CN107557738A - A kind of manufacture method of the high purity boron target of high-compactness high rigidity - Google Patents
A kind of manufacture method of the high purity boron target of high-compactness high rigidity Download PDFInfo
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- CN107557738A CN107557738A CN201710765712.6A CN201710765712A CN107557738A CN 107557738 A CN107557738 A CN 107557738A CN 201710765712 A CN201710765712 A CN 201710765712A CN 107557738 A CN107557738 A CN 107557738A
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Abstract
The invention discloses a kind of manufacture method of the high purity boron target of high-compactness high rigidity, it is to carry out consolidation not less than pure boron powder of the 99.9%, particle diameter no more than 10 μm to purity using discharge plasma sintering technique, 3~10min is incubated after being heated to 1480~1630 DEG C while applying 20~50MPa axial compressive force by step with 50~150 DEG C/min, you can obtain size and be not less than 5mm, consistency not less than 92.0%, the uniform high rigidity high purity boron target of fine microstructures not less than 20mm, thickness.Present invention process is simple, the cycle is short, cost is low, gained boron target through follow-up a small amount of grinding can finished product and be used for the sputter coating in the fields such as nuclear physics, laser physics and functional glass, have a extensive future.
Description
Technical field
The invention belongs to target manufacturing field, more particularly to a kind of method for manufacturing high-melting-point non-metal simple-substance target.
Background technology
Boron target is one of conventional film target in the fields such as nuclear physics, laser physics and functional glass.Traditional target manufacturer
Method be using PM technique by the material powder of certain purity it is compressing after, be made through high temperature sintering.It is but conventional
Sintering method, such as vacuum-sintering, hot pressing, the boron target density that time-consuming, energy consumption is big, efficiency is low and obtained is low, and (consistency is low
In 80%), it is bad mechanical strength, frangible, be not suitable for using during sputter coating.In recent years, according to different application requirements,
The boron target technologies of preparing such as electrostatic vibration, high pressure EFI, centrifugation, the sputtering of focusing HIB and electron bombardment are invented.But
It is the boron target finite thickness (generally only hundreds of microns) that the above method is prepared, and needs substrate to support, be costly.
Discharge plasma sintering (SPS) technology be using flash DC current flow through powder or mould produce Joule heat and
A kind of new technology of rapidly solidified shaping is carried out to powder.The sintering technology can significantly reduce forming temperature and curring time, and
A series of special effectses such as plasma activation, discharge impact pressure and electric field-assisted diffusion effect are produced in powder particle gap,
It is considered as to prepare fine grain, a kind of high efficiency, low cost method of nanocrystalline high compact block material.Importantly, using SPS
Need not both preform be carried out to powder, it is not required that add any lubricant or binder, have short during technology consolidated powder
The advantages that flow, environmental protection, precision form.Therefore, it is expected to break through existing technical bottleneck using SPS technologies, manufacture has high cause
The high purity boron target of density, qualitative leap is realized in performance and cost.
The content of the invention
It is an object of the invention to the deficiency in the method for the high purity boron target for existing manufacture high-compactness high rigidity
Place, by using discharge plasma sintering technique, optimize sintering process parameter, there is provided a kind of high-compactness, high rigidity, tissue are thin
The manufacture method of small uniform high purity boron target, the performance of boron target is increased substantially while reducing cost.
The present invention solves technical problem, adopts the following technical scheme that：
The manufacture method of the high purity boron target of high-compactness high rigidity of the present invention, its feature are：Purity is not less than
99.9% pure boron powder is fitted into precompressed in graphite jig, is then placed in again in discharge plasma sintering system, and step applies 20
3~10min is incubated after being heated to 1480~1630 DEG C while~50MPa axial compressive force with 50~150 DEG C/min, to boron powder
Consolidation is carried out, that is, obtains the high rigidity high purity boron target that consistency is not less than 92%.Specifically comprise the following steps：
Step 1,
From purity not less than pure boron powder of the 99.9%, particle diameter no more than 10 μm；
According to the size of required boron target, a certain amount of pure boron powder is weighed with standby；
Step 2,
Graphite jig is taken, weighted pure boron powder is loaded into graphite jig, then using hand-operated hydraulic press to dress
The graphite jig of good pure boron powder carries out precompressed, and pressure is 8~12MPa；
Step 3,
Graphite jig periphery after the prepressing wraps the thick carbon felts of 4~6mm, is then placed on discharge plasma sintering system
In the burner hearth of system, below 5Pa is evacuated to, is passed through DC pulse current, consolidation, process conditions are carried out to pure boron powder
For：
Axial compressive force：Step applies 20~50MPa axial compressive force；
Heating rate is 50~150 DEG C/min；
Sintering temperature is 1480~1630 DEG C；
Soaking time is 3~10min；
The high purity boron target of high-compactness high rigidity is obtained after furnace cooling.
