CN105441815A - Preparation method for modified superfine low-oxygen water-atomized alloy powder used for diamond tool - Google Patents
Preparation method for modified superfine low-oxygen water-atomized alloy powder used for diamond tool Download PDFInfo
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Abstract
The invention discloses a preparation method for modified superfine low-oxygen water-atomized alloy powder used for a diamond tool. The alloy matrix powder for a tool bit of the diamond tool can be manufactured through the method. The preparation method has the characteristics that the alloy powder is modified by adding multiple strengthening elements and the bending strength of a sintered matrix is improved at the same time; the superfine-grained alloy powder is manufactured through an ultrahigh-pressure water atomization technology, the alloy powder sintering compaction is lowered while the composition uniformity of single powder; the low-oxygen-content alloy powder is obtained through control over a smelting technique and a reduction technique, and the compactness of the sintered matrix is improved.
Description
Technical field
The invention belongs to field of powder metallurgy, relate to a kind of preparation method of diamond tool modified superfine hypoxemia water atomization powdered alloy.Its feature is 3-8 micron in oxygen level lower than 2000ppm, D50, spheroidization particle, powder size normal distribution.Through carbide forming element and rare-earth element modified, alloy has more high-flexural strength and to adamantine hold.
Background technology
Diamond tool is widely used in the processing of the hard and fragile material such as stone material, building materials, refractory materials, pottery, semi-conductor, magneticsubstance, matrix material; most employing mixed metal powder or pre-alloyed powder are binding agent, with the manufacture of diamond particles mixing hot pressed sintering.
The Matrix Wear Resistance that binding agent sintering is formed requires and processed object material matching.If wear resistance is too high, although tool life promotes, working (machining) efficiency can decline, and even causes instrument not use; In like manner, wear resistance is too low, although tool processes efficiency improves, and the corresponding shortening in work-ing life of instrument.
Diamond tool has strict demand to the working (machining) efficiency in its use procedure and life-span simultaneously, and this just requires that the metal-powder performance as carcass must take into account this two aspects simultaneously.The various factors such as Matrix Wear Resistance is subject to powdered ingredients used, oxygen level, size composition, sintered compact bending strength, hardness, be mingled with.
The carcass bending strength that diamond tool requires needs to be greater than 900MPa, otherwise carcass toughness is not enough, easily crackedly in the course of processing causes tool failures.Generally speaking, the higher carcass of bending strength is better to adamantine hold.The compound prescription of the elements such as Fe, Ni, Cu, Sn has higher cost performance in diamond tool field, but its sintered compact bending strength is all at about 1400MPa; For process relatively more soft in the object of hard material time, after often occurring that wear resistance is too high and making the diamond fragmentation of exposure, carcass fails synchronously to wear and tear with diamond, causes the situation of tool processes inefficiency; Especially by the water atomized powder that melting is pre-alloyed, it is more obvious that this defect shows; For this problem, the brittlement phase increased in carcass is effective ways.
Summary of the invention
The object of the invention is by introducing Si in the Composition Design of pre-alloyed powder, carbide forming element, and rare earth element, in tissue of sintered body, form appropriate brittlement phase Fe-Si intermetallic compound, carbide, and YSi
2, improve sintered compact bending strength, make carcass possess moderate wear resistance, meet diamond tool for working (machining) efficiency and the requirement in work-ing life simultaneously.
For achieving the above object, powdered alloy Composition Design proportioning of the present invention is: Cu:27 ~ 67%, Ni:1 ~ 10%, Sn:1 ~ 10%, Si:0.05 ~ 8%, carbide forming element Ti:1 ~ 15%, Cr:1 ~ 20%, rare-earth elements La: 0.03 ~ 5%, Y:0.03 ~ 5%; Fe surplus.Oxygen content in power is less than 1000ppm.Manufacture method comprises: the technique such as smelting, water atomization, filter-press dehydration, vacuum-drying, reduction, screening, conjunction are criticized, vacuum packaging.Its operation steps concrete is as follows:
1) smelt: adopt medium-frequency induction furnace to smelt, its power controls between 180 ~ 240KW; Furnace lining material is magnesia, strictly will control addition sequence and the time of each metallic substance, first add Fe and Ni, add Cu when melting more than half in fusion process, changes clearly and adds Si and Sn; Finally be sequentially added into Cr, Ti, La, Y.Adopt unslaked lime slag making, complete covering alloy solution top layer, 5 ~ 15 minutes heat-preserving deoxidizings.Then control to be atomized after molten steel temperature is skimmed between 1550 ~ 1640 DEG C;
2) water atomization: the mode adopting two groups of nozzle Orthogonal Double V-arrangement secondary atomizations; The installation site of two groups of nozzles is mutually vertical at the line of horizontal plane; One-level atomization angle is 40 ± 1 °, and atomized water flow secondary atomization angle is 30 ± 1 °; The descending diameter 3 ~ 7mm of tundish molten steel, the atomized water flow control of first step atomizing nozzle at 40-80L/min, atomizing pressure 100-120MPa; The atomized water flow control of second stage atomizing nozzle is at 40-60L/min, and atomizing pressure controls at 60-95MPa.
