CN102151839A - ThO2-containing nickel-base binding phase superfine metal ceramic powder and preparation method and application thereof - Google Patents

ThO2-containing nickel-base binding phase superfine metal ceramic powder and preparation method and application thereof Download PDF

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CN102151839A
CN102151839A CN 201110054428 CN201110054428A CN102151839A CN 102151839 A CN102151839 A CN 102151839A CN 201110054428 CN201110054428 CN 201110054428 CN 201110054428 A CN201110054428 A CN 201110054428A CN 102151839 A CN102151839 A CN 102151839A
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powder
tho
metal ceramic
superfine metal
tho2
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CN102151839B (en
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刘沙
许开华
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Shenzhen Gem High Tech Co Ltd
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Shenzhen Gem High Tech Co Ltd
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Abstract

The invention provides a ThO2-containing nickel-base binding phase superfine metal ceramic powder and a preparation method and application thereof. The preparation method disclosed by the invention comprises the steps of: preparing ThO2-containing nickel-base binding phase superfine powder by using a mixing ball milling and reduction process; then putting the obtained ThO2-containing nickel-base binding phase superfine powder into a mixing ball mill together with hard phase TiC powder, TiN powder, Mo powder and carbon black powder and a dispersing agent, a forming agent, a ball milling medium and the like; and after mixing ball milling for a certain time, preparing the mixture into the ThO2-containing nickel-base binding phase superfine metal ceramic powder. The ThO2-containing nickel-base binding phase superfine metal ceramic powder has simple process and low cost, reduces the tendency of nickel cell and ceramic grain gathering and growth easily caused after sintering of the traditional nickel-containing powder material, and has good wear resistance, rigidity, strength and fracture toughness. High-quality superfine metal ceramic material can be prepared by adopting the ThO2-containing nickel-base binding phase superfine metal ceramic powder disclosed by the invention.

