The preparation method of amorphous nano alloy composite powder material
Technical field
The present invention relates to a kind of interpolation composite powder and preparation method thereof for sintered metal product processing, particularly one
Plant the preparation method of the amorphous nano alloy composite powder material of utilization rate height, low cost, diffusion coefficient height, diffusion length length.
Background technology
Sintered metal product, because of its have power consumption less, cutting less, low cost, production efficiency advantages of higher, so in engineering
The mechanical industry fields such as machinery, agricultural machinery, electric tool, weaving, automobile are widely used.But due to domestic technique
Limited, compared with American-European countries, raw material, auxiliary agent moulding process in, however it remains certain gap.In many high-performance
In sintered metal product, the basic dependence on import of raw material, and domestic in metal powder process field, be substantially most basic simple also
The metal dusts such as former iron powder, atomized iron powder, alloyed powder.At present, in sintered metal product production technology, in order to improve powder smelting
The comprehensive physical performance of gold goods, often adds the valuable gold such as some Ni, Co, Mo, Nb, V, rare earth in the proportioning of powder metallurgy
Belong to simple substance or alloy powder.The deficiency adding the precious metal simple substance such as Ni, Co, Mo, Nb, V, rare earth or alloy powder is: one
It is that these precious metal powder price are expensive, improves the production cost of sintered metal product;Two is these precious metal powder
In the range of sintered metal product sintering temperature 1100 DEG C 1300 DEG C, diffusion coefficient is low, diffusion length is shorter, makes diffusibility
Can reduce, often produce segregation depositional phenomenon, thus reduce the comprehensive utilization ratio of metal material, not reach and give full play to its conjunction
The effect of aurification.Through retrieval, have not yet to see the amorphous nano alloy composite powder material added in sintered metal product
Report.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of amorphous nano alloy composite powder material, it is utilized in
Be uniform-distribution with on noncrystal substrate in-situ reducing out, there is the nano-metal particle of specified particle size distribution and other are special
The method that function nano ceramic material is formed.
The preparation method of this amorphous nano alloy composite powder material, it is characterised in that: it includes following production stage system
Become:
(1), metal salt solution is produced: the metallic salt 7.45kgNi(NO containing Ni, Mo, La that will weigh3)2·
6H2O, 1.38kg(NH4)2Mo4O13·2H2O, 1.56kgLa(NO3)3·6H2O, puts in the container being filled with water and dissolves, Bian Jia
Enter, limit is stirred, and measures concentration of ordinary dissolution in time, when concentration of ordinary dissolution reaches 0.75mol/L, then stops adding, and adds aqueous solution weight
The surfactant of the 0.3% of amount, fully dissolves, stirring, i.e. prepares metal salt solution;Described surfactant selects
PEG1000。
(2) oxalic acid solution, is produced: weigh the oxalic acid 2.96kg than precious metal ion excess 5% in molar ratio, put into Sheng
Have in the container of water and dissolve, produce the oxalic acid solution that concentration is 0.4mol/L.
(3), oxalate precursor precipitate is produced: the oxalic acid solution that will prepare in (2nd) step, slow under stirring
In the metal salt solution prepared in slow addition (1st) step, and stir 30min, obtain suspension, then natural sedimentation 30min
After, carry out filtering, washing to PH neutrality, i.e. prepare oxalate precursor precipitate.
(4), the nano zircite in oxalate precursor precipitate and raw material and reduced iron powder mixing:
By the oxalate precursor precipitate prepared in (3rd) step and 7kg nano zircite that mean diameter is 50nm,
Put in the container being filled with water under stirring, be dispersed in water, disperse 20min, then ultrasonic disperse under 15KHz frequency
30min, adds in blender, is stirred, mixing speed 60 revs/min;Carrier material 300 mesh is added under stirring
90.8kg reduced iron powder, stirring mixing 8min, make total solid matters and water quality than controlling as 1:1.5.
