CN1215186C - Powder stainless steel reinforcing and sintering method - Google Patents
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Abstract
The present invention provides a reinforced sintering method of powdered 316L stainless steel. The present invention is characterized in that a proper amount of sintering activating agent, i.e., Cu3P or Fe-Mo-B, with reasonable components is added in a product, and a reasonable sintering technology is established. The activating agent is 2 to 8 wt% of Cu3P or 2 to 8 wt% of Fe-Mo-B, the Cu3P contains 13 to 4% of P, and the Fe-Mo-B contains 30 to 55% of Mo and 2 to 5% of B. The sintering activating agent is premixed in the 316L stainless steel powder, and then the materials are mixed by a ball mill. A sintering temperature is from 1200 to 1350 DEG C. A room temperature is raised to 500 DEG C in 55 to 60 minutes; then the temperature is continuously raised after being preserved for 30 to 40 minutes; the temperature is raised to the sintering temperature in 110 to 130 minutes; then the temperature is cooled down to 800 DEG C in 55 to 65 minutes after being preserved for 85 to 95 minutes; finally the raw materials are cooled to the room temperature with the furnace. The present invention has the advantages of small adding quantity of the activating agent and thermoplasticity and thermoprossing improvement, and is suitable for actual production.
Description
Technical field
The invention belongs to powder metallurgical technology, a kind of powder 316L particularly is provided stainless reinforced sintering method.
Background of invention
Can powder metallurgy 316L stainless steel components substitute fine and close 316L stainless steel components and depend on two principal elements: its intensity and erosion resistance.Usually, the powder metallurgy structural parts organization internal has a certain amount of residual porosity.These residual porosity can reduce the intensity of part.Powder metallurgical technique constantly develops, and has and can eliminate these residual porosity to a great extent such as technology such as temperature and pressure, die wall lubrication and alloyings, increases the intensity of material.The main reference document has: Rutz H G, Harejjo F G, Luk S H. " Warm Compactioon Offers High Density at LowCost " .MPR, 1994,49 (9): 40-47 etc.
Add sintering aid and carry out sintering, be use the widest, the easiest, be studied and spread intensified-sintered process the most widely.If sintering temperature is higher than activator and matrix metal eutectic temperature, be exactly that liquid phase is intensified-sintered.
About employed sintering aid, former research mainly concentrates on monobasic or the binary.Monobasic as B, Si, Al, Ni; Binary is as SiC, Cr
3C
2, CrB, Cu
3P, Fe
3(main literature has P: Molinari, A^Straffelini, G^Pieczonka, T^Kazior, J.Persistent liquid phase sintering of 316L stainless steel.International Journal of Powder Metallurgy, 1998, v34, n2:21-28; Jensen, SK^Maahn, E.Sintering additive for liquid phase sintering of AISI 316L stainless steel.PowderMetallurgy World Congress, 1994, VIII:2113-2116).But these sintering aids all have limitation separately, when surpassing solubleness in austenite as B content, can form low melting point boride eutectic, thus significantly reduce the hot workability of steel and plasticity (Lu Shiying etc. stainless steel. Beijing: Atomic Energy Press, 1995); The raising of Si content can make delta ferrite level increase, and intermetallic phase also can increase rapidly simultaneously, thereby influences the performance of steel; And Al is easy to oxidation; The adding of SiC ceramic particle then can influence stainless plasticity; Cr
3C
2, CrB is not easy to obtain, and they can make stainless coercive force raise with sintering temperature and generally reduce; The adding of the P of 8-10% can make the ductility of steel reduce again.
There is report to adopt pre-alloyed raising density of material (Reen Orville W.Prealloyed stainlesssteel powder for liquid phase sintering.American Patent, US4014680.1977-03-29), the sintered stainless steel density that this method is produced surpasses 95% of theoretical density, complicatedly but institute's addition element is many (comprise≤0.05%C 22～26%Cr, 10～24%Ni, 2.7～5%Mo, 0.1～1%B ,≤2.0%Mn ,≤2.0%Si).
Summary of the invention
The object of the present invention is to provide the stainless reinforced sintering method of a kind of powder 316L.In the density that improves the powder metallurgy structure material effectively, solved and added plasticity and the ductility that sintering aid can reduce material in the past, or the too many problem of prealloy element, make it to be fit to actual production.
Formation of the present invention: in product, add an amount of, the rational sintering activator Cu of composition
3P or Fe-Mo-B, and formulate rational sintering process, concrete grammar is as follows:
1, activator level: Cu
3P:2～8wt% or Fe-Mo-B:2～8wt%.
