CN206263264U - The equipment that a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder - Google Patents
The equipment that a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder Download PDFInfo
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- CN206263264U CN206263264U CN201621259009.5U CN201621259009U CN206263264U CN 206263264 U CN206263264 U CN 206263264U CN 201621259009 U CN201621259009 U CN 201621259009U CN 206263264 U CN206263264 U CN 206263264U
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- Prior art keywords
- logical
- liquid nitrogen
- ball milling
- ball
- temperature
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- 238000000498 ball milling Methods 0.000 title claims abstract description 53
- 239000000843 powder Substances 0.000 title claims abstract description 44
- 230000003534 oscillatory effect Effects 0.000 title claims abstract description 16
- 238000001816 cooling Methods 0.000 title claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 80
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 24
- 230000001681 protective effect Effects 0.000 claims abstract description 22
- 239000011229 interlayer Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 239000012298 atmosphere Substances 0.000 abstract description 5
- 238000003801 milling Methods 0.000 abstract description 5
- 238000001125 extrusion Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 239000004411 aluminium Substances 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 239000012141 concentrate Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 102220043159 rs587780996 Human genes 0.000 description 4
- 238000012387 aerosolization Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002707 nanocrystalline material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
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Abstract
The utility model is related to low temperature ball milling field, the equipment that specially a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder.The equipment includes：Logical protective gas pipeline, logical liquid nitrogen pipeline, temperature feedback circuit, pressure feedback line, ball grinder, spring, eccentric wheel, main shaft, pressure inside the tank and temperature control system; and motor, liquid nitrogen and protective gas source etc.; nanocrystalline powder is prepared using the method for oscillatory type ball milling combination liquid nitrogen refrigerating; raw material granularity is 5~50 μm, the commercial gas-atomised powders of 0.5~5 μm of crystallite dimension.It is different from existing planetary, stirring type low temperature ball-grinding machine, the ball milling principle of the equipment is so that vibration-extrusion is broken, based on compacting, and can flexibly control milling atmosphere, granularity, morphology controllable are prepared in a short time by adjusting ball milling parameter, and the nanocrystalline powder of high thermal stability that size distribution is concentrated.
Description
Technical field：
The utility model is related to the oscillatory type deep cooling ball milling of low temperature ball milling field, specially a kind of use liquid nitrogen refrigerating to prepare
The equipment of nanocrystalline powder.
Background technology：
Ball grinding technique (mechanical alloying) refer to metal or alloy powder ball milling be concentrated through powder granule and abrading-ball it
Between intensely impact for a long time, powder granule is iteratively produced cold welding, fracture, cause powder granule atoms permeating so that
Obtain a kind of Preparation Technique of Powders of alloying powder.
Ball grinding technique is also the important processing method for preparing non-equilibrium material, and metal-powder can be prepared by ball milling
Supersaturated solid solution, the alloy of disordering degree increase and intermetallic compound, amorphous and quasicrystalline alloy, metastable phase and nanocrystalline
Material.
Low temperature ball grinding technique significantly reduces the dynamic recovery energy in powder deformation process due to its relatively low operating temperature
Power.Face-centred cubic structure material is particularly useful for making, such as：The high thermal stability nanocrystalline powder of aluminium, copper, nickel and its alloy.
The advantage of low temperature ball milling includes：(1) compared with conventional ball mill, due to relatively low operating temperature and and during short ball milling
Between, the pollution of oxygen in air is greatly decreased；(2) relatively low operating temperature is conducive to broken toughness material cold welding product；(3) it is relatively low
Operating temperature reduce the dynamic recovery ability of material, significantly reduce by powder grain size be milled to nanoscale when
Between；(4) oxynitrides quantity and disperse degree in can improving material in the environment of liquid nitrogen, improve the thermally-stabilised of material
Property.
Utility model content
The purpose of this utility model is to provide the equipment that a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder, using shaking
The method of dynamic formula ball milling combination liquid nitrogen refrigerating realizes low temperature ball milling, relies on the characteristics of vibrating low temperature ball milling itself, prepares one kind
The high thermal stability nanocrystalline powder that granularity, morphology controllable, size distribution are concentrated.
