CN115383123B - 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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- CN115383123B CN115383123B CN202211298874.0A CN202211298874A CN115383123B CN 115383123 B CN115383123 B CN 115383123B CN 202211298874 A CN202211298874 A CN 202211298874A CN 115383123 B CN115383123 B CN 115383123B
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 238000007639 printing Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 66
- 239000011812 mixed powder Substances 0.000 claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 4
- 239000010937 tungsten Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 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
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000007873 sieving Methods 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 3
- 238000003756 stirring Methods 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 description 40
- 239000000956 alloy Substances 0.000 description 40
- 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
- 230000000052 comparative effect Effects 0.000 description 8
- 229910000881 Cu alloy Inorganic materials 0.000 description 7
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007423 decrease Effects 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
- 238000009826 distribution Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004834 spray adhesive Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
Classifications
-
- 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
Abstract
The invention discloses a preparation method and application of high-density tungsten powder for 3DP printing, comprising the following steps: s1, weighing 20-150 mu m tungsten powder and 0.5-10 mu m tungsten powder according to a proportion; s2, mixing the two tungsten powders, and then carrying out ball milling and powder mixing, wherein the ball material ratio of the ball milling and powder mixing is 1:3, ball milling and powder mixing time is 7-9 h, and mixed powder is obtained after ball milling and powder mixing are completed; and S3, drying the mixed powder at the temperature of 120-180 ℃ for 7-9 hours to obtain high-density tungsten powder after the drying is completed, and 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, wherein the tungsten skeleton formed after 3DP printing has good performance and can 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, and mainly uses a spray head to spray adhesive to print the section of a part on material powder, and the specific process is as follows: after the last layer is bonded, the forming cylinder descends a distance, the powder supply cylinder ascends a height, a plurality of powders are pushed out, and the powder is pushed to the forming cylinder by the powder spreading roller to be spread and compacted. The spray head selectively sprays the adhesive build layer under computer control, pressing the formation data of a build section. The redundant powder is collected by the powder collecting device when the powder spreading roller spreads powder. The powder is sent, spread and sprayed repeatedly, and finally the three-dimensional powder is bonded.
3DP printing is adopted to realize the manufacture of special-shaped pieces and complex pieces, and meanwhile, the powder density can be uniform; the defects of uneven density, difficult pressing of special-shaped pieces, layering, long mold manufacturing period and limited service life which are easy to occur in the traditional molding process are avoided, but the quality of the printing powder can limit the product development of the 3DP printing process.
At present, when a tungsten-copper alloy part is prepared, a tungsten skeleton is required to be printed, then copper infiltration treatment is carried out on the tungsten skeleton to obtain tungsten-copper alloy, and in order to ensure the performance of the tungsten-copper alloy, the tap density of tungsten powder of the printed skeleton slightly exceeds the skeleton density, so that the requirements on granularity and flowability of the printed powder are higher, and special printed powder is adopted during printing, but the powder is expensive and needs to be specially customized, so that the production cost is higher.
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: the preparation method of the high-density tungsten powder for 3DP printing comprises the following steps:
s1, preparing powder
Weighing 20-150 mu m tungsten powder and 0.5-10 mu m tungsten powder according to the proportion;
s2, mixing powder
Mixing the tungsten powder with the particle size of 20-150 mu m and the tungsten powder with the particle size of 0.5-10 mu m, 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 powder mixing time is 7-9 h, and mixed powder is obtained after ball milling and powder mixing are completed;
s3, drying
And drying the mixed powder at the drying temperature of 120-180 ℃ for 7-9 hours to obtain the high-density tungsten powder after the drying is completed.
Description: 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, the tungsten skeleton formed after the 3DP printing is good in performance, and the production cost can be effectively reduced.
Further, in the step S1, the weight ratio of the tungsten powder with the thickness of 20-150 μm to the tungsten powder with the thickness of 0.5-10 μm is 10: 1-2.
Description: the high-density tungsten powder prepared according to the proportion has high tap density and can be printed into a high-density tungsten skeleton.
In the step S1, a 180-mesh screen is used for sieving the 20-150 mu m tungsten powder and the 0.5-10 mu m tungsten powder for one time.
Description: 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 ball material volume of the ball milling mixed powder is less than or equal to 2/3 of the ball milling barrel capacity.
Description: the ball milling effect can be ensured by controlling the ball material volume during ball milling.
Further, in step S3, the high-density tungsten powder is secondarily sieved using a 180 mesh sieve.
Description: the agglomerated powder can be separated after the secondary sieving, so that the agglomerated powder is prevented from affecting the fluidity of the high-density tungsten powder.
Further, the high-density tungsten powder is placed in a drying oven at 80 ℃ for constant temperature storage.
