CN1297685C - Surface modification method for alloy and intermetallic compound - Google Patents
Surface modification method for alloy and intermetallic compound Download PDFInfo
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- CN1297685C CN1297685C CNB200410009715XA CN200410009715A CN1297685C CN 1297685 C CN1297685 C CN 1297685C CN B200410009715X A CNB200410009715X A CN B200410009715XA CN 200410009715 A CN200410009715 A CN 200410009715A CN 1297685 C CN1297685 C CN 1297685C
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Abstract
The present invention provides a method for the surface modification of alloy and intermetallic compounds, which relates to the surface modification of high temperature alloy, particularly to the surface modification by a chemical deposition method. The present invention aims at a basal body which is TiAl alloy with an L1<0> structure, and PC powder is used for the surface modification of L12 type Al3Ti alloy. In the process of the surface modification, the rest fine particle powder is used for embedding and processing, and is used for producing main powder by an extrusion bonding method; the fine powder is firstly coated on the inner surface of a tubby high-purity aluminum oxide crucible, PC powder preprocessed in a vacuum container is filled in the crucible, thick fine powder is covered on the top of the PC powder after a sample is embedded in the PC powder, and a perforated stainless steel disc is covered on the fine powder for heating. The method not only can promote the generation of surface modification layers and increase the chemical and mechanical performance of the surfaces under the conditions of high temperature and room temperature, but also can reduce the cost of the extrusion bonding method.
Description
Technical field
The present invention relates to the high-temperature alloy surface modification, particularly adopt the surface modification of chemical deposition.
Background technology
Generally speaking, high temperature material need have good mechanical properties and chemical property when high temperature, yet many high temperature materials all can't satisfy this two aspects requirement.In this case, use the method for surface modification to improve the surface chemistry performance of high temperature material usually.Chemical vapor deposition method (CVD) is a kind of method of good surface modification, has advantages such as cost is low, subsequent disposal is simple.Extrusion and cementation method (PC) is a kind of of CVD method, as document R.Mevrel, and C.Duret and R.Pichoir, Mater.Sci.Technol.2,201 (1986) are reported, this method is applied in many fields of surface modification, the characteristics that have conveniently, cost are low.Document H.Mabuchi et al., ScriptaMaterialia, vol.41,1999, report among the pp.511-516, the PC method has been applied to the surface modification of intermetallic compound, and successful raising this alloy chemical property at high temperature.But, in PC method treating processes, need in about 20 hours, keep very high vacuum tightness.This often is difficult to realize in actually operating, because vacuum tightness fluctuates through regular meeting.If vacuum tightness is unstable even descend in PC method treating processes, the performance on top layer will reduce after the modification, and for example the top layer crackle can occur or come off, and can't guarantee coating quality, and this mainly is to cause owing to oxidation in the PC method and vying each other of evaporation.This difficult point can be avoided by using high performance instrument, but the expense of instrument will increase considerably, thereby the cost of material modification also can increase thereupon.
Summary of the invention
The present invention is directed to complicated operation when adopting the PC method to carry out the surface modification of alloy and intermetallic compound, the cost problem of higher, proposed in the surface modification process, utilized the main powder remaining particulate powders of (PC powder) process (fine powder) that is used for the PC method in production to carry out the method for embedding treatment.This method not only can promote the generation of surface reforming layer, improves chemistry and mechanical property at high temperature and room temperature condition lower surface, and can reduce the cost of PC method.
Implementing technical scheme of the present invention is: the high purity alumina crucible of using tubbiness is as the container in the PC treating processes, earlier size is coated in the internal surface of crucible less than the fine powder of 13 μ m, again will be through pre-treatment in vacuum vessel 24～48 hours, and the PC powder that is of a size of 47-75 μ m places crucible; After imbedding matrix in the PC powder, PC powder top covers the fine powder of thick about 2 ± 0.5mm, again with the Stainless Steel Disc bedding in a hole that 9-11 diameter arranged is 1 ± 0.2mm on powder.
