CN113510245B - Method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization - Google Patents
Method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 80
- 239000000956 alloy Substances 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000009689 gas atomisation Methods 0.000 title claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 19
- 238000003723 Smelting Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000000889 atomisation Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
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- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 7
- 239000012964 benzotriazole Substances 0.000 claims description 7
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- 229930195725 Mannitol Natural products 0.000 claims description 6
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052758 niobium Inorganic materials 0.000 description 3
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- 229910052726 zirconium Inorganic materials 0.000 description 3
- 238000012387 aerosolization Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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Abstract
The invention discloses a method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization, which comprises the following steps: s1, weighing the raw materials and mixing to obtain alloy powder; s2, uniformly mixing the alloy powder, and performing cold isostatic pressing to obtain an electrode rod; s3, vacuum sintering, namely preheating the electrode rod, then placing the electrode rod into a vacuum sintering furnace for sintering, and then cooling to obtain a sintered blank; s4, taking the sintered blank as a consumable arc melting furnace electrode, and carrying out arc melting in a vacuum consumable arc melting furnace to obtain a melted electrode bar; s5, taking the electrode rod after smelting as an atomizing electrode rod, and carrying out gas atomization powder preparation by using a plasma rotating electrode to obtain CuCrNbZr alloy powder. The invention firstly forms fine Cr in the atomization process by adjusting the proportion of Cr and Nb2The Nb phase is distributed at the edge of the spherical powder and can block the growth of crystal grains under the high-temperature condition, thereby having excellent high-temperature resistance.
Description
Technical Field
The invention relates to the technical field of copper alloy powder preparation, in particular to a method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization.
Background
Due to the excellent heat conducting property of the copper alloy, the copper alloy can be applied to application scenes needing rapid heat transfer, such as a thrust chamber of a rocket engine. However, pure copper, although having a high thermal conductivity, is rarely used in such application scenarios due to its poor mechanical properties. Generally, a rocket engine combustion chamber adopts regenerative cooling to ensure that the temperature of a wall surface is in an allowable range, and the inner wall of the rocket engine combustion chamber is subjected to the action of high-temperature, high-pressure and high-speed gas flow and bears high thermal stress caused by pressure load and temperature gradients on two sides of the inner wall.
Copper alloys have attracted rocket motor components for use as substrates because of two characteristics: compatibility with oxygen and high thermal conductivity. The compatibility with oxygen can avoid oxidation corrosion of the inner wall surface under high temperature conditions, thereby prolonging the service life. On the other hand, the inner side of the liner is exposed to 20 MPa of combustion gas and the outer side is the low temperature propellant. With the increase of the environmental temperature, the fracture of the metal is transited from the common transgranular fracture at normal temperature to the intergranular fracture. This is because the grain strength and grain boundary strength decrease with increasing temperature, but the grain boundary strength decreases faster.
Cu-Cr-Nb-Zr is a dispersion strengthened alloy having excellent electrical conductivity, thermal expansion, strength and ductility. Compared with the traditional copper alloy, the material has more excellent creep resistance and low cycle fatigue performance. With the continuous increase of the pressure and the heat flow in the combustion chamber in the future, the use environment of the inner wall is worse and harsher, and the important significance is achieved for developing the performance and application research of the material as soon as possible.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization.
