CN103114260A - Cryogenic treatment method of tungsten-titanium alloy - Google Patents
Cryogenic treatment method of tungsten-titanium alloy Download PDFInfo
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- CN103114260A CN103114260A CN2013100077348A CN201310007734A CN103114260A CN 103114260 A CN103114260 A CN 103114260A CN 2013100077348 A CN2013100077348 A CN 2013100077348A CN 201310007734 A CN201310007734 A CN 201310007734A CN 103114260 A CN103114260 A CN 103114260A
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- tungsten
- titanium alloy
- cryogenic
- treating process
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 69
- MAKDTFFYCIMFQP-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti].[W] MAKDTFFYCIMFQP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 230000000630 rising effect Effects 0.000 claims abstract description 9
- 239000012530 fluid Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 17
- 238000009689 gas atomisation Methods 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000005611 electricity Effects 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000002826 coolant Substances 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000000903 blocking effect Effects 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-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
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
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- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a cryogenic treatment method of a tungsten-titanium alloy. The method comprises the following steps of: placing the cleaned tungsten-titanium alloy on a specimen holder of cryogenic treatment equipment; opening a valve of a self-pressurized cryogenic fluid conveying device filled with a cryogenic medium; treating the alloy by using a gas spraying method; after the treatment is finished, cutting off a power supply and closing a cryogenic source; and taking out the tungsten-titanium alloy to be put into a water bath of 15 to 25 DEG C to quickly realize the temperature raise at the rising rate of 180 to 200 DEG C/s, thereby obtaining the tungsten-titanium alloy of the cryogenic treatment. The tungsten-titanium alloy obtained by using the cryogenic treatment method has the definite crystal orientation and the good mechanical property, so that a film with a good blocking effect is achieved.
Description
Technical field
The invention belongs to metallic substance sub-zero treatment technical field, be specifically related to a kind of cryogenic treating process of tungsten-titanium alloy.
Background technology
Tungsten-titanium alloy not only is adapted at using under large electric current and hot environment owing to having stable thermomechanical property, but also has the series of advantages such as electronic mobility is low, corrosion resistance is high, chemical stability is good, becomes in copper and silver wiring to stop Cu and Si/SiO
2Between the diffusion the optimal candidate film.Due to the more difficult control of grain orientation in the tungsten-titanium alloy preparation process, need the tungsten-titanium alloy for preparing is processed in use to improve its grain orientation, the existing method of improving the alloy grain orientation mainly contains rolling and forges, but because of tungsten-titanium alloy fragility larger, utilize above-mentioned two kinds of methods to process more difficult, therefore need to seek a kind of grain orientation that can improve alloy, the treatment process of Microstructure and properties that can take into account again alloy is very necessary.
Summary of the invention
The cryogenic treating process that the purpose of this invention is to provide a kind of tungsten-titanium alloy has solved existing rolling and forging hard problem.
The technical solution adopted in the present invention is, a kind of cryogenic treating process of tungsten-titanium alloy, with the tungsten-titanium alloy after cleaning, be positioned on the specimen mounting of deep cold treatment apparatus, open the valve of the self supercharging cryogenic fluids e Foerderanlage that deep cooling medium is housed, adopt gas atomization method alloy to process, cut off the electricity supply after processing, close low-temperature receiver, take out tungsten-titanium alloy and put into the water-bath of 15～25 ℃ with the speed fast temperature rising of 180～220 ℃/s, namely obtain the tungsten-titanium alloy of sub-zero treatment.
Characteristics of the present invention also are,
Then the step of cleaning further cleans residue and the moisture on tungsten-titanium alloy surface for tungsten-titanium alloy is rinsed its surface residue with the fine sandpaper polishing is rear with flowing water with ultrasonic wave and alcohol.
Deep cooling medium adopts liquid nitrogen.
The processing parameter that the above-mentioned gas spray method is processed is: cooling rate is 8～15 ℃/min, and holding temperature is-150～-196 ℃, and soaking time is 2～24h.
Another kind of scheme is, tungsten-titanium alloy is carried out twice sub-zero treatment, and the processing parameter that the gas atomization method is processed is: cooling rate is 8～15 ℃/min, and holding temperature is-150～-196 ℃, and soaking time is 2～4h.
The invention has the beneficial effects as follows,
1. the cryogenic treating process of tungsten-titanium alloy of the present invention, freeze by gasification latent heat and the low temperature nitrogen heat of liquid nitrogen, and cooling temperature is low and tungsten-titanium alloy is not had thermal shocking, reduced the low temperature brittleness fracture of tungsten-titanium alloy.
2. the cryogenic treating process of tungsten-titanium alloy of the present invention, adopt the cryogenic treating process of rapid heat cycle, the mode of fast cooling provides larger internal stress for grain refining and crystal grain rotate, after deep cooling, fast temperature rising has reduced that Yin Wendu raises and the grain growth that causes is consolidated the deep cooling effect and improved production efficiency.
