CN101665881A - Method for preparing superfine hard alloy for PCB tools - Google Patents
Method for preparing superfine hard alloy for PCB tools Download PDFInfo
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- CN101665881A CN101665881A CN200910044493A CN200910044493A CN101665881A CN 101665881 A CN101665881 A CN 101665881A CN 200910044493 A CN200910044493 A CN 200910044493A CN 200910044493 A CN200910044493 A CN 200910044493A CN 101665881 A CN101665881 A CN 101665881A
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Abstract
The invention discloses a method for preparing a superfine hard alloy for PCB tools. The method comprises the steps of proportioning, wetly grinding, drying, forming by pressing and sintering at low pressure. The method is characterized in that WC-Co compound powder whose subgrain size is 50-100 nm is used as material for proportioning, Co powder is added or not to obtain a Co content of 5-10 wt%,0.1-1.0 wt% of Cr3C2 and 0.1-1.0 wt% of VC are also added, the carbon balance value for proportioning calculation is from 0.10% to 0.30%, the temperature for the sintering at low pressure is 1380-1420 DEG C, and the pressure is 7.5-10Mpa. The invention ensures that the prepared superfine hard alloy has uniform metallographical construction and no abnormal grown grains. The wearing resistance andthe hole site accuracy of the PCB tools made of the superfine hard alloy are largely improved.
Description
Technical field
The present invention relates to a kind of preparation method of Wimet, particularly a kind of PCB instrument ultrafine hard alloy preparation method.
Background technology
Wimet has purposes widely with its high rigidity and high strength, in adopting the little brill processing of PCB electronic devices and components industry, along with the continuous miniaturization of electronic devices and components, require little brill brill footpath of use also more and more littler, its requirement to little brill material is also just more and more higher.At present, the little drill tools of the PCB that uses on the market all is to adopt the ultra-fine cemented carbide of traditional hard alloy production process preparation to process, its technical process mainly is to adopt the ultrafine tungsten carbide raw material, and cobalt and a small amount of additive, by wet-milling, drying, compression moulding, sintering is prepared ultra-fine cemented carbide.Such as: Chinese patent " Wimet " (patent No. 200580013951.1) adopts and is no more than 0.3 micron WC is raw material, and it is that 0.3～0.7 micron WC is a raw material that Chinese patent " ultrafine hard alloy preparation method " (patent No. 200310110521.4) adopts Fisher particle size.Ultrafine powder raw material WC, Co etc. that these traditional preparation process ultra-fine cemented carbide methods adopt, specific surface area is big, the tungsten cobalt is difficult to mix in the Wimet of preparation, the ultra-fine cemented carbide of producing often exists metallurgical structure inhomogeneous, the easy appearance crystal grain of growing up unusually, it is not fine causing the wear resistance of cutter in the use and position, hole precision.
Summary of the invention
The present invention seeks to overcome above-mentioned traditional technology method, to prepare the metallurgical structure that ultra-fine cemented carbide exists inhomogeneous, easy appearance technological deficiencies such as crystal grain of growing up unusually, a kind of new PCB instrument ultrafine hard alloy preparation method is provided, make the ultra-fine cemented carbide metallurgical structure of preparation even, the no abnormal crystal grain of growing up, the wear resistance and position, the hole precision of the PCB instrument of producing with this ultra-fine cemented carbide gold improve greatly.
This PCB instrument ultrafine hard alloy preparation method of the present invention, comprise batching, wet-milling, dry, compression moulding, the low pressure sintering operation, the WC-Co composite powder of selecting for use subgrain to be of a size of 50～100nm when different is batching is a raw material, allocating into or not allocating the Co powder into and reach weight percent is 5～10% Co content, also allocates weight percent into and be 0.1～1.0% Cr
3C
2, weight percent is 0.1～1.0% VC, described Co powder, Cr
3C
2Powder and VC powder Fsss granularity are all less than 1.5 μ m, and the carbon balance value of charge calculation is+0.10～+ 0.30%, low pressure sintering temperature be 1380～1420 ℃, pressure is 7.5～10MPa.