Description

Contain ThO<sub〉2</sub〉nickel based binder phase superfine metal ceramic powders and its production and use
Technical field
The present invention relates to the cermet field, relate in particular to and contain ThO 2Nickel based binder phase superfine metal ceramic powders and its production and use.
Background technology
TiC/TiN base metal-ceramic material,, performance cheap because of its cost of material are comparatively excellent, are widely used as cutting tool, mould, wear part etc., are the ideal materials that substitutes some trade mark carbide alloy.Defectives such as because TiC/TiN base metal-ceramic material fragility is bigger, intensity is lower, and service life is short have limited the TiC/TiN base metal-ceramic material and have used widely.
The superfine metal ceramic material has the excellent comprehensive performance, is the important directions of current cermet material both at home and abroad research and development.Preparation superfine metal ceramic material must adopt high-quality superfine metal ceramic powder.Domestic most of enterprises are when preparation superfine metal ceramic powder at present, adopt the thicker pure nickel powder of granularity to make the bonding phase, but the thicker nickel powder (〉=1 μ m) of granularity is difficult to mix with superfine titanium carbide powder, molybdenum powder and carbon powder, this easily produces the nickel pond after causing the superfine metal ceramic post sintering, and increased cermet crystal grain and assemble the trend of growing up, thereby cause that the superfine metal ceramic product is second-rate, service life is lower.In addition, make the bonding phase with pure nickel powder, bonding does not contain dispersion-strengtherning phase particle in mutually, is difficult to guarantee the intensity of superfine metal ceramic product yet.Therefore, the superfine metal pottery be produced and new prescription and technology must be sought.
Summary of the invention
For addressing the above problem, the invention provides the ThO that contains of new prescription 2Nickel based binder phase superfine metal ceramic powders and its production and use, production technology is simple, with low cost, be suitable for conventional production, this superfine metal ceramic powders is used to prepare the superfine metal pottery can be reduced and easily produce nickel pond and crystal grain behind the sintering and assemble the trend of growing up, and improves superfine metal Standpoint of Ceramic Wear-resisting Function, hardness, bending strength and fracture toughness.
One aspect of the present invention provides a kind of ThO of containing 2The preparation method of nickel based binder phase superfine metal ceramic powders may further comprise the steps:
(1) contains ThO 2The preparation of nickel based binder phase superfines: with nickel oxalate or nickelous carbonate and ThO 2Powder is mixed with Ni-1wt%ThO 2Composition is put into agitating ball mill with rotating speed 200rpm ball milling 30 hours, the powder behind the ball milling is put into hydrogen reducing furnace reduce, and reduction temperature is 480 ℃, and hydrogen flowing quantity is 4m 3/ min, the recovery time is 90 minutes, makes powder reduction make ultra-fine Ni-1wt%ThO 2Powder;
(2) preparation of superfine metal ceramic powders: the ultra-fine Ni-1wt%ThO that will prepare 2TiC powder, TiN powder, Mo powder and hydrocarbon black powder are mixed with TiC-15wt%TiN-10wt% (Ni-1wt%ThO to powder mutually with hard 2)-10wt%Mo-0.6wt%C, with ball-milling medium absolute ethyl alcohol 400ml/kg, dispersant 0.3wt% oleic acid, binder 3wt% polyethylene glycol is put into agitating ball mill together, and the ball milling time is 20~40 hours, mixing speed is: 100~200rpm forms the stirring ball-milling slip;
(3) post processing: after the stirring ball-milling slip carried out powder and solution isolated by filtration, the powder after the filtration was 90 ℃ vacuum oven 1.5 hours, made to contain ThO 2Nickel based binder phase superfine metal ceramic powders.
Ni-1wt%ThO described in the present invention 2Be meant by Ni and ThO 2Be mixed and made into, wherein ThO 2Shared weight fraction is 1%, and the content of Ni element is except ThO 2Outside surplus.TiC-15wt%TiN-10wt% (Ni-1wt%ThO 2The understanding of)-10wt%Mo-0.6wt%C herewith, wherein the content of TiC is except TiN, Ni-1wt%ThO 2Surplus outside bonding phase, Mo and the carbon black.
Wherein, ThO 2Adding be the effect of playing dispersion-strengtherning, promptly can be subjected to the dislocation campaign of external force effect when distortion bonding in mutually to play the pinning effect, and the propagation of obstruction micro-crack to pottery.These effects help improving the intensity and the hardness of pottery.
Second aspect present invention provide a kind of prepare according to the method described above contain ThO 2Nickel based binder phase superfine metal ceramic powders.Preferably, the described ThO that contains 2Nickel based binder phase superfine metal ceramic powders Fisher particle size is 0.5~0.7 μ m.
Third aspect present invention provides the ThO that contains that will prepare according to the method described above 2Nickel based binder phase superfine metal ceramic powders is used to prepare the purposes of superfine metal pottery.
Compared with prior art, the present invention has following outstanding advantage:
(1) ThO that contains of the present invention 2Nickel based binder phase superfine metal ceramic powders, not only bonding and other hard mix more evenly mutually, and nickel based binder contains ThO in mutually 2The dispersion-strengtherning phase has reduced the nickel pond and the cermet crystal grain that easily produce behind the superfine metal ceramic post sintering and has assembled the trend of growing up.
