CN117604307A - Rare earth tungsten rod and preparation method thereof - Google Patents
Rare earth tungsten rod and preparation method thereof Download PDFInfo
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- CN117604307A CN117604307A CN202410098979.4A CN202410098979A CN117604307A CN 117604307 A CN117604307 A CN 117604307A CN 202410098979 A CN202410098979 A CN 202410098979A CN 117604307 A CN117604307 A CN 117604307A
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- tungsten rod
- tungsten
- earth oxide
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 118
- 239000010937 tungsten Substances 0.000 title claims abstract description 118
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 79
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 59
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 26
- 238000004321 preservation Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 8
- 238000005056 compaction Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 238000009694 cold isostatic pressing Methods 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000009827 uniform distribution Methods 0.000 abstract description 3
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 229910003440 dysprosium oxide Inorganic materials 0.000 description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- DYIZHKNUQPHNJY-UHFFFAOYSA-N oxorhenium Chemical compound [Re]=O DYIZHKNUQPHNJY-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910003449 rhenium oxide Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Abstract
The invention belongs to the technical field of powder metallurgy, and particularly relates to a rare earth tungsten rod and a preparation method thereof, wherein rare earth oxide is pretreated in advance, the strength of a pressed tungsten rod blank can be improved by controlling the moisture content of the rare earth oxide, the tungsten rod blank is not easy to damage in the process of carrying and sintering, and the tungsten rod blank is well molded; the rare earth oxide powder is prevented from dead angle in the mixer to be mixed unevenly, so that the uniform distribution of the rare earth oxide in the tungsten powder can be improved, and the rare earth oxide of the rare earth tungsten rod is doped evenly after implementation; the density of the rare earth tungsten rod prepared by the invention is 17.8-18.8 g/cm 3 The diameter is 20-22 mm,the number of crystal grains of the radial section of the tungsten rod is 3000-3600, the rare earth element content of different areas is extremely less than 0.05%, and the porosity is less than 5%.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a rare earth tungsten rod and a preparation method thereof.
Background
Along with the progress of the photovoltaic power generation technology, the demands for thinning and increasing the high-strength tungsten wires used for linear cutting of photovoltaic silicon wafers are increased greatly, and the clients control the high-strength tungsten wire breakage rate and the comprehensive slicing yield and bring higher demands for the performance of thin-diameter high-strength tungsten wires. High strength tungsten wires are required to have low breakage rate and Gao Qiege force. The tungsten filament prepared by the prior art has the defects of high breaking rate, low tensile strength and large loss, and can be made up by doping rare earth oxide. The tensile strength of the rare earth tungsten wire is directly related to the uniformity of rare earth elements in a tungsten matrix and the strength of a green compact, the quality of the tungsten wire is directly determined by the quality of a rare earth tungsten rod serving as a raw material of the rare earth tungsten wire, and rare earth oxides for manufacturing the rare earth tungsten rod are characterized by being easy to be subjected to moisture agglomeration, large in specific gravity difference of tungsten powder and the like, and the phenomena of uneven occurrence of rare earth and tungsten mixture, difficult pressing due to moisture pulverization, low strength of a pressed compact and the like easily occur in the process of manufacturing the rare earth tungsten rod, so that the density, the strength and the uniformity of a tungsten rod blank after subsequent pressing molding are greatly disturbed. After being pressed into tungsten bar blanks, the tungsten bar blanks are easy to be pulverized, broken, unqualified in uniformity of rare earth oxide and the like, the sintering cannot be continued, and the sintered tungsten bars are high in porosity and cannot be produced.