2, the composition of activator and preparation: Cu
3P content is 13～14% among the P, adopts Prepared by Ball Milling, granularity≤74 μ m; Mo content is 30～55% among the Fe-Mo-B, B content is 2～5%, adopts earlier hydraulic atomized legal system to be equipped with powdered alloy, get then 〉=powder of 150 μ m is as the activator meal, less than the powder of 150 μ m ball milling 48～72 hours in alcohol or other organic solution, obtain the activator fine powder.
3, the mode of activator adding: the sintering activator premix in the 316L Stainless Steel Powder, is used the ball mill batch mixing.The rotating speed of ball grinder is 50～70 rev/mins, and milling time is 45～65 minutes.
4, sintering temperature and sintering system: sintering temperature is 1200～1350 ℃.Be warmed up to 500 ℃ from room temperature through 55～60 minutes, be incubated 30～40 minutes follow-up temperature of continuing rising, be warmed up to sintering temperature after 110～130 minutes, be incubated 85～95 minutes, begin cooling then, cooled to 800 ℃ through 55～65 minutes, furnace cooling is to room temperature then.
The invention has the advantages that: Cu
3P does sintering aid than foreign literature (Datta, P^Upadhyaya, GS.Sintered duplex stainless steels from premixes of 316L and 434L powders with Cr sub 3 Csub 2 and CrB.Transactions of the Indian Institute of Metals, 2000, v53, addition n6:605-610) is few; When Fe-Mo-B did sintering aid, Fe was identical with matrix element, and Mo can form and stable ferrite phase region, improved the solidity to corrosion of steel in reducing medium, and micro-B can improve the intergranular corrosion resistance of austenitic stainless steel, and improves thermoplasticity and hot workability.In the density that improves the powder metallurgy structure material effectively, solved and added plasticity and the ductility that sintering aid can reduce material in the past, or the too many problem of prealloy element, be fit to actual production.
Description of drawings
Fig. 1 is sample required compression pressure when 40% draught behind each sintering of the present invention, among the figure 1～10th of X-coordinate, and the sequence number of each sample, ordinate zou is compression pressure (unit: MPa).All samples is the sample of 1250 ℃ of sintering temperatures, and wherein, the 1# sample is a premix 0.2%W-special wax, mold heated to 130 ℃, and powder is heated to 120 ℃, the 915MPa compacting; The 2# sample is a premix 0.2%W-special wax, mold heated to 130 ℃, and powder is heated to 120 ℃, the 801MPa compacting; The 3# sample is a premix 0.2%W-special wax, mold heated to 130 ℃, and powder is heated to 120 ℃, the 686MPa compacting; The 4# sample is premix 2%Fe-Mo-B (carefully) and 0.2%EBS wax, mold heated to 110 ℃, and powder is heated to 110 ℃, the 915MPa compacting; The 5# sample is premix 4%Fe-Mo-B (carefully) and 0.2%EBS wax, mold heated to 110 ℃, and powder is heated to 110 ℃, the 915MPa compacting; The 6# sample is premix 2%Fe-Mo-B (carefully) and 0.2%EBS wax, room temperature 915MPa compacting; The 7# sample is premix 4%Fe-Mo-B (carefully) and 0.2%EBS wax, room temperature 915MPa compacting; The 8# sample is premix 2%Cu
3P and 0.2%EBS wax, mould and powder all are heated to 110 ℃, the 915MPa compacting; The 9# sample is premix 6%Cu
3P and 0.2%EBS wax, mould and powder all are heated to 110 ℃, the 915MPa compacting; The 10# sample is premix 4%Cu
3P and 0.2%EBS wax, room temperature 915MPa compacting.
Fig. 2 is Sample A of the present invention and fine and close stainless steel specimen electrode curve stacking diagram.The preparation condition of Sample A is: interior lubricated: 0.2%EBS wax; Die wall lubrication: EBS wax; Pressing pressure: 915MPa; The room temperature compacting; Sintering aid: 6%Fe-Mo-B (carefully); Sintering temperature: 1250 ℃; Sintered density: 7.69g/cm
3Fine and close stainless consisting of: 73.329wt%Fe, 17.410wt%Cr, 7.891wt%Ni, 0.478wt%Si, 0.115wt%Mo, 0.454wt%Cu, 0.100wt%P, 0.137wt%Al.In the similar synthetic perspiration's of self-configuring solution, do electropolarization experiment, in NaCl about 5wt% is arranged, the sodium acetate of 0.5wt% urea and 2wt%, pH value is tested and is about 7.9.
