CN114273497B - Preparation method of tantalum sheath - Google Patents
Preparation method of tantalum sheath Download PDFInfo
- Publication number
- CN114273497B CN114273497B CN202210106152.4A CN202210106152A CN114273497B CN 114273497 B CN114273497 B CN 114273497B CN 202210106152 A CN202210106152 A CN 202210106152A CN 114273497 B CN114273497 B CN 114273497B
- Authority
- CN
- China
- Prior art keywords
- sheath
- heat treatment
- stretch forming
- diameter
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to a preparation method of a tantalum sheath, which comprises the following steps: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and the cover plate to obtain the tantalum sheath; the temperature of the primary heat treatment is 1000-1200 ℃; the temperature of the secondary heat treatment is 700-800 ℃; the temperature of the three heat treatments is 850-970 ℃. Through redesigning the preparation process of the sheath, the problems of deformation and poor air tightness of the sheath at high temperature and high pressure are avoided. The special stretching and heat treatment processes are combined, so that the obtained sheath has good air tightness, and the heat energy ensures good air tightness after high-temperature high-pressure heat treatment.
Description
Technical Field
The invention relates to the field of targets, in particular to a preparation method of a tantalum sheath.
Background
Gadolinium oxysulfide materials are currently used in flat panel detectors for digital radiography because they act as scintillation materials capable of converting high energy rays (X/gamma rays) or particles incident thereon into crystalline energy converters of ultraviolet or visible light.
As disclosed in CN109370583a, a preparation method, a product and an application of a gadolinium oxysulfide fluorescent powder are disclosed, doped gadolinium oxide powder is obtained by a liquid phase precipitation method, the doped gadolinium oxide powder is mixed with a sulfur source and molten salt, and the gadolinium oxysulfide powder is prepared by a solvothermal method, wherein the liquid phase precipitation method is that different rare earth nitrate solutions are uniformly mixed and then reacted with a precipitant to generate a doped rare earth precipitate precursor, and the doped gadolinium oxide precursor is decomposed into doped gadolinium oxide powder after calcination. In the preparation process, the purity of the rare earth oxide powder is improved through the process of nitric acid dissolution and reprecipitation, so that the influence of certain impurities on the luminescent performance of gadolinium oxysulfide fluorescent powder is effectively reduced; the rare earth ions are doped more uniformly, and in a liquid phase, the rare earth ions can be mixed at a molecular level, and the uniformity is incomparable with any solid phase mixing method. The gadolinium oxysulfide fluorescent powder prepared by the method has the characteristics of simple process, high purity, uniform doping and the like.
Gadolinium oxysulfide materials are commonly sintered into ceramic bodies for use in flat panel detectors for digital radiography.
The CN105800663A discloses a hot-pressing reaction sintering method of gadolinium oxysulfide scintillating ceramic, which comprises the following steps: gd is put into 2 O 2 SO 4 Uniformly mixing the powder with reducing agent powder to obtain raw material powder, and carrying out sectional sintering on the raw material powder, wherein the reducing agent comprises active carbon, graphene, coke and charcoal, and the sectional sintering comprises the steps of carrying out first-stage sintering at 820-950 ℃ and 10-75MPa, and carrying out second-stage sintering at 1000-1500 ℃ and 30-150MPa, wherein inert atmosphere, reducing atmosphere or vacuum is kept in the sintering process. The method can provide additional power for densification by utilizing the energy released by the reaction in the sintering process, so that high-density ceramic can be obtained at lower temperature and pressure. In the sintering process, a sintering auxiliary agent is not needed to be added, and interference of foreign ion on scintillation performance is reduced. The method has the advantages of greatly shortening the production period, improving the production efficiency, having the characteristics of simple process, low production cost and the like, and the obtained high-density ceramic has good matching of emission wavelength and a photodiode under the excitation of high-energy rays and has very high detection efficiency.