Disclosure of Invention
In order to solve the problems in the prior art, the main purpose of the invention is to provide a rare earth tungsten rod and a preparation method thereof.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided:
a preparation method of a rare earth tungsten rod comprises the following steps:
s1, pouring rare earth oxide powder into a container, and placing the container in a heat-preservation and moisture-preservation device for a period of time in an open mode to prepare the water-containing rare earth oxide;
s2, mixing the water-containing rare earth oxide and tungsten powder according to the weight ratio of (7.8-9.5) to obtain a mixture, and compacting the mixture to obtain a compacted mixture; when mixing materials, the materials are fed by adopting an equal-part adding method, the water-containing rare earth oxide and tungsten powder are respectively and averagely divided into 5-10 equal parts, and the materials are mixed alternately;
s3, filling the compaction mixture into a die for cold isostatic pressing to prepare a tungsten rod green body;
s4, placing the tungsten rod green compact into a high-temperature sintering furnace for jack sintering, wherein the atmosphere in the furnace is hydrogen, and the atmosphere pressure is 1.2-4.5 KPa.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S1, the thickness of the rare earth oxide powder in the container is controlled to be 12-15 mm, and the container is placed in a heat preservation and moisture preservation device for 24-32 h in an open mode.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S1, the temperature of the heat preservation and moisture preservation device is 40-45 ℃ and the humidity is 75-90%.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S1, the water content of the water-containing rare earth oxide is 15-20wt%.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S1, the rare earth oxide is at least one of lanthanum oxide, rhenium oxide, yttrium oxide, cerium oxide, and dysprosium oxide.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S2, the mixing mode is as follows: firstly adding a first equal part of tungsten powder, then adding a first equal part of water-containing rare earth oxide, and mixing for 3-5 min; then adding a second equal part of tungsten powder, then adding a second equal part of water-containing rare earth oxide, mixing for 3-5 min, and circulating until the mixing is completed.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S2, the temperature of the mixer is 120-180 ℃.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S2, the density of the tap mixture is 7.8-8.5 g/cm 3 。
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S3, the pressing pressure is 150-250 MPa; the strength of the tungsten rod green body is more than 3.0MPa.
As a preferable scheme of the preparation method of the rare earth tungsten rod, the invention comprises the following steps: in the step S4, a sectional sintering process is adopted for sintering:
the sintering temperature in the first stage is 1800-2000 ℃, and the temperature is kept for 40-60 min;
the sintering temperature of the second stage is 2100-2180 ℃, and the temperature is kept for 130-160 min;
the sintering temperature in the third stage is 2400-2520 ℃, and the temperature is kept for 120-180 min.
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
the rare earth tungsten rod is prepared by adopting the preparation method of the rare earth tungsten rod.
As a preferable scheme of the rare earth tungsten rod, the invention comprises the following steps: the density of the rare earth tungsten rod is 17.8-18.8 g/cm 3 The diameter is 20-22 mm, the number of crystal grains of the radial section of the tungsten rod is 3000-3600, the rare earth element content of different areas is extremely less than 0.05%, and the porosity is less than 5%.
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
the application of the rare earth tungsten rod in preparing rare earth tungsten wires.
The beneficial effects of the invention are as follows:
the invention provides a rare earth tungsten rod and a preparation method thereof, wherein rare earth oxide is pretreated in advance, the strength of a pressed tungsten rod blank can be improved by controlling the moisture content of the rare earth oxide, the tungsten rod blank is not easy to damage in the process of carrying and sintering, and the tungsten rod is well molded; the rare earth oxide powder is prevented from dead angle in the mixer to be mixed unevenly, so that the uniform distribution of the rare earth oxide in the tungsten powder can be improved, and the rare earth oxide of the rare earth tungsten rod is doped evenly after implementation; the preparation of the inventionThe density of the rare earth tungsten rod is 17.8-18.8 g/cm 3 The diameter is 20-22 mm, the number of crystal grains of the radial section of the tungsten rod is 3000-3600, the rare earth element content of different areas is extremely less than 0.05%, and the porosity is less than 5%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
Fig. 1 is an SEM image of a rare earth tungsten rod prepared in example 1 of the present invention.
Fig. 2 is an SEM image of the rare earth tungsten rod prepared in comparative example 5 of the present invention.