Embodiment
Example 1: the different Cu of table 1
3Variable density (pressing pressure: 915MPa before and after the sample sintering during P add-on; Interior lubricated: 0.2%EBS wax; Die wall lubrication: EBS wax; Temperature and pressure temperature: 130 ℃ on mould, 120 ℃ in powder)
| Cu 3The P add-on | Density (g/cm before the sintering 3) | Density (g/cm behind 1200 ℃ of sintering 3) | Density (g/cm behind 1250 ℃ of sintering 3) |
| 2% (room temperature) | 6.99 | 7.30 | 7.28 |
| 4% (room temperature) | 7.01 | 7.41 | 7.54 |
| 6% (room temperature) | 7.01 | 7.59 | 7.58 |
| 8% (room temperature) | 7.00 | 7.52 | /* |
| 2% (temperature and pressure) | 7.22 | 7.38 | 7.35 |
| 4% (temperature and pressure) | 7.19 | 7.43 | 7.56 |
| 6% (temperature and pressure) | 7.15 | 7.61 | 7.50 |
| 8% (temperature and pressure) | 7.17 | 7.54 | / |
*"/" expression sample is out of shape in the table
As can be seen from Table 1, when 1200 and 1250 sintering, sintered density is all at Cu respectively in the room temperature compacting
3P content is to reach maximum at 6% o'clock, is respectively 7.59g/cm
3And 7.58g/cm
3And during temperature and pressure, at 1200 sintering, Cu
3P content is 6% o'clock, and it is maximum that sintered density reaches, and is 7.61g/cm
3At 1250 sintering, Cu
3P content is that 4% o'clock sintered density is 7.56g/cm to the maximum
3During 1250 temperature and pressure, sintered density is with Cu
3P content increases than the room temperature compacting and reaches maximum value in advance, and this is because the green density of warm-pressing formation itself generally is higher than the green density of room temperature compacting, and the relative density that can improve by sintering usually than room temperature suppress little.When this explanation, higher sintering temperature, add Cu
3The content of P just can make sintered density reach maximum under fewer situation.In addition, the lower sintering temperature higher sintering temperature of maximum density that can reach wants big.From the test practical situation, when 1300 sintering, add 8%Cu
3The sample of P is badly deformed and caves in.And during 1250 ℃ of sintering, add 6%Cu
3P and 8%Cu
3The sample of P sintering aid also can be found out tangible contraction, and angular edge becomes slick and sly bright.This explanation has just surpassed activator and matrix metal eutectic temperature at 1250 ℃, so the amount of liquid phase of the too high appearance of sintering temperature is too greatly to influence high temperature sintering density than the low density reason of low-temperature sintering.
Example 2: variable density (pressing pressure: 915MPa before and after sample sintering during the different Fe-Mo-B of table 2 (carefully) add-on; Interior lubricated: 0.2%EBS wax; Die wall lubrication: EBS wax; Temperature and pressure temperature: 110 ℃ on mould, 110 ℃ in powder)
| Fe-Mo-B (carefully) add-on | Density (g/cm before the sintering 3) | Density (g/cm behind 1200 ℃ of sintering 3) | Density (g/cm behind 1250 ℃ of sintering 3) |
| 2% (room temperature) | 7.06 | 7.40 | 7.48 |
| 4% (room temperature) | 7.10 | 7.42 | 7.67 |
| 6% (room temperature) | 7.01 | 7.50 | 7.69 |
| 8% (room temperature) | 7.02 | 7.57 | 7.60 |
| 2% (temperature and pressure) | 7.22 | 7.49 | 7.54 |
| 4% (temperature and pressure) | 7.20 | 7.50 | 7.67 |
| 6% (temperature and pressure) | 7.13 | 7.56 | 7.62 |
| 8% (temperature and pressure) | 7.20 | 7.67 | 7.60 |
As can be seen from Table 2, the pressed compact of room temperature compacting and warm-pressing formation is when 1200 sintering, and sintered density all rises with Fe-Mo-B (carefully) content increase always.And when 1250 sintering temperatures, it is 6% o'clock that room temperature is compressed on Fe-Mo-B (carefully) content, and it is maximum that density reaches, and warm-pressing formation is 4% o'clock at Fe-Mo-B (carefully) content, and it is maximum that density reaches.This and interpolation Cu
3The situation of P sintering aid is similar, because along with sintering aid content increases, the amount of liquid phase that occurs under uniform temp is many more, too much liquid phase influences the agglomerating final density.
