DEG C/h is warming up to 210 ~ 320 DEG C of insulation 0.5-2h according to temperature rise rate; Then carbonize, be warming up to 1200 ~ 1800 DEG C according to the temperature rise rate of 20 ~ 40 DEG C/h, roasting 1 ~ 4h obtains inorganic oxide zirconium fiber;
The particle diameter of diadust has three kinds of distributions in described step (3), and massfraction proportioning is: particle diameter 2-8 μm scope account for 5% ~ 30%, particle diameter 15-25 μm scope account for 35% ~ 70%, particle diameter 35-45 μm scope account for 15% ~ 45%; During the mixing of diadust, inorganic oxide zirconium fiber and binder phase, massfraction is respectively diadust 55% ~ 95%, toughner 0.5% ~ 15%, binding agent 2% ~ 35%.
2. according to claim 1 take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, it is characterized in that: the binding agent in described step (3) is at least one in silica flour, boron powder, nickel powder or cobalt powder, its purity is all greater than 99%, and particle diameter is not more than 10 microns.
3. according to claim 1 and 2 take Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase, it is characterized in that: be the test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation in described step (4), put the molybdenum cup installed into graphite jig again, finally load agalmatolite cavity, end socket, is assembled into Synthetic block; Sintering adopts cubic pressure machine equipment to synthesize, and pressure is 4.5 ~ 7.5GPa, and temperature is 1250 ~ 1500
oc, generated time is 5 ~ 30 minutes.
4., according to the polycrystalline diamond taking Zirconium oxide fibre as the preparation method of the polycrystalline diamond of toughness reinforcing phase and obtain according to claim 3, it is characterized in that: the microhardness of described polycrystalline diamond is HV4150-8620, and impelling strength is 426-890 time.
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|---|---|---|---|---|
| CN102277510A (en) * | 2011-07-25 | 2011-12-14 | 哈尔滨工业大学 | Mixing method for preparation of diamond enhanced metal matrix composite material |
| CN103521132A (en) * | 2013-09-13 | 2014-01-22 | 中原工学院 | Synthesis technique of high-grade self-sharpening polycrystalline diamond |
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| CN103938133A (en) | 2014-07-23 |
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