The technical scheme of the invention is as follows: a method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization comprises the following steps:
s1 ingredient
Selecting and weighing corresponding raw materials according to the weight percentage of 0.5-8% of Cr, 0.3-7% of Nb, 0-0.55% of Zr and the balance of Cu and inevitable impurities, and mixing to obtain alloy powder;
s2 prefabricated blank
Fully and uniformly mixing the alloy powder prepared in the step S1, and performing cold isostatic pressing to obtain an electrode rod;
s3 vacuum sintering
Preheating the electrode rod obtained by pressing in the step S2 at the temperature of 400-800 ℃ for 2-6 h, then placing the preheated blank into a vacuum sintering furnace for sintering, wherein the sintering temperature is 900-1100 ℃, and the vacuum degree is kept at 10 during the sintering process-2Below Pa, and then cooling to obtain a sintered blank;
s4 vacuum consumable arc melting
Taking the sintered blank obtained after sintering in the step S3 as a consumable arc melting furnace electrode, and carrying out arc melting in a vacuum consumable arc melting furnace to obtain a melted electrode rod;
s5 plasma rotary electrode gas atomization
Taking the smelted electrode rod obtained by vacuum consumable arc smelting in the step S4 as an atomizing electrode rod, heating the end part of the atomizing electrode rod by using plasma, simultaneously rotating the atomizing electrode rod at a high speed, refining molten liquid drops by means of centrifugal force, solidifying in an inert gas environment and spheroidizing under the action of surface tension to form powder to obtain CuCrNbZr alloy powder, wherein the average particle size of the prepared CuCrNbZr alloy powder is 50 mu m, and a large amount of submicron Cr is formed in the powder preparation process2The Nb strengthening phase particles prevent the particles from growing at high temperature, so the high-temperature-resistant Nb-Nb alloy has excellent high-temperature resistance.
Further, the mass ratio of Cr to Nb in step S1 satisfies: 1 < Cr/Nb < 2. By controlling and adjusting the ratio of Cr to Nb, fine Cr can be formed first in the atomization process2Nb phase of the Cr2The Nb phase is distributed at the edge of the spherical powder, which can hinder the grain growth under high temperature conditions.
Further, the parameters of the cold isostatic pressing in step S2 are: the pressure of the cold isostatic pressing is 100-300 MPa, and the pressure maintaining time is 5-10 min. The CuCrNbZr alloy powder blank obtained by cold isostatic pressing according to the parameters has high density and good uniformity.
Further, the smelting current in the step S4 is: 8-15 KA and 10-25 s of stirring. The electrode bar after smelting can be effectively prepared by performing vacuum consumable arc smelting according to the parameters, and the components of the electrode bar after smelting can be uniform in density by stirring the periphery.
Further, in the step S5, the rotation speed is 13000-. The powder is prepared by carrying out gas atomization on the plasma rotating electrode through the parameters, refining molten liquid drops by means of centrifugal force, solidifying in an inert gas environment and spheroidizing under the action of surface tension to form powder, and the prepared CuCrNbZr alloy powder is uniform in particle size and can keep the average particle size below 50 microns.
As a technical scheme of the present invention, the inert gas environment specifically includes: 15-25 ml/m in inert gas atmosphere3The gasified treatment liquid of (3);
the forming method of the inert gas environment comprises the following steps: gasifying the treatment liquid to obtain gasified treatment liquid, injecting the gasified treatment liquid into an inert gas environment, monitoring the concentration of the gasified treatment liquid in the inert gas environment in real time through a concentration detector, and compensating in real time. The treatment liquid is filled into an inert gas environment in a gasification mode, so that the concentration control of the components of the treatment liquid is more stable, the forming effect of the CuCrNbZr alloy powder of the gasification treatment liquid is better, the surface oxidation of the CuCrNbZr alloy powder can be effectively prevented, and the oxidation rate is only about 2-3%; and the treatment liquid is liquid at normal temperature and normal pressure, so that the treatment liquid is easier to store and prepare for use.
As another improved technical solution, the inert gas environment specifically includes: spraying atomized treatment liquid with the dosage of 3-5 ml/min through a gas distribution plate in an inert gas environment;
the forming method of the inert gas environment comprises the following steps: atomizing the treatment solution into liquid drops with the particle size of 20-40 mu m by utilizing ultrasonic atomization to obtain the atomized treatment solution, uniformly mixing the atomized treatment solution and inert gas, and spraying the mixture through a gas distribution disc. The atomized treatment liquid is mixed into an inert gas environment, the operation is simple, the preparation cost is lower, the surface oxidation of the CuCrNbZr alloy powder can be effectively prevented, and the oxidation rate is only about 4-5%.