Example 3: variable density (pressing pressure: 915MPa before and after sample sintering during the different Fe-Mo-B of table 3 (slightly) add-on; Interior lubricated: 0.2%EBS wax; Die wall lubrication: EBS wax; Temperature and pressure temperature: 110 ℃ on mould, 110 ℃ in powder)
| Fe-Mo-B (slightly) add-on | Density (g/cm before the sintering 3) | Density (g/cm behind 1200 ℃ of sintering 3) | Density (g/cm behind 1250 ℃ of sintering 3) |
| 2% (room temperature) | 7.12 | 7.55 | 7.55 |
| 4% (room temperature) | 7.06 | 7.55 | 7.52 |
| 6% (room temperature) | 7.09 | 7.58 | 7.54 |
| 8% (room temperature) | 7.11 | 7.56 | 7.64 |
| 2% (temperature and pressure) | 7.25 | 7.63 | 7.58 |
| 4% (temperature and pressure) | 7.2 | 7.72 | 7.55 |
| 6% (temperature and pressure) | 7.22 | 7.63 | 7.56 |
| 8% (temperature and pressure) | 7.23 | 7.61 | 7.61 |
As can be seen from Table 3, room temperature compacting pressed compact is behind 1200 ℃ of sintering, and density is little with Fe-Mo-B (slightly) content; During 1250 ℃ of sintering, be 8% o'clock at Fe-Mo-B (slightly) content, it is maximum that sintered density reaches, and is 7.64g/cm
3Fe-Mo-B (slightly) because surface reaction takes place, causes sintered density that acute variation is arranged when content is between 2%～8%.The warm-pressing formation powder compact is that 4% o'clock density reaches maximum at Fe-Mo-B (slightly) content when 1200 ℃ of sintering, and 8% o'clock minimum; During 1250 ℃ of sintering, variation tendency is similar when suppressing with room temperature.
Example 4: fine and close austenite 316L powder of stainless steel goods have good plasticity, and unit elongation reaches 30%, and general powder sintered steel belongs to hard brittle material below 3-5%.The material that powder sintered stainless steel high-density compacting and interpolation activator sinter into is plasticity or hard brittle material, and is quite important for structural parts, and properties for follow is had material impact.
The present invention judges powder sintered stainless steel high-density compacting and adds the material plasticity quality that activator sinters into compression set.Sample is depressed certain altitude (sample thief total height about 40%), sees if there is macrocrack and occurs.Required compression pressure is as shown in Figure 1 when 40% draught for each sample.
From Fig. 1, during identical draught, 4# sample, 6# sample, the required compression pressure of 9# sample maximum illustrate that the ability of these several samples opposing viscous deformation is big, and material hardness is big.2# sample, 3# sample, the required compression pressure of 8# sample minimum illustrate that these sample opposing plastic deformation abilities are poor, and material hardness is low.Above-mentioned 10 kinds of samples, except crackle appears in the 9# sample in compression, all the other all do not have the crack.Explanation is along with Cu
3The raising of P content, the havoc of P element the plastic property of austenitic stainless steel.Bibliographical information is arranged, and the 316L stainless steel adds 8%Cu
3Reduce to 2.5% (Preusse at 1250 ℃ of sintering unit elongation during P, H^Bolton, JD.Use of phosphate phase additions to promote liquid phase sintering in 316Lstainless steels, Powder Metallurgy, 1999, v42, nl:51-62), this illustrates Cu
3The increase of P content strengthens the fragility of material.
Therefore, the interpolation of Fe-Mo-B had both improved the sintering strength of 316L powder of stainless steel pressed compact, and the plasticity of material also is improved within the specific limits thereupon simultaneously; And Cu
3Though the interpolation of P increases the sintering strength of 316L powder of stainless steel pressed compact, has sacrificed the plasticity of material, even makes it to become hard brittle material.
Example 5: an important indicator estimating powder stainless steel part performance is to judge the quality of its corrosion resistance nature.Usually at certain density NaCl or various acidic medium such as H
2SO
4, HNO
3In HCl, measure stainless form of corrosion.