Description: the powder can be stored in a drying oven to prevent powder from being moist and affecting powder fluidity.
Further, in step S2, the mixed powder is modified after the mixed powder is obtained; the modification treatment method comprises the following steps: and (3) 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, gradually reducing the adding amount of the treating agent from 40-60 ml/min along with the temperature rise, reducing the adding amount of the treating agent by 4-6 ml/min when the temperature rises by 5 ℃ until the adding of the treating agent is stopped, and stirring the mixed powder until the heating is completed.
Description: after the mixed powder is modified by the treating agent, the powder fluidity can be improved, the agglomeration phenomenon of tungsten powder can be reduced, and the tungsten skeleton structure is more uniform.
Further, the treating agent comprises the following components in percentage by mass: 20-30% of diethyl succinate, 10-20% of dimethyl phosphite, 15-25% of trimethylmethoxysilane and the balance of absolute ethyl alcohol.
Description: the treating agent can improve the fluidity of powder, reduce the agglomeration of powder, improve the combination of a tungsten skeleton and copper when the tungsten skeleton is permeated with copper, reduce the segregation of copper, uniformly distribute copper, reduce pores, improve the density of tungsten-copper alloy and improve the performance of tungsten-copper alloy.
Further, the invention also discloses application of the high-density tungsten powder in 3DP printing.
Further, the 3DP printing method comprises the following steps:
s1, adding the high-density tungsten powder into a powder cylinder of printing equipment;
s2, pushing a layer of high-density tungsten powder into a forming cylinder by a powder paving roller of the printing equipment, paving 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-sectional shape of a layer of a part, wherein the layer of high-density tungsten powder is 0.013-0.1 mm;
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 formed.
Description: the tungsten framework with fine tissues, uniform powder distribution and higher density can be printed by the 3DP printing method.
The beneficial effects of the invention are as follows:
(1) According to the invention, the high-granularity tungsten powder and the low-granularity tungsten powder are mixed, so that the high-density tungsten powder with the density and the fluidity meeting the requirements is obtained, the tungsten skeleton formed after 3DP printing is good in performance, the preparation cost of the high-density tungsten powder is low, and the production cost can be effectively reduced;
(2) The invention adopts the treating agent to modify the mixed powder, thereby improving the powder fluidity, reducing the agglomeration phenomenon of tungsten powder, ensuring that the tungsten skeleton structure is more uniform, improving the combination property of the tungsten skeleton and copper when the tungsten skeleton is permeated with copper, reducing the segregation of copper, ensuring that the copper is uniformly distributed, reducing the pore space, improving the density of tungsten-copper alloy and improving the performance of tungsten-copper alloy.
Drawings
FIG. 1 is a diagram of the alloy phase of CuW80 prepared from the high density tungsten powder of example 1 of the present invention.
Detailed Description
The invention will be described in further detail with reference to the following embodiments to better embody the advantages of the invention.
Example 1
The preparation method of the high-density tungsten powder for 3DP printing comprises the following steps:
s1, preparing powder
According to 10:1.5, weighing 20-150 mu m tungsten powder and 0.5-10 mu m tungsten powder according to the weight ratio, and sieving the 20-150 mu m tungsten powder and the 0.5-10 mu m tungsten powder by using a 180-mesh screen for one time respectively;
s2, mixing powder
Mixing the tungsten powder with the particle size of 20-150 mu m and the tungsten powder with the particle size of 0.5-10 mu m, 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 8 hours, and obtaining mixed powder after ball milling and mixing, wherein the ball material volume of the ball milling and mixing powder is 2/3 of the volume of a ball milling barrel;
s3, drying
And (3) drying the mixed powder at 150 ℃ for 8 hours to obtain high-density tungsten powder, and secondarily sieving the high-density tungsten powder by using a 180-mesh screen, wherein the high-density tungsten powder is stored in a drying oven at the constant temperature of 80 ℃.
Example 2
This example differs from example 1 in that the ball milling time was 7 hours.
Example 3
This example differs from example 1 in that the ball milling time was 9h.
Example 4
This example differs from example 1 in that the mixed powder was dried at 120℃for 7 hours.
Example 5
This example differs from example 1 in that the mixed powder was dried at 180 ℃ for 9 hours.
Example 6
The difference between this example and example 1 is that the weight ratio of 20-150 μm tungsten powder to 0.5-10 μm tungsten powder is 10:1.
example 7
The difference between this example and example 1 is that the weight ratio of 20-150 μm tungsten powder to 0.5-10 μm tungsten powder is 10:2.
example 8
The present embodiment is different from embodiment 1 in that in step S2, the mixed powder is modified after the mixed powder is obtained;
the modification treatment method comprises the following steps: 500g of the mixed powder is placed in a container, the mixed powder is heated to 140 ℃, the treating agent is gradually added into the container in the heating process, the adding amount of the treating agent gradually decreases from 50ml/min along with the temperature rise, the adding amount of the treating agent is reduced by 5ml/min when the temperature rises by 5 ℃ until the mixed powder is stirred after the adding of the treating agent is stopped, and the heating is completed.