Preferably, the method for 20~50MPa of step application axial compressive force is：When temperature≤1000 DEG C, axially
Pressure is 20MPa；Work as temperature>At 1000 DEG C, axial compressive force 50MPa.
Advantages of the present invention is embodied in：
1st, the present invention uses discharge plasma sintering technique consolidation high-compactness, high rigidity, fine microstructures uniform
High purity boron target, technique is simple, the cycle is short, cost is low；Gained boron target through follow-up a small amount of grinding can finished product and be used for core
The sputter coating in the fields such as physics, laser physics and functional glass, has a extensive future.
2nd, the present invention has given full play to the advantage of the manufacturing process, and it is equal not less than 92%, fine microstructures to have manufactured consistency
Even high rigidity high-purity pure boron target；The manufacturing process of the present invention can be promoted for manufacturing mixing boron target or other are nonmetallic
Simple substance or mixing target.
Embodiment
By following examples, the invention will be further described, but embodiments of the present invention are not limited only to this.
It is in the following embodiments 4N level high purity elemental boron powder from purity, boron powder footpath is less than 10 μm.
Discharge plasma sintering stove used in following embodiments is the LABOX systems of Japanese Sinter Land Inc companies production
Row discharge plasma sintering system, its current type are DC pulse current, pulse train 40:7.
Embodiment 1
The high purity elemental boron target of the present embodiment high-compactness high rigidity is carried out as follows：
Step 1, weigh 3.6g pure boron powder；
Step 2, weighted boron powder is loaded into graphite jig, between the inwall of boron powder and graphite former and boron powder
Separated, then the graphite jig for installing boron powder is carried out using hand-operated hydraulic press pre- using flexible carbon paper between upper and lower pressure head
Pressure, pressure are~10MPa；
Step 3, graphite jig periphery after the prepressing wrap~thick 5mm carbon felt, then it is placed on plasma discharging
In the burner hearth of sintering system, below 5Pa is evacuated to, is passed through DC pulse current, consolidation, process conditions are carried out to boron powder
For：
Axial compressive force is that (room temperature is to 1000 DEG C by 20~50MPa：20MPa；Higher than 1000 DEG C：50MPa)；
Heating rate is 150 DEG C/min；
Sintering temperature is 1630 DEG C；
Soaking time is 3min；
Φ 20mm × 5mm high purity elemental boron target disk is obtained after furnace cooling, its density is 2.20g/cm3It is (fine and close
Spend for 94.0%), fine microstructures are uniform, hardness is HRA 82.7 ± 1.9.
Embodiment 2
The high purity elemental boron target of the present embodiment high-compactness high rigidity is carried out as follows：
Step 1, weigh 46.8g pure boron powder；
Step 2, weighted boron powder is loaded into graphite jig, between boron powder and graphite former inwall and boron powder with
Separated between upper and lower pressure head using flexible carbon paper, precompressed then carried out to the graphite jig for installing boron powder using hand-operated hydraulic press,
Pressure is~10MPa；
Step 3, graphite jig periphery after the prepressing wrap~thick 5mm carbon felt, then it is placed on plasma discharging
In the burner hearth of sintering system, below 5Pa is evacuated to, is passed through DC pulse current, consolidation, process conditions are carried out to boron powder
For：
Axial compressive force is that (room temperature is to 1000 DEG C by 20~50MPa：20MPa；Higher than 1000 DEG C：50MPa)；
Heating rate is 100 DEG C/min；
Sintering temperature is 1530 DEG C；
Soaking time is 8min；
50mm × 50mm × 8mm high purity elemental boron target disk is obtained after furnace cooling, its density is 2.18g/cm3
(consistency 93.2%), fine microstructures are uniform, and hardness is HRA 81.6 ± 1.4.
