CN115383123A - Preparation method and application of high-density tungsten powder for 3DP printing - Google Patents
Preparation method and application of high-density tungsten powder for 3DP printing Download PDFInfo
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- CN115383123A CN115383123A CN202211298874.0A CN202211298874A CN115383123A CN 115383123 A CN115383123 A CN 115383123A CN 202211298874 A CN202211298874 A CN 202211298874A CN 115383123 A CN115383123 A CN 115383123A
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 238000007639 printing Methods 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 67
- 239000011812 mixed powder Substances 0.000 claims abstract description 35
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 238000000498 ball milling Methods 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000004048 modification Effects 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- DKMROQRQHGEIOW-UHFFFAOYSA-N Diethyl succinate Chemical compound CCOC(=O)CCC(=O)OCC DKMROQRQHGEIOW-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 claims description 5
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 4
- 238000003892 spreading Methods 0.000 claims description 4
- 230000007480 spreading Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 abstract description 14
- 239000010937 tungsten Substances 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 229910045601 alloy Inorganic materials 0.000 description 37
- 239000000956 alloy Substances 0.000 description 37
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 229910000881 Cu alloy Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method and application of high-density tungsten powder for 3DP printing, which comprises the following steps: s1, weighing tungsten powder of 20-150 mu m and tungsten powder of 0.5-10 mu m according to a ratio; s2, mixing the two tungsten powders, and performing ball milling and powder mixing, wherein the ball-material ratio of the ball milling and powder mixing is 1:3, ball-milling and mixing for 7 to 9 hours to obtain mixed powder after the ball-milling and mixing are finished; and S3, drying the mixed powder at the drying temperature of 120-180 ℃ for 7-9 h to obtain high-density tungsten powder after drying is completed, mixing the high-granularity tungsten powder with the low-granularity tungsten powder to obtain the high-density tungsten powder with the density and the fluidity meeting the requirements, and finally, forming a tungsten framework through 3DP printing to have good performance and effectively reduce the production cost.
Description
Technical Field
The invention relates to the technical field of metal powder manufacturing, in particular to a preparation method and application of high-density tungsten powder for 3DP printing.
Background
The 3DP printing is an additive manufacturing technology, which mainly prints the section of a part on material powder by spraying adhesive through a spray head, and the specific process comprises the following steps: after the last layer is bonded, the forming cylinder descends for a certain distance, the powder supply cylinder ascends for a certain height, a plurality of powder is pushed out, the powder is pushed to the forming cylinder by the powder paving roller, and the powder is paved and compacted. The spray head, under computer control, selectively sprays adhesive build layers according to the forming data of the next build section. When the powder spreading roller spreads the powder, the redundant powder is collected by the powder collecting device. The powder is fed, spread and sprayed with the binder in cycles, and finally the three-dimensional powder is bonded.
The 3DP printing can be adopted to realize the manufacturing of special-shaped pieces and complex pieces, and the powder density can be uniform; uneven density, difficult pressing of special-shaped parts, layering, long manufacturing period of a die and limitation on service life, which are easily caused by a traditional die pressing process, do not occur, but the quality of printing powder can limit the product development of a 3DP printing process.
At present, when a tungsten-copper alloy part is prepared, a tungsten framework needs to be printed, then copper infiltration treatment is carried out on the tungsten framework to obtain the tungsten-copper alloy, and in order to ensure the performance of the tungsten-copper alloy, the tap density of tungsten powder for printing the framework slightly exceeds the framework density, so that the requirements on the granularity and the flowability of printing powder are high, special printing powder is adopted in printing, but the powder is expensive and needs to be customized specially, and the production cost is high.
Therefore, there is an urgent need for a high-density tungsten powder that is low in cost and can be used for 3DP printing.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method and application of high-density tungsten powder for 3DP printing.
