CN108842106B - Gauge protection ring and preparation method and application thereof - Google Patents
Gauge protection ring and preparation method and application thereof Download PDFInfo
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- CN108842106B CN108842106B CN201810770406.6A CN201810770406A CN108842106B CN 108842106 B CN108842106 B CN 108842106B CN 201810770406 A CN201810770406 A CN 201810770406A CN 108842106 B CN108842106 B CN 108842106B
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- 238000002360 preparation method Methods 0.000 title abstract description 21
- 239000010432 diamond Substances 0.000 claims abstract description 110
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 110
- 239000000956 alloy Substances 0.000 claims abstract description 102
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 102
- 239000002131 composite material Substances 0.000 claims abstract description 37
- 229910052802 copper Inorganic materials 0.000 claims abstract description 26
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 25
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000005520 cutting process Methods 0.000 claims abstract description 22
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 20
- 229910052742 iron Inorganic materials 0.000 claims abstract description 17
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 12
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 39
- 238000005245 sintering Methods 0.000 claims description 35
- 239000011159 matrix material Substances 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 23
- 239000011812 mixed powder Substances 0.000 claims description 16
- 230000007797 corrosion Effects 0.000 claims description 13
- 238000005260 corrosion Methods 0.000 claims description 13
- 238000000713 high-energy ball milling Methods 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 238000005299 abrasion Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims 1
- 238000013461 design Methods 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 2
- 238000004663 powder metallurgy Methods 0.000 abstract 1
- 230000036346 tooth eruption Effects 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 33
- 239000010410 layer Substances 0.000 description 17
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- 239000000463 material Substances 0.000 description 13
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 238000003466 welding Methods 0.000 description 9
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005553 drilling Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
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- 238000002490 spark plasma sintering Methods 0.000 description 3
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- 230000005641 tunneling Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
- B22F5/106—Tube or ring forms
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/06—Alloys containing less than 50% by weight of each constituent containing zinc
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention belongs to the technical field of special equipment design optimization, and particularly relates to a gauge protection ring and a preparation method and application thereof. The gauge protection ring is made of a high-entropy alloy/diamond composite material; in the high-entropy alloy/diamond composite material, diamond accounts for 10-30% of the total mass of the composite material, the diamond is uniformly distributed in the high-entropy alloy in a granular manner, and the grain diameter of diamond grains is 10-150 microns; the high-entropy alloy consists of four elements of Fe, Co, Cr and Ni and at least two elements of Cu, Al, Ti and Zn. The alloy is prepared by a powder metallurgy method, and the obtained product is used as a diameter-keeping device for cutting teeth or drill bits. The invention has reasonable component design, simple and controllable preparation process, excellent product performance, and long service life of 10 times or more than that of the existing similar cutting tooth or drill bit, and is convenient for large-scale industrial application.
Description
The technical field is as follows:
the invention belongs to the technical field of special equipment design optimization, and particularly relates to a gauge protection ring and a preparation method and application thereof.
Background art:
the cutting pick and the drill bit are key elements on a large-scale mining machine, are mainly applied to the mining fields of coal mining, roadway tunneling and the like in a coal field, and along with the increasing of resource requirements, the large-scale mining machine is more and more widely used, so that higher requirements are provided for the performance of the cutting pick. The cutting pick and the drill bit are one of the wearing parts in the tunneling machine and are main tools for breaking and crushing coal. Significant improvements in pick performance will directly reduce drilling costs. In the fields of excavation and drilling such as mining and tunnel excavation, rocks and gravels with higher hardness are often encountered, so that the cutting pick is seriously abraded, even an alloy head falls off, and the service life of the cutting pick is shortened. Alloy bit dropout (also known as "U-turn") is one of the main forms of pick failure. The reason for the 'turning-around' phenomenon is that on one hand, the brazing filler metal does not reach the standard and the strength of a welding seam is insufficient, and on the other hand, the other important reason is that the front end position of the cutting pick (around the alloy head) is excessively exposed due to excessive abrasion, so that the cutting tip directly falls off before the alloy head is not fully used.
