CN102773478A - Sintering method for improving mechanical strength of tantalum block - Google Patents
Sintering method for improving mechanical strength of tantalum block Download PDFInfo
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- CN102773478A CN102773478A CN2012102369613A CN201210236961A CN102773478A CN 102773478 A CN102773478 A CN 102773478A CN 2012102369613 A CN2012102369613 A CN 2012102369613A CN 201210236961 A CN201210236961 A CN 201210236961A CN 102773478 A CN102773478 A CN 102773478A
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- tantalum
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- tantalum piece
- deoxidier
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Abstract
The invention discloses a sintering method for improving the mechanical strength of a tantalum block, which comprises the following steps of: taking the metal which is lower in melting point as deoxidant, and jointly sintering with a pressed tantalum block under the vacuum status, so that the oxidized part of the tantalum block is deoxidized, and continuously heating under the vacuum status after the deoxidization is completed to sinter the tantalum block, so that tantalum power is crystallized. A sintering process comprises the following steps of: putting the deoxidant and the pressed tantalum block into a vacuum sintering furnace, starting heating after the vacuum degree of the vacuum sintering furnace is larger than 3*10<-4> Torr, and stopping heating when the temperature is risen to a melting point of the deoxidant; heating to the deoxidant evaporating temperature after the vacuum degree is larger than 3*10<-4> Torr, and keeping the temperature for 30 minutes after the deoxidant is completely evaporated; and heating to the temperature required by sintering the tantalum block after the vacuum degree is larger than 3*10<-4> Torr. The oxides on the surfaces of the tantalum power grains are removed by the deoxidant steam, micro-melting layers on the surfaces of the tantalum power grains can not be baffled by the oxides, crystallization regions are formed among the micro-melting layers, and the mechanical strength of the tantalum block can be greatly improved after the tantalum block is naturally cooled under the vacuum environment.
Description
Technical field
The present invention relates to the metal smelt technical field, particularly a kind of sintering method that improves tantalum piece mechanical strength.
Background technology
Along with the development of complete electronic set to miniaturization, digitlization, high frequencyization, highly reliable direction, require that tantalum electrolytic capacitor is increasingly high with the specific volume of tantalum powder, particle is more and more littler, so tantalum powder adsorption of oxygen and the degree of oxidation is also more and more serious in air.When sintering tantalum piece, because there is layer oxide film on tantalum powder particles surface, blocked flowing of adjacent tantalum powder particles melt surface layer, its mutual crystallizing power is descended, thereby reduced the intensity of tantalum piece.If improve tantalum piece mechanical strength its specific volume will be reduced, not reach the purpose of reduced volume through the raising sintering temperature; Directly cause back working procedure processing difficulty if strengthen pressed density.
Summary of the invention
To the problems referred to above; The present invention discloses a kind of sintering method that improves tantalum piece mechanical strength; Concrete technical scheme is; With fusing point lower enliven tantalum piece under vacuum state the co-sintered of metal as deoxidier and compression moulding, make the oxidized part deoxidation of tantalum piece, deoxidation is accomplished continued and under vacuum state, is heated up the tantalum piece is carried out sintering and makes the crystallization of tantalum powder.
In sintering process, get into vacuum sintering furnace after the tantalum piece of deoxidier and compression moulding put into tantalum crucible, in the vacuum that makes vacuum sintering furnace greater than 3 * 10
-4Begin behind the Torr to heat up, when being warming up to the fusing point of deoxidier, stop to heat up; The vacuum that makes vacuum sintering furnace again is greater than 3 * 10
-4Torr, temperature continues to rise to the deoxidier vapourizing temperature, deoxidier is vaporized fully afterwards be incubated 30 minutes; The vacuum that makes vacuum sintering furnace again is greater than 3 * 10
-4Torr continues to be warmed up to the required temperature of sintering tantalum piece.Because the oxide on tantalum powder particles 1 surface is removed by deoxidier steam, little melting zone 2 on tantalum powder particles surface does not have stopping of oxide, forms crystal region 3 to each other, and after under vacuum environment, cooling off naturally, the mechanical strength of tantalum piece significantly improves.
In the method, for making the abundant deoxidation of tantalum powder that is pressed into the tantalum piece, the mass ratio of deoxidier and tantalum piece is 0.1:3～0.1:15, and optimum quality ratio is 0.1:4～0.1:10.Through selecting for use different metal,, and magnesium is made into the magnesium paper tinsel is tiled in best results under the tantalum piece with the best results of magnesium as deoxidier as the deoxidier comparison that experimentizes.
