CN1321940C - Precision rolling material of self-flexible silicon nitride ceramic wire rod and prepartion process thereof - Google Patents
Precision rolling material of self-flexible silicon nitride ceramic wire rod and prepartion process thereof Download PDFInfo
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- CN1321940C CN1321940C CNB2005100964154A CN200510096415A CN1321940C CN 1321940 C CN1321940 C CN 1321940C CN B2005100964154 A CNB2005100964154 A CN B2005100964154A CN 200510096415 A CN200510096415 A CN 200510096415A CN 1321940 C CN1321940 C CN 1321940C
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 84
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 39
- 239000000919 ceramic Substances 0.000 title claims abstract description 29
- 238000005096 rolling process Methods 0.000 title abstract description 12
- 238000000034 method Methods 0.000 title description 4
- 239000000843 powder Substances 0.000 claims abstract description 110
- 239000013078 crystal Substances 0.000 claims abstract description 43
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 30
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 30
- 238000003825 pressing Methods 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 30
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229940075624 ytterbium oxide Drugs 0.000 claims abstract description 15
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims abstract description 15
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 28
- 238000009413 insulation Methods 0.000 claims description 28
- 239000011812 mixed powder Substances 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 27
- 206010013786 Dry skin Diseases 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 18
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 16
- 239000012467 final product Substances 0.000 claims description 14
- 229910052779 Neodymium Inorganic materials 0.000 claims description 6
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 229910052765 Lutetium Inorganic materials 0.000 claims description 5
- 229910052772 Samarium Inorganic materials 0.000 claims description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract description 2
- 238000007731 hot pressing Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 230000003245 working effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to self-flexible silicon nitride ceramic wire precision rolling material of and a preparation method thereof. Firstly, ytterbium oxide powder is added to alpha phase silicon nitride powder, then is added with absolute ethyl alcohol or acetone to confect slurry, and is sintered at high temperature under nitrogen atmosphere to prepare beta-Si3N4 seed crystal after processed through ball milling and dried. Secondly, the alpha phase silicon nitride powder, rare earth oxide, the beta-Si3N4 crystal seed and titanium carbide are evenly mixed then are added with the absolute ethyl alcohol or the acetone to prepare the slurry which is formed by dry pressing after processed through ball milling and dried. Finally, the material formed by dry pressing is sintered by hot pressing at high temperature under nitrogen atmosphere, and the temperature is reduced to room temperature. The planishing roll material prepared according to the preparation method of the present invention has high toughness (8 to 11MPam<1/2>), strength (900 to 1100MPa of bending strength at ordinary temperature, 700 to 900MPa of bending strength at 1200 DEG C), hardness (90 to 94HRA) and abrasion resistance. The service life of the planishing roll material is 2 to 3 times longer than the service life of hard alloy wire planishing rolls, and the work efficiency of high-speed wire rolling mills can be greatly enhanced.
Description
Technical field
The present invention relates to a kind of preparation method of stupalith, particularly a kind of self-flexible silicon nitride ceramic wire rod finishing roll preparation methods.
Background technology
High-speed rod-rolling mill is with its accurate pass design, reasonable tension and kink control, do not have and turn round high-speed and continuous rolling mode and enough attrition resistant finishing rolls of milling train rigidity and employing pony roll footpath, the higher roll speed and the quality of product have been guaranteed, and finishing roll is the important component part in the high speed wire rod finishing block, plays key effect for the section precision and the surface quality that keep wire rod.
In the wire rod operation of rolling, steel billet is rolled into required section form and size with higher temperature (900～1250 ℃) and higher speed (more than the 50m/s) by finishing roll.Be the temperature of cooling roll, at operation of rolling kind needs ceaselessly to the water coolant of its jet surface certain pressure.Therefore finishing roll will bear higher shock load, rolling stress, frictional force, rapid heat cycle impact in the operation of rolling, and working conditions is very abominable, so just causes the loss even the inefficacy of finishing roll easily.Above factor all causes huge finishing roll materials consumption and changes finishing roll continually, and this has become one of bottleneck that restraining wire production normally carries out.