Detailed Description
The following description will be made clearly and fully with reference to the technical solutions in the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a rare earth tungsten rod and a preparation method thereof, and the rare earth tungsten rod has the following advantages:
(1) The strength of the pressed tungsten rod blank can be improved by controlling the moisture content of the rare earth oxide, the tungsten rod blank is not easy to damage in the process of carrying and sintering, and the tungsten rod blank is well molded;
(2) The rare earth content of the rare earth tungsten mixed powder prepared by equal parts of alternate mixing is uniformly distributed;
(3) The mixed powder prepared by the invention is smooth in powder filling in the pressing process, and the surface of the green body is smooth and has no bulge;
(4) The green body prepared by the invention has no phenomena of pulverization, fracture and the like when being placed in air, and has high green body strength.
According to one aspect of the invention, the invention provides the following technical scheme:
a preparation method of a rare earth tungsten rod comprises the following steps:
s1, pouring rare earth oxide powder into a container, and placing the container in a heat-preservation and moisture-preservation device for a period of time in an open mode to prepare the water-containing rare earth oxide;
s2, mixing the water-containing rare earth oxide and tungsten powder according to the weight ratio of (7.8-9.5) to obtain a mixture, and compacting the mixture to obtain a compacted mixture; when mixing materials, the materials are fed by adopting an equal-part adding method, the water-containing rare earth oxide and tungsten powder are respectively and averagely divided into 5-10 equal parts, and the materials are mixed alternately;
s3, filling the compaction mixture into a die for cold isostatic pressing to prepare a tungsten rod green body;
s4, placing the tungsten rod green compact into a high-temperature sintering furnace for jack sintering, wherein the atmosphere in the furnace is hydrogen, and the atmosphere pressure is 1.2-4.5 KPa.
Preferably, in the step S1, the thickness of the rare earth oxide powder in the container is controlled to be 12-15 mm, and the container is placed in a heat-preservation and moisture-preservation device for 24-32 hours in an open mode; the temperature of the heat preservation and moisture preservation device is 40-45 ℃ and the humidity is 75-90%; the water content of the hydrous rare earth oxide is 15-20wt%; the rare earth oxide is at least one of lanthanum oxide, rhenium oxide, yttrium oxide, cerium oxide and dysprosium oxide.
Preferably, in the step S2, the mixing manner is as follows: firstly adding a first equal part of tungsten powder, then adding a first equal part of water-containing rare earth oxide, and mixing for 3-5 min; then adding a second equal part of tungsten powder, then adding a second equal part of water-containing rare earth oxide, mixing for 3-5 min, and circulating until the mixing is completed; the temperature of the mixer is 120-180 ℃; the density of the compaction mixture is 7.8-8.5 g/cm 3 。
Preferably, in the step S3, the pressing pressure is 150 to 250MPa; the strength of the tungsten rod green body is more than 3.0MPa.
Further preferably, in the step S4, the rare earth tungsten rod prepared by the three-stage sintering process has high density and high crystallization degree; the sintering adopts a sectional sintering process:
the sintering temperature in the first stage is 1800-2000 ℃, and the temperature is kept for 40-60 min;
the sintering temperature of the second stage is 2100-2180 ℃, and the temperature is kept for 130-160 min;
the sintering temperature in the third stage is 2400-2520 ℃, and the temperature is kept for 120-180 min.
In order to provide another aspect of the invention, the invention provides the following technical scheme:
the rare earth tungsten rod is prepared by adopting the preparation method of the rare earth tungsten rod.
Preferably, the density of the rare earth tungsten rod is 17.8-18.8 g/cm 3 The diameter is 20-22 mm, the number of crystal grains of the radial section of the tungsten rod is 3000-3600, the rare earth element content of different areas is extremely less than 0.05%, and the porosity is less than 5%. The radial section of the tungsten rod refers to a section perpendicular to the axial direction of the tungsten rod, the number of grains in a unit area is obtained by counting the number of grains in a certain area, and the number of grains in the radial section can be obtained according to the area of the radial section.
The technical scheme of the invention is further described below by combining specific embodiments.
Example 1
A preparation method of a rare earth tungsten rod comprises the following steps:
s1, pouring rare earth oxide powder into a container, and placing the container in a heat-preservation and moisture-preservation device for a period of time in an open mode to prepare the water-containing rare earth oxide; controlling the thickness of the rare earth oxide powder in the container to be 12mm, and placing the container in a heat-preservation and moisture-preservation device for 24 hours in an open mode; the temperature of the heat preservation and moisture preservation device is 40 ℃ and the humidity is 90%. The water content of the water-containing rare earth oxide is 17wt%; the rare earth oxide is lanthanum oxide.
