CN103938145B - The preparation method of the corrosion of resistance to copper cermet material - Google Patents
The preparation method of the corrosion of resistance to copper cermet material Download PDFInfo
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- CN103938145B CN103938145B CN201310019100.4A CN201310019100A CN103938145B CN 103938145 B CN103938145 B CN 103938145B CN 201310019100 A CN201310019100 A CN 201310019100A CN 103938145 B CN103938145 B CN 103938145B
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Abstract
The invention discloses a kind of preparation method of the corrosion of resistance to copper cermet material, comprise the following steps: a, alloy base material surface treatment; B, batching mixing and ball milling; C, pulverizing drying; D, plasma spraying.The compactness simplify production technique, reducing production cost, greatly improve ceramic-metal composite, thus corrosion resistance nature and the work-ing life of improving ceramic-metal composite.
Description
Technical field:
The present invention relates to the corrosion of resistance to copper Material Field, particularly relate to a kind of plasma spraying technology that adopts on austenite stainless steel substrate, deposited cermet preparation method of composite coating.
Background technology:
In copper alloy castingprocesses; the mensuration of copper liquid temperature is very important; the height of copper liquid temperature is directly relevant to casting quality, along with the increase of following brass work demand, proposes requirements at the higher level to the performance of dress metallic copper liquid and thermocouple temperature measurement protective casing etc. material.For a long time; internal copper processing enterprise have employed multiple temp measuring method; as optical pyrometer and contact temperature-measuring; but what only obtain is surface temperature; also adopt the stupaliths such as quartz high temperature pottery, corundum, silicon carbide to be used as the thermocouple temperature measurement protective casing material of mensuration copper liquid in addition, all in all due to metal protective sleeve pipe non-refractory, corrosion-resistant, although and nonmetal protective sleeve is high temperature resistant, erosion resistance is high; but red brittleness is responsive, easy to crack.
As far back as the nineties later stage in last century, the people such as Harbin Institute of Technology Zhu Chun one-tenth once reported that employing metal titanium, norbide, copper powder and nickel by powder were that raw material prepares TiB2-TiC/Cu-Ni anti-yaw damper material by pressurization from climing combustion high temperature synthesis techniques, but because the ceramic phase crystal grain bonding strength in the matrix material of preparation is lower, the thermal shock resistance of matrix material is lower, has no the report of subsequent applications.China national Department of Intellectual Property discloses the manufacture method of a CN201110075071.4 ceramic/copper composite material throat insert, comprise the steps: the first step: the preparation of ceramic skeleton: 1.1 ball millings: get metallic titanium powder and boron carbide powder 2.6: 1 proportionings in mass ratio, abrading-ball is made, ratio of grinding media to material (8-12): 1 with sintered carbide ball; Make ball-milling medium with analytical pure alcohol, ball milling 20 ~ 28 hours, obtains mixed powder; 1.2 granulate: in 1.1 gained mixed powders, add the paraffin accounting for mixed powder quality 0.8 ~ 1.2%, granulate, obtain mixed powder particle with 40 mesh sieves; 1.3 shaping: it is in the mould of 65 ~ 75 DEG C that the mixed powder heating particles that 1.2 obtain is filled into mould temperature to 60 ~ 70 DEG C, apply the compacting pressure of 100 ~ 120Mpa, pressurize demoulding after 60 ~ 75 seconds; Obtain the larynx lining blank be shaped; 1.4 pre-burning degreasings: the larynx lining blank obtained 1.3 is placed in vacuum oven with the speed of 1-3 DEG C/min from room temperature to 320-350 DEG C, insulation 1-1.5 hour; 650-700 DEG C is warming up to subsequently and furnace cooling after being incubated 1-1.5 hour with same heat-up rate; In whole skimming processes, control vacuum tightness in stove and be less than or equal to 10Pa; 1.5 high temperature sinterings: the larynx lining blank after 1.4 degreasings is placed in vacuum sintering furnace, 1550-1750 DEG C is risen to from room temperature with the heat-up rate of 3-5 DEG C/min, and after being incubated 60-120 minute, cool to room temperature with the furnace, obtain the porous ceramic skeleton blank for the preparation of larynx lining; In whole high-temperature sintering process, control vacuum tightness in stove and be less than or equal to 0.1Pa; Second step: the infiltration of copper alloy: be that-200 object copper nickeline au-alloy powder to be placed on the obtained porous ceramic skeleton blank of the first step the 1.5th and to imbed-40 object high purity graphite particles by granularity, push together in molybdenum filament sintering oven with burning boat and be heated to 1450-1500 DEG C, be incubated and push cooling zone furnace cooling after 30-45 minute, obtain ceramic/copper composite material throat insert.