With the temperature rise rate of the crucible of powder and matrix with 0.01～0.03K/s is housed, be heated to 570～580K from room temperature lentamente and carry out preheating, preheating is finished post-heating speed and is increased to 0.08～1.0K/s, controlled temperature in 1373-1473K, L1
2The thickness on phase top layer is 35 ± 2 μ m, L1 in 1273-1323K
2The thickness on phase top layer is 13 ± 1 μ m.Here, matrix is to have L1
0The TiAl alloy of structure, the PC powder is L1
2Type Al
3The Ti alloy.
The dominant mechanism of this invention is that in the starting stage that the PC method is handled, fine powder is used for obtaining environmental gas, then as protective layer, prevents the oxidation of PC powder in long-time PC treating processes after the sintering process.
Generally, the material powder that is used for PC method preparation coating is than the easier oxidation of body material, but some exceptions, for example aluminum oxide are also arranged.Therefore, when this powder of preparation, should adopt the method for mechanical workout, rather than chemical process, as atomizer.A large amount of residual powders that mechanical workout goes out PC powder more used than PC method is thin, and the size of PC powder depends on sintering and the atomization temperature in the PC treating processes.But in mechanical processing process, if do not consider dimensional problem, the quantity of those residual powders is to be used for three times of PC powder quantity of the PC method even more, so thin residual powder is easy to obtain.
Compared with prior art, the invention has the advantages that:
Fig. 2,3,4 shows that fine powder is forming L1
2Role during the phase top layer.When not adding fine powder,, can see that the top layer is the extremely thin film of one deck as Fig. 2.Yet, when having covered fine powder on the PC powder, can see having generated clear and thick top layer on the matrix, as Fig. 3, observe row's alumina particulate simultaneously on the surface on top layer.Fig. 4 shows the microstructure that has formed good oxygen-free aluminium particulate after covering fine powder on inner surface of crucible and the PC powder.Utilize X-ray diffraction method to confirm that the top layer that forms on the matrix is L1
2Phase.
Temperature L1 in 1373-1473K in this invention
2The thickness on phase top layer is 35 ± 2 μ m, and thickness is 13 ± 1 μ m in 1273-1323K.L1
2Phase top layer and matrix have good avidity, can find out matrix and L1 on the face with the milling cutter cutting
2There is not crackle on the interface on phase top layer, by the three-point bending test, at L1
2The phase top layer is crackle according to qualifications, and scratch test does not find that any top layer peels off from matrix yet in addition.
L1
2The phase top layer shows combination stability, has good provide protection in the cyclic oxidation process of room temperature → 1253K (relaxation time 800s) → room temperature, through behind 12 cyclic oxidations, and L1
2The composition on phase top layer does not change, matrix and L1
2Do not observe any crackle on the interface on phase top layer yet.
More than about fine powder at L1
2Role shows in the forming process on phase top layer, there is no need the used instrument of this experiment is improved.
Description of drawings
Figure 1 shows that the microstructure of the example cross section of handling through PC.When the turning of not considering sample and parallel surfaces, handling later on by the PC method, matrix has just been covered by top layer (coating).
The cross section composition that Figure 2 shows that the PC method processing back sample that does not use fine powder changes, and the top layer is very thin.
Figure 3 shows that the cross section that has covered the sample that the PC method at crucible top handles with fine powder: near the top layer of Fig. 2, formed the thick film that contains alumina particulate of one deck.
Figure 4 shows that the cross section of the sample that the PC method after with fine powder the internal surface of crucible and top all being covered is handled: the film that has formed the thick oxygen-free aluminium particulate of one deck.
Embodiment
Use diameter as the 30mm height as the high purity alumina crucible of 30mm tubbiness as the container in the PC treating processes.Earlier manual size is coated in the internal surface of crucible less than the fine powder of 13 μ m, the PC powder that will be of a size of 47-75 μ m again places crucible.After imbedding matrix in the PC powder, PC powder top covers the fine powder of thick 2mm.In addition, again with a heavy 20g, the Stainless Steel Disc bedding in the hole that 9 diameters are arranged is 1mm is on powder.