The present invention preferentially selects be weight percentage 5～7% WC-Co composite powder of Co content for use when implementing.
The present invention is when implementing, and the ratio of grinding media to material of wet-milling is preferably 5～8: 1, and milling time is 60～100 hours.
Advantage of the present invention is that to select nano level WC-Co composite powder for use be raw material, and allocates proper C r into
3C
2, VC makes grain inhibitor, the WC mean grain size reaches (0.5～0.7) μ m in the ultra-fine cemented carbide that makes, the hardness of Wimet reaches HV
3: 1700～2000, bending strength TRS 〉=4000N/mm
2Owing to adopt 1380～1420 ℃ of low pressure sinterings, make Wimet can keep weave construction even, stable performance.It is mutually even that the Wimet that uses the inventive method to prepare has cobalt, grain growing is complete, have good fracture toughness property, can satisfy diameter is the use technology requirement of the little brill of the following PCB of 0.5mm, and little wear resistance and position, the hole precision that is drilled in the use that is processed into is fine.
Description of drawings
Fig. 1 is the SEM photo (10000 *) of the ultra-fine cemented carbide for preparing of the present invention;
Fig. 2 is the ultra-fine cemented carbide SEM photo (10000 *) that traditional technology is produced.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1: select the WC-Co composite powder that Co weight percent (below be abbreviated as wt%) is 5%, subgrain is of a size of 50～100nm for use, allocate the Cr3C2 of 1.0wt% into, the VC of 0.1wt%, the carbon balance value of charge calculation is+0.10%, the material for preparing is carried out wet-milling, the ratio of grinding media to material of wet-milling is 5～6: 1, and milling time is 60～70 hours.Compound after wet-milling technology routinely carries out drying, and being pressed into diameter is the excellent base of the little brill of PCB of 3.5mm, then the blank after the moulding is carried out low pressure sintering, and the agglomerating temperature is 1380～1420 ℃, and pressure is 7.5～8.5MPa.Reach 5200 holes work-ing life with the little little brill of 0.30mm that bores that rod is processed into of the qualified PCB of sinter molding.
The nano level WC-Co composite powder that the present invention selects for use is to adopt soluble tungsten salt to carry out molecular level with cobalt salt to be mixed with into tungsten cobalt composite powder precursor solution, spray-dried again or pyrolysis is prepared into tungsten cobalt composite powder oxidation of precursor thing, after carbonization and a kind of WC-Co composite powder raw material of being prepared into, superfine tungsten carbide and cobalt powder with respect to preparation Wimet use in the traditional method, nano level WC-Co composite powder has remarkable advantages on mixing uniformity, be aided with suitable production technique again, it is even to have a metallurgical structure with the ultra-fine cemented carbide of nano level WC-Co composite powder production, the no abnormal crystal grain of growing up, the little brill of PCB with (such as 0.3mm) below its preparation 0.5mm also just has tangible technical superiority, and the wear resistance of product and position, hole precision are better than traditional ultra-fine cemented carbide.