(2) with the ThO that contains of the present invention 2Superfine metal ceramic abrasive resistance and hardness that nickel based binder phase superfine metal ceramic powders is prepared, bending strength and fracture toughness all improve a lot.
(3) preparation technology of the present invention is simple, and is with low cost, is suitable for conventional production.
The specific embodiment
The following stated is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Embodiment one
Preparation TiC-15wt%TiN-10wt% (Ni-1wt%ThO 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.
With the Fei Shi particle mean size is nickel oxalate (nickeliferous 31wt%) 400g of≤3 μ m, with the Fei Shi particle mean size be the ThO of≤1 μ m 2Powder 1.24g puts into agitating ball mill with rotating speed 200rpm ball milling 30 hours, and the powder behind the ball milling is put into hydrogen reducing furnace, is 4m at 480 ℃, hydrogen flowing quantity 3Under/min, 90 minutes the condition, making powder reduction make the Fei Shi particle mean size is the ultra-fine Ni-1wt%ThO of 0.8 μ m 2Powder is as the bonding phase of superfine metal pottery.
With the ultra-fine Ni-1wt%ThO for preparing 2Powder 100g, with the Fei Shi particle mean size be TiC powder 650g, TiN powder 150g, Mo powder 100g and the hydrocarbon black powder 6g of≤1 μ m, with ball-milling medium absolute ethyl alcohol 400ml/kg, dispersant 0.3wt% oleic acid, binder 3wt% polyethylene glycol together, putting into agitating ball mill, is 200rpm stirring ball-milling 20 hours with the mixing speed.
After the stirring ball-milling slip carried out powder and solution isolated by filtration, 90 ℃ vacuum oven 1.5 hours, making the Fei Shi particle mean size was the TiC-10wt% (Ni-1wt%ThO of 0.7 μ m 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.
Embodiment two
Preparation TiC-15wt%TiN-10wt% (Ni-1wt%ThO 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.
With the Fei Shi particle mean size is nickelous carbonate (nickeliferous 44wt%) 400g of≤3 μ m and the Fei Shi particle mean size ThO for≤1 μ m 2Powder 1.76g puts into agitating ball mill with rotating speed 200rpm ball milling 30 hours, and the powder behind the ball milling is put into hydrogen reducing furnace, is 4m at 480 ℃, hydrogen flowing quantity 3Under/min, 90 minutes the condition, making powder reduction make the Fei Shi particle mean size is the ultra-fine Ni-1wt%ThO of 0.8 μ m 2Powder is as the bonding phase of superfine metal pottery.
With the ultra-fine Ni-1wt%ThO for preparing 2Powder 100g, with the Fei Shi particle mean size be TiC powder 650g, TiN powder 150g, Mo powder 100g and the hydrocarbon black powder 6g of≤1 μ m, with ball-milling medium absolute ethyl alcohol 400ml/kg, dispersant 0.3wt% oleic acid, binder 3wt% polyethylene glycol together, putting into agitating ball mill, is 200rpm stirring ball-milling 20 hours with the mixing speed.
After the stirring ball-milling slip carried out powder and solution isolated by filtration, 90 ℃ vacuum oven 1.5 hours, making the Fei Shi particle mean size was the TiC-10wt% (Ni-1wt%ThO of 0.7 μ m 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.
Embodiment three
Preparation TiC-15wt%TiN-10wt% (Ni-1wt%ThO 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.
With the Fei Shi particle mean size is nickel oxalate (nickeliferous 31wt%) 400g of≤3 μ m, with the Fei Shi particle mean size be the ThO of≤1 μ m 2Powder 1.24g puts into agitating ball mill with rotating speed 200rpm ball milling 30 hours, and the powder behind the ball milling is put into hydrogen reducing furnace, is 4m at 480 ℃, hydrogen flowing quantity 3Under/min, 90 minutes the condition, making powder reduction make the Fei Shi particle mean size is the ultra-fine Ni-1wt%ThO of 0.8 μ m 2Powder is as the bonding phase of superfine metal pottery.
With the ultra-fine Ni-1wt%ThO for preparing 2Powder 100g, with the Fei Shi particle mean size be TiC powder 650g, TiN powder 150g, Mo powder 100g and the hydrocarbon black powder 6g of≤1 μ m, with ball-milling medium absolute ethyl alcohol 400ml/kg, dispersant 0.3wt% oleic acid, binder 3wt% polyethylene glycol together, putting into agitating ball mill, is 100rpm stirring ball-milling 40 hours with the mixing speed.
After the stirring ball-milling slip carried out powder and solution isolated by filtration, 90 ℃ vacuum oven 1.5 hours, making the Fei Shi particle mean size was the TiC-10wt% (Ni-1wt%ThO of 0.5 μ m 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.
Embodiment four
Preparation TiC-15wt%TiN-10wt% (Ni-1wt%ThO 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.
With the Fei Shi particle mean size is nickelous carbonate (nickeliferous 44wt%) 400g of≤3 μ m and the Fei Shi particle mean size ThO for≤1 μ m 2Powder 1.76g puts into agitating ball mill with rotating speed 200rpm ball milling 30 hours, and the powder behind the ball milling is put into hydrogen reducing furnace, is 4m at 480 ℃, hydrogen flowing quantity 3Under/min, 90 minutes the condition, making powder reduction make the Fei Shi particle mean size is the ultra-fine Ni-1wt%ThO of 0.8 μ m 2Powder is as the bonding phase of superfine metal pottery.
With the ultra-fine Ni-1wt%ThO for preparing 2Powder 100g, with the Fei Shi particle mean size be TiC powder 650g, TiN powder 150g, Mo powder 100g and the hydrocarbon black powder 6g of≤1 μ m, with ball-milling medium absolute ethyl alcohol 400ml/kg, dispersant 0.3wt% oleic acid, binder 3wt% polyethylene glycol together, putting into agitating ball mill, is 100rpm stirring ball-milling 40 hours with the mixing speed.
After the stirring ball-milling slip carried out powder and solution isolated by filtration, 90 ℃ vacuum oven 1.5 hours, making the Fei Shi particle mean size was the TiC-10wt% (Ni-1wt%ThO of 0.5 μ m 2)-10wt%Mo-0.6wt%C superfine metal ceramic powders.