The technical scheme of the invention is as follows: a preparation method of high-density tungsten powder for 3DP printing comprises the following steps:
s1, preparing powder
Weighing tungsten powder of 20 to 150 mu m and tungsten powder of 0.5 to 10 mu m according to the proportion;
s2, mixing the powder
Mixing the tungsten powder with the diameter of 20-150 mu m and the tungsten powder with the diameter of 0.5-10 mu m, and then carrying out ball milling and powder mixing, wherein the ball-to-material ratio of the ball milling and powder mixing is 1:3, ball-milling and mixing for 7 to 9 hours to obtain mixed powder after the ball-milling and mixing are finished;
s3, drying
And drying the mixed powder at the drying temperature of 120-180 ℃ for 7-9 h to obtain the high-density tungsten powder.
Description of the drawings: according to the method, the high-density tungsten powder with the density and the fluidity meeting the requirements is obtained by mixing the high-granularity tungsten powder and the low-granularity tungsten powder according to a certain proportion, and finally, the tungsten skeleton formed after 3DP printing has good performance, and the production cost can be effectively reduced.
Further, in the step S1, the weight ratio of the tungsten powder with the diameter of 20 to 150 μm to the tungsten powder with the diameter of 0.5 to 10 μm is 10:1 to 2.
Description of the invention: the high-density tungsten powder prepared according to the proportion has high tap density, and can print a high-density tungsten framework.
Further, in step S1, the tungsten powder of 20 to 150 μm and the tungsten powder of 0.5 to 10 μm are respectively sieved once by using a 180-mesh screen.
Description of the invention: the agglomerated powder in the tungsten powder can be separated by one-time sieving, so that the tungsten powder is easier to mix uniformly.
Further, in the step S2, the volume of the ball material of the ball milling mixed powder is less than or equal to 2/3 of the volume of the ball milling barrel.
Description of the drawings: the ball milling effect can be ensured by controlling the volume of the ball material during ball milling.
Further, in step S3, the high-density tungsten powder is sieved twice using a 180-mesh screen.
Description of the invention: after secondary sieving, agglomerated powder can be separated, and the influence of the agglomerated powder on the fluidity of the high-density tungsten powder is avoided.
Further, the high-density tungsten powder is placed in a drying oven at the temperature of 80 ℃ for constant-temperature storage.
Description of the invention: the preservation in the drying oven can prevent the powder from getting damp and influencing the powder flowability.
Further, in step S2, after the mixed powder is obtained, modifying the mixed powder; the modification treatment method comprises the following steps: putting 500g of mixed powder into a container, heating the mixed powder to 120-160 ℃, gradually adding a treating agent into the container in the heating process, wherein the addition amount of the treating agent is gradually reduced along with the temperature rise from 40-60ml/min, and the addition amount of the treating agent is reduced by 4-6 ml/min when the temperature rises by 5 ℃ every time, and stirring the mixed powder until the heating is finished after the adding of the treating agent is stopped.
Description of the drawings: the mixed powder is modified by the treating agent, so that the powder fluidity can be improved, the agglomeration phenomenon of the tungsten powder is reduced, and the tungsten skeleton structure is more uniform.
Further, the components of the treating agent comprise the following components in percentage by mass: 20-30% of diethyl succinate, 10-20% of dimethyl phosphite, 15-25% of trimethyl methoxysilane and the balance of absolute ethyl alcohol.
Description of the invention: the treating agent can improve the powder fluidity, reduce the agglomeration of the powder, improve the bonding property of the tungsten framework and the copper when the tungsten framework is infiltrated with the copper, reduce the segregation of the copper, ensure that the copper is uniformly distributed, reduce the pores, improve the density of the tungsten-copper alloy and improve the performance of the tungsten-copper alloy.
Further, the invention also discloses application of the high-density tungsten powder in 3DP printing.
Further, the 3DP printing method is:
s1, adding the high-density tungsten powder into a powder cylinder of printing equipment;
s2, pushing the high-density tungsten powder with one layer thickness into a forming cylinder from a powder cylinder by a powder spreading roller of the printing equipment, flattening and compacting, and spraying an adhesive on the high-density tungsten powder of the forming cylinder by a spray head of the printing equipment according to the cross section shape of one layer of the part, wherein the one layer thickness is 0.013-0.1mm;
and S3, after the adhesive is sprayed, repeating the step S2 to finish the next layer of printing of the part until the part is molded.