At present, the following common solutions for solving the phenomenon of turning around caused by over-grinding are available: firstly, a surfacing mode is adopted, a welding wire (or welding flux) with better wear resistance is used for welding a cutter head, and an annular band with certain width and height is formed around the position of the cutter head in a surfacing mode; secondly, slotting at the position below the cutter head, and putting a certain number of hard alloy strips for welding and fixing; and finally, welding and fixing the high-hardness ball at the platform position around the cutter head. The surfacing process is complex and long, strict requirements are placed on the selection of welding materials and the width of a welding seam, and the quality is difficult to guarantee; the production cost of the cutting pick can be increased by adopting the hard alloy strips and the high-hardness balls; and the life of the delay equipment is generally 3-5 times.
The high-entropy alloy is also called multi-principal-element high-disorder-degree alloy, and has a simple crystal structure and excellent physical properties (such as higher hardness and wear resistance, good corrosion resistance, high temperature resistance and magnetic properties, excellent resistance property and hydrogen storage property, and the like).
Although the high-entropy alloy has good advantages as a matrix material, related research documents are rarely found in the aspect of diamond/high-entropy alloy composite materials. Particularly, no relevant report of the application of the diamond/high-entropy alloy composite material as a gauge protection ring on cutting picks and drill bits is found.
Disclosure of Invention
The technical problem to be solved by the present invention is to overcome the deficiencies and defects raised in the above background art, and to provide a gauge protection ring, a preparation method and an application thereof.
The invention relates to a gauge protection ring; the material is a high-entropy alloy/diamond composite material; in the high-entropy alloy/diamond composite material, diamond accounts for 10-30% of the total mass of the composite material, preferably 12-28%, the diamond is uniformly distributed in the high-entropy alloy in a granular manner, and the grain diameter of diamond grains is 10-150 microns;
the high-entropy alloy consists of four elements of Fe, Co, Cr and Ni and at least two elements of Cu, Al and Ti; wherein the mol ratio of any two elements in the four elements of Fe, Co, Cr and Ni is 0.95-1.05: 0.95-1.05; the molar ratio of any one element of Cu, Al, Ti and Zn to Fe is 0.5-1: 1;
the density of the high-entropy alloy/diamond composite material is greater than or equal to 99%.
The invention relates to a gauge protection ring; the average microhardness of the high-entropy alloy/diamond composite material is more than or equal to 345HV, the tensile strength is 700-1400MPa, the yield strength is 230-400MPa, the abrasion loss is 0.06-0.13mg/min, and the corrosion potential is-180 to-116 mV in 1mol/L NaCl solution.
In the present invention, the abrasion loss test conditions are: carrying out a ball disc reciprocating friction experiment by using agate balls as dual balls; the loading load is 50N; the friction speed is 900 revolutions per minute.
The invention relates to a preparation method of a gauge protection ring; the method comprises the following steps:
step one
Selecting four elements of Fe, Co, Cr and Ni to mix according to an equal molar ratio or a close molar ratio, adding at least two elements of Al, Cu and Ti according to a set proportion, mixing and atomizing to obtain high-entropy matrix powder;
step two
Carrying out high-energy ball milling treatment on the high-entropy matrix powder obtained in the step one to obtain surface-activated high-entropy alloy powder;
step three
According to a set proportion; uniformly mixing the surface-activated high-entropy alloy powder with diamond particles to obtain high-entropy alloy/diamond mixed powder; the surface of the diamond particle is plated with a surface metal layer; the surface metal layer contains at least one of zero-valent Ti, zero-valent Ni, zero-valent Cr and zero-valent W;
step four
Placing the mixed powder into a die, and performing spark plasma sintering to obtain the gauge protection ring; and during spark plasma sintering, controlling the sintering temperature to be 850-1000 ℃, keeping the temperature for 5-10 min, and controlling the sintering pressure to be 30-50 MPa.
As a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; in high entropy matrix powders, in terms of mole ratios; fe, Co, Ni, Al, Cu 1: 1: 1: 1: 1: 1.
as a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; in high entropy matrix powders, in terms of mole ratios; fe, Co, Ni, Al, Cu 1: 1: 1: 1: 0.5: 1.
as a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; in high entropy matrix powders, in terms of mole ratios; fe, Co, Ni, Al, Cu 1: 1: 1: 1: 0.5: 0.5.
as a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; in the high-entropy matrix powder, the molar ratio of Fe, Co, Cr, Ni, Al, Cu and Zn is (1): 1: 1: 1: 0.5:0.5:0.5 to 1.