Its application places of copper material that oxygen level is different is different, and such as oxygen free copper cable is widely used in karaoke machine.Copper material can control the oxygen level of copper liquid in smelting process by smelting technology, but only under the prerequisite measuring oxygen level in copper liquid exactly, effectively could control the copper material that smelting technology produces different oxygen level.At present, measuring oxygen level in copper liquid is with the experience estimation of experienced technician in smelting process, also there is no the instrument of oxygen level in a kind of Measurement accuracy copper liquid, there is error unavoidably in this experience estimation, this error causes the copper material smelting not meet required oxygen level requirement, thus causes underproof copper material to overstock and waste.China national Department of Intellectual Property discloses CN03153877.0 copper liquid and determines oxygen sensor making method, its processing step is: cobalt powder and cobalt oxide powder are (70%-90%) by (1) by weight percentage: the ratio of (10%-30%) is put into non-metallic container and mixed, and then grinds half an hour more than; (2) by one end sharpening of iron wire, apart from most advanced and sophisticated 2 millimeters of curved straight hooks in 90 ° in place, then inserted one end of buckle bottom the one end of shutting in vitrified pipe, the other end of iron wire is exposed at the top of vitrified pipe open at one end; (3) in vitrified pipe, pour into the good cobalt powder of barreling and cobalt oxide powder mixed powder, Bu Duan Dun is real, makes mixed powder account for the 10%-90% of vitrified pipe volume, and makes iron wire be positioned at the centre of vitrified pipe; (4) pour into aluminum oxide powder or cobalt powder at the first half of vitrified pipe, Bu Duan Dun is real, to filling vitrified pipe; (5) vitrified pipe opening end is sealed with high-temperature plastic, seasoning more than 24 hours; (6) packaged vitrified pipe is toasted more than 16 hours in an oven, oven temperature remains on 60 DEG C ± 5 DEG C.
A kind of high temperature resistant, anticorrosive, intensity is high, plasticity and toughness are moderate protective casing material of domestic exploitation of still needing in high-temperature copper liquid thermometric protective casing material.Cermet material effectively can improve the fragility of single stupalith, makes overall to mould, toughness is improved, become a kind of material of the comparatively excellent corrosion of resistance to copper.
Summary of the invention:
The object of the present invention is to provide a kind of preparation process simple, material structure is fine and close, has the preparation method of the corrosion of the resistance to copper cermet material of stronger corrosion resistance nature.
The present invention is achieved by the following technical solution:
1, the preparation method of the corrosion of resistance to copper cermet material, comprises the following steps:
A, alloy base material surface treatment: oil removal treatment and frosting treatment are carried out in the alloy base material surface for the treatment of plasma spray;
B, batching mixing and ball milling: get Al
2o
3powder, Ti powder and Mo powder, by mass percentage 60 ~ 80%Al
2o
3, 10 ~ 35%Ti and 1 ~ 10%Mo takes powder, first by Ti powder and Mo powder, load ball mill ball milling, Ball-milling Time is after 6-8 hour, then adds Al
2o
3powder, carries out secondary ball milling, and Ball-milling Time is 8-12 hour;
C, pulverize dry: the powder mixed after ball milling to be pulverized, dry;
D, plasma spraying: adopt plasma spray coating process, by step c gained mix powder spraying described in step a alloy base material surface, described plasma spray coating process parameter is: electric current: 700 ~ 750A, plasma gas H
2: 14 ~ 23 standard liter/min, plasma gas Ar:50 ~ 55 standard liter/min, powder carrier gas Ar:3.7 ~ 4.5 standard liter/min, spray distance 50 ~ 100mm.