And the finishing roll material adopts tungsten carbide base carbide alloy to make mostly at present, and its main component is tungsten carbide particle and metal adhesive (often being cobalt).Although Hardmetal materials at room temperature has very high intensity and hardness, performances such as its intensity and hardness can raise and decline rapidly along with temperature.In the wire rod high-speed rolling process, the temperature of wire rod is at 700-1000 ℃, and also to produce a large amount of deformation heat in the deformation process, the degradation that causes Wimet, its metal adhesive also will be subjected to can taking place when contacting with the high temperature wire rod that passes through at a high speed the corrosive nature of oxygenizement and water coolant simultaneously, easily produce corrosion product particles such as oxide compound, aggravated the wearing and tearing of finishing roll after coming off.In addition, the composition of Wimet exists the place of contradiction in design, and desire improves its hardness and intensity, needs to add more wolfram varbide, this causes the toughness of material, the decline of thermal shock resistance again, shows the phenomenon that produces be full of cracks even broken roller at roll easily in the use.Above factor has all directly influenced the use of Wimet finishing roll.
Find that after deliberation for high line hot fine rolling roller, its material requirements is very strict, must have characteristics: 1, hot strength height; 2, good in oxidation resistance; 3, and be rolled between the material (iron and steel, non-ferrous metal etc.) and do not react; 4, high wearability (comprising anti-surface roughening ability); 5, good thermal shock; 6, toughness height; 7, ability of anti-deformation strong (high-temperature elastic modulus is big).
Compare with Wimet, stupalith all has superiority on the 1st, 2,3,4,5,7.In addition, because half of the not enough Wimet of the density of ceramic roll is that ceramic roll also has the effect that reduces labor intensity changing roll.In stupalith, can be at the normal material that uses of more than 1000 degree, and have both above-mentioned performance have only the silicon nitride series material.Thereby in order to overcome the deficiency of hard alloy roll performance, in nineteen nineties, Japan has proposed the imagination of full ceramic roll, and the patented technology of several enforcements has been arranged in order further to improve the quality of wire rod working (machining) efficiency and processing wire rod.Patent in 1993 (spy opens flat 5-337518) has proposed to make roll to improve the technology of heat-shock resistance with Sialon; At the deficiency of silicon nitride ceramics wear resistance, patent in 1997 (spy opens flat 9-278529) has proposed to disperse Cr in silicon nitride ceramics
2The N particle is to strengthen the technology of roll wearability; The special permission communique the dispersed carbon silicon carbide particle has been proposed in silicon nitride ceramics to increase the technology of wearability for No. 2920138; Another patent of Japan in 1998 has proposed to add the design (spy opens flat 10-101436) of high heat conductance AlN at the heat-shock resistance problem of pottery, has proposed to use Si
3N
4-Y
2O
3The technology of-MgO-AlN ceramic sintered bodies manufacturing revolution processing component; Hot strength at stupalith, the flat 10-81566 of patent EP0726236A2 and Te Kai has proposed to add Y and Yb element in silicon nitride, through sintering again 1100-1300 ℃ of tempering heat treatment to form the technology of crystal boundary J phase, to increase the hot strength of roll material.But these patents all are at the improvement of waiting to expect some aspect of performances, and the over-all properties of ceramic roll is the restriction that is subjected to the many aspects factor, and effect is unsatisfactory.
Summary of the invention
Order of the present invention is to overcome the shortcoming of above-mentioned prior art, and a kind of self-flexible silicon nitride ceramic wire rod finishing roll preparation methods with high tenacity, hot strength is provided.
For achieving the above object, the technical solution used in the present invention is: the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 8-20% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol or acetone is made into slurry with 1: 2 mass ratio, obtain powder 80-100 ℃ of following drying after ball milling 12-48 hour, this powder was made β-Si in 0.5～3 hour with 1550 ℃～1750 ℃ insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 55～80% α phase silicon nitride powder, 10～20% rare earth oxide, β-Si of 5～15%
3N
4The titanium carbide of crystal seed and 5-10% mixes, and then in this mixture, add dehydrated alcohol or acetone is mixed with slurry with 1: 2 mass ratio, obtain powder 80-100 ℃ of following drying after ball milling 12-48 hour, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 50-100MPa; With dry-pressing formed material pressure with 15-40MPa under nitrogen atmosphere, 1700-1800 ℃ sintering temperature insulation was reduced to room temperature with 400-800 ℃ of speed hourly and is got final product after 30-120 minute at last.
Rare earth oxide of the present invention is Lu, Yb, Y, Ce, Nd, Sm, Gd, the oxide compound of Dy or Er.
According to the finishing roll material that preparation method of the present invention makes, comprise the α phase silicon nitride powder of weight percent 55～80%, 10～20% rare earth oxide, β-Si of 5～15%
3N
4The titanium carbide of crystal seed and 5-10%.