However, when gadolinium oxysulfide ceramic is fired by hot isostatic pressing, the high sintering temperature, the high pressure and the reaction in the sintering process cause the problem that sulfur vapor fills the sheath and causes the sheath to be damaged or contracted. While also affecting the properties of the resulting sintered ceramic.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a preparation method of a tantalum sheath, which aims to solve the problems of insufficient air tightness and larger deformation rate of the current sheath in the high-temperature use process.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a tantalum sheath, which comprises the following steps: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and the cover plate to obtain the tantalum sheath;
the diameter of the sheath obtained by the primary stretch forming is larger than the diameter of the sheath obtained by the secondary stretch forming;
the diameter of the sheath obtained by the three-time stretch forming is smaller than the diameter of the sheath obtained by the two-time stretch forming;
the diameter of the sheath obtained by the three times of stretching molding is smaller than the diameter of the sheath obtained by the four times of stretching molding;
the temperature of the primary heat treatment is 1000-1200 ℃; the temperature of the secondary heat treatment is 700-800 ℃; the temperature of the three heat treatments is 850-970 ℃.
According to the preparation method provided by the invention, through redesigning the preparation process of the sheath, the problems of deformation and poor air tightness of the sheath at high temperature and high pressure are avoided. The special stretching and heat treatment processes are combined, so that the obtained sheath has good air tightness, and the heat energy ensures good air tightness after high-temperature high-pressure heat treatment. In the heat treatment process, the deformation of the sheath in the use process is obviously reduced due to the adoption of a specific temperature system.
In the invention, the sheet material is formed into a certain direct cylindrical sheath by one-step stretch forming, and the shape is similar to a barrel shape, namely one side is opened. The subsequent stretch forming is similar.
In the present invention, the temperature of the primary heat treatment may be 1000 to 1200 ℃, for example, 1000 ℃, 1010 ℃, 1020 ℃, 1030 ℃, 1040 ℃, 1050 ℃, 1060 ℃, 1070 ℃, 1080 ℃, 1090 ℃, 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃, 1160 ℃, 1170 ℃, 1180 ℃, 1190 ℃, 1200 ℃, or the like, but the present invention is not limited to the above-mentioned values, and other combinations not mentioned in the above range are equally applicable.
In the present invention, the temperature of the secondary heat treatment is 700 to 800 ℃, and for example, 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, or 800 ℃ may be used, but the present invention is not limited to the above-mentioned values, and other combinations not mentioned in the above range are equally applicable.
In the present invention, the temperature of the three heat treatments is 850 to 970 ℃, and may be 850 ℃, 860 ℃, 870 ℃, 880 ℃, 890 ℃, 900 ℃, 910 ℃, 920 ℃, 930 ℃, 940 ℃, 950 ℃, 960 ℃, 970 ℃, or the like, for example, but the present invention is not limited to the above-mentioned values, and other combinations not mentioned in the above range are equally applicable.
In a preferred embodiment of the present invention, the tantalum plate has a thickness of 1.5 to 2.5mm, for example, 1.5mm, 1.6mm, 1.7mm, 1.8mm, 1.9mm, 2mm, 2.1mm, 2.2mm, 2.3mm, 2.4mm, or 2.5mm, etc., but the tantalum plate is not limited to the recited values, and other combinations not recited in the range are equally applicable.
In the invention, the grain in the tantalum plate is redistributed by sintering at a higher temperature, the grain structure is redistributed, and then the surface property of the sheath is further optimized by adopting heat treatment at a lower temperature, so that the final sheath has good deformation resistance.
In a preferred embodiment of the present invention, the diameter of the sheath obtained by the one-time stretch forming is 180 to 200mm, and for example, 180mm, 181mm, 182mm, 183mm, 184mm, 185mm, 186mm, 187mm, 188mm, 189mm, 190mm, 191mm, 192mm, 193mm, 194mm, 195mm, 196mm, 197mm, 198mm, 199mm, 200mm, or the like may be used, but the present invention is not limited to the above-mentioned values, and other combinations not shown in the above-mentioned ranges are equally applicable.