Alloy base material in described step a is austenitic stainless steel.
Described Al
2o
3the purity > of powder 97.9%, granularity < 20 micron.
The purity > of described Ti powder and Mo powder 97.9%, granularity < 10 micron.
Ball-milling medium in described step b twice mechanical milling process is ethanol, mixed powder in twice mechanical milling process: ball: the mass ratio of ethanol is 1:2:1.
The present invention compared with prior art has following row beneficial effect:
The present invention proposes a kind of preparation method of the plasma spraying corrosion of resistance to copper cermet material, simplify production technique, reduce production cost, greatly improve the compactness of ceramic-metal composite, thus improve the corrosion resistance nature of ceramic-metal composite, improve the work-ing life of cermet material simultaneously, the metal-ceramic coating of prepared by the present invention be coated on alloy surface is combined with alloy surface closely, can ensure coat and copper liquid nonwetting, and there is high heat shock resistance, corrosion-resistant characteristic, can the workpiece that contacts with copper liquid phase of significant prolongation, the work-ing life of container, this material has high erosion resistance and obdurability in copper liquid, has very important engineer applied and is worth.
Accompanying drawing illustrates:
Fig. 1 is the scanning electron microscopy tissue of cermet material prepared by the present invention;
Fig. 2 is the XRD diffraction analysis collection of illustrative plates of cermet material prepared by the present invention.
Fig. 3 is the Cross Section Morphology of cermet material prepared by the present invention.
Fig. 4 is the partial enlarged drawing in A portion in Fig. 3.
Sequence number in figure: 1, coat, 2, austenitic stainless steel.
Embodiment:
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
Embodiment one: see Fig. 1, Fig. 2, Fig. 3 and Fig. 4, a kind of preparation method of the corrosion of resistance to copper cermet material, comprises the following steps:
A, alloy base material surface treatment: the surface 240# emery paper treating the austenite stainless steel substrate 304 of plasma spray is polished, object is the surface of alligatoring austenite stainless steel substrate 304, be beneficial to the inlaying of powder and stainless steel substrate, clog, and with washes of absolute alcohol, remove by the various impurity greasy dirts on cladding surface, be beneficial to the wetting and metallurgical binding of powder and matrix surface;
B, batching mixing and ball milling: get Al2O3 powder, Ti powder and Mo powder, 60%Al2O3,30%Ti and 10%Mo take powder by mass percentage, first by Ti powder and Mo powder, load ball mill ball milling, the purity > of described Ti powder and Mo powder 97.9%, granularity < 10 micron, ball-milling medium is ethanol, material: ball: ethanol is 1:2:1, start ball milling, Ball-milling Time is 6 hours; Al2O3 powder is added again, the purity > of described Al2O3 powder 97.9%, granularity < 20 micron in ball mill, and according to material: ball: ethanol is that 1:2:1 carries out secondary ball milling, and Ball-milling Time is 12 hours;
C, pulverizing drying: after ball milling completes, take out the titanium mixed, molybdenum, alumina mixed powder, dries and grind at 120 DEG C;
D, plasma spraying: adopt plasma spray coating process, described plasma spray coating process parameter is: electric current: 720A, plasma gas H2:21 standard liter/min, plasma gas Ar:50 standard liter/min, powder carrier gas Ar:4 standard liter/min, spray distance 50mm, by step c gained mix powder spraying described in step a alloy base material surface.
Cermet material prepared by the present invention has higher erosion resistance and obdurability in copper liquid.The cermet material adopting the present invention to prepare is produced thermocouple temperature measurement protective casing and is had the higher corrosion of resistance to copper performance, improves the work-ing life of protective casing.
Cermet material prepared by the present invention carries out corrosion test in copper liquid, and comparatively other metallic substance such as corrosion resistance nature such as stainless steel, cast iron significantly improves.