Because silicon nitride is the strong covalent bond compound, ionicly only account for 0.3, and self-diffusion coefficient is very little, necessary volume diffusion of densification and crystal boundary velocity of diffusion are very little, its sintering motivating force Δ γ (Δ γ=Y
Sv/ Y
Gb, Y
SvBe the surface energy of powder, Y
GbCrystal boundary energy for sintered compact) very little, and at high temperature easily resolve into nitrogen and silicon, these inherent person's characters have just caused it to be difficult to densified sintering product, and must add small amounts of additives, make its at high temperature with the SiO of silicon nitride surface
2The reaction solution phase, in the hope of reaching dense sintering, and rare earth oxide can greatly improve the silicon nitride mechanical behavior under high temperature, so the present invention adds rare earth oxide and promotes material agglomerating densification and improve its high-temperature behavior in silicon nitride, add the hardness of titanium carbide raising material, thereby improve the work-ing life and the result of use of finishing wire roller, improve the production efficiency of high-speed rod-rolling mill.Do not exist by endergonic mechanism such as crystal boundary slippage and dislocations owing in the stupalith in addition, so, in order to improve the toughness of stupalith, added β-Si
3N
4Crystal seed utilizes β-Si
3N
4The anisotropy of grain growing obtains the β-Si of long column shape
3N
4Crystal grain.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1, at first the ytterbium oxide powder that adds α phase silicon nitride weight percent 8% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 100 ℃ of following dryings after 26 hours, and this powder was made β-Si in 3 hours with 1550 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 55% α phase silicon nitride powder, the oxide compound of 20% Lu, β-Si of 15%
3N
4Crystal seed and 10% titanium carbide mix, and then add dehydrated alcohol with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 85 ℃ of following dryings after 37 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 100MPa; With dry-pressing formed material pressure with 18MPa under nitrogen atmosphere, 1720 ℃ sintering temperature insulation was reduced to room temperature with 600 ℃ of speed hourly and is got final product after 100 minutes at last; The self-flexible silicon nitride ceramic wire rod finishing roll material of gained contains the α phase silicon nitride powder of weight percent 55%, the oxide compound of 20% Lu, β-Si of 15%
3N
4Crystal seed and 10% titanium carbide.
Embodiment 2, at first the ytterbium oxide powder that adds α phase silicon nitride weight percent 15% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add acetone with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 92 ℃ of following dryings after 12 hours, and this powder was made β-Si in 2.0 hours with 1620 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 80% α phase silicon nitride powder, the oxide compound of 10% Yb, β-Si of 5%
3N
4Crystal seed and 5% titanium carbide mix, and then add acetone with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 100 ℃ of following dryings after 12 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 80MPa; With dry-pressing formed material pressure with 36MPa under nitrogen atmosphere, 1750 ℃ sintering temperature insulation was reduced to room temperature with 400 ℃ of speed hourly and is got final product after 70 minutes at last; The self-flexible silicon nitride ceramic wire rod finishing roll material of gained contains the α phase silicon nitride powder of weight percent 80%, the oxide compound of 10% Yb, β-Si of 5%
3N
4Crystal seed and 5% titanium carbide.
Embodiment 3, at first the ytterbium oxide powder that adds α phase silicon nitride weight percent 10% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 85 ℃ of following dryings after 37 hours, and this powder was made β-Si in 0.8 hour with 1730 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 70% α phase silicon nitride powder, the oxide compound of 15% Y, β-Si of 6%
3N
4Crystal seed and 9% titanium carbide mix, and then add dehydrated alcohol with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 80 ℃ of following dryings after 48 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 60MPa; With dry-pressing formed material pressure with 25MPa under nitrogen atmosphere, 1700 ℃ sintering temperature insulation was reduced to room temperature with 700 ℃ of speed hourly and is got final product after 120 minutes at last; The self-flexible silicon nitride ceramic wire rod finishing roll material of gained contains the α phase silicon nitride powder of weight percent 70%, the oxide compound of 15% Y, β-Si of 6%
3N
4Crystal seed and 9% titanium carbide.
Embodiment 4, at first the ytterbium oxide powder that adds α phase silicon nitride weight percent 17% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add acetone with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 96 ℃ of following dryings after 48 hours, and this powder was made β-Si in 2.5 hours with 1580 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 65% α phase silicon nitride powder, the oxide compound of 18% Ce, β-Si of 10%
3N
4Crystal seed and 7% titanium carbide mix, and then add acetone with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 96 ℃ of following dryings after 26 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 90MPa; With dry-pressing formed material pressure with 15MPa under nitrogen atmosphere, 1780 ℃ sintering temperature insulation was reduced to room temperature with 500 ℃ of speed hourly and is got final product after 45 minutes at last; The self-flexible silicon nitride ceramic wire rod finishing roll material of gained contains the α phase silicon nitride powder of weight percent 65%, the oxide compound of 18% Ce, β-Si of 10%
3N
4Crystal seed and 7% titanium carbide.
