The present invention relates to a method of making a cemented carbide with submicron WC grain size with a powder metallurgical technique including milling, pressing and sintering. The method includes milling all components except WC for about three hours, then adding the WC powder and milling for about ten additional hours. In this way a cemented carbide powder with acceptable low compacting pressure is obtained.
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#2# 1. A method of making a submicron cemented carbide powder comprising a plurality of components including submicron WC and binder metal, the powder having a low compacting pressure, the method comprising the steps of:
(i) pre-milling a mixture of components which does not include the WC for more than 2 hours;
(ii) adding the WC to the mixture of step (i) and milling for approximately 10 hours; and
(iii) drying the milled mixture to obtain a powder.
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According to the method of the present invention, the milling procedure is started with a >2 hours, preferably about 3 hours, pre-milling step including wet milling in ethanol with cemented carbide milling bodies of all components except of WC such as grain growth inhibitors, carbon black or tungsten powder, binder metal and pressing agent, respectively. The pre-milling step is followed by a further final milling step of about 10 hours with the WC powder included. The amount of milling bodies during the pre-milling and final milling shall be such that the weight ratio milling bodies: WC powder is about 4-7. The cemented carbide powder is then dried preferably by spray drying, pressed to inserts and sintered.
WC-powder with submicron grain size distribution according to the invention with no grains greater than 1.5 μm is prepared by milling/sieving such as in a jetmill-classifier. According to the present invention, a minimal change in grain size and/or grain size distribution results from the final milling step.
A submicron cemented carbide powder with the composition including WC and 0.5 weight % Cr, 0.4 weight % V and 10 weight % Co with a grain size of 0.4 μm were produced according to the invention. The milling was carried out in ethanol (0.3 l fluid per kg cemented carbide powder) in a 30 l mill with 120 kg milling balls. The batch size was 20 kg. An initial milling step was carried out with all components added (C3C2, VC and Co) except WC for approximately 3 hours. Furthermore, 0.4 kg (2 weight %) lubricant, was added to the slurry and the carbon content was adjusted with carbon black such that a binder phase alloyed with W having a CW-ratio of 0.85 is obtained. The milling procedure was then completed with a 10 hour final milling step with the raw WC material included. A well deagglomerated WC, dwc=0.4 μm (jetmilled and sieved) was used. After spray drying, inserts of the type N151.2-400-4E were compacted and sintered according to standard practice. A compacting pressure of 165 MPa (18% shrinkage) and excellent inserts with no crack tendencies were obtained. Furthermore dense sintered structures with no porosity and hardness HV3=1800 were obtained.
Cemented carbide tool inserts of the type N151.2-400-4 E were produced in the same way as in Example 1 but with the composition having 0.5 weight % Cr, 0.3 weight % V and 8 weight % Co. The same result as in Example 1 was obtained except that a compacting pressure of 170 MPa (18% shrinkage) and a hardness of HV3=1890 resulted.
Cemented carbide tool inserts of the type N151.2-400-4 E were produced in the same way as in Example 1 but with the composition having 0.5 weight % Cr, 0.3 weight % V and 10 weight % Co and a grain size of 0.6 μm. The same result as in Example 1 was obtained except that a compacting pressure of 160 MPa (18% shrinkage) and a hardness of HV3-1740 resulted.
Cemented carbide standard tool inserts of the type N151.2-400-4 E were produced with the same chemical composition, average grain size of WC and CW-ratio as in Example 1 but from powder manufactured with conventional ball milling techniques and with a milling time of 80 hours. Roughly the same physical properties (porosity A00; HV3=1820) were obtained as in Example 1, but a considerably higher compacting pressure resulted, 290 MPa, (18% shrinkage) and because of this inserts with pronounced crack and chipping tendencies were obtained.
The foregoing has described the principles, preferred embodiments and modes of operation of the present invention. However, the invention should not be construed as being limited to the particular embodiments discussed. Thus the above-described embodiments should be regarded as illustrative rather than restrictive, and it should be appreciated that variations may be made in those embodiments by workers skilled in the art without departing from the scope of the present invention as defined by the following claims.
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