Claims (4)

1. one kind contains ThO 2The preparation method of nickel based binder phase superfine metal ceramic powders is characterized in that, may further comprise the steps:
(1) contains ThO 2The preparation of nickel based binder phase superfines: with nickel oxalate or nickelous carbonate and ThO 2Powder is mixed with Ni-1wt%ThO 2Composition is put into agitating ball mill with rotating speed 200rpm ball milling 30 hours, the powder behind the ball milling is put into hydrogen reducing furnace reduce, and reduction temperature is 480 ℃, and hydrogen flowing quantity is 4m 3/ min, the recovery time is 90 minutes, makes powder reduction make ultra-fine Ni-1wt%ThO 2Powder;
(2) preparation of superfine metal ceramic powders: the described ultra-fine Ni-1wt%ThO that will prepare 2TiC powder, TiN powder, Mo powder and hydrocarbon black powder are mixed with TiC-15wt%TiN-10wt% (Ni-1wt%ThO to powder mutually with hard 2)-10wt%Mo-0.6wt%C, with ball-milling medium absolute ethyl alcohol 400ml/kg, dispersant 0.3wt% oleic acid, binder 3wt% polyethylene glycol is put into agitating ball mill together, and the ball milling time is 20~40 hours, mixing speed is: 100~200rpm forms the stirring ball-milling slip;
(3) post processing: after described stirring ball-milling slip carried out powder and solution isolated by filtration, the powder after the filtration was 90 ℃ vacuum oven 1.5 hours, made to contain ThO 2Nickel based binder phase superfine metal ceramic powders.
One kind according to claim 1 method prepare contain ThO 2Nickel based binder phase superfine metal ceramic powders.
3. the ThO that contains as claimed in claim 1 2Nickel based binder phase superfine metal ceramic powders is characterized in that, Fisher particle size is 0.5~0.7 μ m.
4. ThO that contains as claimed in claim 2 2Nickel based binder phase superfine metal ceramic powders is used to prepare the purposes of superfine metal pottery.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103350224A (en) * 2013-06-18 2013-10-16 江苏和昊激光科技有限公司 Special nickel metal ceramal powder for laser cladding of crankshaft
CN115323218A (en) * 2022-08-16 2022-11-11 自贡硬质合金有限责任公司 Light high-strength snow shoveling sheet and preparation method thereof

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CN104858436B (en) * 2014-02-21 2018-01-16 宁夏东方钽业股份有限公司 The preparation method of highly reliable Fabrication of High Specific Capacitance electrolytic capacitor tantalum powder

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CN101967594A (en) * 2010-10-27 2011-02-09 合肥工业大学 Titanium carbide-based hard alloy taking nickel-molybdenum alloy as adhesive and preparation method thereof

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GB1170520A (en) * 1966-11-30 1969-11-12 Sherritt Gordon Mines Ltd Production of Nickel-Thoria Powders
US4133680A (en) * 1976-05-27 1979-01-09 Babaskin Jury Z Method of producing dopant material for iron or nickel-base alloys
CN101333616A (en) * 2008-07-29 2008-12-31 华中科技大学 Whisker- toughened cermet cutting tool and method for preparing same
CN101967594A (en) * 2010-10-27 2011-02-09 合肥工业大学 Titanium carbide-based hard alloy taking nickel-molybdenum alloy as adhesive and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103350224A (en) * 2013-06-18 2013-10-16 江苏和昊激光科技有限公司 Special nickel metal ceramal powder for laser cladding of crankshaft
CN115323218A (en) * 2022-08-16 2022-11-11 自贡硬质合金有限责任公司 Light high-strength snow shoveling sheet and preparation method thereof
CN115323218B (en) * 2022-08-16 2024-04-26 自贡硬质合金有限责任公司 Light high-strength snow shoveling sheet and preparation method thereof

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