For the tantalum piece of accomplishing deoxidation and sintering; After temperature is reduced to room temperature under the vacuum state of vacuum sintering furnace; For the metal deoxidier of removing tantalum piece remained on surface and the oxide of this deoxidier, the tantalum piece is put into diluted acid soaked 20 minutes, use deionized water rinsing again 3～4 times.Soaked 20 minutes with dilute acid soln again with the tantalum piece that deionized water soaks for this operation, take out in the baking oven that is put into 150 ℃ then and dry by the fire more than 30 minutes.
Because the present invention has adopted technique scheme, the mechanical strength of tantalum piece improves, and the shearing force on the minimum direction of cuboid tantalum piece size can be brought up to about 1.2kg from about 0.8kg.
Description of drawings
Fig. 1 is sintering curre figure of the present invention.
Fig. 2 is tantalum powder particles crystallization sketch map behind the sintering of the present invention.
The specific embodiment
As deoxidier, sintering curre as shown in Figure 1 carries out sintering with magnesium, gets into vacuum sintering furnace after the tantalum piece of magnesium and compression moulding is put into tantalum crucible, adopts the magnesium pool to be tiled in the tantalum crucible bottom, and the tantalum piece evenly is placed on the magnesium pool.In the vacuum that makes vacuum sintering furnace greater than 3 * 10
-4Begin behind the Torr to heat up, when 650 ℃ of fusing points that is warming up to magnesium, stop to heat up, this moment, vacuum can decrease because the distillation of magnesium and reduction tantalum piece; Start the vacuum extractor of vacuum sintering furnace, the vacuum that makes vacuum sintering furnace again is greater than 3 * 10
-4Torr, temperature continues to rise to 1107 ℃ of magnesium vapourizing temperatures, magnesium is vaporized fully afterwards be incubated 30 minutes, and this moment, magnesium was with the tantalum powder Restore All in the tantalum piece; Vacuumize, the vacuum that makes vacuum sintering furnace is greater than 3 * 10 again
-4Torr continues to be warmed up to the required temperature of sintering tantalum piece as 1300 ℃.This moment is as shown in Figure 2; Because the oxide on tantalum powder particles 1 surface is removed by deoxidier steam, little melting zone 2 on tantalum powder particles 1 surface does not have stopping of oxide, forms crystal region 3 to each other; After under vacuum environment, cooling off naturally, the mechanical strength of tantalum piece significantly improves.
In this method; For making the abundant deoxidation of tantalum powder particles that is pressed into the tantalum piece; The applicant gropes the mass ratio of deoxidier and tantalum piece; Contrasted deoxidier and tantalum piece ratio and be the technique effect of each value between 0.1:1 ~ 0.1:20, drawn deoxidier and tantalum piece ratio effect between 0.1:3～0.1:15 is preferable, wherein optimal proportion is 0.1:4～0.1:10.Through selecting for use different metals such as sodium, magnesium, aluminium as the deoxidier comparison that experimentizes, with the best results of magnesium as deoxidier.
For confirming the beneficial effect of sintering method of the present invention, the applicant has carried out confirmatory experiment.
Confirmatory experiment 1:
Using the CV value is the tantalum powder of 50000 μ F.V/g; Be pressed into 100 of tantalum pieces that are of a size of 7.5 * 2.0 * 1.8mm, quality 150mg; Add 150mg magnesium paper tinsel in magnesium and tantalum piece ratio 0.1:10 and be sintered to 1550 ℃ of insulations 20 minutes, take out 5 minimum thickness direction up cut shear such as following tables of samples inspection tantalum piece size by the sintering curre deoxidation of accompanying drawing 1:
| Sample number into spectrum | Tantalum piece thickness direction shearing force (kg) |
| 1 | 1.18 |
| 2 | 1.23 |
| 3 | 1.16 |
| 4 | 1.24 |
| 5 | 1.21 |
Confirmatory experiment 2:
Using the CV value is the tantalum powder of 80000 μ F.V/g; Be pressed into 100 of tantalum pieces that are of a size of 8.3 * 2.0 * 1.8mm, quality 150mg; Add the deoxidation of 150mg magnesium paper tinsel in magnesium and tantalum piece ratio 0.1:10 and be sintered to 1400 ℃ of insulations 20 minutes, take out 5 minimum thickness direction up cut shear such as following tables of sample inspection tantalum piece size:
| Sample number into spectrum | Tantalum piece thickness direction shearing force (kg) |
| 1 | 1.16 |
| 2 | 1.14 |
| 3 | 1.17 |
| 4 | 1.13 |
| 5 | 1.15 |
Confirmatory experiment 3:
Using the CV value is the tantalum powder of 120000 μ F.V/g; Be pressed into 100 of tantalum pieces that are of a size of 5.5 * 2.0 * 1.8mm, tantalum grain weight amount 100mg; Add the deoxidation of 100mg magnesium paper tinsel in magnesium and tantalum piece ratio 0.1:10 and be sintered to 1300 ℃ of insulations 20 minutes, take out 5 minimum thickness direction up cut shear such as following tables of sample inspection tantalum piece size:
| Sample number into spectrum | Tantalum piece thickness direction shearing force (kg) |
| 1 | 1.14 |
| 2 | 1.13 |
| 3 | 1.15 |
| 4 | 1.14 |
| 5 | 1.15 |
Make respectively and the identical tantalum piece of above-mentioned 3 confirmatory experiment parameters according to prior art, do not add 100 of each sintering of deoxidier, respectively take out minimum thickness direction up cut shear and the confirmatory experiment contrast of 5 sample inspection tantalum piece sizes according to identical sintering temperature curve:
Contrast can know that the tantalum piece that adopts sintering method sintering of the present invention is under identical testing conditions, and the shearing force that can bear is higher, for the tantalum point electrolysis condenser of making high-quality has been created condition.