3. the cryogenic treating process of tungsten-titanium alloy of the present invention is processed the tungsten-titanium alloy obtain and is not only had certain crystalline orientation, and has good mechanical property, thereby obtains film with good barrier effect.
Description of drawings
Fig. 1 is the figure of tissue topography without the tungsten-titanium alloy of sub-zero treatment;
Fig. 2 is the figure of tissue topography of the tungsten-titanium alloy of the embodiment of the present invention 1 sub-zero treatment.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The cryogenic treating process of tungsten-titanium alloy of the present invention, concrete steps are as follows:
Step 1 is polished tungsten-titanium alloy except rinsing its surface residue with flowing water after descaling and line cutting vestige with fine sandpaper, then further cleans residue and the moisture on tungsten-titanium alloy surface with ultrasonic wave and alcohol;
Step 2, tungsten-titanium alloy after step 1 is cleaned, be positioned on the specimen mounting of deep cold treatment apparatus, open the valve of the self supercharging cryogenic fluids e Foerderanlage that liquid nitrogen is housed, adopt gas atomization method alloy to process, processing parameter is: cooling rate is 8～15 ℃/min, holding temperature is-150～-196 ℃, soaking time is 2～24h, cut off the electricity supply after processing, close low-temperature receiver, take out the speed fast temperature rising that tungsten-titanium alloy is put into 180～220 ℃/s of water-bath of 15～25 ℃, namely obtain the tungsten-titanium alloy of sub-zero treatment.
Tungsten-titanium alloy is carried out twice sub-zero treatment, and the processing parameter that the gas atomization method is processed is: cooling rate is 8～15 ℃/min, and holding temperature is-150～-196 ℃, and soaking time is 2～4h.
The cryogenic treating process of tungsten-titanium alloy of the present invention freezes by gasification latent heat and the low temperature nitrogen heat of liquid nitrogen, and cooling temperature is low and tungsten-titanium alloy is not had thermal shocking, has reduced the low temperature brittleness fracture of tungsten-titanium alloy; Adopt the cryogenic treating process of rapid heat cycle, the mode of fast cooling provides larger internal stress for grain refining and crystal grain rotate, and after deep cooling, fast temperature rising has reduced that Yin Wendu raises and the grain growth that causes is consolidated the deep cooling effect and improved production efficiency.
Tungsten-titanium alloy through sub-zero treatment not only has certain crystalline orientation, and has good mechanical property, thus the film that acquisition has the good barrier effect.
Embodiment 1
Step 1 is polished tungsten-titanium alloy except rinsing its surface residue with flowing water after descaling and line cutting vestige with fine sandpaper, then further cleans residue and the moisture on tungsten-titanium alloy surface with ultrasonic wave and alcohol;
Step 2, tungsten-titanium alloy after step 1 is cleaned, be positioned on the specimen mounting of deep cold treatment apparatus, open the valve of the self supercharging cryogenic fluids e Foerderanlage that liquid nitrogen is housed, adopt gas atomization method alloy to process, processing parameter is: cooling rate is 15 ℃/min, holding temperature is-196 ℃, and soaking time is 2h, cuts off the electricity supply after processing, close low-temperature receiver, take out the speed fast temperature rising that tungsten-titanium alloy is put into the 220 ℃/s of water-bath of 25 ℃.
Then, repeat above-mentioned steps 1 and step 2, the tungsten-titanium alloy after sub-zero treatment is carried out sub-zero treatment for the second time.
Embodiment 2
Step 1 is polished tungsten-titanium alloy except rinsing its surface residue with flowing water after descaling and line cutting vestige with fine sandpaper, then further cleans residue and the moisture on tungsten-titanium alloy surface with ultrasonic wave and alcohol;
Step 2, tungsten-titanium alloy after step 1 is cleaned, be positioned on the specimen mounting of deep cold treatment apparatus, open the valve of the self supercharging cryogenic fluids e Foerderanlage that liquid nitrogen is housed, adopt gas atomization method alloy to process, processing parameter is: cooling rate is 8 ℃/min, holding temperature is-150 ℃, and soaking time is 4h, cuts off the electricity supply after processing, close low-temperature receiver, take out the speed fast temperature rising that tungsten-titanium alloy is put into the 180 ℃/s of water-bath of 15 ℃.
Then, repeat above-mentioned steps 1 and step 2, the tungsten-titanium alloy after sub-zero treatment is carried out sub-zero treatment for the second time.
Embodiment 3
Step 1 is polished tungsten-titanium alloy except rinsing its surface residue with flowing water after descaling and line cutting vestige with fine sandpaper, then further cleans residue and the moisture on tungsten-titanium alloy surface with ultrasonic wave and alcohol;
Step 2, tungsten-titanium alloy after step 1 is cleaned, be positioned on the specimen mounting of deep cold treatment apparatus, open the valve of the self supercharging cryogenic fluids e Foerderanlage that liquid nitrogen is housed, adopt gas atomization method alloy to process, processing parameter is: cooling rate is 13 ℃/min, holding temperature is-175 ℃, soaking time is 24h, cut off the electricity supply after processing, close low-temperature receiver, take out the speed fast temperature rising that tungsten-titanium alloy is put into the 200 ℃/s of water-bath of 20 ℃ with fixture from deep cold treatment apparatus, namely obtain the tungsten-titanium alloy of sub-zero treatment.