Embodiment two: a kind of preparation method of the corrosion of resistance to copper cermet material, comprise the following steps: a, alloy base material surface treatment: the surface 240# emery paper treating the austenite stainless steel substrate 304 of plasma spray is polished, object is the surface of alligatoring austenite stainless steel substrate 304, be beneficial to the inlaying of powder and stainless steel substrate, clog, and with washes of absolute alcohol, remove by the various impurity greasy dirts on cladding surface, be beneficial to the wetting and metallurgical binding of powder and matrix surface;
B, batching mixing and ball milling: get Al2O3 powder, Ti powder and Mo powder, 70%Al2O3,25%Ti and 5%Mo take powder by mass percentage, first by Ti powder and Mo powder, load ball mill ball milling, the purity > of described Ti powder and Mo powder 97.9%, granularity < 10 micron, ball-milling medium is ethanol, material: ball: ethanol is 1:2:1, start ball milling, Ball-milling Time is 7 hours; Al2O3 powder is added again, the purity > of described Al2O3 powder 97.9%, granularity < 20 micron in ball mill, and according to material: ball: ethanol is that 1:2:1 carries out secondary ball milling, and Ball-milling Time is 10 hours;
C, pulverizing drying: after ball milling completes, take out the titanium mixed, molybdenum, alumina mixed powder, dries and grind at 120 DEG C;
D, plasma spraying: adopt plasma spray coating process, described plasma spray coating process parameter is: electric current: 700A, plasma gas H2:14 standard liter/min, plasma gas Ar:55 standard liter/min, powder carrier gas Ar:4.5 standard liter/min, spray distance 80mm, by step c gained mix powder spraying described in step a alloy base material surface.
Embodiment three: a kind of preparation method of the corrosion of resistance to copper cermet material, comprises the following steps:
Sandblasting is carried out on a, the surface of austenite stainless steel substrate 304 for the treatment of plasma spray, object is the surface of alligatoring austenite stainless steel substrate 304, be beneficial to the inlaying of powder and stainless steel substrate, clog, and with washes of absolute alcohol, remove by the various impurity greasy dirts on cladding surface, be beneficial to the wetting and metallurgical binding of powder and matrix surface;
B, batching mixing and ball milling: get Al2O3 powder, Ti powder and Mo powder, 80%Al2O3,15%Ti and 5%Mo take powder by mass percentage, first by Ti powder and Mo powder, load ball mill ball milling, the purity > of described Ti powder and Mo powder 97.9%, granularity < 10 micron, ball-milling medium is ethanol, material: ball: ethanol is 1:2:1, start ball milling, Ball-milling Time is 8 hours; Al2O3 powder is added again, the purity > of described Al2O3 powder 97.9%, granularity < 20 micron in ball mill, and according to material: ball: ethanol is that 1:2:1 carries out secondary ball milling, and Ball-milling Time is 8 hours;
C, pulverizing drying: after ball milling completes, take out the titanium mixed, molybdenum, alumina mixed powder, dries and grind at 120 DEG C;
D, plasma spraying: adopt plasma spray coating process, described plasma spray coating process parameter is: electric current: 750A, plasma gas H2:23 standard liter/min, plasma gas Ar:52 standard liter/min, powder carrier gas Ar:3.7 standard liter/min, spray distance 60mm, by step c gained mix powder spraying described in step a alloy base material surface.
Adopt the cermet material prepared by embodiment one, two, three, carry out the corrosion of resistance to copper test, corrosion experiment condition is: have the austenite stainless steel substrate 2 of cermet material coat 1 of the present invention to put into the copper alloy solution 10h of melting respectively on austenitic stainless steel, surface, contrast the corrosion of the resistance to copper performance of the material of containing metal ceramic coating from etching extent.