Embodiment 2: selecting Co content for use is the WC-Co composite powder that 6wt%, subgrain are of a size of 50～70nm, allocates the Cr of 0.6wt% into
3C
2, the VC of 0.3wt%, the carbon balance value of charge calculation is+0.15%, and the ratio of grinding media to material of wet-milling is 5～6: 1, and milling time is 60～70 hours.Compound after wet-milling technology routinely carries out drying, and being pressed into diameter is the excellent base of the little brill of PCB of 3.5mm, then the blank after the moulding is carried out low pressure sintering, and the agglomerating temperature is 1380～1420 ℃, and pressure is 7.5～8.5MPa.Reach 5700 holes work-ing life with the little little brill of 0.3mm that bores that rod is processed into of the qualified PCB of sinter molding.(all the other technological processs and controlled variable are with embodiment 1)
Embodiment 3: selecting Co content for use is the WC-Co composite powder that 7wt%, subgrain are of a size of 70～90nm, allocates the Co powder (the Fsss granularity is less than 1.5 μ m, and following examples are identical) of 1wt% into and reaches the Co content of 8wt%, allocates the Cr of 0.45wt% into
3C
2(the Fsss granularity is less than 1.5 μ m, and following examples are identical), (the Fsss granularity is less than 1.5 μ m for the VC of 0.55wt%, following examples are identical), the carbon balance value of charge calculation is+0.20%, and the material for preparing is carried out wet-milling, the ratio of grinding media to material of wet-milling is 6～7: 1, and milling time is 75～85 hours.Compound after wet-milling technology routinely carries out drying, and being pressed into diameter is the excellent base of the little brill of PCB of 3.5mm, then the blank after the moulding is carried out low pressure sintering, and the agglomerating temperature is 1380～1420 ℃, and pressure is 8.5～9.5MPa.Reach 6100 holes work-ing life with the little little brill of 0.3mm that bores that rod is processed into of the qualified PCB of sinter molding.(all the other technological processs and controlled variable are with embodiment 1)
Embodiment 4: selecting Co content for use is the WC-Co composite powder that 7wt%, subgrain are of a size of 80～100nm, allocates the Co powder of 2wt% into and reaches the Co content of 9wt%, allocates the Cr of 0.35wt% into
3C
2, the VC of 0.65wt%, the carbon balance value of charge calculation is+0.25%, and the material for preparing is carried out wet-milling, and the ratio of grinding media to material of wet-milling is 7～8: 1, and milling time is 85～95 hours.Compound after wet-milling technology routinely carries out drying, and being pressed into diameter is the excellent base of the little brill of PCB of 3.5mm, then the blank after the moulding is carried out low pressure sintering, and the agglomerating temperature is 1380～1420 ℃, and pressure is 9.0～9.5MPa.Reach 6700 holes work-ing life with the little little brill of 0.3mm that bores that rod is processed into of the qualified PCB of sinter molding.(all the other technological processs and controlled variable are with embodiment 1)
Embodiment 5: selecting Co content for use is the WC-Co composite powder that 7wt%, subgrain are of a size of 80～100nm, allocates the Co powder of 3wt% into and reaches the Co content of 10wt%, allocates the Cr3C of 0.1wt% into
2, the VC of 1.0wt%, the carbon balance value of charge calculation is+0.30%, and the material for preparing is carried out wet-milling, and the ratio of grinding media to material of wet-milling is 7～8: 1, and milling time is 95～100 hours.Compound after wet-milling technology routinely carries out drying, and being pressed into diameter is the excellent base of the little brill of PCB of 3.5mm, then the blank after the moulding is carried out low pressure sintering, and the agglomerating temperature is 1380～1420 ℃, and pressure is 9.0～10.0MPa.Reach 7000 holes work-ing life with the little little brill of 3.5mm that bores that rod is processed into of the qualified PCB of sinter molding.
The PCB instrument of embodiment 1～5 preparation is listed in table 1 with the physical and mechanical property of ultra-fine cemented carbide:
Table 1
| Embodiment | Density (g/cm 3) | ??Hc(KA/m) | ??Com(％) | ??TRS(N/mm 2) | ??HV 3 |
| ??1 | ??14.90 | ??31.6 | ??4.9 | ??4030 | ??1980 |
| ??2 | ??14.82 | ??29.3 | ??5.2 | ??4200 | ??1900 |
| ??3 | ??14.56 | ??27.5 | ??7.1 | ??4300 | ??1850 |
| ??4 | ??14.38 | ??25.4 | ??7.8 | ??4260 | ??1780 |
| ??5 | ??14.20 | ??23.3 | ??8.5 | ??4350 | ??1720 |
Claims (3)
1, a kind of PCB instrument ultrafine hard alloy preparation method, comprise batching, wet-milling, dry, compression moulding, the low pressure sintering operation, the WC-Co composite powder of selecting for use subgrain to be of a size of 50～100nm when it is characterized in that preparing burden is a raw material, allocating into or not allocating the Co powder into and reach weight percent is 5～10% Co content, also allocates weight percent into and be 0.1～1.0% Cr
3C
2, weight percent is 0.1～1.0% VC, described Co powder, Cr
3C
2Powder and VC powder Fsss granularity are all less than 1.5 μ m, and the carbon balance value of charge calculation is+0.10～+ 0.30%, low pressure sintering temperature be 1380～1420 ℃, pressure is 7.5～10MPa.