Embodiment 5, at first the ytterbium oxide powder that adds α phase silicon nitride weight percent 13% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 80 ℃ of following dryings after 20 hours, and this powder was made β-Si in 0.5 hour with 1750 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 68% α phase silicon nitride powder, the oxide compound of 13% Nd, β-Si of 13%
3N
4Crystal seed and 6% titanium carbide mix, and then add dehydrated alcohol with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 92 ℃ of following dryings after 41 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 50MPa; With dry-pressing formed material pressure with 30MPa under nitrogen atmosphere, 1800 ℃ sintering temperature insulation was reduced to room temperature with 800 ℃ of speed hourly and is got final product after 30 minutes at last; The self-flexible silicon nitride ceramic wire rod finishing roll material of gained contains the α phase silicon nitride powder of weight percent 68%, the oxide compound of 13% Nd, β-Si of 13%
3N
4Crystal seed and 6% titanium carbide.
Embodiment 6, at first the ytterbium oxide powder that adds α phase silicon nitride weight percent 20% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add acetone with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 90 ℃ of following dryings after 41 hours, and this powder was made β-Si in 1.0 hours with 1700 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 70% α phase silicon nitride powder, the oxide compound of 12% Sm, β-Si of 8%
3N
4Crystal seed and 10% titanium carbide mix, and then add acetone with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 90 ℃ of following dryings after 20 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 70MPa; With dry-pressing formed material pressure with 40MPa under nitrogen atmosphere, 1760 ℃ sintering temperature insulation was reduced to room temperature with 570 ℃ of speed hourly and is got final product after 60 minutes at last; The self-flexible silicon nitride ceramic wire rod finishing roll material of gained contains the α phase silicon nitride powder of weight percent 70%, the oxide compound of 12% Sm, β-Si of 8%
3N
4Crystal seed and 10% titanium carbide.
Adopt the silicon nitride ceramic material of the finishing roll shape that method of the present invention makes, have characteristics such as high temperature resistant, high strength, high tenacity, high rigidity and high abrasion resistance.The finishing wire roller of employed self-flexible silicon nitride material preparation has characteristics such as high toughness, hot strength and hardness.Its fracture toughness property is 8-11MPam
1/2, intensity is (room temperature bending strength 900-1100MPa, bending strength 700-900MPa in the time of 1200 ℃), hardness is 90-94HRA.Be used to be made into the finishing wire roller, in the high speed hot rolling processing of metal wire, can reach the high effect of wire product quality that prolong, process work-ing life.Be applied in the actual production, self-toughening ceramic finishing wire roller is than improving 1-2 the work-ing life of Wimet finishing wire roller doubly.
Claims (8)
1, a kind of self-flexible silicon nitride ceramic wire rod finishing roll preparation methods is characterized in that:
1) the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 8-20% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol or acetone is made into slurry with 1: 2 mass ratio, obtain powder 80-100 ℃ of following drying after ball milling 12-48 hour, this powder was made 3-Si in 0.5～3 hour with 1550 ℃～1750 ℃ insulations under nitrogen atmosphere
3N
4Crystal seed;
Secondly 2) by weight percentage with 55～80% α phase silicon nitride powder, 10～20% rare earth oxide, β-Si of 5～15%
3N
4The titanium carbide of crystal seed and 5-10% mixes, and then in this mixture, add dehydrated alcohol or acetone is mixed with slurry with 1: 2 mass ratio, obtain powder 80-100 ℃ of following drying after ball milling 12-48 hour, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 50-100MPa;
3) at last with dry-pressing formed material pressure with 15-40MPa under nitrogen atmosphere, 1700-1800 ℃ sintering temperature insulation was reduced to room temperature with 400-800 ℃ of speed hourly and is got final product after 30-120 minute.
2, self-flexible silicon nitride ceramic wire rod finishing roll preparation methods according to claim 1, it is characterized in that: said rare earth oxide is Lu, Yb, Y, Ce, Nd, Sm, Gd, the oxide compound of Dy or Er.
3, self-flexible silicon nitride ceramic wire rod finishing roll preparation methods according to claim 1, it is characterized in that: the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 8% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 100 ℃ of following dryings after 26 hours, and this powder was made β-Si in 3 hours with 1550 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 55% α phase silicon nitride powder, the oxide compound of 20% Lu, β-Si of 15%
3N
4Crystal seed and 10% titanium carbide mix, and then add dehydrated alcohol with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 85 ℃ of following dryings after 37 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 100MPa; With dry-pressing formed material pressure with 18 MPa under nitrogen atmosphere, 1720 ℃ sintering temperature insulation was reduced to room temperature with 600 ℃ of speed hourly and is got final product after 100 minutes at last.