In a preferred embodiment of the present invention, the diameter of the sheath obtained by the secondary stretch forming is 140 to 150mm, and may be 140mm, 141mm, 142mm, 143mm, 144mm, 145mm, 146mm, 147mm, 148mm, 149mm, 150mm, or the like, for example, but not limited to the values recited, and other values not recited in the range are equally applicable.
In a preferred embodiment of the present invention, the diameter of the sheath obtained by the three-time stretch forming is 100 to 110mm, and for example, 100mm, 101mm, 102mm, 103mm, 104mm, 105mm, 106mm, 107mm, 108mm, 109mm or 110mm may be used, but the sheath is not limited to the above-mentioned values, and other combinations not mentioned in the above range are equally applicable.
In a preferred embodiment of the present invention, the diameter of the sheath obtained by the four-time stretch forming is 120 to 125mm, for example, 120mm, 120.5mm, 121mm, 121.5mm, 122mm, 122.5mm, 123mm, 123.5mm, 124mm, 124.5mm or 125mm, etc., but the sheath is not limited to the above-mentioned values, and other combinations not mentioned in the above range are equally applicable.
In a preferred embodiment of the present invention, the time of the primary heat treatment is 1 to 2 hours, for example, 1 hour, 1.1 hour, 1.2 hours, 1.3 hours, 1.4 hours, 1.5 hours, 1.6 hours, 1.7 hours, 1.8 hours, 1.9 hours or 2 hours, etc., but the present invention is not limited to the recited values, and other combinations not recited in the range are equally applicable.
The temperature rising rate of the primary heat treatment is preferably 10 to 15 ℃ per minute, and may be, for example, 10 ℃ per minute, 10.5 ℃ per minute, 11 ℃ per minute, 11.5 ℃ per minute, 12 ℃ per minute, 12.5 ℃ per minute, 13 ℃ per minute, 13.5 ℃ per minute, 14 ℃ per minute, 14.5 ℃ per minute, 15 ℃ per minute, etc., but not limited to the recited values, and other non-recited combinations within the range are equally applicable.
In a preferred embodiment of the present invention, the time of the secondary heat treatment is 30 to 45min, for example, 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min, 44min or 45min, etc., but not limited to the recited values, and other combinations not recited in the range are equally applicable.
Preferably, the temperature rising rate of the secondary heat treatment is 2-7 ℃ per minute, for example, 2 ℃/min, 2.5 ℃/min, 3 ℃/min, 3.5 ℃/min, 4 ℃/min, 4.5 ℃/min, 5 ℃/min, 5.5 ℃/min, 6 ℃/min, 6.5 ℃/min or 7 ℃/min, etc., but not limited to the recited values, and other non-recited combinations within the range are equally applicable.
In a preferred embodiment of the present invention, the time of the three heat treatments is 40-60min, for example, 40min, 41min, 42min, 43min, 44min, 45min, 46min, 47min, 48min, 49min, 50min, 51min, 52min, 53min, 54min, 55min, 56min, 57min, 58min, 59min or 60min, etc., but not limited to the recited values, and other non-recited combinations are equally applicable in the range.
Preferably, the time of the three heat treatments is 15-25 ℃ per minute, for example, 15 ℃ per minute, 16 ℃ per minute, 17 ℃ per minute, 18 ℃ per minute, 19 ℃ per minute, 20 ℃ per minute, 21 ℃ per minute, 22 ℃ per minute, 23 ℃ per minute, 24 ℃ per minute, 25 ℃ per minute, etc., but not limited to the recited values, other non-recited combinations within the range are also applicable.