Further, the composition of the treatment liquid is as follows: 1-2 g of benzotriazole, 5-10 ml of phytic acid, 9-15 ml of hydrogen peroxide, 10-20 ml of polyethylene glycol and 10-20 ml of mannitol. The matched material components are selected under a large amount of experimental researches, so that the molten liquid drops of the atomized electrode rod are solidified to form powder in the inert gas environment containing the treatment liquid, the oxidation phenomenon of the CuCrNbZr alloy powder finished product is effectively prevented, and the economic benefit is obvious.
The invention has the beneficial effects that: the preparation method of the invention firstly forms fine Cr in the atomization process by adjusting the component proportion of Cr and Nb2The Nb phase is distributed at the edge of the spherical powder, the growth of crystal grains can be hindered under the high-temperature condition, and the prepared CuCrNbZr alloy powder has excellent high-temperature resistance.
Drawings
FIG. 1 is a diagram of the gold phase of a CuCrNbZr alloy prepared in the experimental example, group 1;
FIG. 2 is an SEM topography of the CuCrNbZr alloy powder prepared in example 1 of the invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments thereof for better understanding the advantages of the invention.
Example 1
A method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization comprises the following steps:
s1 ingredient
Selecting and weighing corresponding raw materials according to the weight percentage of 3.6 percent of Cr, 2.3 percent of Nb, 0.25 percent of Zr and the balance of Cu and inevitable impurities, and mixing to obtain alloy powder; by controlling and adjusting the ratio of Cr to Nb, fine Cr can be formed first in the atomization process2Nb phase of the Cr2The Nb phase is distributed at the edge of the spherical powder, so that the growth of crystal grains can be hindered under the high-temperature condition;
s2 prefabricated blank
Fully and uniformly mixing the alloy powder prepared in the step S1, and performing cold isostatic pressing to obtain an electrode rod; the pressure of cold isostatic pressing is 240 MPa, the pressure maintaining time is 7 min, the CuCrNbZr alloy powder blank obtained by cold isostatic pressing according to the parameters is high in density, and the uniformity of the CuCrNbZr alloy powder blank is good;
s3 vacuum sintering
Preheating the electrode rod pressed in the step S2 at 700 ℃ for 4 h, then putting the preheated blank into a vacuum sintering furnace for sintering, wherein the sintering temperature is 1000 ℃, and the vacuum degree is kept at 10 in the sintering process-2Pa, then cooling to obtain a sintered blank;
s4 vacuum consumable arc melting
And (4) taking the sintered blank obtained after sintering in the step (S3) as an electrode of a consumable arc melting furnace, and carrying out arc melting in the vacuum consumable arc melting furnace, wherein the melting current is as follows: 10 KA, stirring the surrounding for 15 s at the same time to obtain a smelted electrode rod; the electrode bar after smelting can be effectively prepared by performing vacuum consumable arc smelting according to the parameters, and the density of each component of the electrode bar after smelting can be uniform and consistent by stirring the periphery;
s5 plasma rotary electrode gas atomization
Taking the smelted electrode rod obtained by vacuum consumable arc smelting in the step S4 as an atomizing electrode rod, heating the end part of the atomizing electrode rod by using plasma, simultaneously rotating the atomizing electrode rod at a high speed with the rotation speed of 15000 r/min, the current of 2500A and the feeding speed of 1.5 mm/S, refining molten liquid drops by virtue of centrifugal force, solidifying in an inert gas environment and spheroidizing under the action of surface tension to form powder to obtain CuCrNbZr alloy powder, wherein the average particle size of the prepared CuCrNbZr alloy powder is 50 mu m, and a large amount of submicron Cr is formed in the powder preparation process2Nb strengthening phase particles block the growth of the particles at high temperature, so the powder has excellent high temperature resistance, plasma rotating electrode gas atomization is carried out to prepare powder through the parameters, molten liquid drops are refined by means of centrifugal force, the molten liquid drops are solidified in an inert gas environment and are spheroidized under the action of surface tension to form powder, and the prepared CuCrNbZr alloy powder has uniform particle size, and the average particle size can be kept below 50 microns.