Embodiment 3
The high purity elemental boron target of the present embodiment high-compactness high rigidity is carried out as follows：
Step 1, weigh 275.0g pure boron powder；
Step 2, weighted boron powder is loaded into graphite jig, between boron powder and graphite former inwall and boron powder with
Separated between upper and lower pressure head using flexible carbon paper, precompressed then carried out to the graphite jig for installing boron powder using hand-operated hydraulic press,
Pressure is~10MPa；
Step 3, graphite jig periphery after the prepressing wrap~thick 5mm carbon felt, then it is placed on plasma discharging
In the burner hearth of sintering system, below 5Pa is evacuated to, is passed through DC pulse current, consolidation, process conditions are carried out to boron powder
For：
Axial compressive force is that (room temperature is to 1000 DEG C by 20~50MPa：20MPa；Higher than 1000 DEG C：50MPa)；
Heating rate is 50 DEG C/min；
Sintering temperature is 1480 DEG C；
Soaking time is 10min；
Φ 100mm × 15mm high purity elemental boron target disk is obtained after furnace cooling, its density is 2.17g/cm3(cause
Density is that 92.8%), fine microstructures are uniform, and hardness is HRA 81.3 ± 1.5.
Claims (4)
- A kind of 1. manufacture method of the high purity boron target of high-compactness high rigidity, it is characterised in that：Pure boron powder of the purity not less than 99.9% is fitted into precompressed in graphite jig, is then placed in discharge plasma sintering system again In system, step is incubated after being heated to 1480~1630 DEG C while applying 20~50MPa axial compressive force with 50~150 DEG C/min 3~10min, consolidation is carried out to boron powder, that is, obtains the high rigidity high purity boron target that consistency is not less than 92%.
- 2. manufacture method according to claim 1, it is characterised in that comprise the following steps：Step 1,From purity not less than pure boron powder of the 99.9%, particle diameter no more than 10 μm；According to the size of required boron target, the pure boron powder of constant weight is weighed with standby；Step 2,Graphite jig is taken, weighted pure boron powder is loaded into the graphite jig；Then using hand-operated hydraulic press to dress The graphite jig of good pure boron powder carries out precompressed, and pressure is 8~12MPa；Step 3,Graphite jig periphery after the prepressing wraps the thick carbon felts of 4~6mm, is then placed on discharge plasma sintering system In burner hearth, below 5Pa is evacuated to, is passed through DC pulse current, consolidation is carried out to pure boron powder, process conditions are：Axial compressive force：Step applies 20~50MPa axial compressive force；Heating rate is 50~150 DEG C/min；Sintering temperature is 1480~1630 DEG C；Soaking time is 3~10min；The high purity boron target of high-compactness high rigidity is obtained after furnace cooling.
- 3. manufacture method according to claim 1 or 2, it is characterised in that：The step applies 20~50MPa axial direction pressure The method of power is：When temperature≤1000 DEG C, axial compressive force 20MPa；Work as temperature>At 1000 DEG C, axial compressive force 50MPa.
- 4. manufacture method according to claim 1 or 2, it is characterised in that：The size of manufactured high purity boron target is：Directly Footpath or length and width are not less than 5mm not less than 20mm, thickness.
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| CN201710765712.6A CN107557738A (en) | 2017-08-30 | 2017-08-30 | A kind of manufacture method of the high purity boron target of high-compactness high rigidity |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108274009A (en) * | 2018-02-08 | 2018-07-13 | 合肥工业大学 | A kind of restorative procedure of Cr targets |
| CN108817405A (en) * | 2018-07-12 | 2018-11-16 | 合肥工业大学 | A kind of restorative procedure of W target |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103567440A (en) * | 2013-08-15 | 2014-02-12 | 厦门虹鹭钨钼工业有限公司 | Preparation method for tungsten carbide target material for film coating of oil exploration drill bit |
| CN106498205A (en) * | 2016-12-13 | 2017-03-15 | 合肥工业大学 | A kind of manufacture method of the CuCr alloys of large scale high-compactness high uniformity |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103567440A (en) * | 2013-08-15 | 2014-02-12 | 厦门虹鹭钨钼工业有限公司 | Preparation method for tungsten carbide target material for film coating of oil exploration drill bit |
| CN106498205A (en) * | 2016-12-13 | 2017-03-15 | 合肥工业大学 | A kind of manufacture method of the CuCr alloys of large scale high-compactness high uniformity |
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| 易丹青等: "《金属硅化物》", 30 September 2012, 冶金工业出版社 * |
| 林其壬: "《铁氧体工作原理》", 30 April 1987, 上海科学技术出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108274009A (en) * | 2018-02-08 | 2018-07-13 | 合肥工业大学 | A kind of restorative procedure of Cr targets |
| CN108817405A (en) * | 2018-07-12 | 2018-11-16 | 合肥工业大学 | A kind of restorative procedure of W target |
| CN108817405B (en) * | 2018-07-12 | 2020-12-29 | 合肥工业大学 | W target repairing method |
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