As a preferable technical scheme of the invention, the preparation method comprises the following steps: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and a tantalum cover plate to obtain the tantalum sheath;
the thickness of the tantalum plate is 1.5-2.5mm;
the diameter of the sheath obtained by the primary stretch forming is larger than the diameter of the sheath obtained by the secondary stretch forming;
the diameter of the sheath obtained by the three-time stretch forming is smaller than the diameter of the sheath obtained by the two-time stretch forming;
the diameter of the sheath obtained by the three times of stretching molding is smaller than the diameter of the sheath obtained by the four times of stretching molding; the diameter of the sheath obtained by the primary stretch forming is 180-200mm; the diameter of the sheath obtained by the secondary stretch forming is 140-150mm; the diameter of the sheath obtained by the three times of stretching molding is 100-110mm; the diameter of the sheath obtained by the four-time stretch forming is 120-125mm;
the temperature of the primary heat treatment is 1000-1200 ℃; the time of the primary heat treatment is 1-2h; the heating rate of the primary heat treatment is 10-15 ℃/min;
the temperature of the secondary heat treatment is 700-800 ℃; the time of the secondary heat treatment is 30-45min; the temperature rising rate of the secondary heat treatment is 2-7 ℃/min;
the temperature of the three heat treatments is 850-970 ℃; the time of the three heat treatments is 40-60min; the time of the three heat treatments is 15-25 ℃/min.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) According to the preparation method of the sheath, provided by the invention, the preparation of the high-performance sheath made of the specific material is realized by adopting the coupling of the specific stretching process and the heat treatment process, wherein the airtight performance of the sheath is improved by adopting the matching and lifting of the stretching process and the heat treatment process for the specific times; furthermore, the temperature system of heat treatment is controlled to realize that the obtained sheath has good mechanical property, and the deformation rate before and after use is obviously reduced.
(2) The obtained sheath has good air tightness and almost no change in air tightness and deformation rate before and after use. Helium concentration in the air tightness detection is less than or equal to 1 x 10 -12 Pa, deformation rate of the sheath is less than or equal to 1.6% before and after use.
Detailed Description
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
example 1
The embodiment provides a preparation method of a tantalum sheath, which comprises the following steps: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and a tantalum cover plate to obtain the tantalum sheath;
the thickness of the tantalum plate is 2mm;
the diameter of the sheath obtained by the primary stretch forming is larger than the diameter of the sheath obtained by the secondary stretch forming;
the diameter of the sheath obtained by the three-time stretch forming is smaller than the diameter of the sheath obtained by the two-time stretch forming;
the diameter of the sheath obtained by the three times of stretching molding is smaller than the diameter of the sheath obtained by the four times of stretching molding; the diameter of the sheath obtained by the primary stretch forming is 190mm; the diameter of the sheath obtained by the secondary stretch forming is 145mm; the diameter of the sheath obtained by the three-time stretch forming is 105mm; the diameter of the sheath obtained by the four-time stretch forming is 122mm;
the temperature of the primary heat treatment is 1100 ℃; the time of the primary heat treatment is 1.5h; the heating rate of the primary heat treatment is 12 ℃/min;
the temperature of the secondary heat treatment is 750 ℃; the time of the secondary heat treatment is 37min; the temperature rising rate of the secondary heat treatment is 4 ℃/min;
the temperature of the three heat treatments is 900 ℃; the time of the three heat treatments is 50min; the time of the three heat treatments is that the heating rate is 20 ℃/min.
The properties of the resulting sheath are shown in Table 1.
