CN1911568A - Control method of powder oxygen content in manufacturing process of ultrafine hard alloy - Google Patents
Control method of powder oxygen content in manufacturing process of ultrafine hard alloy Download PDFInfo
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- CN1911568A CN1911568A CN 200610088494 CN200610088494A CN1911568A CN 1911568 A CN1911568 A CN 1911568A CN 200610088494 CN200610088494 CN 200610088494 CN 200610088494 A CN200610088494 A CN 200610088494A CN 1911568 A CN1911568 A CN 1911568A
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Abstract
The present invention is a method of controlling oxygen content in superfine hard alloy powder, and features that before or during ball milling, methyl benzotriazole in the amount of 0.1-2 wt% is added into the mixed powder material directly or through dissolving in organic solvent. The technological scheme of the present invention can control the oxygen content in superfine powder effective in 0.5-0.6 wt%, so as to avoid no-carbon phase in the alloy and raise the use performance of the superfine hard alloy obviously.
Description
Technical field
The present invention relates to the manufacturing of carbide alloy, relate in particular to the control method of superfine powder oxygen content in the manufacturing process of ultrafine hard alloy.
Background technology
Ultra-fine cemented carbide is owing to have high rigidity, high strength and high tenacity, and is widely used in making the precision bit of drill of metal cutting and precision instruments such as little brill that milling cutter, printed circuit board drilling are used, tape cutting knife.It is very little to make the ultra-fine raw-material granularity that ultra-fine cemented carbide adopted, and wherein the particle diameter of superfine tungsten carbide is 0.1～0.2 μ m, and the particle diameter of super-fine cobalt powder is 0.4～1.0 μ m.In these powder processes of processing, the rolling ball milling through 24～72 hours exists very big surface energy and distortion of lattice energy in the powder, and the activity of powder is stronger, is easy to the oxygen uptake oxidation.If oxidation is serious, even can cause the scarce carbon phase of appearance in the alloy, the appearance of this scarce carbon phase constitution is with the serviceability of severe exacerbation ultra-fine cemented carbide.Therefore, the instability of superfine powder oxygen content has brought very big difficulty for production high-quality ultra-fine cemented carbide.
Summary of the invention
The control method that the purpose of this invention is to provide superfine powder oxygen content in a kind of manufacturing process of ultrafine hard alloy is intended to effectively solve the problem that superfine powder causes the superfine powder oxygen content to exceed standard, cause the alloy serviceability to descend because of the oxygen uptake oxidation in the alloy production process.
Purpose of the present invention is achieved through the following technical solutions:
The control method of powder oxygen content in the manufacturing process of ultrafine hard alloy, various raw material are made into mixed powder and add wet grinding media by certain weight ratio, carry out ball milling a few hours, powder mixes the forming agent press forming again through super-dry behind the ball milling, sintering gets finished product, it is characterized in that: before ball milling or in the mechanical milling process, also add TTA.
Further, the control method of powder oxygen content in the above-mentioned manufacturing process of ultrafine hard alloy, described TTA dissolves in organic solvent earlier, and then joins by in the middle of the composite material of ball milling.
Again further, the control method of powder oxygen content in the above-mentioned manufacturing process of ultrafine hard alloy, the addition of TTA are 0.1～2% of mixed powder weight.
Further, the control method of powder oxygen content in the above-mentioned manufacturing process of ultrafine hard alloy, described wet grinding media are any one or any two kinds mixture or three kinds the mixture in industrial alcohol, acetone, the n-hexane; Described raw material comprise tungsten carbide powder, and the grain specification of tungsten carbide powder is of a size of sub-micro thin level 0.5～0.8 μ m or ultra-fine level 0.2～0.5 μ m or nanoscale＜0.2 μ m.
The outstanding substantive distinguishing features and the obvious improvement of technical solution of the present invention is mainly reflected in:
1. before ball milling or in the mechanical milling process, in mixed powder, add TTA, can effectively control the oxygen content of superfine powder, thereby the carbon content of more accurate control ultra-fine cemented carbide, avoid occurring in the alloy lacking the carbon phase, the quality of stable alloy, the serviceability of prepared ultra-fine cemented carbide significantly improves;
2. this scheme enforcement easy and simple to handle, easy is applicable to the processing and manufacturing of various precision instruments such as the precision bit of drill of metal cutting and little brill that milling cutter, printed circuit board drilling are used, tape cutting knife, applied range, and economic benefit is very remarkable.