3) filter-press dehydration: the sealed gas supercharging in powder collecting pot of the pigment mixture after atomization, bottom powder collecting pot, water outlet installs 1200 order filter clothes additional, and under 0.1 ~ 0.5MPa pressure, pressurize is to water outlet is discharged without obvious gas-vapor mix.
4) vacuum-drying: adopt DoubletaperedVacuumdrier, first loads moisture eliminator by the wet-milling after dehydration, and powder filling port seals, and starts vacuum pump, starts power switch and makes the vertical single direction rotation of moisture eliminator, then start heater switch.Vacuumdrier setting vacuum tightness is less than-0.09MPa, Heating temperature 40 ~ 120 DEG C.
5) reduce: adopt stepped start-stop system to push away boat reduction furnace, the hydrogen that cracked ammonium produces, the mixed gas of nitrogen, hydrogen ratio is higher than 75%.Reduction temperature is 560 ~ 620 DEG C, and powder at the uniform velocity advances in reduction furnace isothermal region, and the recovery time is 30 ~ 60 minutes.
6) sieve: sieve according to the screen cloth of corresponding-200 orders of required granularity selection ,-300 orders or-400 specifications.
7) conjunction batch: concentrated by the screen underflow after screening, adds the mixing of vacuum mixing machine, makes it even particle size distribution.
8) vacuum packaging: adopting plastic vacuum packaging bag vacuum packaging by closing the powder after criticizing, every bag of packed weight can be selected as required.
In the present invention, raw material adopt purity be greater than 99.95% pure iron, electrolytic copper plate, sheet nickel, tin slab and simple substance silico briquette, simple substance Cr block, electrolysis Ti plate, simple substance La, simple substance Y; Composition based on iron and copper in formula; The object adding nickel is solution strengthening, improves hardness, the bending strength of sintered powder, thus improves the hold to diamond particles, improves the work-ing life of diamond tool.If nickel content is too low, strengthening effect is not obvious, and life tools are not enough; If nickel too high levels, sintered compact hardness and wear resistance too high, diamond tool self-sharpening can be caused poor, and sharpness is not enough, and working (machining) efficiency is low.The object adding tin reduces powdered alloy fusing point and powder sintering temperatures, if content is too low, do not reach ideal effect; If Theil indices is too high, liquid phase can be there is too early in hot pressed sintering process, reduce die life, cause sintered density not enough simultaneously.The object adding silicon forms brittlement phase Fe-Si intermetallic compound, improves the sharpness of instrument when ensureing sintered compact toughness; If it is too high to add silicone content, sintered compact can be caused to become fragile, toughness is not enough, and instrument cannot use; If add-on is too low, then cannot play the effect of material modification.The object adding rare earth element y is in powder organization, form the tiny YSi of disperse
2, serve dispersion-strengthened effect.The inhibiting grain growth when object adding La is sintering, and play solution strengthening effect, improve alloy bending strength.Add Ti, the object of Cr forms TiC at diamond surface, Cr
3c
2intermetallic compound, increase and adamantine Chemical bond, and be uniformly distributed in boundary surfaces, carry heavy alloyed Grain-boundary Junctions and make a concerted effort.
Compared with other pre-alloyed powders, powdered alloy prepared by the present invention has Ultra-fine, the feature of low oxygen content, therefore good low-temperature sintering temperature performance is possessed, and sintering range is wider: equal hot pressing sintering within the scope of 760 DEG C ~ 880 DEG C, and sintered density reaches more than 99%, due to the interpolation of modifying element, the bending strength of agglomerate is made to be greater than 1900MPa.With the diamond tool that it manufactures, tool life and working (machining) efficiency improve all significantly.
Embodiment 1.
Use the Medium frequency induction smelting furnace of industrial production 250kg furnace capacity, furnace lining material is magnesia, uses raw material and weight as following table 1:
Table 1. raw material uses kind and proportioning table (embodiment 1)
| Raw material name | Technically pure iron | Electrolysis Ni plate | Electrolysis Cu plate | Si | Sn | Cr | Ti | La | Y | Gross weight, kg |
| Weight | 104.5 | 12.5 | 100 | 7.5 | 10 | 12.5 | 2.5 | 0.25 | 0.25 | 250 |
Raw material addition sequence is as follows:
The first step: add pure iron, in the middle of pure iron, insert Ni plate, power controls at 230KW, and fusing starts.