As a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; and in the second step, the high-energy ball milling speed is controlled to be 250-350 r/min for 10-24 h during high-energy ball milling treatment.
As a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; in the second step, the granularity of the surface-activated high-entropy alloy powder is 45-150 um, the fluidity is more than 20g/s, and the oxygen content is less than 500 ppm.
As a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; the diamond particles have a particle size of 50 to 325 mesh. The thickness of the metal layer coated on the surface of the diamond particles is 20-50 um microns.
As a preference; the invention relates to a preparation method of a gauge protection ring; the average particle size ratio of the diamond particles to the surface-activated high-entropy alloy powder is preferably 3: 1.5-4.
The process for coating the metal layer on the surface of the diamond is a plasma sputtering and/or chemical plating process.
As a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; in the third step, mixing the high-entropy matrix powder and the diamond particles for 5-8 hours; obtaining mixed powder which is mixed uniformly; during mixing, a mechanical mixing mode is adopted for mixing; when mixing materials, the rotating speed is controlled to be 250-350 r/min.
As a preferred embodiment; the invention relates to a preparation method of a gauge protection ring; and putting the mixed powder into a mold, vacuumizing until the vacuum degree of a sintering cavity is less than 20Pa, heating to 850-1000 ℃ at a heating rate of 80-120 ℃/min, preferably 850-950 ℃, keeping the temperature for 5-10 min, and sintering at the pressure of 30-50 MPa.
In the present invention, the technique of preparing powder by gas atomization is the prior art.
The invention discloses a gauge protection ring which is used as a gauge protection device for a cutting pick or a drill bit. The industry of its connection to a pick or bit may be prior art.
When the material and the processing technology of the cutting tooth or the drill bit are completely consistent; under the premise that the connection between the gauge ring and the cutting tooth or the drill bit is completely consistent, under the same working condition; the service life of the cutting tooth or the drill bit containing the gauge protection ring designed by the invention is 10 times or more than that of similar products on the market.
When the gauge protection ring designed and prepared by the invention is used on a cutting pick or a drill bit as a gauge protection device, and is used for deep sea drilling and deep sea operation, the service life of the gauge protection ring is far longer than that of the existing product. Meanwhile, theoretically; the gauge protection ring designed and prepared by the invention can be suitable for outer space when being used as a gauge protection device on a cutting pick or a drill bit.
The high-entropy alloy designed by the invention; because the diamond composite material has the advantages of high hardness, good toughness, controllable alloy components, excellent wear resistance, excellent hot hardness and thermal stability and the like, the diamond composite material can be completely used as a matrix material of the diamond composite material. This provides the necessary condition for inventing the cutting pick and the drill bit with ultra-long service life.
The invention utilizes the spark plasma sintering process to rapidly prepare the high-entropy alloy/diamond composite material at a lower temperature; the problems of severe thermal corrosion and graphitization of the diamond in the traditional sintering process are solved, the performance of the single-particle diamond is protected from being reduced in the sintering process, the mechanical property of the composite material is ensured, and the composite material has good corrosion resistance.
In the research and development process of the invention, because the melting point of the high-entropy alloy is higher, the invention adds a proper amount of low-melting-point elements such as Cu, Al, Zn, Ti and the like, so that the sintering temperature is reduced, and simultaneously, the FCC + BCC bidirectional structure is convenient to generate, and the mechanical property of the composite material is further improved. Meanwhile, the sintering temperature is reduced, so that the original appearance of the diamond is kept as far as possible, and the condition that the diamond loses efficacy due to graphitization is avoided. In addition, the added proper amount of zero-valent Cu, Al, Zn, Ti and the like is beneficial to the subsequent connection of the product with a cutting tooth or a drill bit; in particular by a welding process. This provides the necessary conditions for obtaining a product with an ultra-long life.
The surface functionalized diamond particles adopted by the invention have two functions of protection and activation. The surface functionalization of the diamond hinders the mutual diffusion reaction of carbon atoms and a substrate, avoids the thermal erosion of the diamond and maintains the complete crystal form of the diamond; meanwhile, the functionalized layer can be in full metallurgical bonding with the high-entropy alloy matrix and the diamond, so that the bonding strength of an interface is improved, and the wettability and holding force of the matrix to the diamond are increased.