The soaking time of gas atomization method can also be got 8h, 12h, 16h and 20h.
As shown in Figure 1, organizing without the tungsten-titanium alloy of sub-zero treatment is mainly rich titanium phase composite by rich tungsten phase and the darker regions of light areas, and wherein rich titanium is compared tinyly, also exists the part hole but have in agglomeration and tissue.
As shown in Figure 2, the tungsten-titanium alloy of processing through embodiment 1 is compared untreated alloy structure by rich tungsten phase and rich titanium phase composite, rich titanium mutually more tiny, be evenly distributed, the hole in tissue also disappears substantially; This is mainly that this internal stress causes the compression closures of subsurface defect in alloy (micropore etc.) because form larger internal stress in alloy because of difference variation in sub-zero treatment.
Before and after the tungsten-titanium alloy sub-zero treatment, the contrast of performance and preferred orientation, as shown in table 1.
Performance and preferred orientation contrast before and after the sub-zero treatment of table 1 tungsten-titanium alloy
Claims (5)
1. the cryogenic treating process of a tungsten-titanium alloy, it is characterized in that: the tungsten-titanium alloy after cleaning, be positioned on the specimen mounting of deep cold treatment apparatus, open the valve of the self supercharging cryogenic fluids e Foerderanlage that deep cooling medium is housed, adopt gas atomization method alloy to process, cut off the electricity supply after processing, close low-temperature receiver, take out tungsten-titanium alloy and put into the speed fast temperature rising of 180～220 ℃/s of water-bath of 15～25 ℃, namely obtain the tungsten-titanium alloy of sub-zero treatment.
2. the cryogenic treating process of tungsten-titanium alloy according to claim 1, it is characterized in that: then the step of described cleaning further cleans residue and the moisture on tungsten-titanium alloy surface for tungsten-titanium alloy is rinsed its surface residue with the fine sandpaper polishing is rear with flowing water with ultrasonic wave and alcohol.
3. the cryogenic treating process of tungsten-titanium alloy according to claim 1 and 2, is characterized in that: described deep cooling medium employing liquid nitrogen.
4. the cryogenic treating process of tungsten-titanium alloy according to claim 3 is characterized in that: the processing parameter that described gas atomization method is processed is: cooling rate is 8～15 ℃/min, and holding temperature is-150～-196 ℃, and soaking time is 2～24h.
5. the cryogenic treating process of tungsten-titanium alloy according to claim 3, it is characterized in that: tungsten-titanium alloy is carried out twice sub-zero treatment, the processing parameter that described gas atomization method is processed is: cooling rate is 8～15 ℃/min, and holding temperature is-150～-196 ℃, and soaking time is 2～4h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559934A (en) * | 2018-03-30 | 2018-09-21 | 江苏大学 | A kind of cryogenic treatment process of TC6 titanium alloy forgings |
| CN109604957A (en) * | 2018-12-14 | 2019-04-12 | 中国航空工业集团公司北京航空精密机械研究所 | A kind of processing method of the open thin-wall titanium alloy part of high-precision configuration |
| CN109848834A (en) * | 2018-12-06 | 2019-06-07 | 太原理工大学 | A kind of combined type processing method improving titanium alloy surface quality |
| CN110819923A (en) * | 2019-11-22 | 2020-02-21 | 西安庄信新材料科技有限公司 | Heat treatment process of titanium plate blank |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201261796Y (en) * | 2008-09-18 | 2009-06-24 | 浙江工业大学 | Conveyer belt type cryogenic treatment apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201261796Y (en) * | 2008-09-18 | 2009-06-24 | 浙江工业大学 | Conveyer belt type cryogenic treatment apparatus |
Non-Patent Citations (1)
| Title |
|---|
| 陈绍甫等: "深冷处理及其应用研究", 《云南农业大学学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559934A (en) * | 2018-03-30 | 2018-09-21 | 江苏大学 | A kind of cryogenic treatment process of TC6 titanium alloy forgings |
| CN108559934B (en) * | 2018-03-30 | 2020-02-21 | 江苏大学 | Cryogenic treatment process for TC6 titanium alloy forging |
| CN109848834A (en) * | 2018-12-06 | 2019-06-07 | 太原理工大学 | A kind of combined type processing method improving titanium alloy surface quality |
| CN109604957A (en) * | 2018-12-14 | 2019-04-12 | 中国航空工业集团公司北京航空精密机械研究所 | A kind of processing method of the open thin-wall titanium alloy part of high-precision configuration |
| CN110819923A (en) * | 2019-11-22 | 2020-02-21 | 西安庄信新材料科技有限公司 | Heat treatment process of titanium plate blank |
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| CN103114260B (en) | 2015-01-21 |
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