The specific embodiment
In order effectively to solve the problem that superfine powder causes the superfine powder oxygen content to exceed standard, cause the alloy serviceability to descend because of the oxygen uptake oxidation in production processes such as ball milling, storage, the invention provides the control method of superfine powder oxygen content in a kind of manufacturing process of ultrafine hard alloy.
The main process of manufacturing process of ultrafine hard alloy is: at first various raw material are made into mixed powder by certain weight ratio, add wet grinding media then and carry out ball milling, the ball milling powder is through super-dry and mix the forming agent press forming after a few hours, and last sintering gets hard alloy finished product.Main feature of the present invention is in the above-mentioned process, so that oxygen content is controlled, to guarantee the quality of ultra-fine cemented carbide finished product at ball milling operation adding TTA.
During concrete enforcement, generally comprised tungsten carbide powder in the middle of the raw material, the grain specification of this tungsten carbide powder can be the thin level of sub-micro 0.5～0.8 μ m, or ultra-fine level 0.2～0.5 μ m, or nanoscale＜0.2 μ m.Before ball milling or in the mechanical milling process, both can directly add TTA, also can in advance TTA be dissolved in the middle of organic solvents such as acetone, n-hexane, and then join the ball milling system.Wet grinding media be in industrial alcohol, acetone, the n-hexane any one, two or three mixture.
Usually, the addition of TTA is 0.1～2% of a raw material mixed powder weight.After the adding, TTA is adsorbed on the superfine powder surface, changes the state of charge and the interfacial property on superfine powder surface on the one hand, and ultra-fine grain surface energy state is tended towards stability, and slows down oxidation rate; The TTA molecule that is adsorbed on the other hand forms layer protecting film in the metal surface, hinders the electric charge relevant with oxidation reaction or the transfer of material, and the oxidation rate of powder is obviously reduced.Be adsorbed on the organic protective film on superfines surface, except in mechanical milling process, playing the effect that prevents the powder oxidation, can continue to play a role at the storage stage (not before the press forming) of powder, thereby delay the powder oxidation.Comparative test result shows that the oxygen content that does not add the mixed powder of TTA is 1.0～1.2% (percentage by weights), and the oxygen content that has added the mixed powder of TTA is reduced to 0.5～0.6% (percentage by weight).
" embodiment one "
It is ultrafine tungsten carbide (WC) powder of 0.2 μ m and ultra-fine cobalt (Co) powder that granularity is 0.8 μ m that raw material adopt granularity, by weight WC: Co=9: 1 is made into mixed powder puts in the ball grinder, the weight ratio of alloying pellet and mixed powder is 5: 1, the per kilogram mixed powder adds the alcohol of 350ml, press 0.5% of mixed powder weight again and add TTA, ball milling 48 hours, powder behind the ball milling is dry under 100 ℃ temperature, mix the forming agent press forming after the drying again, 1390 ℃ of following sintering 60min in the low pressure sintering stove get finished product.
" Comparative Examples "
Except not adding the TTA, other condition and embodiment one are identical, make finished product to contrast.
After testing, embodiment one and Comparative Examples gained ultra-fine cemented carbide performance indications separately are as shown in table 1.
Table 1
| Oxygen content (%) | Density (g/cm 3) | Hardness (HV10) | Bending strength (MPa) | Porosity (100X) | |||
| A | B | C | |||||
| Embodiment one | 0.58 | 14.47 | 2055 | 3689 | 02 | 00 | 00 |
| Comparative Examples | 1.08 | 14.38 | 1972 | 2824 | 04 | 00 | 00 |
From the listed data of table 1 as can be seen, adopt after the technical solution of the present invention, oxygen content obviously reduces, and the alloy bending strength significantly improves, and porosity also decreases, and promptly 100 power microscopes are observed the visual field following hole quantity of 10 μ m and reduced to some extent.