2. PCB instrument ultrafine hard alloy preparation method according to claim 1 is characterized in that the Co content of described WC-Co composite powder is weight percentage 5～7%.
3. PCB instrument ultrafine hard alloy preparation method according to claim 1 and 2, the ratio of grinding media to material that it is characterized in that described wet-milling is 5～8: 1, milling time is 60～100 hours.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818275A (en) * | 2010-05-11 | 2010-09-01 | 杭州天石硬质合金有限公司 | Preparation method of ultrafine hard alloy |
| CN102198514A (en) * | 2011-05-12 | 2011-09-28 | 中南大学 | Method for preparing ultrafine grain wolfram carbide/cobalt composite powder |
| CN103042257A (en) * | 2013-01-17 | 2013-04-17 | 河南省大地合金股份有限公司 | Micro drill for printed circuit board (PCB) and preparation method thereof |
| CN104451217A (en) * | 2013-09-17 | 2015-03-25 | 自贡硬质合金有限责任公司 | Preparation method of ultrafine cemented carbide |
| US9518308B2 (en) | 2013-12-23 | 2016-12-13 | King Fahd University Of Petroleum And Minerals | High-density and high-strength WC-based cemented carbide |
| CN109022997A (en) * | 2018-09-14 | 2018-12-18 | 河源富马硬质合金股份有限公司 | A kind of high tough high-wearing feature polycrystalline cemented carbide material |
| CN115896519A (en) * | 2022-11-16 | 2023-04-04 | 河南大地合金有限公司 | Method for preparing hard alloy from WC ultrafine powder and hard alloy |
-
2009
- 2009-10-09 CN CN200910044493A patent/CN101665881A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818275A (en) * | 2010-05-11 | 2010-09-01 | 杭州天石硬质合金有限公司 | Preparation method of ultrafine hard alloy |
| CN101818275B (en) * | 2010-05-11 | 2012-06-20 | 杭州天石硬质合金有限公司 | Preparation method of ultrafine hard alloy |
| CN102198514A (en) * | 2011-05-12 | 2011-09-28 | 中南大学 | Method for preparing ultrafine grain wolfram carbide/cobalt composite powder |
| CN102198514B (en) * | 2011-05-12 | 2012-11-07 | 中南大学 | Method for preparing ultrafine grain wolfram carbide/cobalt composite powder |
| CN103042257A (en) * | 2013-01-17 | 2013-04-17 | 河南省大地合金股份有限公司 | Micro drill for printed circuit board (PCB) and preparation method thereof |
| CN104451217A (en) * | 2013-09-17 | 2015-03-25 | 自贡硬质合金有限责任公司 | Preparation method of ultrafine cemented carbide |
| CN104451217B (en) * | 2013-09-17 | 2017-05-03 | 自贡硬质合金有限责任公司 | Preparation method of ultrafine cemented carbide |
| US9518308B2 (en) | 2013-12-23 | 2016-12-13 | King Fahd University Of Petroleum And Minerals | High-density and high-strength WC-based cemented carbide |
| CN109022997A (en) * | 2018-09-14 | 2018-12-18 | 河源富马硬质合金股份有限公司 | A kind of high tough high-wearing feature polycrystalline cemented carbide material |
| CN115896519A (en) * | 2022-11-16 | 2023-04-04 | 河南大地合金有限公司 | Method for preparing hard alloy from WC ultrafine powder and hard alloy |
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Application publication date: 20100310 |