Compared with the prior art, the invention has the advantages that:
(1) the discharge plasma sintering process adopted by the invention can ensure the compactness of the diamond/high-entropy alloy composite material and the metallurgical bonding between the diamond and the high-entropy alloy matrix to the maximum extent, and ensure that the diamond is not ablated and graphitized on a large scale.
(2) The diamond surface functionalization technology adopted by the invention can enhance the holding force of the high-entropy alloy matrix to the diamond, improve the bonding strength between the diamond and the high-entropy alloy matrix, reduce the graphitization degree of the diamond, maintain the good crystal form and mechanical property of the diamond, and finally enable the gauge protection ring to have excellent wear resistance (reaching the level of oil lubrication) and higher hardness and bending strength. Meanwhile, the graphitization of the diamond surface layer can be reduced to the greatest extent by coating the metal layer with proper thickness on the surface layer; the condition that the diamond falls off in the early stage in the use process is avoided.
(3) The diamond addition amount adopted by the invention can ensure the hardness and the bending strength of the composite material, simultaneously improve the wear resistance of the composite material to the greatest extent, greatly prolong the service life of the cutting pick, and reduce the drilling and excavating costs.
(4) The invention is annular in shape, and carries out covering protection on the position around the alloy head;
(5) the invention relates to a gauge protection ring made of a diamond/high-entropy alloy composite material and a processing method thereof; the method has the advantages of low cost, short process flow, high controllability, easy realization of industrial production, environmental protection and the like.
Drawings
FIG. 1 is a high entropy alloy/diamond gauge ring prepared in example 1 of the present invention;
FIG. 2 is a sintering curve of a high entropy alloy/diamond gauge ring prepared in example 2 of the present invention;
FIG. 3 is an SEM photograph of a high entropy alloy/diamond gauge ring prepared in example 3 of the present invention;
FIG. 4 is a pictorial view of the high entropy alloy/diamond gauge ring prepared in example 1 with cutting picks attached thereto;
FIG. 5 shows the high entropy alloy/diamond gauge ring prepared in example 1 with an attached cutting pick and mounted to the apparatus;
fig. 6 is diamond particles with a Ni layer plated on the surface prepared in example 1;
FIG. 7 shows that the friction coefficient of the high-entropy alloy/diamond gauge-protection ring prepared in example 3 and the material is 42CrMo
And comparing the friction coefficients of the test samples.
Detailed Description
Example 1:
the invention relates to a high-entropy alloy/diamond composite gauge protection ring, which takes high-entropy alloy as a matrix phase and diamond as a reinforcing phase; the matrix phase high-entropy alloy mainly contains six elements of Fe, Co, Cr, Ni, Al and Cu, the molar weight of the six elements are equal, and the content of diamond is 12 wt%.
The preparation method of the high-entropy alloy/diamond composite material gauge protection ring comprises the following steps:
(1) selecting Fe, Co, Cr, Ni, Al and Cu plates or blocks with the purity higher than 99.9 percent (mass percentage), and mixing the materials according to the molar ratio of Fe to Co to Cr to Ni to Al to Cu of 1: 1: 1: 1: 1:1, carrying out melting atomization to obtain high-entropy alloy powder;
(2) and (3) carrying out high-energy ball milling treatment on the high-entropy alloy powder at the rotating speed of 250 revolutions per minute for 10 hours. The powder obtained has a flowability of greater than 20g/s and an oxygen content of less than 500 ppm.
(3) The alloy is prepared from the following high-entropy alloys in percentage by mass: diamond 88: 12, weighing high-entropy alloy powder with the granularity of less than or equal to 45um and diamond particles with the granularity of 10-50 microns, and uniformly mixing for 5 hours (the rotating speed is 300 revolutions per minute) to obtain mixed powder. The surface of the diamond particle is plated with a Ni layer; the thickness of the Ni layer was 25 microns;
(4) and (3) loading the mixed powder into a graphite grinding tool, sintering by adopting a rapid discharge plasma sintering process (the sintering temperature is 950 ℃, the sintering time is 8min, the pressure is 40MPa, and the vacuum degree is 5 Pa), and finally obtaining the high-entropy alloy/diamond composite material gauge-protecting ring.
Metallographic observation of the high-entropy alloy/diamond gauge-protecting ring prepared by the embodiment shows that the diamond particles in the material have obvious edges and corners and do not generate obvious thermal corrosion.