Example 2
This example is substantially the same as example 1, except that the inert gas atmosphere is different from the inert gas atmosphere, specifically: 21 ml/m in inert gas atmosphere3The gasified treatment liquid of (3);
the forming method of the inert gas environment comprises the following steps: gasifying the treatment liquid to obtain a gasified treatment liquid, specifically, injecting the gasified treatment liquid into an inert gas environment at the temperature of 230 ℃ and the pressure of 0.75 standard atmospheric pressure, monitoring the concentration of the gasified treatment liquid in the inert gas environment in real time through a concentration detector and compensating in real time, and gasifying the treatment liquid into the inert gas environment to ensure that the concentration control of the components of the treatment liquid is more stable, the forming effect of the CuCrNbZr alloy powder of the gasified treatment liquid is better, the surface oxidation of the CuCrNbZr alloy powder can be effectively prevented, and the oxidation rate is only 2-3%; the treatment liquid is liquid at normal temperature and normal pressure, so that the treatment liquid is easy to store and prepare for use;
wherein the treating fluid comprises the following components: 1.5 g of benzotriazole, 7 ml of phytic acid, 12 ml of hydrogen peroxide, 15 ml of polyethylene glycol and 15 ml of mannitol, and the material components are selected under a large amount of experimental researches, so that the requirements of gasifying and atomizing the treating fluid of the CuCrNbZr alloy powder in the atomization powder preparation process are met, the oxidation phenomenon of the finished CuCrNbZr alloy powder is effectively prevented, and the economic benefit is remarkable.
Example 3
This example is substantially the same as example 1, except that the inert gas atmosphere is different from the inert gas atmosphere, specifically: spraying 4 ml/min of atomized treatment liquid in an inert gas environment through a gas distribution plate;
the forming method of the inert gas environment comprises the following steps: atomizing the treatment liquid into liquid drops with the particle size of 20-40 mu m by utilizing ultrasonic atomization to obtain the atomized treatment liquid, uniformly mixing the atomized treatment liquid with inert gas, spraying the mixture through a gas distribution disc, mixing the atomized treatment liquid into an inert gas environment, and effectively preventing the surface of the CuCrNbZr alloy powder from being oxidized with the oxidation rate of only 4-5%, wherein the operation is simple, the preparation cost is lower;
wherein the treating fluid comprises the following components: 1.5 g of benzotriazole, 7 ml of phytic acid, 12 ml of hydrogen peroxide, 15 ml of polyethylene glycol and 15 ml of mannitol, and the material components are selected under a large amount of experimental researches, so that the requirements of gasifying and atomizing the treating fluid of the CuCrNbZr alloy powder in the atomization powder preparation process are met, the oxidation phenomenon of the finished CuCrNbZr alloy powder is effectively prevented, and the economic benefit is remarkable.
Example 4
The embodiment is basically the same as embodiment 1, and is different from embodiment 1 in that the ingredients in step S1 are different, specifically: according to the weight percentage of 0.5 percent of Cr, 0.3 percent of Nb, 0 percent of Zr and the balance of Cu and inevitable impurities, corresponding raw materials are selected and weighed and mixed to obtain alloy powder.
Example 5
The embodiment is basically the same as embodiment 1, and is different from embodiment 1 in that the ingredients in step S1 are different, specifically: according to 8 wt% of Cr, 7 wt% of Nb, 0.55 wt% of Zr and the balance of Cu and inevitable impurities, selecting and weighing corresponding raw materials, and mixing to obtain alloy powder.
Example 6
The present embodiment is substantially the same as embodiment 1, except that the cold isostatic pressing parameters in step S2 are different, specifically: the pressure of the cold isostatic pressing is 100 MPa, and the pressure maintaining time is 5 min.
Example 7
The present embodiment is substantially the same as embodiment 1, except that the cold isostatic pressing parameters in step S2 are different, specifically: the pressure of the cold isostatic pressing is 300 MPa, and the pressure maintaining time is 10 min.
Example 8
The present embodiment is substantially the same as embodiment 1, and differs therefrom in that the preheating parameters in step S3 are different, specifically: the electrode rod pressed in step S2 was preheated at 400 ℃ for 2 hours.