Second step: when melting more than half, adds Cu plate.
3rd step: add Si ingot and Sn ingot after the fusing of Cu plate.
4th step: add Cr ingot, Ti plate, La and Y powder
After melting sources, on molten metal surface, lime covers, and after 10 minutes, lime fusing, starts to skim.Measure melt temperature, start high-pressure hydraulic pump when temperature reaches 1580 DEG C, inflated with nitrogen in atomization bucket, adjustments atomizing pressure is 100MPa, topples over liquation and enters middle bottom pour ladle and start to be atomized.The sealed gas supercharging in powder collecting pot of pigment mixture after atomization, bottom powder collecting pot, water outlet installs 1200 order filter clothes additional, and under 0.5MPa pressure, pressurize is to water outlet is discharged without obvious gas-vapor mix.First the wet-milling after dehydration is loaded moisture eliminator, powder filling port seals, and starts vacuum pump, starts power switch and makes the vertical single direction rotation of moisture eliminator, then start heater switch.Vacuumdrier setting vacuum tightness is less than-0.09MPa, Heating temperature 110 DEG C, closes heating after dry 4 hours, waits for that dryer temperature drops to less than 50 DEG C, closes vacuum pump, open meal outlet powder delivery.Powder after drying is loaded graphite boat, puts into stepped start-stop system and push away boat reduction furnace, pass into the hydrogen of cracked ammonium generation, the mixed gas of nitrogen in stove, hydrogen ratio is higher than 75%.Setting reduction temperature is 600 DEG C, and powder at the uniform velocity advances in reduction furnace isothermal region, and the recovery time is 30 minutes.Sieved by reduced powder 400 eye mesh screens, collection undersize powder adds vacuum mixing machine and mixes.The finished product powder detected result is as table 2:
The performance of table 2. water atomization powdered alloy (embodiment 1) the finished product
Embodiment 2.
Use the Medium frequency induction smelting furnace of industrial production 250kg furnace capacity, furnace lining material is magnesia, uses raw material and weight as following table 3:
Table 3. raw material uses kind and proportioning table (embodiment 2)
Raw material addition sequence is identical with embodiment 1.
After melting sources, on molten metal surface, lime covers, and after 10 minutes, lime fusing, starts to skim.Measure melt temperature, start high-pressure hydraulic pump when temperature reaches 1600 DEG C, inflated with nitrogen in atomization bucket, adjustments atomizing pressure is 110MPa, topples over liquation and enters middle bottom pour ladle and start to be atomized.The sealed gas supercharging in powder collecting pot of pigment mixture after atomization, bottom powder collecting pot, water outlet installs 1200 order filter clothes additional, and under 0.5MPa pressure, pressurize is to water outlet is discharged without obvious gas-vapor mix.First the wet-milling after dehydration is loaded moisture eliminator, powder filling port seals, and starts vacuum pump, starts power switch and makes the vertical single direction rotation of moisture eliminator, then start heater switch.Vacuumdrier setting vacuum tightness is less than-0.09MPa, Heating temperature 110 DEG C, closes heating after dry 4 hours, waits for that dryer temperature drops to less than 50 DEG C, closes vacuum pump, open meal outlet powder delivery.Powder after drying is loaded graphite boat, puts into stepped start-stop system and push away boat reduction furnace, pass into the hydrogen of cracked ammonium generation, the mixed gas of nitrogen in stove, hydrogen ratio is higher than 75%.Setting reduction temperature is 600 DEG C, and powder at the uniform velocity advances in reduction furnace isothermal region, and the recovery time is 30 minutes.Sieved by reduced powder 400 eye mesh screens, collection undersize powder adds vacuum mixing machine and mixes.The finished product powder detected result is as table 4:
The performance of table 4. water atomization powdered alloy (embodiment 2) the finished product
Claims (14)
1. a diamond tool modified superfine hypoxemia water atomization powdered alloy, is characterized in that chemical composition is composed as follows by weight percentage, Cu27 ~ 67%, Ni1 ~ 10%, Sn1 ~ 10%, Si0.05 ~ 8%, Ti1 ~ 15%, Cr1 ~ 20%, La0.03 ~ 5%, Y0.03 ~ 5%; Fe surplus.
2. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, is characterized in that comprising step: smelt, water atomization, filter-press dehydration, vacuum-drying, reduction, and screening is closed and criticized, vacuum packaging.
3. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, is characterized in that, adopts medium-frequency induction furnace to smelt, its power controls between 180 ~ 240KW, furnace lining material is magnesia, strictly will control the addition sequence of each metallic substance, first add Fe and Ni in fusion process, Cu is added when melting more than half, change clear after add Si and Sn, after be sequentially added into Cr, Ti, La, Y.Adopt unslaked lime slag making, complete covering alloy solution top layer, 5 ~ 15 minutes heat-preserving deoxidizings.Then control to be atomized after molten steel temperature is skimmed between 1550 ~ 1640 DEG C.
4. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, is characterized in that, adopt the mode of two groups of nozzle Orthogonal Double V-arrangement secondary atomizations, the installation site of two groups of nozzles is mutually vertical at the line of horizontal plane; One-level atomization angle is 40 ± 1 °, and atomized water flow secondary atomization angle is 30 ± 1 °.
5. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, is characterized in that, the descending diameter 3 ~ 7mm of tundish molten steel.
6. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, it is characterized in that, the atomized water flow control of first step atomizing nozzle is at 40-80L/min, atomizing pressure 100-120MPa, the atomized water flow control of second stage atomizing nozzle is at 40-60L/min, and atomizing pressure controls at 60-95MPa.
7. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, it is characterized in that, the sealed gas supercharging in powder collecting pot of pigment mixture after atomization, bottom powder collecting pot, water outlet installs 1200 order filter clothes additional, and under 0.1 ~ 0.5MPa pressure, pressurize is to water outlet is discharged without obvious gas-vapor mix.
8. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, it is characterized in that, adopt DoubletaperedVacuumdrier, first the wet-milling after dehydration is loaded moisture eliminator, powder filling port seals, start vacuum pump, start power switch and make the vertical single direction rotation of moisture eliminator, then start heater switch.Vacuumdrier setting vacuum tightness is less than-0.09MPa, Heating temperature 40 ~ 120 DEG C.
9. a diamond tool modified superfine hypoxemia water atomization Alloy powder manufacturing approach as claimed in claim 1, is characterized in that, adopts stepped start-stop system to push away boat reduction furnace, and the hydrogen that cracked ammonium produces, the mixed gas of nitrogen, hydrogen ratio is higher than 75%.Reduction temperature is 560 ~ 620 DEG C, and powder at the uniform velocity advances in reduction furnace isothermal region, and the recovery time is 30 ~ 60 minutes.
10. a manufacture method as claimed in claim 1, is characterized in that Si added in preparing burden, forms appropriate brittlement phase Fe-Si intermetallic compound in powder organization, simultaneously owing to adding rare earth element y, form the YSi that disperse is tiny in powder organization
2, serve dispersion-strengthened effect, joint account Si its in smelting process, play the scaling loss amount of reductor effect, make smelting technology only need CaO slag making, without the need to adding other reductors, technique simple and stable is easy to operate.
11. 1 kinds of manufacture method as claimed in claim 1, is characterized in that Ti added in its batching, Cr, form TiC, Cr at diamond surface
3c
2intermetallic compound, increase with adamantine Chemical bond, be uniformly distributed in boundary surfaces, carry heavy alloyed Grain-boundary Junctions make a concerted effort.
12. 1 kinds of manufacture method as claimed in claim 1, it is characterized in that La added in its batching, Y rare earth element, inhibiting grain growth during sintering, plays solution strengthening effect, improves alloy bending strength.
13. 1 kinds of manufacture method as claimed in claim 1, the powder average particle size produced (D50) is between 3 ~ 8 microns, and oxygen content in power is less than 2000ppm, and spheroidization is good, and powder size is normal distribution.
14. 1 kinds of manufacture method as claimed in claim 2, it is characterized in that the powder size that it is atomized is thinner, the temperature reduction being less than 620 DEG C can be adopted, avoid the powder bonded in reduction process, reducing powder does not need fragmentation, directly can sieve, ensure that finished product powder average particle size (D50) is less than 8 microns, be conducive to the sintering process in diamond tool manufacturing processed.
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| CN113500198B (en) * | 2021-07-08 | 2023-07-25 | 河南黄河旋风股份有限公司 | Preparation method of high zinc alloy powder |
| CN115156543A (en) * | 2022-07-15 | 2022-10-11 | 河南弘博新材料有限公司 | Iron-nickel alloy powder production process |
| CN115138844A (en) * | 2022-07-18 | 2022-10-04 | 江苏精研科技股份有限公司 | Method for preparing ultrahigh-strength wear-resistant steel complex part by adopting powder metallurgy |
| CN115740469A (en) * | 2022-11-28 | 2023-03-07 | 江苏萌达新材料科技有限公司 | Superfine low-oxygen iron-nickel alloy powder and preparation method thereof |
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