4, self-flexible silicon nitride ceramic wire rod finishing roll preparation methods according to claim 1, it is characterized in that: the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 15% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add acetone with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 92 ℃ of following dryings after 12 hours, and this powder was made β-Si in 2.0 hours with 1620 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 80% α phase silicon nitride powder, the oxide compound of 10% Yb, 5% 3-Si
3N
4Crystal seed and 5% titanium carbide mix, and then add acetone with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 100 ℃ of following dryings after 12 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 80MPa; With dry-pressing formed material pressure with 36MPa under nitrogen atmosphere, 1750 ℃ sintering temperature insulation was reduced to room temperature with 400 ℃ of speed hourly and is got final product after 70 minutes at last.
5, self-flexible silicon nitride ceramic wire rod finishing roll preparation methods according to claim 1, it is characterized in that: the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 10% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 85 ℃ of following dryings after 37 hours, and this powder was made β-Si in 0.8 hour with 1730 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 70% α phase silicon nitride powder, the oxide compound of 15% Y, β-Si of 6%
3N
4Crystal seed and 9% titanium carbide mix, and then add dehydrated alcohol with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 80 ℃ of following dryings after 48 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 60MPa; With dry-pressing formed material pressure with 25MPa under nitrogen atmosphere, 1700 ℃ sintering temperature insulation was reduced to room temperature with 700 ℃ of speed hourly and is got final product after 120 minutes at last.
6, self-flexible silicon nitride ceramic wire rod finishing roll preparation methods according to claim 1, it is characterized in that: the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 17% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add acetone with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 96 ℃ of following dryings after 48 hours, and this powder was made β-Si in 2.5 hours with 1580 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 65% α phase silicon nitride powder, the oxide compound of 18% Ce, β-Si of 10%
3N
4Crystal seed and 7% titanium carbide mix, and then add acetone with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 96 ℃ of following dryings after 26 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 90MPa; With dry-pressing formed material pressure with 15MPa under nitrogen atmosphere, 1780 ℃ sintering temperature insulation was reduced to room temperature with 500 ℃ of speed hourly and is got final product after 45 minutes at last.
7, self-flexible silicon nitride ceramic wire rod finishing roll preparation methods according to claim 1, it is characterized in that: the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 13% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add dehydrated alcohol with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 80 ℃ of following dryings after 20 hours, and this powder was made β-Si in 0.5 hour with 1750 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed; Secondly by weight percentage with 68% α phase silicon nitride powder, the oxide compound of 13% Nd, β-Si of 13%
3N
4Crystal seed and 6% titanium carbide mix, and then add dehydrated alcohol with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 92 ℃ of following dryings after 41 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 50MPa; With dry-pressing formed material pressure with 30MPa under nitrogen atmosphere, 1800 ℃ sintering temperature insulation was reduced to room temperature with 800 ℃ of speed hourly and is got final product after 30 minutes at last; The self-flexible silicon nitride ceramic wire rod finishing roll material of gained contains the α phase silicon nitride powder of weight percent 68%, the oxide compound of 13% Nd, β-Si of 13%
3N
4Crystal seed and 6% titanium carbide.
8, self-flexible silicon nitride ceramic wire rod finishing roll preparation methods according to claim 1, it is characterized in that: the ytterbium oxide powder that at first adds α phase silicon nitride weight percent 20% in α phase silicon nitride powder is made mixed powder, and then in mixed powder, add acetone with 1: 2 mass ratio and be made into slurry, ball milling obtained powder 90 ℃ of following dryings after 41 hours, and this powder was made β-Si in 1.0 hours with 1700 ℃ of insulations under nitrogen atmosphere
3N
4Crystal seed: secondly by weight percentage with 70% α phase silicon nitride powder, the oxide compound of 12% Sm, β-Si of 8%
3N
4Crystal seed and 10% titanium carbide mix, and then add acetone with 1: 2 mass ratio in this mixture and be mixed with slurry, and ball milling obtained powder 90 ℃ of following dryings after 20 hours, cross behind 80 mesh sieves powder that obtains dry-pressing formed under 70MPa; With dry-pressing formed material pressure with 40MPa under nitrogen atmosphere, 1760 ℃ sintering temperature insulation was reduced to room temperature with 570 ℃ of speed hourly and is got final product after 60 minutes at last.
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