Example 9
The present embodiment is substantially the same as embodiment 1, and differs therefrom in that the preheating parameters in step S3 are different, specifically: the electrode rod pressed in step S2 was preheated at 800 ℃ for 6 hours.
Example 10
This example is substantially the same as example 1, except that the sintering temperature in step S3 is different, specifically: the sintering temperature was 900 ℃.
Example 11
This example is substantially the same as example 1, except that the sintering temperature in step S3 is different, specifically: the sintering temperature was 1100 ℃.
Example 12
The present embodiment is substantially the same as embodiment 1, and is different from embodiment 1 in that the melting parameters in step S4 are different, specifically: the smelting current is as follows: 8 KA, and stirring for 10 s.
Example 13
The present embodiment is substantially the same as embodiment 1, and is different from embodiment 1 in that the melting parameters in step S4 are different, specifically: the smelting current is as follows: 15 KA, while stirring for 25 s.
Example 14
The present embodiment is substantially the same as embodiment 1, and is different from embodiment 1 in that the parameters of plasma rotating electrode aerosolization are different, specifically: the rotating speed is 13000 r/min, the current is 2000A, and the feeding speed is 1 mm/s.
Example 15
The present embodiment is substantially the same as embodiment 1, and is different from embodiment 1 in that the parameters of plasma rotating electrode aerosolization are different, specifically: the rotating speed is 18000 r/min, the current is 2500A, and the feeding speed is 2 mm/s.
Example 16
The present embodiment is substantially the same as embodiment 2, and is different from embodiment 2 in that the content of the gasified treatment liquid contained in the inert gas environment is different, specifically: contains 15 ml/m in inert gas atmosphere3The gasified treatment liquid of (2).
Example 17
This example is substantially the same as example 2 except that the gaseous treating solution contained in the inert gas atmosphere containsThe different amounts are specifically: the content of the active component in the inert gas environment is 25 ml/m3The gasified treatment liquid of (2).
Example 18
The present embodiment is substantially the same as embodiment 2, and the difference is that the preparation of the treatment solution is different, specifically: the treating fluid comprises the following components: 1 g of benzotriazole, 5 ml of phytic acid, 9 ml of hydrogen peroxide, 10 ml of polyethylene glycol and 10 ml of mannitol.
Example 19
The present embodiment is substantially the same as embodiment 2, and the difference is that the preparation of the treatment solution is different, specifically: the treating fluid comprises the following components: 2 g of benzotriazole, 10 ml of phytic acid, 15 ml of hydrogen peroxide, 20 ml of polyethylene glycol and 20 ml of mannitol.
Example 20
This example is substantially the same as example 3, except that the amount of the atomized treatment liquid sprayed in the inert gas atmosphere is different, specifically: spraying atomized treatment liquid with the dosage of 3 ml/min through a gas distribution plate in an inert gas environment.
Example 21
This example is substantially the same as example 3, except that the amount of the atomized treatment liquid sprayed in the inert gas atmosphere is different, specifically: spraying 5 ml/min of atomized treatment liquid through a gas distribution plate in an inert gas environment.
Examples of the experiments
Aiming at the CuCrNbZr alloy powder prepared by each embodiment, hot isostatic pressing is carried out on the CuCrNbZr alloy powder to prepare a bulk material, and the softening temperature, hardness and conductivity of the bulk material are respectively tested, and the following specific researches are carried out:
1. the influence of different inert gas environments on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 1, 2, 3 are shown in table 1 below:
table 1 examples 1-3 table for testing the properties of each block material
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 1 | 867 | 158 | 70 |
Example 2 | 868 | 157 | 75 |
Example 3 | 864 | 158 | 73 |
From the results in table 1, it can be seen that different inert gas environments have no influence on the softening temperature and hardness of the bulk material subjected to hot isostatic pressing of the prepared CuCrNbZr alloy powder, while the inert gas environments of examples 2 and 3 have a certain improvement on the electrical conductivity of the bulk material subjected to hot isostatic pressing of the prepared CuCrNbZr alloy powder, and the comparison shows that the CuCrNbZr alloy powder prepared by the preparation method of example 2 has better overall performance.