In the preparatory stage that PC handles, the needed powder of PC treatment process is kept in the vacuum vessel 35 hours.In the initial stage that PC handles, with PC equipment, the crucible that powder and matrix promptly are housed is heated to 570K from room temperature lentamente, and temperature rise rate is lower than 0.02K/s.Preheating is finished post-heating speed and is increased to 0.09K/s.Here, matrix is to have L1
0The TiAl alloy of structure, the PC powder is L1
2Type Al
3The Ti alloy.These diameters less than the sintering temperature of 13 μ m fine powders at 1273K.Diameter is that the PC powder of 47-75 μ m and the temperature of matrix fusion are 1473K.As seen from Figure 3, generated clear and thick top layer on the matrix, L1
2Phase top layer and matrix have good avidity, and the top layer has good oxidation-resistance.
Claims (2)
1, the method for a kind of alloy and intermetallic compound surface modification, the needed powder of PC treatment process is kept in the vacuum vessel 24～48 hours, be contained in then in the PC equipment, it is characterized in that, the high purity alumina crucible of using tubbiness is as the container in the PC treating processes, earlier size is coated in the internal surface of crucible less than the fine powder of 13 μ m, the PC powder that will be of a size of 47-75 μ m again places crucible; After imbedding matrix in the PC powder, PC powder top covers the fine powder of thick 2 ± 0.5mm, again with the Stainless Steel Disc bedding in a hole that 9-11 diameter arranged is 1 ± 0.2mm on powder; With the temperature rise rate of the crucible of powder and matrix with 0.01～0.03K/s is housed, be heated to 570～580K from room temperature lentamente and carry out preheating, preheating is finished post-heating speed and is increased to 0.08～1.0K/s, controlled temperature in 1373-1473K, L1
2The thickness on phase top layer is 35 ± 2 μ m, L1 in 1273-1323K
2The thickness on phase top layer is 13 ± 1 μ m.
2, the method for alloy as claimed in claim 1 and intermetallic compound surface modification is characterized in that, matrix is to have L1
0The TiAl alloy of structure, the PC powder is L1
2Type Al
3The Ti alloy.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410009715XA CN1297685C (en) | 2004-10-28 | 2004-10-28 | Surface modification method for alloy and intermetallic compound |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200410009715XA CN1297685C (en) | 2004-10-28 | 2004-10-28 | Surface modification method for alloy and intermetallic compound |
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| CN1603462A CN1603462A (en) | 2005-04-06 |
| CN1297685C true CN1297685C (en) | 2007-01-31 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5139824A (en) * | 1990-08-28 | 1992-08-18 | Liburdi Engineering Limited | Method of coating complex substrates |
| US5334417A (en) * | 1992-11-04 | 1994-08-02 | Kevin Rafferty | Method for forming a pack cementation coating on a metal surface by a coating tape |
| CN1114984A (en) * | 1994-07-14 | 1996-01-17 | 中国科学院兰州化学物理研究所 | Common-sputtering solid lubricating film |
| JP2615107B2 (en) * | 1986-12-23 | 1997-05-28 | エムテーウー・モートレン−ウント・ツルビーネン−ウニオン・ミュンヘン・ゲーエムベーハー | Erosion-resistant lacquer protective coating for plastic substrates |
| CN1320717A (en) * | 2001-02-28 | 2001-11-07 | 山东大学 | Mechanical energy diffusion-assistant technique for modifying metal surface |
-
2004
- 2004-10-28 CN CNB200410009715XA patent/CN1297685C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2615107B2 (en) * | 1986-12-23 | 1997-05-28 | エムテーウー・モートレン−ウント・ツルビーネン−ウニオン・ミュンヘン・ゲーエムベーハー | Erosion-resistant lacquer protective coating for plastic substrates |
| US5139824A (en) * | 1990-08-28 | 1992-08-18 | Liburdi Engineering Limited | Method of coating complex substrates |
| US5334417A (en) * | 1992-11-04 | 1994-08-02 | Kevin Rafferty | Method for forming a pack cementation coating on a metal surface by a coating tape |
| CN1114984A (en) * | 1994-07-14 | 1996-01-17 | 中国科学院兰州化学物理研究所 | Common-sputtering solid lubricating film |
| CN1320717A (en) * | 2001-02-28 | 2001-11-07 | 山东大学 | Mechanical energy diffusion-assistant technique for modifying metal surface |
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| CN1603462A (en) | 2005-04-06 |
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