S2, mixing 117kg of water-containing rare earth oxide with 920kg of tungsten powder to obtain a mixture, and compacting the mixture to obtain a compacted mixture; when mixing materials, feeding by adopting an equal-part adding method, respectively equally dividing the water-containing rare earth oxide and tungsten powder into 5 equal parts, and alternately mixing materials; the mixing mode is as follows: firstly adding 184kg of tungsten powder in the first part, then adding 23.4kg of water-containing rare earth oxide in the first part, and mixing for 5min; then add the first184kg of tungsten powder in two equal parts, adding 23.4kg of aqueous rare earth oxide in the second equal part, mixing for 5min, and circulating until mixing is completed; the temperature of the mixer is 120 ℃; the density of the tap mixture was 8.3g/cm 3 。
S3, filling the compaction mixture into a die for cold isostatic pressing to prepare a tungsten rod green body; the pressing pressure is 150MPa; the green strength of the tungsten rod was 3.5MPa.
S4, placing the tungsten rod green compact into a high-temperature sintering furnace for jack sintering, wherein the atmosphere in the furnace is hydrogen, and the atmosphere pressure is 2.45KPa; the sintering adopts a sectional sintering process: the sintering temperature in the first stage is 1900 ℃, and the temperature is kept for 50min; the sintering temperature in the second stage is 2140 ℃, and the temperature is kept for 145min; the sintering temperature in the third stage is 2480 ℃, and the temperature is kept for 150min.
The SEM image of the rare earth tungsten rod prepared in this example is as shown in FIG. 1, and has a diameter of 20.5mm and a density of 18.2g/cm 3 The number of grains of the radial section of the tungsten rod is 3452, the rare earth element content of 5 different areas is 0.041%, and the porosity is 4.5%.
Example 2
The difference from example 1 is that the thickness of the rare earth oxide powder in the container is controlled to be 15mm, and the container is placed in a heat-preservation and moisture-preservation device for 32 hours in an open manner; the temperature of the heat preservation and moisture preservation device is 45 ℃ and the humidity is 90%. The water content of the hydrous rare earth oxide is 19wt%;
the strength of the tungsten rod green compact prepared in the embodiment is 3.4MPa, and the density of the rare earth tungsten rod is 18.02g/cm 3 The number of grains of the radial section of the tungsten rod is 3313, the rare earth element content of 5 different areas is 0.044% and the porosity is 4.7%.
Example 3
The difference from example 1 is that the aqueous rare earth oxide and tungsten powder are divided into 10 equal parts on average, respectively.
The density of the tapped mix of this example was 8.15g/cm 3 The strength of the prepared tungsten rod green compact is 3.55MPa, and the density of the rare earth tungsten rod is 18.40g/cm 3 The number of crystal grains of the radial section of the tungsten rod is 3266, the rare earth element content of 5 different areas is extremely poor and is 0.039%, and the porosity is 4.3%.
Comparative example 1
The difference from example 1 is that step S1 is not performed.
The tungsten rod green compact prepared in this comparative example has poor strength and low molding rate, and the sintering of the tungsten rod cannot be performed.
Comparative example 2
The difference from example 1 is that the aqueous rare earth oxide and tungsten powder are added and mixed at once.
The strength of the tungsten rod green compact prepared in this comparative example was 3.25MPa, and the density of the rare earth tungsten rod was 18.10g/cm 3 The number of crystal grains of the radial section of the tungsten rod is 2675, the rare earth element content of 5 different areas is extremely poor and is 0.14%, and the porosity is 5.9%.
Comparative example 3
The difference from example 1 is that the humidity of the heat and moisture retaining device is 40%.
The water content of the aqueous rare earth oxide of this comparative example was 9wt%; the strength of the prepared tungsten rod green body is 2.25MPa, and the density of the rare earth tungsten rod is 16.40g/cm 3 The number of crystal grains of the radial section of the tungsten rod is 2451, the rare earth element content of 5 different areas is 0.042%, and the porosity is 7.8%.