2. The influence of different ingredients on the prepared CuCrNbZr alloy powder is explored
The results of the experimental comparisons of examples 1, 4 and 5 with 7 groups of CuCrNbZr alloy powders with different compositions are shown in table 2 below:
TABLE 2 Performance test Table for bulk material of each ingredient of CuCrNbZr alloy powder
Group of | Cr(wt%) | Nb(wt%) | Zr(wt%) | Cu(wt%) | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 1 | 3.6 | 2.3 | 0.25 | Balance of | 867 | 158 | 70 |
Example 4 | 0.5 | 0.3 | 0 | Balance of | 560 | 145 | 97 |
Example 5 | 8 | 7 | 0.55 | Balance of | 957 | 186 | 61 |
Matching group 1 | 3.5 | 2 | 0 | Balance of | 850 | 154 | 75 |
Matching group 2 | 3.7 | 2.6 | 0.31 | Balance of | 875 | 164 | 68 |
Group 3 | 6.48 | 5.32 | 0.25 | Balance of | 948 | 169 | 66 |
Matching group 4 | 6.5 | 5.5 | 0.25 | Balance of | 968 | 173 | 65 |
Make up 5 | 6.58 | 5.41 | 0.36 | Balance of | 955 | 162 | 68 |
Matching group 6 | 6.67 | 5.86 | 0.31 | Balance of | 952 | 170 | 69 |
Matching group 7 | 1.1 | 0 | 0.08 | Balance of | 550 | 140 | 85 |
The results in the table 2 show that different proportions of Cr, Nb, Zr, and Cu have certain influence on the properties of the bulk material of the CuCrNbZr alloy powder, and the CuCrNbZr alloy powder with different proportions can be selected according to actual requirements for preparation;
meanwhile, as shown in fig. 1, a gold phase diagram of the CuCrNbZr alloy in example 1, and as shown in fig. 2, an SEM topography diagram of the CuCrNbZr alloy powder in group 1, it can be seen that the CuCrNbZr alloy powder prepared by the method of the present invention has high sphericity and uniform particle size.
3. The influence of different cold isostatic pressing parameters on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 1, 6, 7 are shown in table 3 below:
table 3 table for testing properties of each block material of examples 1, 6 and 7
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 1 | 867 | 158 | 70 |
Example 6 | 854 | 145 | 67 |
Example 7 | 859 | 152 | 69 |
From the results of table 3 above, it can be seen that different cold isostatic pressing parameters have some influence on the softening temperature, hardness and electrical conductivity of the bulk material hot isostatically pressed with the prepared CuCrNbZr alloy powder, and the cold isostatic pressing parameters of example 1 are relatively better.
4. The influence of different preheating parameters on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 1, 8, 9 are shown in table 4 below:
table 4 table for testing properties of each block material of examples 1, 8 and 9
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 1 | 867 | 158 | 70 |
Example 6 | 849 | 141 | 65 |
Example 7 | 857 | 149 | 68 |
From the results of table 4 above, it can be seen that different preheating parameters have certain influence on the softening temperature, hardness and conductivity of the bulk material subjected to hot isostatic pressing by the prepared CuCrNbZr alloy powder, and the preheating parameters of example 1 are relatively better.
5. The influence of different sintering temperatures on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 1, 10, 11 are shown in table 5 below:
table 5 table for testing properties of each block material of examples 1, 10 and 11
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 1 | 867 | 158 | 70 |
Example 10 | 863 | 154 | 68 |
Example 11 | 869 | 159 | 70 |
From the results of table 5, it can be seen that different sintering temperatures have some influence on the softening temperature, hardness and electrical conductivity of the bulk material subjected to hot isostatic pressing by the prepared CuCrNbZr alloy powder, but the influence is not great, and the sintering temperature of example 11 is relatively better, but the performance difference between example 11 and example 1 is not obvious, and the sintering temperature of example 1 is more economic from the economic viewpoint.
