CN107190195A - A kind of W-REO alloys crucible and its manufacture method - Google Patents
A kind of W-REO alloys crucible and its manufacture method Download PDFInfo
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- CN107190195A CN107190195A CN201710323888.6A CN201710323888A CN107190195A CN 107190195 A CN107190195 A CN 107190195A CN 201710323888 A CN201710323888 A CN 201710323888A CN 107190195 A CN107190195 A CN 107190195A
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- crucible
- reo alloys
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
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- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of W-REO alloys crucible and its manufacture method, 1.3%~2.5% lanthana and 97.5%~98.7% tungsten is included by hundred parts of ratios of quality.A kind of manufacture method of W-REO alloys crucible, comprises the following steps：Step (1)：Prepare W-REO alloys, step (2)：Prepare W-REO alloys crucible blank, step (3)：Prepare finished product.Mechanical behavior under high temperature of the present invention is excellent, and creep strength is high, and tensile strength and good toughness, durability are strong, reduces use cost.
Description
Technical field
The present invention relates to a kind of crucible, and in particular to a kind of W-REO alloys crucible and its manufacture method.
Background technology
Tungsten crucible has that excellent resistance to elevated temperatures and electric conductivity are high, and thermal coefficient of expansion is low, is widely used in LED wafer
Production.Tungsten crucible of the prior art is usually that pure tungsten is made, and pure tungsten easily aoxidizes and generates oxygen at high operating temperatures
Compound, is enriched with crystal boundary and reduces grain-boundary strength, reduces resistance to elevated temperatures, creep strength and tensile strength, causes toughness
Difference, reduces the service life of tungsten crucible.Therefore, in order to avoid shortcoming present in prior art, it is necessary to prior art
Make improvement.
The content of the invention
It is an object of the invention to overcome shortcoming and deficiency of the prior art there is provided a kind of durable performance it is high, using into
This low W-REO alloys crucible.
It is another object of the present invention to provide a kind of manufacture method of W-REO alloys crucible.
The present invention is realized by following technical scheme：
A kind of W-REO alloys crucible, by hundred parts of ratios of quality include 1.3%~2.5% lanthana and 97.5%~
98.7% tungsten.
Further, the content of the lanthana is 1.5%~2.2%.
Further, the content of the lanthana is 2%.
A kind of manufacture method of W-REO alloys crucible, comprises the following steps：
Step (1)：Prepare W-REO alloys, by hundred parts of ratios of quality weigh 94.6%~96.8% ammonium paratungstate and
Ammonium paratungstate, is added reactor and is heated to 70 DEG C~90 DEG C, then added in a kettle. by 3.2%~5.4% rare earth
Rare earth, continues to heat and stir until becoming dry composite powder, then high temperature reduction obtains rare earth under the protection of hydrogen
Tungsten alloy powder, the W-REO alloys powder contains 1.3%~2.5% lanthana；
Step (2)：W-REO alloys crucible blank is prepared, W-REO alloys powder made from step (1) is loaded rubber moulding
In, be reloaded into isostatic pressing machine enter horizontal high voltage compacting obtain W-REO alloys crucible blank material；To W-REO alloys crucible blank
Material carries out pre-sintering, and pre-sintering temperature is 1100 DEG C~1250 DEG C, and the pre-sintered time is 30min~45min, and Rare-Earth Tungsten is made and closes
The smart blank of golden crucible；
Step (3)：Finished product is prepared, height is carried out to the smart blank of W-REO alloys crucible of step (2) in intermediate frequency furnace
Temperature sintering, high temperature sintering temperature is 2350 DEG C~2420 DEG C, and the high temperature sintering time is 12h, be made W-REO alloys crucible half into
Product；Surface smoothness is carried out to W-REO alloys crucible semi-finished product and precision working process obtains W-REO alloys crucible finished product.
Further, the step (1) rare earth contains more than 99% lanthanum nitrate.
Further, step (1) the W-REO alloys powder contains 2% lanthana.
Further, the high temperature reduction temperature in the step (1) is 900 DEG C.
Further, the step (1) weighs 95% ammonium paratungstate and 5% rare earth.
Further, step (2) pre-sintering temperature is 1200 DEG C, and the pre-sintered time is 40min.