The technical solution of the utility model is as follows：
A kind of equipment that oscillatory type deep cooling ball milling prepares nanocrystalline powder, the equipment includes：Logical protective gas pipeline, logical liquid
Nitrogen pipeline, pressure feedback line, temperature feedback circuit, pressure inside the tank and temperature control system, ball grinder, motor, main shaft,
Eccentric wheel, spring and liquid nitrogen and protective gas source, concrete structure are as follows：
Ball grinder is connected by logical protective gas pipeline, logical liquid nitrogen pipeline with liquid nitrogen and protective gas source respectively, described
Valve is respectively provided with logical protective gas pipeline, logical liquid nitrogen pipeline；Pressure feedback line, one end of temperature feedback circuit are connected to ball
Grinding jar, the other end of pressure feedback line is connected to the valve on logical protective gas pipeline, and the other end of temperature feedback circuit is connected to
Valve on logical liquid nitrogen pipeline, sets pressure inside the tank and temperature control system, in tank on pressure feedback line, temperature feedback circuit
The pressure and temperature signal of pressure and temperature control system in ball grinder, control pressure feedback line, temperature feedback circuit
The aperture of upper valve and keying；
Ball grinder is rigidly connected with main shaft, and main shaft is connected with motor, eccentric wheel is set on main shaft and one end is connected and consolidated
Fixed spring.
The equipment that described oscillatory type deep cooling ball milling prepares nanocrystalline powder, the shell of ball grinder sets logical nitrogen interlayer, leads to
Liquid nitrogen pipeline point two-way, is connected in ball grinder all the way, and another road is connected in logical nitrogen interlayer.
Advantage of the present utility model and beneficial effect are：
1st, the utility model uses oscillatory type low temperature ball-grinding machine, and the nanocrystalline aluminium powder of preparation has higher thermally-stabilised
Property.
2nd, the utility model can with prepared sizes distribution concentrate etc. the nanocrystalline aluminium powder of shaft-like, and precise control powder grain
Degree scope (D50=15~500 μm).
3rd, the utility model can prepare two-dimensional slice that thickness is 100~200nm into the nanocrystalline aluminium powder of shape.
Brief description of the drawings
Fig. 1 is oscillatory type deep cooling ball-grinding machine schematic diagram.In figure, 1 logical protective gas pipeline；2 logical liquid nitrogen pipelines；3 pressure
Feedback line；4 temperature feedback circuits；5 pressure inside the tanks and temperature control system；6 ball grinders；7 motors；8 main shafts；9 is eccentric
Wheel；10 springs.
Specific embodiment
As shown in figure 1, the equipment that the utility model oscillatory type deep cooling ball milling prepares nanocrystalline powder, by vibrating device, many
Function ball grinder, external auxiliary control system composition, realize low temperature ball milling, equipment master by oscillatory type ball milling combination liquid nitrogen refrigerating
Including：Logical protective gas pipeline 1, logical liquid nitrogen pipeline 2, pressure feedback line 3, temperature feedback circuit 4, pressure inside the tank and temperature
Control system 5, ball grinder 6, motor 7, main shaft 8, eccentric wheel 9, spring 10 and liquid nitrogen and protective gas source etc., concrete structure
It is as follows：
Ball grinder 6 is connected by logical protective gas pipeline 1, logical liquid nitrogen pipeline 2 with liquid nitrogen and protective gas source respectively, in institute
State and be respectively provided with valve on logical protective gas pipeline 1, logical liquid nitrogen pipeline 2；One end of pressure feedback line 3, temperature feedback circuit 4
Ball grinder 6 is connected to, the other end of pressure feedback line 3 is connected to the valve on logical protective gas pipeline 1, temperature feedback circuit 4
The other end is connected to the valve on logical liquid nitrogen pipeline 2, and pressure inside the tank and temperature are set on pressure feedback line 3, temperature feedback circuit 4
Control system 5, the pressure and temperature signal of pressure inside the tank and temperature control system 5 in ball grinder 6, control pressure feedback line
The aperture of valve and keying on road 3, temperature feedback circuit 4.