Cermet material prepared by embodiment one, two, three and the stainless steel corrosion of resistance to copper Performance comparision as follows:
| Be coated with the austenite stainless steel substrate of cermet material prepared by the present invention | Stainless steel | Remarks | |
| Average corrosion rate (mm/h) | 5.3Х10-6 | 6.5Х10-2 | Embodiment 1 |
| 2.3Х10-6 | 6.5Х10-2 | Embodiment 2 | |
| 6.5Х10-6 | 6.5Х10-2 | Embodiment 3 |
Embodiment is just for the ease of understanding technical scheme of the present invention; do not form limiting the scope of the invention; step a of the present invention also can carry out after step c or step a and step b, step c carry out simultaneously; every do not depart from technical solution of the present invention interior perhaps above scheme is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong within scope.
Claims (6)
1. the preparation method of the corrosion of resistance to copper cermet material, comprises the following steps:
A, alloy base material surface treatment: oil removal treatment and frosting treatment are carried out in the alloy base material surface for the treatment of plasma spray;
B, batching mixing and ball milling: get Al
2o
3powder, Ti powder and Mo powder, by mass percentage 60 ~ 80%Al
2o
3, 10 ~ 35%Ti and 1 ~ 10%Mo takes powder, first by Ti powder and Mo powder, load ball mill ball milling, Ball-milling Time is after 6-8 hour, then adds Al
2o
3powder, carries out secondary ball milling, and Ball-milling Time is 8-12 hour;
C, pulverize dry: the powder mixed after ball milling to be pulverized, dry;
D, plasma spraying: adopt plasma spray coating process, by step c gained mix powder spraying described in step a alloy base material surface, described plasma spray coating process parameter is: electric current: 700 ~ 750A, plasma gas H
2: 14 ~ 23 standard liter/min, plasma gas Ar:50 ~ 55 standard liter/min, powder carrier gas Ar:3.7 ~ 4.5 standard liter/min, spray distance 50 ~ 100mm.
2. the preparation method of the corrosion of resistance to copper cermet material according to claim 1, is characterized in that: the alloy base material in described step a is austenitic stainless steel.
3. the preparation method of the corrosion of resistance to copper cermet material according to claim 1, is characterized in that: described Al
2o
3the purity > of powder 97.9%, granularity < 20 micron.
4. the preparation method of the corrosion of the resistance to copper cermet material according to claim 1,2 or 3, is characterized in that: the purity > of described Ti powder and Mo powder 97.9%, granularity < 10 micron.
5. the preparation method of the corrosion of the resistance to copper cermet material according to claim 1,2 or 3, it is characterized in that: the ball-milling medium in described step b twice mechanical milling process is ethanol, mixed powder in twice mechanical milling process: ball: the mass ratio of ethanol is 1:2:1.
6. the preparation method of the corrosion of resistance to copper cermet material according to claim 4, is characterized in that: the ball-milling medium in described step b twice mechanical milling process is ethanol, mixed powder in twice mechanical milling process: ball: the mass ratio of ethanol is 1:2:1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1271706A (en) * | 2000-05-26 | 2000-11-01 | 清华大学 | High-antiwear composite ceramet material for cutting tools |
| CN1740380A (en) * | 2004-08-23 | 2006-03-01 | 胡学儒 | Composite ceramet material preparing process |
| CN102115884A (en) * | 2011-03-23 | 2011-07-06 | 北京矿冶研究总院 | Preparation method of wear-resistant and corrosion-resistant composite coating |
| CN102676971A (en) * | 2012-05-14 | 2012-09-19 | 新兴铸管股份有限公司 | Preparation method for composite coating of outer surface of nodular cast iron pipe |
-
2013
- 2013-01-20 CN CN201310019100.4A patent/CN103938145B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1271706A (en) * | 2000-05-26 | 2000-11-01 | 清华大学 | High-antiwear composite ceramet material for cutting tools |
| CN1740380A (en) * | 2004-08-23 | 2006-03-01 | 胡学儒 | Composite ceramet material preparing process |
| CN102115884A (en) * | 2011-03-23 | 2011-07-06 | 北京矿冶研究总院 | Preparation method of wear-resistant and corrosion-resistant composite coating |
| CN102676971A (en) * | 2012-05-14 | 2012-09-19 | 新兴铸管股份有限公司 | Preparation method for composite coating of outer surface of nodular cast iron pipe |
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