Example 2
The embodiment provides a preparation method of a tantalum sheath, which comprises the following steps: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and a tantalum cover plate to obtain the tantalum sheath;
the thickness of the tantalum plate is 1.5mm;
the diameter of the sheath obtained by the primary stretch forming is larger than the diameter of the sheath obtained by the secondary stretch forming;
the diameter of the sheath obtained by the three-time stretch forming is smaller than the diameter of the sheath obtained by the two-time stretch forming;
the diameter of the sheath obtained by the three times of stretching molding is smaller than the diameter of the sheath obtained by the four times of stretching molding; the diameter of the sheath obtained by the primary stretch forming is 200mm; the diameter of the sheath obtained by the secondary stretch forming is 140mm; the diameter of the sheath obtained by the three-time stretch forming is 110mm; the diameter of the sheath obtained by the four-time stretch forming is 125mm;
the temperature of the primary heat treatment is 1000 ℃; the time of the primary heat treatment is 2 hours; the heating rate of the primary heat treatment is 10 ℃/min;
the temperature of the secondary heat treatment is 700 ℃; the time of the secondary heat treatment is 45min; the temperature rising rate of the secondary heat treatment is 2 ℃/min;
the temperature of the three heat treatments is 850 ℃; the time of the three heat treatments is 60min; the time of the three heat treatments is that the heating rate is 25 ℃/min.
The properties of the resulting sheath are shown in Table 1.
Example 3
The embodiment provides a preparation method of a tantalum sheath, which comprises the following steps: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and a tantalum cover plate to obtain the tantalum sheath;
the thickness of the tantalum plate is 2.5mm;
the diameter of the sheath obtained by the primary stretch forming is larger than the diameter of the sheath obtained by the secondary stretch forming;
the diameter of the sheath obtained by the three-time stretch forming is smaller than the diameter of the sheath obtained by the two-time stretch forming;
the diameter of the sheath obtained by the three times of stretching molding is smaller than the diameter of the sheath obtained by the four times of stretching molding; the diameter of the sheath obtained by the primary stretch forming is 180mm; the diameter of the sheath obtained by the secondary stretch forming is 150mm; the diameter of the sheath obtained by the three-time stretch forming is 100mm; the diameter of the sheath obtained by the four-time stretch forming is 120mm;
the temperature of the primary heat treatment is 1200 ℃; the time of the primary heat treatment is 1h; the heating rate of the primary heat treatment is 15 ℃/min;
the temperature of the secondary heat treatment is 800 ℃; the time of the secondary heat treatment is 30min; the temperature rising rate of the secondary heat treatment is 7 ℃/min;
the temperature of the three heat treatments is 970 ℃; the time of the three heat treatments is 40min; the time of the three heat treatments is 15 ℃/min.
The properties of the resulting sheath are shown in Table 1.
Comparative example 1
The difference from example 1 is that the primary stretch forming is not performed. The properties of the resulting sheath are shown in Table 1.
Comparative example 2
The difference from example 1 is only that the secondary stretch forming is not performed. The properties of the resulting sheath are shown in Table 1.
Comparative example 3
The difference from example 1 is only that no three stretch forming is performed. The properties of the resulting sheath are shown in Table 1.
Comparative example 4
The difference from example 1 is only that the four stretch forming is not performed. The properties of the resulting sheath are shown in Table 1.
Comparative example 5
The difference from example 1 is that only one heat treatment was not performed. The properties of the resulting sheath are shown in Table 1.
Comparative example 6
The difference from example 1 is only that no secondary heat treatment was performed. The properties of the resulting sheath are shown in Table 1.
Comparative example 7
The difference from example 1 is only that no heat treatment was performed three times. The properties of the resulting sheath are shown in Table 1.
Comparative example 8
The only difference from example 1 is that the three stretch forming and four stretch forming are combined and stretched directly to a jacket diameter of 122mm. The properties of the resulting sheath are shown in Table 1.
Comparative example 9
The difference from example 1 is only that the temperature of the three heat treatments is 1200 ℃. The properties of the resulting sheath are shown in Table 1.
Gadolinium oxysulfide powder was sintered by hot isostatic pressing using the sheaths obtained in examples 1 to 3 and comparative examples 1 to 9, at a sintering temperature of 1900℃and a pressure of 200MPa. The properties of the capsule after the hot isostatic pressing treatment are shown in Table 1.
The detection of the air tightness of the sheath is as follows: by butt-wrappingVacuumizing to 1.0 x 10 -12 Pa, and carrying out helium leak detection on the vacuum body; air tightness of the sheath after use: and whether the sheath bulges or not is observed as a standard.