Further, step (3) the high temperature sintering temperature is 2400 DEG C.
Relative to prior art, the present invention produces tungsten alloy by the lanthanum element in rare earth and tungsten reaction, due to tungsten
Lanthana energy even dispersion distribution in alloy, has refined the crystal grain of material, can significantly improve the mechanical property of tungsten alloy, so that
The plasticity and cracking resistance for strengthening tungsten alloy become tensile strength.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
A kind of W-REO alloys crucible, by hundred parts of ratios of quality include 1.3%~2.5% lanthana and 97.5%~
98.7% tungsten.The content of lanthana is 1.5%~2.2% preferable.As a kind of embodiment, the content of lanthana is
2%.
A kind of manufacture method of W-REO alloys crucible, comprises the following steps：
Step (1)：Prepare W-REO alloys, by hundred parts of ratios of quality weigh 94.6%~96.8% ammonium paratungstate and
Ammonium paratungstate, is added reactor and is heated to 70 DEG C~90 DEG C, then added in a kettle. by 3.2%~5.4% rare earth
Rare earth, continues to heat and stir until becoming dry composite powder, then high temperature reduction obtains rare earth under the protection of hydrogen
Tungsten alloy powder, W-REO alloys powder contains 1.3%~2.5% lanthana；As a kind of embodiment, weigh
95% ammonium paratungstate and 5% rare earth, rare earth contain more than 99% lanthanum nitrate, and W-REO alloys powder contains 2% oxygen
Change lanthanum, high temperature reduction temperature is 900 DEG C.
Step (2)：W-REO alloys crucible blank is prepared, W-REO alloys powder made from step (1) is loaded rubber moulding
In, be reloaded into isostatic pressing machine enter horizontal high voltage compacting obtain W-REO alloys crucible blank material；To W-REO alloys crucible blank
Material carries out pre-sintering, and pre-sintering temperature is 1100 DEG C~1250 DEG C, and the pre-sintered time is 30min~45min, and Rare-Earth Tungsten is made and closes
The smart blank of golden crucible；Pre-sintering temperature is 1200 DEG C, and the pre-sintered time is 40min.
Step (3)：Finished product is prepared, height is carried out to the smart blank of W-REO alloys crucible of step (2) in intermediate frequency furnace
Temperature sintering, high temperature sintering temperature is 2350 DEG C~2420 DEG C, and the high temperature sintering time is 12h, be made W-REO alloys crucible half into
Product；Surface smoothness is carried out to W-REO alloys crucible semi-finished product and precision working process obtains W-REO alloys crucible finished product.
High temperature sintering temperature is 2400 DEG C.
The W-REO alloys crucible of the present invention can hinder the growth of crystal grain in applied at elevated temperature, enhance the antioxygen of tungsten crucible
Change, resistance to elevated temperatures, so as to improve tungsten crucible tensile strength, improve plasticity and toughness, comprehensive mechanical property is improved,
Durable performance improves more than 30%, reduces use cost.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (10)
1. a kind of W-REO alloys crucible, it is characterised in that：By hundred parts of ratios of quality include 1.3%~2.5% lanthana and
97.5%~98.7% tungsten.
2. W-REO alloys crucible according to claim 1, it is characterised in that：The content of the lanthana be 1.5%~
2.2%.
3. W-REO alloys crucible according to claim 1, it is characterised in that：The content of the lanthana is 2%.
4. a kind of manufacture method of W-REO alloys crucible, it is characterised in that：Comprise the following steps：
Step (1)：Prepare W-REO alloys, by hundred parts of ratios of quality weigh 94.6%~96.8% ammonium paratungstate and 3.2%~
Ammonium paratungstate, is added reactor and is heated to 70 DEG C~90 DEG C, rare earth is then added in a kettle. by 5.4% rare earth, after
Continuous to heat and stir until becoming dry composite powder, then high temperature reduction obtains W-REO alloys powder under the protection of hydrogen
End, the W-REO alloys powder contains 1.3%~2.5% lanthana；
Step (2)：W-REO alloys crucible blank is prepared, W-REO alloys powder made from step (1) is fitted into rubber moulding, then
Enter horizontal high voltage compacting in loading isostatic pressing machine and obtain W-REO alloys crucible blank material；W-REO alloys crucible blank material is carried out
Pre-sintering, pre-sintering temperature is 1100 DEG C~1250 DEG C, and the pre-sintered time is 30min~45min, and W-REO alloys crucible is made
Smart blank；
Step (3)：Finished product is prepared, high temperature burning is carried out to the smart blank of W-REO alloys crucible of step (2) in intermediate frequency furnace
Knot, high temperature sintering temperature is 2350 DEG C~2420 DEG C, and the high temperature sintering time is 12h, and W-REO alloys crucible semi-finished product are made；It is right
W-REO alloys crucible semi-finished product carry out surface smoothness and precision working process obtains W-REO alloys crucible finished product.