6. The influence of different smelting parameters on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 1, 12, 13 are shown in table 6 below:
table 6 table for testing properties of each block material of examples 1, 12 and 13
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 1 | 867 | 158 | 70 |
Example 12 | 862 | 153 | 66 |
Example 13 | 870 | 161 | 71 |
From the results of table 6, it can be seen that different melting parameters have certain effects on the softening temperature, hardness and conductivity of the bulk material subjected to hot isostatic pressing by the prepared CuCrNbZr alloy powder, and the cold isostatic pressing parameter of example 13 is relatively better, but the performance difference between example 13 and example 1 is not obvious, and the melting parameter of example 1 is more economic from the economic viewpoint.
7. The influence of different plasma rotating electrode gas atomization parameters on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 1, 14, 15 are shown in table 7 below:
table 7 table for testing properties of bulk materials of examples 1, 14 and 15
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 1 | 867 | 158 | 70 |
Example 14 | 865 | 154 | 68 |
Example 15 | 871 | 160 | 70 |
From the results in table 7, it can be seen that different parameters of gas atomization by using a plasma rotary electrode have certain effects on the softening temperature, hardness and conductivity of the bulk material subjected to hot isostatic pressing by the prepared CuCrNbZr alloy powder, and the parameters of gas atomization by using a plasma rotary electrode in example 15 are relatively better, but the performance difference between example 15 and example 1 is not obvious, and the parameters of gas atomization by using a plasma rotary electrode in example 1 are better in economical efficiency from the viewpoint of economical efficiency.
8. The influence of the inert gas environments of the gasified treatment liquids with different contents on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 2, 16, 17 are shown in table 8 below:
table 8 table for testing properties of each of the bulk materials of examples 2, 16 and 17
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 2 | 868 | 157 | 75 |
Example 16 | 866 | 157 | 72 |
Example 17 | 868 | 158 | 76 |
From the results of table 8, it can be seen that the content of the liquefied treatment solution contained in different inert gas environments has no influence on the softening temperature and hardness of the bulk material subjected to hot isostatic pressing of the prepared CuCrNbZr alloy powder, but the conductivity has a certain influence, and the comparison shows that the performance of the CuCrNbZr alloy powder prepared by the preparation method of example 17 is better as a whole, but the comparison between example 2 and example 16, and between example 2 and example 17 shows that the effect is remarkably reduced with the increase of the dosage from example 2 to example 17, so the treatment effect of example 2 is relatively better from the economical point of view.
9. The influence of different treatment liquid preparation groups on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons made with examples 2, 18, 19 are shown in table 9 below:
table 9 table for testing properties of each block material of examples 2, 18 and 19
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 2 | 868 | 157 | 75 |
Example 18 | 869 | 158 | 73 |
Example 19 | 867 | 157 | 73 |
Comparative example | 867 | 158 | 71 |
The results in table 9 show that different treatment liquid formulations have no influence on the softening temperature and hardness of the bulk material subjected to hot isostatic pressing of the prepared CuCrNbZr alloy powder, but the conductivity has a certain influence, and the comparison shows that the CuCrNbZr alloy powder prepared by the preparation method in example 2 has better overall performance;
meanwhile, the comparative example adopts 1.5 g of benzotriazole with the same dosage, and other components are complemented by polyethylene glycol to serve as the comparative example, and the conductivity of the comparative example is obviously lower than that of the examples 2, 18 and 19.
10. The influence of the inert gas environments of the atomized treatment liquids with different contents on the prepared CuCrNbZr alloy powder is explored
The results of experimental comparisons of examples 3, 20, 21 are shown in table 10 below:
table 10 table for testing properties of each block material of examples 3, 20 and 21
Group of | Softening temperature/. degree.C | hardness/HB | Conductivity/% IACS |
Example 3 | 864 | 158 | 73 |
Example 20 | 863 | 158 | 72 |
Example 21 | 864 | 157 | 73 |
From the results in table 10, it can be seen that the content of the atomized treatment solution in different inert gas environments has no influence on the softening temperature and hardness of the bulk material subjected to hot isostatic pressing by the prepared CuCrNbZr alloy powder, but has a certain influence on the electrical conductivity, and it can be seen by comparison that the CuCrNbZr alloy powder prepared by the preparation methods of examples 3 and 21 has better overall performance, but the economy of example 3 is relatively better in consideration of the preparation cost and other factors, and can be selected according to actual requirements.