(5), again precipitate and be dried: after 450g polyacrylamide is first dissolved in 50kg water in advance, being slowly added to (4th)
In mixture obtained in step, re-form precipitation, and make oxalate precursor precipitate and 7kg nano zircite with
The 90.8kg reduced iron powder of 300 mesh forms caking property precipitation, stops, natural subsidence 30min, filter-press dehydration after stirring 20min,
150 DEG C of vacuum drying 3.5h, make water content control below 1%;Wherein polyacrylamide is precipitant, and addition is solid-liquid thing
The 0.15% of matter total amount.
(6), the broken amorphous nano alloy composite powder material finished product for preparing of reduction: the dry matter that will prepare in (5th)
It is crushed to 50 mesh, loads reduction furnace, under the reducing atmosphere of nitrogen hydrogen mol ratio 1:3,850 DEG C of reductase 12 h;It is crushed to 400 mesh again,
It is 100kg amorphous nano alloy composite powder material finished product.
The ultimate principle of the preparation method of this amorphous nano alloy composite powder material is: be uniformly distributed on noncrystal substrate
In-situ reducing out, there are the nano-metal particle of specified particle size distribution, and other specific function nano ceramics materials
Material, the metal nano ceramic composite structures material of formation, after adding in sintered metal product, due to its granularity of nano-metal particle
Reaching nanoscale, under the effect of the nano effect of nano metal material, nano metal material has the sintering of 400-1000 DEG C
Temperature, has high diffusion velocity and alloying activity simultaneously, thus significantly improves the valuable gold such as Ni, Co, Mo, Nb, V, rare earth
Belong to the utilization rate of material.And nano-ceramic particle nano-oxide or the existence of nano nitride, one is can be non-
During brilliant diffusion alloy material reduction, disperse and regulate the grain graininess that precious metal material produces in reducing process;Two
In sintered metal product sintering circuit, nano ceramic material along iron powder or other alloy powders crystal boundary disperse and with gold
Belong to crystal grain to combine, form the effect of particle dispersion strengthening, thus improve the physical property of sintered metal product.
The beneficial effects of the present invention is: compared with the alloy powder material being currently used for powder metallurgy, not only have excellent
Different physical property, and low cost;It it is the Nanoalloy composite of a kind of brand-new Powder Metallurgy Industry.At powder metallurgy
In goods, adding the present invention, can improve the comprehensive physical performance of powder metallurgy, particularly excellent physical property, ratio is at powder
Metallurgical proportioning directly adds the precious metal simple substance such as Ni, Co, Mo, Nb, V, rare earth or alloy powder is compared, not only reduce
The production cost of sintered metal product, and can expand in the range of sintered metal product sintering temperature 1100 DEG C 1300 DEG C
Scattered coefficient is high, diffusion length is longer, makes diffusion improve, and has reached the mesh of the comprehensive physical performance improving sintered metal product
's.
Detailed description of the invention
Produce 100kg amorphous nano alloy composite powder material.First 7.45kgNi(NO is weighed by demand proportioning3)2·
6H2O, 1.38kg(NH4)2Mo4O13·2H2O, 1.56kgLa(NO3)3·6H2O;Oxalic acid 2.96kg;Mean diameter is 50nm's
7kg nano zircite;450g polyacrylamide;Granularity is the 90.8kg reduced iron powder of 300 mesh.
Its production stage is:
(1), metal salt solution is produced: the metallic salt 7.45kgNi(NO containing Ni, Mo, La that will weigh3)2·
6H2O, 1.38kg(NH4)2Mo4O13·2H2O, 1.56kgLa(NO3)3·6H2O, puts in the container being filled with water and dissolves, Bian Jia
Enter, limit is stirred, and measures concentration of ordinary dissolution in time, when concentration of ordinary dissolution reaches 0.75mol/L, then stops adding, and adds aqueous solution weight
The surfactant of the 0.3% of amount, fully dissolve, stirring, i.e. prepare metal salt solution;Described surfactant selects
PEG1000。
(2) oxalic acid solution, is produced: weigh the oxalic acid 2.96kg than precious metal ion excess 5% in molar ratio, put into Sheng
Have in the container of water and dissolve, produce the oxalic acid solution that concentration is 0.4mol/L.