The high entropy alloy/diamond gauge ring prepared in this example was tested to have an average microhardness of 547 HV. The bending strength is 1360MPa, the yield strength is 360MPa, the abrasion loss is 0.1mg/min, and the corrosion potential is-142 mV in 1mol/L NaCl solution.
Example 1 was repeated; the yield is 100 percent after 50 times.
Example 2:
the invention relates to a high-entropy alloy/diamond composite gauge protection ring, which takes high-entropy alloy as a matrix phase and diamond as a reinforcing phase; the matrix phase high-entropy alloy mainly contains six elements of Fe, Co, Cr, Ni, Al and Cu.
The preparation method of the high-entropy alloy/diamond composite material gauge protection ring comprises the following steps:
(1) selecting a plate or a block of Fe, Co, Cr, Ni, Al and Cu with the purity of more than 99.9 percent (mass percentage), and mixing the materials in a molar ratio of Fe to Co to Cr to Ni to Al to Cu of 1: 1: 1: 1: 0.5: 1, carrying out melting atomization to obtain high-entropy alloy powder;
(2) and (3) carrying out high-energy ball milling treatment on the high-entropy alloy powder at the rotating speed of 250 revolutions per minute for 16 hours. The powder obtained has a flowability of greater than 20g/s and an oxygen content of less than 500 ppm.
(3) The alloy is prepared from the following high-entropy alloys in percentage by mass: diamond 4: 1, weighing high-entropy alloy powder with the granularity of 45-90 um and diamond particles with the granularity of 50-90 microns, and uniformly mixing for 8 hours to obtain mixed powder. The surface of the diamond particle is plated with a Ni layer; the average thickness of the Ni layer was 27 microns.
(4) And (3) putting the mixed powder into a graphite grinding tool, and sintering by adopting a rapid discharge plasma sintering process (the sintering temperature is 1000 ℃, the sintering time is 8min, the pressure is 40MPa, and the vacuum degree is 8Pa), so as to finally obtain the high-entropy alloy/diamond composite material gauge-protection ring.
Metallographic observation of the high-entropy alloy/diamond gauge-protecting ring prepared by the embodiment shows that the diamond particles in the material have obvious edges and corners and do not generate obvious thermal corrosion.
The average microhardness of the high entropy alloy/diamond gauge ring prepared in this example was tested to be 421 HV. The bending strength is 1267MPa, the yield strength is 324MPa, the abrasion loss is 0.12mg/min, and the corrosion potential is-180 mV in 1mol/L NaCl solution.
Example 2 was repeated; the yield is 100 percent after 50 times.
Example 3:
the invention relates to a high-entropy alloy/diamond composite gauge protection ring, which takes high-entropy alloy as a matrix phase and diamond as a reinforcing phase; the matrix phase high-entropy alloy mainly contains six elements of Fe, Co, Cr, Ni, Al and Cu.
The preparation method of the high-entropy alloy/diamond composite material gauge protection ring comprises the following steps:
(1) selecting a plate or a block of Fe, Co, Cr, Ni, Al, Cu and Zn with the purity of more than 99.9 percent (mass percentage), and mixing the materials in a molar ratio of Fe to Co to Cr to Ni to Al to Cu to Zn to 1: 1: 1: 1: 0.5:0.5: 1, carrying out melting atomization to obtain high-entropy alloy powder;
(2) and (3) carrying out high-energy ball milling treatment on the high-entropy alloy powder at the rotating speed of 250 revolutions per minute for 18 hours. The powder obtained has a flowability of greater than 20g/s and an oxygen content of less than 500 ppm.
(3) The alloy is prepared from the following high-entropy alloys in percentage by mass: diamond 4: 1, weighing high-entropy alloy powder with the granularity of 45-90 um and diamond particles with the granularity of 90-110 microns, and uniformly mixing for 8 hours (the rotating speed is 250 revolutions per minute) to obtain mixed powder. The surface of the diamond particle is plated with a Ni layer; the thickness of the Ni layer was 2 microns;
(4) and (3) putting the mixed powder into a graphite grinding tool, and sintering by adopting a rapid discharge plasma sintering process (the sintering temperature is 900 ℃, the sintering time is 8min, the pressure is 40MPa, and the vacuum degree is 8Pa), so as to finally obtain the high-entropy alloy/diamond composite material gauge-protection ring.