The density that an important factor of restriction powder stainless steel structural parts development is a part is low, this means that there are a large amount of residual porosity part inside.These residual porosity, particularly open pore not only obviously lower the mechanical property of material, and worsen the erosion resistance of part.Because the present invention is intended to make the Stainless Steel Products that can be advantageously applied to wrist-watch and some medicine equipments, so it requires sample to have good anti-corrosion under the environment that is similar to sweat, body fluid etc.The similar synthetic perspiration's of self-configuring solution, in NaCl about 5wt% is arranged, the sodium acetate of 0.5wt% urea and 2wt%, the test of pH value is about 7.9.
With the solution of self-configuring solution as the electric polarization curve test.If contain dissolved oxygen in the erosion electrolyte solution, then hydrogen reduction divides the electric current can be superimposed with the branch electric current of dissolving metal and liberation of hydrogen, and this specific form of corrosion has especially important meaning in the solution of roughly neutral (6＜pH＜8).Therefore, anode mainly is the solubilizing reaction of metal in the solution of self-configuring, and negative electrode is that hydrogen reduction reaches the evolving hydrogen reaction that is caused by water decomposition.
Select Sample A to do electric polarization curve in configuration solution, its preparation condition is: interior lubricated: 0.2%EBS wax; Die wall lubrication: EBS wax; Pressing pressure: 915MPa; The room temperature compacting; Sintering aid: 6%Fe-Mo-B (carefully); Sintering temperature: 1250 ℃; Sintered density: 7.69g/cm
3
Under identical conditions, measure electric polarization curve with a fine and close stainless steel sample simultaneously, to make comparisons.It consists of: 73.329wt%Fe, 17.410wt%Cr, 7.891wt%Ni, 0.478wt%Si, 0.115wt%Mo, 0.454wt%Cu, 0.100wt%P, 0.137wt%Al.
The sample pattern after the corrosion test is finished in observation, and pit is almost can't see on the Sample A surface, shows that its corrosion resistance nature is fine, with the electric polarization curve stack of fine and close sample and Sample A, as shown in Figure 2.
Three different electrochemical behavior zones are arranged: region of activation (A), passivation region (P) and trans-passive region (T) among the figure.Beginning is owing to polarized action, and along with the increase of corrosion current intensity, anode potential raises, and reaches the maximum current intensity I on anodic polarization curves
p, the respective electrode current potential is ε
pThe time, having produced anode passivation, anodic process is subjected to great retardance, at this moment strength of current I
pDrop to minimum value I suddenly
Minimum, in very wide anode passivation potential range, almost keep I always
MinimumCorrosion current intensity, this moment anode be in passivation region (P), corrosion speed reduces greatly.Corrosion potential is elevated to ε
TAfter, corrosion current intensity increases again, and this phenomenon is called transpassivation.Surpass ε
T, anode is in trans-passive region (T), and this moment, corrosion of metal speed increased again.ε
P-ε
TPotential range for the passivation attitude.Can observe out the I of sample 1 by Fig. 2
pBe greater than fine and close sample, ε
pLess than fine and close sample, the fine and close sample of passivation region (P) is better than sample 1, but sample 1 secondary passivity occurred behind the trans-passive region (T) about 0.18V, and this is the unexistent phenomenon of fine and close sample.
Claims (1)
1, the stainless reinforced sintering method of a kind of powder 316L is characterized in that: add an amount of, the rational sintering activator Fe-Mo-B of composition in product, and formulate rational sintering process, concrete grammar is as follows:
A, activator level: Fe-Mo-B:2～8wt%;
The composition of b, activator and preparation: Mo content is 30～55% among the Fe-Mo-B, B content is 2～5%, adopt hydraulic atomized legal system to be equipped with powdered alloy earlier, get then 〉=powder of 150 μ m is as the activator meal, less than the powder of 150 μ m ball milling 48～72 hours in alcohol, obtain the activator fine powder;
The mode that c, activator add: sintering activator meal or fine powder premix in the 316L Stainless Steel Powder, are used the ball mill batch mixing, and the rotating speed of ball grinder is 50～70 rev/mins, and milling time is 45～65 minutes;
D, sintering temperature and sintering system: sintering temperature is 1200～1350 ℃, be warmed up to 500 ℃ from room temperature through 55～60 minutes, be incubated 30～40 minutes follow-up temperature of continuing rising, after 110～130 minutes, be warmed up to sintering temperature, be incubated 85～95 minutes, begin cooling then, cooled to 800 ℃ through 55～65 minutes, furnace cooling is to room temperature then.
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