Description of the drawings: the tungsten skeleton with fine structure, uniform powder distribution and high density can be printed by the 3DP printing method.
The beneficial effects of the invention are:
(1) According to the invention, high-density tungsten powder with the density and the fluidity meeting the requirements is obtained by mixing high-granularity tungsten powder and low-granularity tungsten powder, and finally, the tungsten skeleton formed after 3DP printing has good performance, and the high-density tungsten powder has low preparation cost, so that the production cost can be effectively reduced;
(2) According to the invention, the treating agent is adopted to modify the mixed powder, so that the powder fluidity can be improved, the agglomeration phenomenon of tungsten powder is reduced, the tungsten framework structure is more uniform, the associativity of the tungsten framework and copper can be improved when the tungsten framework is infiltrated with copper, the segregation of copper is reduced, the copper is uniformly distributed, the pores are reduced, the density of the tungsten-copper alloy is improved, and the performance of the tungsten-copper alloy is improved.
Drawings
FIG. 1 is a diagram of the gold phase of a CuW80 alloy prepared from the high-density tungsten powder of example 1 of the present 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 preparation method of high-density tungsten powder for 3DP printing comprises the following steps:
s1, preparing powder
According to the following steps: weighing tungsten powder of 20 to 150 mu m and tungsten powder of 0.5 to 10 mu m according to the weight proportion of 1.5, and sieving the tungsten powder of 20 to 150 mu m and the tungsten powder of 0.5 to 10 mu m for one time by using a 180-mesh sieve;
s2, mixing the powder
Mixing the tungsten powder with the diameter of 20-150 mu m and the tungsten powder with the diameter of 0.5-10 mu m, and then carrying out ball milling and powder mixing, wherein the ball-to-material ratio of the ball milling and powder mixing is 1:3, ball milling and powder mixing time is 8 hours, mixed powder is obtained after ball milling and powder mixing are finished, and the volume of ball materials of the ball milling and powder mixing is 2/3 of the volume of a ball milling barrel;
s3, drying
And drying the mixed powder at the drying temperature of 150 ℃ for 8h to obtain high-density tungsten powder, secondarily sieving the high-density tungsten powder by using a 180-mesh sieve, and storing the high-density tungsten powder in a drying oven at the constant temperature of 80 ℃.
Example 2
The difference between this example and example 1 is that the ball milling and powder mixing time is 7 hours.
Example 3
The difference between this example and example 1 is that the ball milling and powder mixing time is 9h.
Example 4
The difference between the embodiment and embodiment 1 is that the mixed powder is dried, the drying temperature is 120 ℃, and the drying time is 7h.
Example 5
The difference between the embodiment and the embodiment 1 is that the mixed powder is dried, the drying temperature is 180 ℃, and the drying time is 9h.
Example 6
The difference between the embodiment and the embodiment 1 is that the weight ratio of the tungsten powder with the particle size of 20 to 150 μm to the tungsten powder with the particle size of 0.5 to 10 μm is 10:1.
example 7
The difference between the embodiment and the embodiment 1 is that the weight ratio of the tungsten powder with the particle size of 20 to 150 μm to the tungsten powder with the particle size of 0.5 to 10 μm is 10:2.
example 8
The difference between this example and example 1 is that, in step S2, after the mixed powder is obtained, the mixed powder is subjected to modification treatment;
the modification treatment method comprises the following steps: 500g of mixed powder is placed into a container, the mixed powder is heated to 140 ℃, a treating agent is gradually added into the container in the heating process, the adding amount of the treating agent is gradually reduced along with the temperature rise from 50ml/min, the adding amount of the treating agent is reduced by 5ml/min when the temperature rises by 5 ℃, and the mixed powder is stirred until the heating is finished after the adding of the treating agent is stopped.
The treating agent comprises the following components in percentage by mass: 25% of diethyl succinate, 15% of dimethyl phosphite, 20% of trimethyl methoxy silane and the balance of absolute ethyl alcohol.
Example 9
This example differs from example 8 in that the mixed powder was placed in a container and heated to 120 ℃.
Example 10
This example is different from example 8 in that the mixed powder was put in a container and the mixed powder was heated to 160 ℃.
Example 11
This example is different from example 8 in that the addition amount of the treating agent gradually decreased from 40ml/min with the increase in temperature, and the addition amount of the treating agent decreased by 4ml/min for every 5 ℃ increase in temperature.
Example 12
The difference between the embodiment and the embodiment 8 is that the addition amount of the treating agent is gradually reduced from 60ml/min along with the increase of the temperature, and the addition amount of the treating agent is reduced by 6ml/min for every 5 ℃ increase of the temperature.
Example 13
The difference between the embodiment and the embodiment 8 is that the treating agent comprises the following components in percentage by mass: 20% of diethyl succinate, 10% of dimethyl phosphite, 15% of trimethyl methoxysilane and the balance of absolute ethyl alcohol.
Example 14
The difference between the embodiment and the embodiment 8 is that the treating agent comprises the following components in percentage by mass: 30% of diethyl succinate, 20% of dimethyl phosphite, 25% of trimethyl methoxysilane and the balance of absolute ethyl alcohol.
Example 15
This example provides the use of the high density tungsten powder prepared in example 14 in 3DP printing;
the 3DP printing method comprises the following steps:
s1, adding the high-density tungsten powder into a powder cylinder of printing equipment;
s2, pushing the mixed powder with one layer thickness into a forming cylinder from a powder cylinder by a powder spreading roller of the printing equipment, flattening and compacting, spraying an adhesive on the high-density tungsten powder of the forming cylinder by a spray head of the printing equipment according to the cross section shape of a tungsten framework, wherein the one layer thickness is 0.05mm;
and S3, after the adhesive is sprayed, repeating the step S2 to finish the next layer of printing of the tungsten framework until the tungsten framework is molded.
Example 16
This example differs from example 15 in that the one layer thickness is 0.013mm.
Example 17
This example differs from example 15 in that the one layer thickness is 0.1mm.
Examples of the experiments
In order to explore the influence of the high-density tungsten powder obtained by different parameters on the performance of a finished product, a tungsten framework is printed from the high-density tungsten powder obtained in each embodiment by a 3DP printing technology and is prepared into a CuW80 alloy; metallographic detection is carried out on the CuW80 alloy obtained in the embodiment 1, and as shown in figure 1, the CuW80 alloy obtained in the embodiment 1 has a compact structure and no obvious structure defects;
meanwhile, the performance of the CuW80 alloy obtained in each embodiment is tested to investigate the influence of the high-density tungsten powder prepared under different process parameters on the performance of the CuW80 alloy, and the specific investigation is as follows:
1. the influence of the ball milling powder mixing time on the performance of the CuW80 alloy is researched:
the properties of the CuW80 alloy obtained by comparing examples 1, 2 and 3 are shown in table 1:
TABLE 1 comparison of CuW80 alloy properties obtained at different ball-milling powder-mixing times
| Group of | Density (g/cm) 3 ） | Hardness (HB) |
| Example 1 | 14.52 | 188.7 |
| Example 2 | 13.24 | 168.9 |
| Example 3 | 14.77 | 191.3 |
As can be seen from the data in table 1, the CuW80 obtained in example 1 has higher density and hardness and better performance compared to example 2, which indicates that the ball milling powder mixing time of example 2 is slightly shorter, while the ball milling powder mixing time of example 1 is more sufficient, so that the powder can be mixed more uniformly, and compared to example 3, the performance of example 1 is not much different, so that the ball milling powder mixing time selected in example 1 is better in terms of time cost.
2. The influence of drying parameters on the performance of the CuW80 alloy is explored:
the performance data of the CuW80 alloy obtained by using examples 1, 4 and 5 as experimental comparisons are shown in Table 2:
TABLE 2 comparison of the properties of CuW80 alloys obtained with different drying parameters
| Group of | Density (g/cm) 3 ） | Hardness (HB) |
| Example 1 | 14.52 | 188.7 |
| Example 4 | 13.56 | 170.1 |
| Example 5 | 14.63 | 189.0 |
As can be seen from the data in Table 2, compared with the example 4, the CuW80 alloy obtained by the drying parameters selected in the example 1 has better performance; compared with the embodiment 5, the embodiment 1 has the advantages that the performance is not greatly different, and the drying parameters selected by the embodiment 1 are better in view of time cost.
3. The influence of the powder ratio on the properties of the CuW80 alloy is explored:
the properties of the CuW80 alloy obtained by using examples 1, 6 and 7 as experimental comparisons are shown in Table 3:
TABLE 3 comparison of the properties of the CuW80 alloys obtained at different powder ratios
| Group of | Density (g/cm) 3 ） | Hardness (HB) |
| Example 1 | 14.52 | 188.7 |
| Example 6 | 13.74 | 172.8 |
| Example 7 | 13.68 | 170.5 |
From the data in Table 3, it is clear that the CuW80 alloy obtained with the powder ratio selected in example 1 has the best performance, and the powder ratio selected in example 1 is the best.
4. The influence of modification treatment on the performance of the CuW80 alloy is researched:
the properties of the CuW80 alloy obtained by comparing examples 1 and 8 are shown in table 4:
TABLE 4 comparison of the properties of the CuW80 alloys obtained by the modification treatment
| Group of | Density (g/cm) 3 ） | Hardness (HB) |
| Example 1 | 14.52 | 188.7 |
| Example 8 | 16.75 | 202.4 |
As can be seen from the data in Table 4, the density and hardness of the CuW80 alloy prepared from the modified mixed powder are higher than those of the unmodified mixed powder, which indicates that the modification treatment can effectively improve the performance of the prepared CuW80 alloy.
5. The influence of the heating temperature on the performance of the CuW80 alloy in the modification treatment is explored:
the properties of the CuW80 alloy obtained by comparing examples 8, 9 and 10 are shown in Table 5:
TABLE 5 comparison of the properties of CuW80 alloys obtained at different heating temperatures in the modification treatment
| Group of | Density (g/cm) 3 ） | Hardness (HB) |
| Example 8 | 16.75 | 202.4 |
| Example 9 | 15.59 | 194.3 |
| Example 10 | 15.96 | 195.7 |
As is clear from the data in Table 5, the CuW80 alloy obtained at the heating temperature selected in example 8 exhibited the best performance, and the heating temperature selected in example 8 was the best.
6. The influence of the addition amount of the treating agent on the performance of the CuW80 alloy is researched:
the performance data of the CuW80 alloy obtained by using examples 8, 11 and 12 as experimental comparisons and using example 8 as a reference and using the treating agent in a one-time addition manner as comparative example 1 are shown in Table 6:
TABLE 6 comparison of the properties of CuW80 alloys obtained with different amounts of treating agents
| Group of | Density (g/cm) 3 ） | Hardness (HB) |
| Example 8 | 16.75 | 202.4 |
| Example 11 | 15.34 | 193.4 |
| Example 12 | 16.13 | 198.2 |
| Comparative example 1 | 14.98 | 190.6 |
From the data in Table 6, it is clear that the CuW80 alloy obtained with the treatment agent addition amount selected in example 8 is the best, and the CuW80 alloy obtained with the treatment agent addition method selected in example 8 is better, compared with comparative example 1, in example 8, and the treatment agent addition method of example 8 is better.