Metallographic observation of the high-entropy alloy/diamond gauge-protecting ring prepared by the embodiment shows that the diamond particles in the material have obvious edges and corners and do not generate obvious thermal corrosion.
The average microhardness of the high-entropy alloy/diamond gauge ring prepared by the embodiment is tested to be 386 HV. The tensile strength is 928MPa, the yield strength is 260MPa, the abrasion loss is 0.14mg/min, and the corrosion potential is-116 mV in 1mol/L NaCl solution.
Example 3 was repeated; the yield is 100 percent after 50 times.
Example 4:
the invention relates to a high-entropy alloy/diamond composite gauge protection ring, which takes high-entropy alloy as a matrix phase and diamond as a reinforcing phase; the matrix phase high-entropy alloy mainly contains seven elements of Fe, Co, Cr, Ni, Al, Cu and Zn.
The preparation method of the high-entropy alloy/diamond composite material gauge protection ring comprises the following steps:
(1) selecting a plate or a block of Fe, Co, Cr, Ni, Al, Cu and Zn with the purity of more than 99.9 percent (mass percentage), and mixing the materials in a molar ratio of Fe to Co to Cr to Ni to Al to Cu to Zn to 1: 1: 1: 1: carrying out melting atomization at a ratio of 0.5:0.5:0.5 to obtain high-entropy alloy powder;
(2) and (3) carrying out high-energy ball milling treatment on the high-entropy alloy powder at the rotating speed of 350 r/min for 24 hours. The powder obtained has a flowability of greater than 20g/s and an oxygen content of less than 500 ppm.
(3) The alloy is prepared from the following high-entropy alloys in percentage by mass: diamond 4: 1, weighing high-entropy alloy powder with the granularity of 90-150 um and diamond particles with the granularity of 110-150 microns, and uniformly mixing for 12 hours to obtain mixed powder. The surface of the diamond particle is plated with a Ni layer; the thickness of the Ni layer was 26 microns;
(4) and (3) putting the mixed powder into a graphite grinding tool, and sintering by adopting a rapid discharge plasma sintering process (the sintering temperature is 850 ℃, the sintering time is 8min, the pressure is 40MPa, and the vacuum degree is 8Pa), so as to finally obtain the high-entropy alloy/diamond composite material gauge-protection ring.
Metallographic observation of the high-entropy alloy/diamond gauge-protecting ring prepared by the embodiment shows that the diamond particles in the material have obvious edges and corners and do not generate obvious thermal corrosion.
The average microhardness of the high entropy alloy/diamond gauge ring prepared in this example was tested to be 345 HV. The bending strength is 726MPa, the yield strength is 281MPa, the abrasion loss is 0.16mg/min, and the corrosion potential is-137 mV in 1mol/L NaCl solution.
Example 1 was repeated; the yield is 100 percent after 50 times.
Comparative example 1: other conditions were consistent with the examples; the difference is that when the sintering temperature of 1050 ℃ or above is adopted, the sintering sample generates liquid phase, which causes the sintering to be interrupted.
Comparative example 2: other conditions were consistent with the examples; only the diamond coated with the nickel layer is not added; the microhardness of the obtained product is 300 HV.
Comparative example 3
Other conditions were consistent with the examples; al and Cu are not added into the high-entropy alloy; a dense product cannot be obtained.
Comparative example 4
Other conditions were consistent with the examples; only the diamond is not coated with the nickel layer; the microhardness of the obtained product is 340 HV. And the yield is only 50-75%.