Sheath formability: and (3) whether the sheath can be in good condition to achieve the final size.
The deformation rate is detected by determining the volume of the sheath before and after use, and specifically comparing the volume of water in the sheath before and after use.
The deformation rate is the amount of water that the sheath can hold after use/the amount of water that the sheath can hold before use is 100%.
TABLE 1
As can be seen from the results of the above examples and comparative examples, the preparation method provided by the present invention avoids the problems of deformation and poor air tightness of the sheath at high temperature and high pressure by redesigning the preparation process of the sheath. The special stretching and heat treatment processes are combined, so that the obtained sheath has good air tightness, and the heat energy ensures good air tightness after high-temperature high-pressure heat treatment. In the heat treatment process, the deformation of the sheath in the use process is obviously reduced due to the adoption of a specific temperature system.
It is stated that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e., it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (13)
1. A method for preparing a tantalum sheath, comprising the steps of: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and the cover plate to obtain the tantalum sheath;
the diameter of the sheath obtained by the primary stretch forming is larger than the diameter of the sheath obtained by the secondary stretch forming;
the diameter of the sheath obtained by the three-time stretch forming is smaller than the diameter of the sheath obtained by the two-time stretch forming;
the diameter of the sheath obtained by the three times of stretching molding is smaller than the diameter of the sheath obtained by the four times of stretching molding;
the temperature of the primary heat treatment is 1000-1200 ℃; the temperature of the secondary heat treatment is 700-800 ℃; the temperature of the three heat treatments is 850-970 ℃.
2. The method of manufacturing according to claim 1, wherein the tantalum plate has a thickness of 1.5-2.5mm.
3. The method of claim 1, wherein the diameter of the sheath obtained by the one-time stretch forming is 180-200mm.
4. The method of claim 1, wherein the diameter of the jacket obtained by the secondary stretch forming is 140-150mm.
5. The method of claim 1, wherein the diameter of the sheath obtained by the three stretch forming is 100-110mm.
6. The method of claim 1, wherein the sheath formed by four stretching processes has a diameter of 120-125mm.
7. The method of claim 1, wherein the time of the one heat treatment is 1 to 2 hours.
8. The method according to claim 1, wherein the temperature rise rate of the primary heat treatment is 10 to 15 ℃/min.
9. The method of claim 1, wherein the secondary heat treatment is performed for a period of 30 to 45 minutes.
10. The method according to claim 1, wherein the rate of temperature rise of the secondary heat treatment is 2 to 7 ℃/min.
11. The method of claim 1, wherein the three heat treatments are performed for a period of 40 to 60 minutes.
12. The method according to claim 1, wherein the time of the three heat treatments is 15-25 ℃/min.
13. The method of any one of claims 1-12, wherein the method of preparation comprises: sequentially carrying out primary stretch forming, primary heat treatment, secondary stretch forming, secondary heat treatment, tertiary stretch forming, quaternary stretch forming and tertiary heat treatment on the tantalum plate to obtain a sheath cavity; then welding the sheath cavity and a tantalum cover plate to obtain the tantalum sheath;
the thickness of the tantalum plate is 1.5-2.5mm;
the diameter of the sheath obtained by the primary stretch forming is larger than the diameter of the sheath obtained by the secondary stretch forming;