Ball grinder 6 is rigidly connected with main shaft 8, and main shaft 8 is connected with motor 7, and eccentric wheel 9 is set on main shaft 8；Spring 10
One end fix, the other end of spring 10 connection main shaft 8.
The shell of ball grinder 6 sets logical nitrogen interlayer, leads to liquid nitrogen 2 points of two-way of pipeline, is connected to all the way in ball grinder 6, Ling Yilu
It is connected in the logical nitrogen interlayer of ball grinder 6.
It is as follows that the utility model prepares the adjustable technological parameter of nanocrystalline powder using the said equipment：Liquid nitrogen atmosphere or guarantor
Ball milling under shield gas atmosphere, ball milling temperature is in room temperature to -196 DEG C of scope adjustment, ball milling 2~8mm of amplitude, vibration frequency 50Hz.
Also, by adjusting Material quality of grinding balls, size, and process control agent addition, ball material mass ratio and fill factor etc., Neng Goujing
The high thermal stability manocrystalline powders that the granularity of milling body, prepared sizes, morphology controllable, and size distribution are concentrated are received in really control.
Particularly, the utility model can be in normal temperature to freely controlling ball milling in the range of -196 DEG C by adjusting liquid nitrogen flow
Temperature；The utility model can control ball milling amplitude and vibration frequency by adjusting eccentric wheel angle, quality and motor power
Rate.The utility model can irrigate liquid nitrogen with ball milling in ball grinder, or liquid nitrogen refrigerating is filled in tank outside sandwich, and in tank
The protective gas of certain pressure is filled with ball milling, freely controlling for milling atmosphere is realized.
Below, the utility model is further elaborated on by embodiment.
Embodiment 1
In the present embodiment, ball milling initial grain size is about 1~5 μm of commercial aerosolization aluminium powder.- 180 DEG C of ball milling temperature,
Ball milling amplitude 5mm, vibration frequency 50Hz, Ball-milling Time 2 hours, using stainless steel abrading-ball, ball material mass ratio 10:1, add stearic
Acid amount is abrasive material quality 2%, prepares two-dimensional slice that thickness is 100~200nm into shape nanocrystalline powder, and crystallite dimension is about
35nm。
Embodiment 2
In the present embodiment, ball milling initial grain size is about 1~5 μm of commercial aerosolization aluminium powder.- 180 DEG C of ball milling temperature,
Ball milling amplitude 6mm, vibration frequency 50Hz, Ball-milling Time 4 hours, using stainless steel abrading-ball, ball material mass ratio 10:1, adjust abrading-ball
Can be prepared after size size distribution concentrate, D50 in 15~500 μ ms precise control etc. shaft-like nanocrystalline powder,
Crystallite dimension is about 50nm.
Embodiment 3
In the present embodiment, ball milling initial grain size is about 1~5 μm of commercial aerosolization aluminium powder.- 180 DEG C of ball milling temperature,
Ball milling amplitude 4mm, vibration frequency 50Hz, Ball-milling Time 2 hours, using stainless steel abrading-ball, ball material mass ratio 10:1, adjust abrading-ball
Can be prepared after size size distribution concentrate, D50 in 15~500 μ ms precise control etc. shaft-like Ultra-fine Grained powder,
Crystallite dimension is about 200nm.
It is in micro-meter scale, two-dimensional slice in two dimensions using the two-dimensional slice of the utility model ball milling preparation into shape powder
Thickness into shape powder is about 100~200nm.
Using prepared by the utility model ball milling D50=400 μm and D50=100 μm of nanocrystalline powder, in equiaxial piece
Shape, concentrates with good mobility and Pneumatic acceleration effect, and size distribution.