5. the manufacture method of W-REO alloys crucible according to claim 4, it is characterised in that：The step (1) is described
Rare earth contains more than 99% lanthanum nitrate.
6. the manufacture method of W-REO alloys crucible according to claim 4, it is characterised in that：The step (1) is described
W-REO alloys powder contains 2% lanthana.
7. the manufacture method of W-REO alloys crucible according to claim 4, it is characterised in that：In the step (1)
High temperature reduction temperature is 900 DEG C.
8. the manufacture method of W-REO alloys crucible according to claim 4, it is characterised in that：The step (1) weighs
95% ammonium paratungstate and 5% rare earth.
9. the manufacture method of W-REO alloys crucible according to claim 4, it is characterised in that：Step (2) pre-burning
Junction temperature is 1200 DEG C, and the pre-sintered time is 40min.
10. the manufacture method of W-REO alloys crucible according to claim 4, it is characterised in that：Step (3) high temperature
Sintering temperature is 2400 DEG C.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710323888.6A CN107190195A (en) | 2017-05-04 | 2017-05-04 | A kind of W-REO alloys crucible and its manufacture method |
| PCT/CN2017/112281 WO2018201702A1 (en) | 2017-05-04 | 2017-11-22 | Rare earth tungsten alloy crucible and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710323888.6A CN107190195A (en) | 2017-05-04 | 2017-05-04 | A kind of W-REO alloys crucible and its manufacture method |
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| Publication Number | Publication Date |
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| CN107190195A true CN107190195A (en) | 2017-09-22 |
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ID=59872674
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710323888.6A Pending CN107190195A (en) | 2017-05-04 | 2017-05-04 | A kind of W-REO alloys crucible and its manufacture method |
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| WO (1) | WO2018201702A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018201702A1 (en) * | 2017-05-04 | 2018-11-08 | 鹤山市沃得钨钼实业有限公司 | Rare earth tungsten alloy crucible and manufacturing method thereof |
| CN108772558A (en) * | 2018-06-15 | 2018-11-09 | 赣州有色冶金研究所 | A kind of compound tungsten crucible of multielement rare earth and its preparation method and application |
| CN111960648A (en) * | 2020-06-24 | 2020-11-20 | 江苏太平洋石英股份有限公司 | Multifunctional electric melting furnace |
| CN113913665A (en) * | 2021-09-30 | 2022-01-11 | 中国科学院重庆绿色智能技术研究院 | Nano lanthanum oxide reinforced tungsten-based composite material and preparation method thereof |
| CN115029597A (en) * | 2022-06-02 | 2022-09-09 | 安泰天龙钨钼科技有限公司 | Method for preparing tungsten and tungsten alloy sheets |
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- 2017-11-22 WO PCT/CN2017/112281 patent/WO2018201702A1/en active Application Filing
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| CN108772558A (en) * | 2018-06-15 | 2018-11-09 | 赣州有色冶金研究所 | A kind of compound tungsten crucible of multielement rare earth and its preparation method and application |
| CN111960648A (en) * | 2020-06-24 | 2020-11-20 | 江苏太平洋石英股份有限公司 | Multifunctional electric melting furnace |
| CN113913665A (en) * | 2021-09-30 | 2022-01-11 | 中国科学院重庆绿色智能技术研究院 | Nano lanthanum oxide reinforced tungsten-based composite material and preparation method thereof |
| CN115029597A (en) * | 2022-06-02 | 2022-09-09 | 安泰天龙钨钼科技有限公司 | Method for preparing tungsten and tungsten alloy sheets |
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| WO2018201702A1 (en) | 2018-11-08 |
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