Comparative example 4
The difference from example 1 is that 220kg of hydrous lanthanum oxide and 920kg of tungsten powder are used in step S2.
The strength of the tungsten rod green compact prepared in this comparative example was 3.21MPa, and the density of the rare earth tungsten rod was 16.80g/cm 3 The number of grains of the radial section of the tungsten rod is 2382, the rare earth element content of 5 different areas is 0.094% extremely, and the porosity is 6.3%.
Comparative example 5
The difference from example 1 is that the pressing pressure in step S3 is 100MPa.
The strength of the green tungsten rod produced in this comparative example was 2.23MPa, and the density of the rare earth tungsten rod (as shown in FIG. 2) was 14.84g/cm 3 The number of grains of the radial section of the tungsten rod is 2863, the rare earth element content of 5 different areas is 0.041%, and the porosity is 8.2%.
From the above embodimentThe example and the comparative example show that the rare earth oxide is pretreated in advance, the strength of the pressed tungsten rod blank can be improved by controlling the moisture content of the rare earth oxide, the tungsten rod blank is not easy to be damaged in the process of carrying and sintering, and the tungsten rod blank is well molded; the rare earth oxide powder is prevented from dead angle in the mixer to be mixed unevenly, so that the uniform distribution of the rare earth oxide in the tungsten powder can be improved, and the rare earth oxide of the rare earth tungsten rod is doped evenly after implementation; the density of the rare earth tungsten rod prepared by the invention is 17.8-18.8 g/cm 3 The diameter is 20-22 mm, the number of crystal grains of the radial section of the tungsten rod is 3000-3600, the rare earth element content of different areas is extremely less than 0.05%, and the porosity is less than 5%.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. The preparation method of the rare earth tungsten rod is characterized by comprising the following steps:
s1, pouring rare earth oxide powder into a container, and placing the container in a heat-preservation and moisture-preservation device for a period of time in an open mode to prepare the water-containing rare earth oxide;
s2, mixing the water-containing rare earth oxide and tungsten powder according to the weight ratio of (7.8-9.5) to obtain a mixture, and compacting the mixture to obtain a compacted mixture; when mixing materials, the materials are fed by adopting an equal-part adding method, the water-containing rare earth oxide and tungsten powder are respectively and averagely divided into 5-10 equal parts, and the materials are mixed alternately;
s3, filling the compaction mixture into a die for cold isostatic pressing to prepare a tungsten rod green body;
s4, placing the tungsten rod green compact into a high-temperature sintering furnace for jack sintering, wherein the atmosphere in the furnace is hydrogen, and the atmosphere pressure is 1.2-4.5 KPa.
2. The method for preparing a rare earth tungsten rod according to claim 1, wherein in the step S1, the thickness of the rare earth oxide powder in the container is controlled to be 12-15 mm, and the container is placed in the heat-preserving and moisture-preserving device for 24-32 h.
3. The method for preparing a rare earth tungsten rod according to claim 1, wherein in the step S1, the temperature of the heat-preserving and moisture-preserving device is 40-45 ℃ and the humidity is 75-90%.
4. The method for producing a rare earth tungsten rod according to claim 1, wherein the water content of the hydrous rare earth oxide in step S1 is 15 to 20wt%.
5. The method for preparing a rare earth tungsten rod according to claim 1, wherein in the step S2, the mixing mode is as follows: firstly adding a first equal part of tungsten powder, then adding a first equal part of water-containing rare earth oxide, and mixing for 3-5 min; then adding a second equal part of tungsten powder, then adding a second equal part of water-containing rare earth oxide, mixing for 3-5 min, and circulating until the mixing is completed.
6. The method of producing rare earth tungsten rod according to claim 1, wherein in step S2, the density of the tap mixture is 7.8 to 8.5g/cm 3 。
7. The method for preparing a rare earth tungsten rod according to claim 1, wherein in the step S3, the pressing pressure is 150 to 250MPa; the strength of the tungsten rod green body is more than 3.0MPa.
8. A rare earth tungsten rod, characterized in that it is prepared by the method of any one of claims 1 to 7.
9. A rare earth tungsten rod according to claim 8, wherein the density of the rare earth tungsten rod is 17.8-18.8 g/cm 3 The diameter is 20-22 mm, the number of crystal grains of the radial section of the tungsten rod is 3000-3600, the rare earth element content of different areas is extremely less than 0.05%, and the porosity is less than 5%.
10. Use of a rare earth tungsten rod according to any one of claims 8-9 in the preparation of a rare earth tungsten filament.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5284614A (en) * | 1992-06-01 | 1994-02-08 | General Electric Company | Method of forming fine dispersion of ceria in tungsten |
| CN103225032A (en) * | 2013-05-17 | 2013-07-31 | 中国兵器工业第五九研究所 | Rare-earth-oxide-doped W-Cu composite material and preparation method thereof |
| CN107009093A (en) * | 2017-01-12 | 2017-08-04 | 厦门虹鹭钨钼工业有限公司 | A kind of preparation method of rear-earth-doped tungsten pipe |
| CN109226748A (en) * | 2018-08-15 | 2019-01-18 | 赣州虹飞钨钼材料有限公司 | A kind of preparation method of composite tungsten electrode material |
| CN109834285A (en) * | 2019-03-08 | 2019-06-04 | 北京矿冶科技集团有限公司 | A kind of method of accurate control tungsten alloy powder doping component content |
| CN110256042A (en) * | 2019-06-26 | 2019-09-20 | 福建省德化县邦威陶瓷有限公司 | The anti-folding heatproof and shockproof ceramic blank of one kind, anti-folding heatproof and shockproof ceramic product and preparation method thereof |
| CN110549032A (en) * | 2019-08-21 | 2019-12-10 | 河南机电职业学院 | copper-based brazing filler metal with gradient thermal expansion coefficient and preparation method thereof |
| CN112476820A (en) * | 2020-10-30 | 2021-03-12 | 罗小怀 | Compounding agent adding system for mixing raw rubber |
| KR20210056548A (en) * | 2019-11-11 | 2021-05-20 | 한국생산기술연구원 | Manufacturing method of Ta-Cu alloy and Ta-Cu alloy using thereof |
-
2024
- 2024-01-24 CN CN202410098979.4A patent/CN117604307B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5284614A (en) * | 1992-06-01 | 1994-02-08 | General Electric Company | Method of forming fine dispersion of ceria in tungsten |
| CN103225032A (en) * | 2013-05-17 | 2013-07-31 | 中国兵器工业第五九研究所 | Rare-earth-oxide-doped W-Cu composite material and preparation method thereof |
| CN107009093A (en) * | 2017-01-12 | 2017-08-04 | 厦门虹鹭钨钼工业有限公司 | A kind of preparation method of rear-earth-doped tungsten pipe |
| CN109226748A (en) * | 2018-08-15 | 2019-01-18 | 赣州虹飞钨钼材料有限公司 | A kind of preparation method of composite tungsten electrode material |
| CN109834285A (en) * | 2019-03-08 | 2019-06-04 | 北京矿冶科技集团有限公司 | A kind of method of accurate control tungsten alloy powder doping component content |
| CN110256042A (en) * | 2019-06-26 | 2019-09-20 | 福建省德化县邦威陶瓷有限公司 | The anti-folding heatproof and shockproof ceramic blank of one kind, anti-folding heatproof and shockproof ceramic product and preparation method thereof |
| CN110549032A (en) * | 2019-08-21 | 2019-12-10 | 河南机电职业学院 | copper-based brazing filler metal with gradient thermal expansion coefficient and preparation method thereof |
| KR20210056548A (en) * | 2019-11-11 | 2021-05-20 | 한국생산기술연구원 | Manufacturing method of Ta-Cu alloy and Ta-Cu alloy using thereof |
| CN112476820A (en) * | 2020-10-30 | 2021-03-12 | 罗小怀 | Compounding agent adding system for mixing raw rubber |
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