Claims (5)
1. A method for preparing CuCrNbZr alloy powder by utilizing plasma rotating electrode gas atomization is characterized by comprising the following steps:
s1 ingredient
Selecting and weighing corresponding raw materials according to the weight percentage of 0.5-8% of Cr, 0.3-7% of Nb, 0-0.55% of Zr and the balance of Cu and inevitable impurities, and mixing to obtain alloy powder;
s2 prefabricated blank
Fully and uniformly mixing the alloy powder prepared in the step S1, and performing cold isostatic pressing to obtain an electrode rod;
s3 vacuum sintering
Preheating the electrode rod obtained by pressing in the step S2 at the temperature of 400-800 ℃ for 2-6 h, then placing the preheated blank into a vacuum sintering furnace for sintering, wherein the sintering temperature is 900-1100 ℃, and the vacuum degree is kept at 10 during the sintering process-2Below Pa, and then cooling to obtain a sintered blank;
s4 vacuum consumable arc melting
Taking the sintered blank obtained after sintering in the step S3 as a consumable arc melting furnace electrode, and carrying out arc melting in a vacuum consumable arc melting furnace to obtain a melted electrode rod;
s5 plasma rotary electrode gas atomization
Taking the smelted electrode rod obtained by vacuum consumable arc smelting in the step S4 as an atomizing electrode rod, heating the end part of the atomizing electrode rod by using plasma, simultaneously rotating the atomizing electrode rod at a high speed, refining molten liquid drops by means of centrifugal force, solidifying in an inert gas environment and spheroidizing under the action of surface tension to form powder to obtain CuCrNbZr alloy powder;
the inert gas environment is as follows: 15-25 ml/m in inert gas atmosphere3Spraying the atomized treatment liquid with the dosage of 3-5 ml/min through a gas distribution plate in an inert gas environment;
15-25 ml/m in inert gas atmosphere3The method for forming the gasified treatment liquid of (2) is: gasifying the treatment liquid to obtain a gasified treatment liquid, injecting the gasified treatment liquid into an inert gas environment under the same air pressure environment, monitoring the concentration of the gasified treatment liquid in the inert gas environment in real time through a concentration detector, and compensating in real time;
spraying atomized treatment liquid with the dosage of 3-5 ml/min through a gas distribution plate in an inert gas environment, wherein the forming method comprises the following steps: atomizing the treatment solution into liquid drops with the particle size of 20-40 mu m by utilizing ultrasonic atomization to obtain the atomized treatment solution, uniformly mixing the atomized treatment solution with inert gas, and spraying the mixture through a gas distribution disc;
wherein the treating fluid comprises the following components: 1-2 g of benzotriazole, 5-10 ml of phytic acid, 9-15 ml of hydrogen peroxide, 10-20 ml of polyethylene glycol and 10-20 ml of mannitol.
2. The method for preparing the CuCrNbZr alloy powder by using the plasma rotary electrode gas atomization, according to the claim 1, wherein the mass ratio of Cr to Nb in the step S1 satisfies the following condition: 1 < Cr/Nb < 2.
3. The method for preparing the CuCrNbZr alloy powder by using the plasma rotary electrode gas atomization, according to claim 1, wherein the parameters of the cold isostatic pressing in the step S2 are as follows: the pressure of the cold isostatic pressing is 100-300 MPa, and the pressure maintaining time is 5-10 min.
4. The method for preparing the CuCrNbZr alloy powder by using the plasma rotating electrode for gas atomization as claimed in claim 1, wherein the smelting current in the step S4 is as follows: 8-15 KA and 10-25 s of stirring.
5. The method as claimed in claim 1, wherein the rotation speed in step S5 is 13000-.
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