the diameter of the sheath obtained by the three-time stretch forming is smaller than the diameter of the sheath obtained by the two-time stretch forming;
the diameter of the sheath obtained by the three times of stretching molding is smaller than the diameter of the sheath obtained by the four times of stretching molding; the diameter of the sheath obtained by the primary stretch forming is 180-200mm; the diameter of the sheath obtained by the secondary stretch forming is 140-150mm; the diameter of the sheath obtained by the three times of stretching molding is 100-110mm; the diameter of the sheath obtained by the four-time stretch forming is 120-125mm;
the temperature of the primary heat treatment is 1000-1200 ℃; the time of the primary heat treatment is 1-2h; the heating rate of the primary heat treatment is 10-15 ℃/min;
the temperature of the secondary heat treatment is 700-800 ℃; the time of the secondary heat treatment is 30-45min; the temperature rising rate of the secondary heat treatment is 2-7 ℃/min;
the temperature of the three heat treatments is 850-970 ℃; the time of the three heat treatments is 40-60min; the time of the three heat treatments is 15-25 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210106152.4A CN114273497B (en) | 2022-01-28 | 2022-01-28 | Preparation method of tantalum sheath |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210106152.4A CN114273497B (en) | 2022-01-28 | 2022-01-28 | Preparation method of tantalum sheath |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114273497A CN114273497A (en) | 2022-04-05 |
| CN114273497B true CN114273497B (en) | 2023-07-25 |
Family
ID=80881832
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210106152.4A Active CN114273497B (en) | 2022-01-28 | 2022-01-28 | Preparation method of tantalum sheath |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114273497B (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0452541A2 (en) * | 1990-04-14 | 1991-10-23 | W.C. Heraeus GmbH | Method of manufacturing hollow objects from tantalum |
| JP2002192248A (en) * | 2000-12-27 | 2002-07-10 | Asahi-Seiki Mfg Co Ltd | Titanium plate drawing method and drawn product |
| JP2004209533A (en) * | 2003-01-07 | 2004-07-29 | Matsushita Electric Ind Co Ltd | Drawing method of small diameter |
| JP2014018854A (en) * | 2012-07-23 | 2014-02-03 | Nippon Steel & Sumitomo Metal | Method for manufacturing aluminum alloy formed body |
| JP6133965B1 (en) * | 2015-12-17 | 2017-05-24 | 日新製鋼株式会社 | Evaluation method of stretch flangeability |
| WO2017145856A1 (en) * | 2016-02-22 | 2017-08-31 | 日新製鋼株式会社 | Molding material production method and molding material thereof |
| CN107321833A (en) * | 2017-06-30 | 2017-11-07 | 成都市翻鑫家科技有限公司 | A kind of high rigidity gas cylinder Hot drawing manufacture method |
| CN109201837A (en) * | 2018-08-15 | 2019-01-15 | 东莞市瑞成精密模具有限公司 | A kind of battery steel shell drawing process |
| CN110802153A (en) * | 2019-11-06 | 2020-02-18 | 四川航天中天动力装备有限责任公司 | Deep drawing forming process for aluminum alloy deep paraboloid cylindrical part |
| CN110952064A (en) * | 2019-11-25 | 2020-04-03 | 宁波江丰电子材料股份有限公司 | Tantalum-silicon alloy sputtering target material and preparation method thereof |
| CN111185539A (en) * | 2020-01-16 | 2020-05-22 | 浙江安胜科技股份有限公司 | Special-shaped stretch-formed heat-preservation lunch box and preparation method thereof |
| CN112453165A (en) * | 2020-11-19 | 2021-03-09 | 台州竞美工贸有限公司 | Hot water circulating pump stator shielding sleeve mirror surface bright extrusion forming process |
-
2022
- 2022-01-28 CN CN202210106152.4A patent/CN114273497B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0452541A2 (en) * | 1990-04-14 | 1991-10-23 | W.C. Heraeus GmbH | Method of manufacturing hollow objects from tantalum |
| JP2002192248A (en) * | 2000-12-27 | 2002-07-10 | Asahi-Seiki Mfg Co Ltd | Titanium plate drawing method and drawn product |
| JP2004209533A (en) * | 2003-01-07 | 2004-07-29 | Matsushita Electric Ind Co Ltd | Drawing method of small diameter |