The treating agent comprises the following components in percentage by mass: 25% of diethyl succinate, 15% of dimethyl phosphite, 20% of trimethylmethoxysilane and the balance of absolute ethyl alcohol.
Example 9
This example differs from example 8 in that the mixed powder is placed in a container and the mixed powder is heated to 120 ℃.
Example 10
This example differs from example 8 in that the mixed powder is placed in a container and the mixed powder is heated to 160 ℃.
Example 11
This example is different from example 8 in that the addition amount of the treating agent is gradually decreased from 40ml/min with the increase in temperature, and the addition amount of the treating agent is decreased by 4ml/min every 5℃increase in temperature.
Example 12
This example is different from example 8 in that the addition amount of the treating agent is gradually decreased from 60ml/min with the increase in temperature, and the addition amount of the treating agent is decreased by 6ml/min per 5℃increase in temperature.
Example 13
The present embodiment is different from embodiment 8 in that the treating agent comprises the following components in percentage by mass: 20% of diethyl succinate, 10% of dimethyl phosphite, 15% of trimethylmethoxysilane and the balance of absolute ethyl alcohol.
Example 14
The present embodiment is different from embodiment 8 in that the treating agent comprises the following components in percentage by mass: 30% of diethyl succinate, 20% of dimethyl phosphite, 25% of trimethylmethoxysilane and the balance of absolute ethyl alcohol.
Example 15
This example provides the application of the high density tungsten powder prepared in example 14 to 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 a layer of mixed powder into a forming cylinder from a powder cylinder by a powder paving roller of the printing equipment, paving and compacting, and spraying an adhesive on 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 skeleton, wherein the layer thickness is 0.05mm;
and S3, after the adhesive is sprayed, repeating the step S2 to finish printing the next layer of the tungsten skeleton until the tungsten skeleton is formed.
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.
Experimental example
In order to explore the influence of high-density tungsten powder obtained by different parameters on the performance of a finished product, the high-density tungsten powder obtained by each embodiment is printed out to form a tungsten skeleton 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 fig. 1, the CuW80 alloy in the embodiment 1 has compact structure and no obvious structural defect;
meanwhile, performance tests are carried out on the CuW80 alloy obtained in each embodiment so as to explore the influence of the high-density tungsten powder prepared under different technological parameter conditions on the performance of the CuW80 alloy, and the specific exploration is as follows:
1. the influence of ball milling powder mixing time on the performance of CuW80 alloy is explored:
the performance data of the obtained CuW80 alloy are shown in table 1, using examples 1, 2 and 3 as experimental comparisons:
TABLE 1 comparison of CuW80 alloy Performance obtained at different ball milling and 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 density and hardness obtained in example 1 were higher and the performance was better than that obtained in example 2, which means that the ball milling time of example 2 was slightly shorter, whereas the ball milling time of example 1 was more sufficient to allow more uniform powder mixing, whereas the performance of example 1 was not much different from that of example 3, and the ball milling time selected in example 1 was better from the time cost point of view.
2. The influence of the drying parameters on the performance of the CuW80 alloy is explored:
the performance data of the CuW80 alloy obtained by comparing examples 1, 4 and 5 are shown in table 2:
table 2 comparison of CuW80 alloy Performance 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, the CuW80 alloy obtained by the drying parameters selected in example 1 has better properties than those obtained in example 4; example 1 has comparable performance to example 5, and the drying parameters selected in example 1 are better from the time cost standpoint.
3. The effect of powder ratio on CuW80 alloy properties was investigated:
the performance data of the CuW80 alloy obtained by comparing examples 1, 6 and 7 are shown in table 3:
TABLE 3 comparison of CuW80 alloy properties obtained with 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 |
As can be seen from the data in Table 3, the CuW80 alloy obtained by selecting the powder ratio in example 1 had the best performance, and the powder ratio in example 1 was the best.
4. The influence of modification treatment on the performance of CuW80 alloy is explored:
the performance data of the CuW80 alloy obtained by comparing examples 1 and 8 are shown in table 4:
TABLE 4 comparison of the properties of CuW80 alloys obtained by modification
| 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 mixed powder which is not modified, which indicates that the modification treatment can effectively improve the performance of the prepared CuW80 alloy.