Claims (7)
1. sintering method that improves tantalum piece mechanical strength, it is characterized in that: the metal that fusing point is lower is as tantalum piece co-sintered under vacuum state of deoxidier and compression moulding.
2. a kind of sintering method that improves tantalum piece mechanical strength as claimed in claim 1 is characterized in that: in sintering process, get into vacuum sintering furnace after the tantalum piece of deoxidier and compression moulding put into tantalum crucible, in the vacuum that makes vacuum sintering furnace greater than 3 * 10
-4Begin behind the Torr to heat up, when being warming up to the fusing point of deoxidier, stop to heat up; The vacuum that makes vacuum sintering furnace again is greater than 3 * 10
-4Torr, temperature continues to rise to the deoxidier vapourizing temperature, deoxidier is vaporized fully afterwards be incubated 30 minutes; The vacuum that makes vacuum sintering furnace again is greater than 3 * 10
-4Torr continues to be warmed up to the required temperature of sintering tantalum piece.
3. a kind of sintering method that improves tantalum piece mechanical strength as claimed in claim 1 is characterized in that: the mass ratio of deoxidier and tantalum piece is 0.1:3～0.1:15.
4. a kind of sintering method that improves tantalum piece mechanical strength as claimed in claim 1 is characterized in that: the mass ratio of deoxidier and tantalum piece is 0.1:4～0.1:10.
5. a kind of sintering method that improves tantalum piece mechanical strength as claimed in claim 1 is characterized in that: described deoxidier adopts magnesium.
6. a kind of sintering method that improves tantalum piece mechanical strength as claimed in claim 1 is characterized in that: deoxidier adopts the magnesium paper tinsel, and the magnesium paper tinsel is tiled under the tantalum piece.
7. a kind of sintering method that improves tantalum piece mechanical strength as claimed in claim 1 is characterized in that: the tantalum piece that will accomplish deoxidation and sintering is put into diluted acid immersion 20 minutes, uses deionized water rinsing again 3～4 times.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103700504A (en) * | 2013-12-17 | 2014-04-02 | 中国振华（集团）新云电子元器件有限责任公司 | Sintering method for enhancing tantalum wire tension on anode block of tantalum capacitor |
| CN113077989A (en) * | 2021-03-31 | 2021-07-06 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Preparation method of anode tantalum block of low-oxygen-content solid electrolyte tantalum capacitor |
| CN114093676A (en) * | 2021-11-12 | 2022-02-25 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Sintering method of anode block of tantalum capacitor |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103700504A (en) * | 2013-12-17 | 2014-04-02 | 中国振华（集团）新云电子元器件有限责任公司 | Sintering method for enhancing tantalum wire tension on anode block of tantalum capacitor |
| CN103700504B (en) * | 2013-12-17 | 2016-07-20 | 中国振华（集团）新云电子元器件有限责任公司 | Improve the sintering method of anode block of tantalum capacitor tantalum wire pulling force |
| CN113077989A (en) * | 2021-03-31 | 2021-07-06 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Preparation method of anode tantalum block of low-oxygen-content solid electrolyte tantalum capacitor |
| CN113077989B (en) * | 2021-03-31 | 2023-05-12 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Preparation method of anode tantalum block of low-oxygen-content solid electrolyte tantalum capacitor |
| CN114093676A (en) * | 2021-11-12 | 2022-02-25 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Sintering method of anode block of tantalum capacitor |
| CN114093676B (en) * | 2021-11-12 | 2023-03-24 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Sintering method of anode block of tantalum capacitor |
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Application publication date: 20121114 |