(3), oxalate precursor precipitate is produced: the oxalic acid solution that will prepare in (2nd) step, slow under stirring
In the metal salt solution prepared in slow addition (1st) step, and stir 30min, obtain suspension, then natural sedimentation 30min
After, carry out filtering, washing to PH neutrality, i.e. prepare oxalate precursor precipitate.
(4), the nano zircite in oxalate precursor precipitate and raw material and reduced iron powder mixing:
By the oxalate precursor precipitate prepared in (3rd) step and 7kg nano zircite that mean diameter is 50nm,
Put in the container being filled with water under stirring, be dispersed in water, disperse 20min, then ultrasonic disperse under 15KHz frequency
30min, adds in blender, is stirred, mixing speed 60 revs/min;Carrier material 300 mesh is added under stirring
90.8kg reduced iron powder, stirring mixing 8min, make total solid matters and water quality than controlling as 1:1.5.
(5), again precipitate and be dried: after 450g polyacrylamide is first dissolved in 50kg water in advance, being slowly added to (4th)
In mixture obtained in step, re-form precipitation, and make oxalate precursor precipitate and 7kg nano zircite with
The 90.8kg reduced iron powder of 300 mesh forms caking property precipitation, stops, natural subsidence 30min, filter-press dehydration after stirring 20min,
150 DEG C of vacuum drying 3.5h, make water content control below 1%;Wherein polyacrylamide is precipitant, and addition is solid-liquid thing
The 0.15% of matter total amount.
(6), the broken amorphous nano alloy composite powder material finished product for preparing of reduction: the dry matter that will prepare in (5th)
It is crushed to 50 mesh, loads reduction furnace, under the reducing atmosphere of nitrogen hydrogen mol ratio 1:3,850 DEG C of reductase 12 h;It is crushed to 400 mesh again,
It is 100kg amorphous nano alloy composite powder material finished product.
The quality of the amorphous nano alloy composite powder material that this embodiment is produced, after testing, its technical specification is: nickel
Content 1.47%, molybdenum content 0.19%, lanthanum oxide content 0.56%, precious metal total amount is 2.22%;Nano oxidized zirconium content 7%;Remaining
Amount is ferrum;Nickel, molybdenum particle diameter 1000nm.
Four kinds of application modes are used to carry out comparative illustration below:
|
Fe surplus |
C:0.7% |
Cu:1.5% |
Amorphous nano alloy composite powder
Powder material: 2% |
Micro mist wax: 0.6% |
Self-control cutting agent 0.4% |
1 |
Atomized iron powder 5Kg |
35g |
75g |
100g |
30g |
20g |
2 |
Ibid |
Ibid |
Ibid |
Nikel powder 500 mesh |
Ibid |
Ibid |
3 |
Reduced iron powder 5Kg |
Ibid |
Ibid |
Ibid |
Ibid |
Ibid |
4 |
Ibid |
Ibid |
Ibid |
Nikel powder 500 mesh |
Ibid |
Ibid |
Above-mentioned dispensing is equivalent to U.S.'s powdered metallurgical material standard FN-208.
In table: atomized iron powder is Laigang LAP100.29;Reduced iron powder is Laigang FHY100.25;Graphite is Qingdao Hua Tai
800 mesh high-quality graphite powders;Copper powder is that FTD-2 electrolytic copper powder is ground in Beijing.
After above-mentioned four kinds of examination powder mix 30 minutes, require to prepare tensile sample according to GB/T7963-1987, high through 1120 DEG C
Temperature sintering is after 30 minutes, according to GB/T7964-1987 sintered metal materials (not including hard alloy) tensile testing at ambient temperature
Obtain a result (meansigma methods).
|
Density |
Hardness (HRB) |
Stretching (KN) |
1 |
6.75 |
67.2 |
17.8 |
2 |
6.76 |
63.6 |
15.75 |
3 |
6.68 |
71.3 |
16.6 |
4 |
6.69 |
68.5 |
15.50 |