5. The influence of the heating temperature in the modification treatment on the performance of the CuW80 alloy is explored:
the performance data of the CuW80 alloy obtained by comparing examples 8, 9 and 10 are shown in table 5:
TABLE 5 comparison of the performance of CuW80 alloys obtained at different heating temperatures during modification
| 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 can be seen from the data in Table 5, the heating temperature selected in example 8 gave the best performance of the CuW80 alloy, and the heating temperature selected in example 8 was the best.
6. The influence of the additive amount of the treating agent on the performance of the CuW80 alloy is explored:
with examples 8, 11 and 12 as experimental comparison and with example 8 as reference, the treating agent was used as comparative example 1 in a one-time addition manner, and the obtained CuW80 alloy performance data are shown in table 6:
table 6 comparison of CuW80 alloy Performance obtained with different additive amounts of the 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 |
As is clear from the data in table 6, the CuW80 alloy obtained by the additive amount of the treatment agent selected in example 8 had the best performance, and the CuW80 alloy obtained by the additive method of the treatment agent selected in example 8 had the better performance, which means that the additive method of the treatment agent of example 8 was better than that of comparative example 1.
7. The effect of the composition of the treating agent on the performance of the CuW80 alloy was investigated:
the performance data of the CuW80 alloy obtained by using examples 8, 13 and 14 as experimental comparison and using example 8 as reference and using absolute ethyl alcohol as the reference to replace diethyl succinate in the treating agent as comparative example 2 are shown in table 7:
TABLE 7 comparison of the performance of 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 obtained from the treatment composition of example 8 has better performance than the CuW80 alloy obtained from the treatment composition of example 8, and the treatment composition selected in example 8 has better performance than the CuW80 alloy obtained in comparative example 2, but the CuW80 alloy obtained in example 8 has improved performance than the CuW80 alloy obtained in comparative example 2, but the CuW80 alloy obtained in comparative example 2 has smaller amplitude, which indicates that the CuW80 alloy performance is improved by the combined action of diethyl succinate in the treatment and other components in the treatment.
Claims (6)
1. The preparation method of the high-density tungsten powder for 3DP printing is characterized by comprising the following steps of:
s1, preparing powder
Weighing 20-150 mu m tungsten powder and 0.5-10 mu m tungsten powder according to a proportion, and sieving the two tungsten powders by using a 180-mesh screen for one time respectively;
s2, mixing powder
Mixing the two tungsten powders, and then carrying out ball milling and powder mixing, wherein the ball material ratio of the ball milling and powder mixing is 1:3, ball milling and powder mixing time is 7-9 h, and mixed powder is obtained after ball milling and powder mixing are completed;
s3, drying
Drying the mixed powder at the drying temperature of 120-180 ℃ for 7-9 hours to obtain high-density tungsten powder after the drying is completed;
in the step S2, modifying the mixed powder after the mixed powder is obtained;
the modification treatment method comprises the following steps: placing 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, gradually reducing the adding amount of the treating agent from 40-60 ml/min along with the temperature rise, reducing the adding amount of the treating agent by 4-6 ml/min when the temperature rises by 5 ℃ until the adding of the treating agent is stopped, and stirring the mixed powder until the heating is completed;
the treating agent comprises the following components in percentage by mass: 20-30% of diethyl succinate, 10-20% of dimethyl phosphite, 15-25% of trimethylmethoxysilane and the balance of absolute ethyl alcohol.
2. The method for preparing high-density tungsten powder for 3DP printing according to claim 1, wherein in step S1, the weight ratio of 20-150 μm tungsten powder to 0.5-10 μm tungsten powder is 10: 1-2.
3. The method for preparing high-density tungsten powder for 3DP printing according to claim 1, wherein in step S2, the ball volume of the ball milling mixed powder is less than or equal to 2/3 of the ball milling barrel capacity.
4. The method for producing a high-density tungsten powder for 3DP printing according to claim 3, wherein in step S3, the high-density tungsten powder is secondarily sieved using a 180-mesh sieve.
5. The method for preparing the high-density tungsten powder for 3DP printing according to claim 1, wherein the high-density tungsten powder is stored at a constant temperature in a drying oven at 80 ℃.
6. The application of the high-density tungsten powder for 3DP printing prepared by the method according to any one of claims 1-5, wherein the high-density tungsten powder is applied to 3DP printing, and the 3DP printing method comprises the following steps:
s1, adding the high-density tungsten powder into a powder cylinder of printing equipment;
s2, pushing a layer of high-density tungsten powder into a forming cylinder by a powder paving roller of the printing equipment, paving 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 a part, wherein the layer thickness is 0.013-0.1 mm;
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 formed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211298874.0A CN115383123B (en) | 2022-10-24 | 2022-10-24 | Preparation method and application of high-density tungsten powder for 3DP printing |
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