Claims (9)
1. A gauge protection ring is characterized in that the gauge protection ring is made of a high-entropy alloy/diamond composite material, wherein diamond accounts for 12 ~ 28% of the total mass of the composite material, the diamond is uniformly distributed in the high-entropy alloy in a granular manner, and the grain size of diamond grains is 10-150 micrometers;
the high-entropy alloy consists of four elements of Fe, Co, Cr and Ni and at least two elements of Cu, Al, Ti and Zn; wherein the mol ratio of any two elements in the four elements of Fe, Co, Cr and Ni is 0.95-1.05: 0.95-1.05; the mol ratio of any one element of Cu, Al, Ti and Zn to Fe is 0.5-1: 1;
the gauge protection ring is prepared by the following steps:
step one
Selecting and mixing four elements of Fe, Co, Cr and Ni according to a set proportion, adding at least two elements of Al, Cu, Ti and Zn according to a set proportion, mixing and atomizing to obtain high-entropy matrix powder;
step two
Carrying out high-energy ball milling treatment on the high-entropy matrix powder obtained in the step one to obtain surface-activated high-entropy alloy powder;
step three
According to a set proportion; uniformly mixing the surface-activated high-entropy alloy powder with diamond particles to obtain high-entropy alloy/diamond mixed powder; the surface of the diamond particle is plated with a surface metal layer; the surface metal layer contains at least one of zero-valent Ti, zero-valent Ni, zero-valent Cr and zero-valent W;
step four
And (3) placing the mixed powder into a die, and performing discharge plasma sintering to obtain the gauge protection ring, wherein the sintering temperature is controlled to be 850 ~ 1000 ℃, the heat preservation time is 5 ~ 10min, and the sintering pressure is 30 ~ 50MPa during the discharge plasma sintering.
2. A gage ring as defined in claim 1; the method is characterized in that: the density of the high-entropy alloy/diamond composite material is greater than or equal to 99%.
3. The gauge protection ring as claimed in claim 1, wherein the average microhardness of the high-entropy alloy/diamond composite material is greater than or equal to 345HV, the bending strength is 700-1400MPa, the yield strength is 200-400MPa, the abrasion loss is 0.06-0.13mg/min, and the corrosion potential is 150 ~ 230 mV.
4. A gage ring as defined in claim 1; the method is characterized in that:
in high entropy matrix powders, in terms of mole ratios; fe, Co, Cr, Ni, Al, Cu = 1: 1: 1: 1: 1: 1;
or
In high entropy matrix powders, in terms of mole ratios; fe, Co, Cr, Ni, Al, Cu = 1: 1: 1: 1: 0.5: 1;
or
In high entropy matrix powders, in terms of mole ratios; fe, Co, Cr, Ni, Al, Cu = 1: 1: 1: 1: 0.5: 0.5; or
In the high-entropy matrix powder, the molar ratio of Fe, Co, Cr, Ni, Al, Cu, Zn = 1: 1: 1: 0.5:0.5:0.5 ~ 1 is.
5. A gage ring as defined in claim 1; the method is characterized in that:
in the second step, the high-energy ball milling speed is controlled to be 250 ~ 350 rpm for 10 ~ 24h during the high-energy ball milling treatment;
in the second step, the particle size of the surface-activated high-entropy alloy powder is 45 ~ 150 μm, the fluidity is more than 20g/s, and the oxygen content is less than 500 ppm.
6. The gauge protection ring of claim 1, wherein the diamond particles have a size of 50 mesh ~ 325 mesh 325, and the metal layer coated on the surface of the diamond particles has a thickness of 20 ~ 50 μm.
7. A gage ring as defined in claim 1; the method is characterized in that:
and in the third step, mixing the high-entropy matrix powder and the diamond particles for 5 ~ 8 hours to obtain uniformly mixed powder, and during mixing, mixing the powder in a mechanical mixing mode, wherein during mixing, the rotating speed is controlled to be 250-350 revolutions per minute.
8. A gage ring as defined in claim 1; the method is characterized in that:
and step four, placing the mixed powder into a mold, vacuumizing until the vacuum degree of a sintering cavity is less than 20Pa, heating to 850 ~ 1000 ℃ at the heating rate of 80 ~ 120 ℃/min to 5 ~ 10min, and sintering at the pressure of 30 ~ 50 MPa.
9. Use of a gauge ring according to any of claims 1-8, wherein: the gauge protection ring is used as a gauge protection device for a cutting pick or a drill bit.
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| CN110202145A (en) * | 2019-06-20 | 2019-09-06 | 蓬莱市超硬复合材料有限公司 | Preparation method based on laser gain material manufacture high-entropy alloy diamond composite |
| CN112622057A (en) * | 2020-12-22 | 2021-04-09 | 中南大学 | Diamond composite material, preparation method thereof, wire saw bead and wire saw machine |
| CN113399670B (en) * | 2021-05-19 | 2023-04-07 | 西安理工大学 | Double-element equivalent transformation high-entropy alloy powder and preparation method thereof |
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