More than by instantiation technical solution of the present invention has been done to further specify, the example that provides only is an exemplary applications, can not be interpreted as a kind of restriction to claim protection domain of the present invention.
Claims (5)
1. the control method of powder oxygen content in the manufacturing process of ultrafine hard alloy, various raw material are made into mixed powder and add wet grinding media by certain weight ratio, carry out ball milling a few hours, powder mixes the forming agent press forming again through super-dry behind the ball milling, sintering gets finished product, it is characterized in that: before ball milling or in the mechanical milling process, also add TTA.
2. the control method of powder oxygen content in the manufacturing process of ultrafine hard alloy according to claim 1 is characterized in that: described TTA dissolves in organic solvent earlier, and then joins by in the middle of the composite material of ball milling.
3. the control method of powder oxygen content in the manufacturing process of ultrafine hard alloy according to claim 1 and 2 is characterized in that: the addition of described TTA is 0.1～2% of a mixed powder weight.
4. the control method of powder oxygen content in the manufacturing process of ultrafine hard alloy according to claim 1 is characterized in that: described wet grinding media is any one or any two kinds mixture or three kinds the mixture in industrial alcohol, acetone, the n-hexane.
5. the control method of powder oxygen content in the manufacturing process of ultrafine hard alloy according to claim 1, it is characterized in that: described raw material comprise tungsten carbide powder, and the grain specification of tungsten carbide powder is of a size of sub-micro thin level 0.5～0.8 μ m or ultra-fine level 0.2～0.5 μ m or nanoscale＜0.2 μ m.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106312074A (en) * | 2016-08-25 | 2017-01-11 | 苏州赛特锐精密机械配件有限公司 | Preparation method for superfine hard alloy cutter blank with preformed cutter groove |
| CN106544538A (en) * | 2016-12-23 | 2017-03-29 | 苏州新锐合金工具股份有限公司 | The control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process |
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| JPS5943962B2 (en) * | 1978-06-06 | 1984-10-25 | 東洋紡績株式会社 | Method for producing ultrafine metal powder |
| JPS61136606A (en) * | 1984-12-06 | 1986-06-24 | Toyobo Co Ltd | Production of ultrafine powder |
| US6030429A (en) * | 1996-08-06 | 2000-02-29 | Toyo Kohan Co., Ltd. | Hard sintered alloy |
| CN1212191A (en) * | 1997-09-23 | 1999-03-31 | 上海华明高技术（集团）有限公司 | Method for manufacturing WC/CO composite nanometre powder |
| CN100443219C (en) * | 2001-06-26 | 2008-12-17 | 中国科学院长春应用化学研究所 | Tungsten aluminium carbide hard alloy nanometer powder preparation method |
| CN1207121C (en) * | 2002-10-30 | 2005-06-22 | 株洲硬质合金集团有限公司 | Method for preventing super fine hard alloy from oxidation in producing process |
| CN1687336B (en) * | 2005-04-06 | 2010-10-13 | 上海纳克润滑技术有限公司 | High temperature composite additive for chain oil and preparation method thereof |
| CN100507038C (en) * | 2006-01-17 | 2009-07-01 | 武汉理工大学 | Preparation process of tungsten carbide/inhibitor composite powder and superfine hard alloy thereof |
| CN1817516A (en) * | 2006-03-17 | 2006-08-16 | 金川集团有限公司 | Production of superfine cobalt powder by air-flow breaking process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106312074A (en) * | 2016-08-25 | 2017-01-11 | 苏州赛特锐精密机械配件有限公司 | Preparation method for superfine hard alloy cutter blank with preformed cutter groove |
| CN106312074B (en) * | 2016-08-25 | 2018-02-02 | 苏州赛特锐精密机械配件有限公司 | A kind of preparation method of the preforming cutter groove solid tool base substrate of ultra-fine cemented carbide |
| CN106544538A (en) * | 2016-12-23 | 2017-03-29 | 苏州新锐合金工具股份有限公司 | The control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process |
| CN106544538B (en) * | 2016-12-23 | 2018-09-07 | 苏州新锐合金工具股份有限公司 | The control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process |
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