7. The influence of the components of the treating agent on the performance of the CuW80 alloy is researched:
the performance data of the CuW80 alloy obtained by using examples 8, 13 and 14 as experimental comparisons and using example 8 as a reference and absolute ethyl alcohol instead of diethyl succinate in the treating agent as comparative example 2 is shown in Table 7:
TABLE 7 comparison of the properties of the CuW80 alloys obtained with different treating agent compositions
| Group of | Density (g/cm) 3 ） | Hardness (HB) |
| Example 8 | 16.75 | 202.4 |
| Example 13 | 15.54 | 194.2 |
| Example 14 | 15.87 | 195.1 |
| Comparative example 2 | 15.16 | 190.8 |
As can be seen from the data in Table 7, the CuW80 alloy performance obtained by the treating agent components in example 8 is better in examples 8, 13 and 14, the treating agent components selected in example 8 are better, and the CuW80 alloy performance in comparative example 2 is improved but the amplitude is not large in example 8 compared with comparative example 2, which shows that the CuW80 alloy performance is improved by the combined action of diethyl succinate in the treating agent and other components in the treating agent.
Claims (9)
1. A preparation method of high-density tungsten powder for 3DP printing is characterized by comprising the following steps:
s1, preparing powder
Weighing 20 to 150 mu m tungsten powder and 0.5 to 10 mu m tungsten powder according to the proportion;
s2, mixing the powder
Mixing the tungsten powder of 20 to 150 mu m and the tungsten powder of 0.5 to 10 mu m, and then carrying out ball milling and powder mixing, wherein the ball-to-feed ratio of the ball-milling mixed powder is 1:3, performing ball milling and powder mixing for 7 to 9 hours to obtain mixed powder after the ball milling and powder mixing are completed;
s3, drying
And drying the mixed powder at the drying temperature of 120 to 180 ℃ for 7 to 9h to obtain the high-density tungsten powder after drying.
2. The method for preparing the high-density tungsten powder for 3DP printing according to claim 1, wherein in step S1, the weight ratio of the tungsten powder of 20 to 150 μm to the tungsten powder of 0.5 to 10 μm is 10:1 to 2.
3. The method for preparing the high-density tungsten powder for 3DP printing according to claim 1, wherein in step S1, the tungsten powder of 20 to 150 μm and the tungsten powder of 0.5 to 10 μm are sieved once by using a 180-mesh sieve.
4. The method for preparing high-density tungsten powder for 3DP printing according to claim 1, wherein in step S2, the volume of the ball material of the ball-milling mixed powder is less than or equal to 2/3 of the volume of the ball-milling barrel.
5. The method of claim 3, wherein in step S3, the high-density tungsten powder is sieved twice by using a 180-mesh screen.
6. The method for preparing the high-density tungsten powder for 3DP printing according to claim 1, wherein the high-density tungsten powder is stored in a drying oven at a constant temperature of 80 ℃.
7. The method for preparing high-density tungsten powder for 3DP printing according to claim 1, wherein in step S2, the mixed powder is modified after being obtained;
the modification treatment method comprises the following steps: putting 500g of mixed powder into a container, heating the mixed powder to 120-160 ℃, gradually adding a treating agent into the container in the heating process, wherein the addition amount of the treating agent is gradually reduced along with the temperature rise from 40-60ml/min, and the addition amount of the treating agent is reduced by 4-6 ml/min when the temperature rises by 5 ℃ every time, and stirring the mixed powder until the heating is finished after the adding of the treating agent is stopped.
8. The preparation method of the high-density tungsten powder for 3DP printing according to claim 7, wherein the components of the treating agent include, by mass: 20-30% of diethyl succinate, 10-20% of dimethyl phosphite, 15-25% of trimethyl methoxy silane and the balance of absolute ethyl alcohol.
9. Use of the high-density tungsten powder for 3DP printing prepared according to any one of claims 1 to 8, wherein said high-density tungsten powder is used in 3DP printing by:
s1, adding the high-density tungsten powder into a powder cylinder of printing equipment;
s2, pushing high-density tungsten powder with one layer thickness into a forming cylinder from a powder cylinder by a powder spreading roller of the printing equipment, flattening and compacting, and spraying an adhesive on the high-density tungsten powder of the forming cylinder by a spray head of the printing equipment according to the cross section shape of the part, wherein the one layer thickness is 0.013-0.1mm;
and S3, after the adhesive is sprayed, repeating the step S2 to finish the next layer of printing of the part until the part is molded.
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