The TEM diffraction patterns for using D50=400 μm of nanocrystalline powder of the utility model ball milling preparation are annular, are allusion quotations
The nanocrystalline structure diffraction pattern of type, the average grain size of powder is about 50nm.
Embodiment result is shown, is freezed using oscillatory type ball-milling technology combination liquid nitrogen (liquid nitrogen) and realize oscillatory type low temperature ball milling
Powder processed, is different from existing planetary, stirring type low temperature ball-grinding machine, and the ball milling principle of the equipment is crushed with vibration-extrusion, rammed
Actually lead, and can flexibly control milling atmosphere.It is thus possible to pass through to adjust ball milling parameter prepare in a short time granularity,
Morphology controllable, and size distribution concentrate high thermal stability nanocrystalline powder.Can be selected in protective gas in mechanical milling process
Ball milling in atmosphere, to reduce the pollution of oxygen, also may be selected the ball milling in liquid nitrogen atmosphere, make to be contained Dispersed precipitate by milling body
Nitrogen oxides, strengthen powder stability.
Claims (2)
1. the equipment that a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder, it is characterised in that：The equipment includes：Logical protective gas
Pipeline, logical liquid nitrogen pipeline, pressure feedback line, temperature feedback circuit, pressure inside the tank and temperature control system, ball grinder, driving
Motor, main shaft, eccentric wheel, spring and liquid nitrogen and protective gas source, concrete structure are as follows：
Ball grinder is connected by logical protective gas pipeline, logical liquid nitrogen pipeline with liquid nitrogen and protective gas source respectively, in the logical guarantor
Valve is respectively provided with shield gas piping, logical liquid nitrogen pipeline；Pressure feedback line, one end of temperature feedback circuit are connected to ball milling
Tank, the other end of pressure feedback line is connected to the valve on logical protective gas pipeline, and the other end of temperature feedback circuit is connected to logical
Valve on liquid nitrogen pipeline, sets pressure inside the tank and temperature control system, tank internal pressure on pressure feedback line, temperature feedback circuit
The pressure and temperature signal of power and temperature control system in ball grinder, on control pressure feedback line, temperature feedback circuit
The aperture of valve and keying；
Ball grinder is rigidly connected with main shaft, and main shaft is connected with motor, and eccentric wheel is set on main shaft and one end fixation is connected
Spring.
2. the equipment for preparing nanocrystalline powder according to the oscillatory type deep cooling ball milling described in claim 1, it is characterised in that：Ball grinder
Shell logical nitrogen interlayer is set, lead to liquid nitrogen pipeline point two-way, be connected in ball grinder all the way, another road is connected in logical nitrogen interlayer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621259009.5U CN206263264U (en) | 2016-11-23 | 2016-11-23 | The equipment that a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621259009.5U CN206263264U (en) | 2016-11-23 | 2016-11-23 | The equipment that a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206263264U true CN206263264U (en) | 2017-06-20 |
Family
ID=59040363
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201621259009.5U Expired - Fee Related CN206263264U (en) | 2016-11-23 | 2016-11-23 | The equipment that a kind of oscillatory type deep cooling ball milling prepares nanocrystalline powder |
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| Country | Link |
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| CN (1) | CN206263264U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106623951A (en) * | 2016-11-23 | 2017-05-10 | 中国科学院金属研究所 | Equipment and method for preparing nanocrystal powder through vibration type copious cooling ball milling |
| CN115194165A (en) * | 2022-09-14 | 2022-10-18 | 四川泽丰锂能新能源科技有限公司 | Low-temperature brittle metal powder grinding device |
-
2016
- 2016-11-23 CN CN201621259009.5U patent/CN206263264U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106623951A (en) * | 2016-11-23 | 2017-05-10 | 中国科学院金属研究所 | Equipment and method for preparing nanocrystal powder through vibration type copious cooling ball milling |
| CN115194165A (en) * | 2022-09-14 | 2022-10-18 | 四川泽丰锂能新能源科技有限公司 | Low-temperature brittle metal powder grinding device |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20170620 Termination date: 20201123 |