| JP2014018854A (en) * | 2012-07-23 | 2014-02-03 | Nippon Steel & Sumitomo Metal | Method for manufacturing aluminum alloy formed body |
| JP6133965B1 (en) * | 2015-12-17 | 2017-05-24 | 日新製鋼株式会社 | Evaluation method of stretch flangeability |
| WO2017145856A1 (en) * | 2016-02-22 | 2017-08-31 | 日新製鋼株式会社 | Molding material production method and molding material thereof |
| CN107321833A (en) * | 2017-06-30 | 2017-11-07 | 成都市翻鑫家科技有限公司 | A kind of high rigidity gas cylinder Hot drawing manufacture method |
| CN109201837A (en) * | 2018-08-15 | 2019-01-15 | 东莞市瑞成精密模具有限公司 | A kind of battery steel shell drawing process |
| CN110802153A (en) * | 2019-11-06 | 2020-02-18 | 四川航天中天动力装备有限责任公司 | Deep drawing forming process for aluminum alloy deep paraboloid cylindrical part |
| CN110952064A (en) * | 2019-11-25 | 2020-04-03 | 宁波江丰电子材料股份有限公司 | Tantalum-silicon alloy sputtering target material and preparation method thereof |
| CN111185539A (en) * | 2020-01-16 | 2020-05-22 | 浙江安胜科技股份有限公司 | Special-shaped stretch-formed heat-preservation lunch box and preparation method thereof |
| CN112453165A (en) * | 2020-11-19 | 2021-03-09 | 台州竞美工贸有限公司 | Hot water circulating pump stator shielding sleeve mirror surface bright extrusion forming process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114273497A (en) | 2022-04-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111394706B (en) | Preparation method of ITO ceramic target material with controllable grain size | |
| JP5764828B2 (en) | Oxide sintered body and tablet processed the same | |
| CN114273497B (en) | Preparation method of tantalum sheath | |
| WO2013021737A1 (en) | Zn-Sn-O TYPE OXIDE SINTERED BODY AND METHOD FOR PRODUCING SAME | |
| JP6649959B2 (en) | Manufacturing method of transparent alumina sintered body | |
| DE112011100972T5 (en) | Transparent conductive film | |
| US20210206697A1 (en) | Sn-Zn-O-BASED OXIDE SINTERED BODY AND METHOD FOR PRODUCING THE SAME | |
| EP2573059A1 (en) | Sintered zinc oxide tablet and process for producing same | |
| CN112919907A (en) | Lead-free ferroelectric ceramic material with enhanced energy storage efficiency and high energy storage capacity and preparation method thereof | |
| KR20050106475A (en) | Sputtering target and process for producing the same | |
| CN1289439C (en) | Lanthanum hafnate base transparent ceramics and its preparing method | |
| CN1142218A (en) | Silicon nitride sinter and process for producing the same | |
| JP2020105064A (en) | Ruthenium aluminum garnet sintered with praseodymium and a method for producing the same | |
| CN113045310B (en) | Method for preparing lanthanum gadolinium zirconate transparent ceramic by AM gel casting process | |
| CN113213927A (en) | High-energy-storage silver niobate-based ceramic with mismatch of stoichiometry and preparation method thereof | |
| CN111943650B (en) | IWO target material for activated plasma deposition technology and preparation method thereof | |
| CN116120057B (en) | High-density ytterbium hafnate transparent ceramic material and preparation method and application thereof | |
| WO2012121298A1 (en) | Oxide sintered body, method for manufacturing same, and target using same | |
| CN113149614A (en) | Sintered body, target material and preparation method thereof | |
| JPWO2014021374A1 (en) | Oxide sintered body and tablet processed the same | |
| JP5613926B2 (en) | Sputtering target for transparent conductive film and method for producing the same | |
| KR20140103097A (en) | Complex oxide sintered body, sputtering target, transparent conductive oxide film, and method for producing same | |
| JPH06171930A (en) | Spinel powder for light transmitting spinel sintered compact and its production | |
| US3897257A (en) | Light transmitting polycrystalline magnesia member and method of making | |
| CN116253558B (en) | Preparation method of graphene-coated electronic compound and preparation method of film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |