CN1292866C - Nanometer nickel powder preparing process - Google Patents
Nanometer nickel powder preparing process Download PDFInfo
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- CN1292866C CN1292866C CNB2005100002949A CN200510000294A CN1292866C CN 1292866 C CN1292866 C CN 1292866C CN B2005100002949 A CNB2005100002949 A CN B2005100002949A CN 200510000294 A CN200510000294 A CN 200510000294A CN 1292866 C CN1292866 C CN 1292866C
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 13
- 208000032544 Cicatrix Diseases 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 231100000241 scar Toxicity 0.000 claims description 6
- 230000037387 scars Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 abstract description 7
- 239000002244 precipitate Substances 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract description 3
- 239000012190 activator Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 235000017550 sodium carbonate Nutrition 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000004663 powder metallurgy Methods 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 21
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 17
- 229910052708 sodium Inorganic materials 0.000 description 17
- 241000209094 Oryza Species 0.000 description 15
- 235000007164 Oryza sativa Nutrition 0.000 description 15
- 235000009566 rice Nutrition 0.000 description 15
- 239000012153 distilled water Substances 0.000 description 12
- 239000013078 crystal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005352 clarification Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 230000002500 effect on skin Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention belongs to the field of powder metallurgy. No relevant reports on the research of nanometer nickel powder preparation by the freeze drying technology exist at home at abroad up to now. The present invention is characterized in that the present invention comprises: a nickel nitrate Ni (NO) 2.6H2O solution is mixed with a sodium carbonate Na2CO3 solution to obtain precipitates which are washed and then dissolved in ammonia water to obtain a clear solution; a universal nitrogen lance is used for dispersing the clear solution in universal liquid nitrogen to be prefreezed; congelation prefreezed in the liquid nitrogen is put in a freezedryer for vacuum drying to obtain precursors; dried precursors are treated by two times of hydrogen reduction, the hydrogen flow rate is 0.1 to 0.3 m3 / hr, the first reduction is carried out at the temperature of 100 to 160 DEG C, and the temperature is preserved for 1 to 7 hours; for the second reduction, the temperature is raised to 140 to 200 DEG C and preserved for 2 to 6 hours. Nanometer nickel powder has broad application prospects in the aspects of catalysts, sintering activators, electrocondution slurry, batteries, hard alloys, etc.
Description
Technical field
A kind of preparation method of sodium rice nickel powder belongs to powder metallurgical technology.
Background technology
Nickel is that a kind of argenteous metal has magnetic, electric conductivity and better chemical stability, high-temperature stability, mechanical stability.Sodium rice nickel powder has great skin effect and bulk effect because surface-active height, surperficial purity height, pore-free infiltration, specific area are big, is a kind of hydrogenation catalyst of novel, efficient, high selectivity.Owing to have magnetic property, sodium rice nickel powder can be used as magnetic material; Sodium rice nickel powder has good wetability and good suppression performance, sintering character to metal carbides (as WC, TiC, TaC etc.) and graphite etc. in addition, thereby is a kind of important carbide alloy and diamond carcass binding metal dusty material; Sodium rice nickel powder has good electrical conductivity, and cost is low, is widely used in electrocondution slurry, multilayer ceramic capacitor and nickel-cadmium cell etc.Therefore sodium rice nickel powder has broad application prospects at aspects such as catalyst, sintering activator, electrocondution slurry, battery, carbide alloy.
There are abundant nickel resources and powerful smelting ability in China.The growth momentum of automobile, electronics, machinery, information industry attracts people's attention, and the application of nickel powder is constantly widened.If can be at nickel powder particularly in the preparation of extra-fine nickel powder with use and get along with, to making full use of resource, increasing economic efficiency, shorten and developed country between gap all significant.
The result of literature survey shows that Freeze Drying Technique prepares the research of sodium rice nickel powder, does not also have relevant report so far both at home and abroad.
Summary of the invention
The preparation method of a kind of sodium rice nickel powder provided by the present invention, it is characterized in that: it may further comprise the steps:
(1) nickel nitrate solution is mixed with sodium carbonate liquor can obtain the precipitation, with its washing after, be dissolved in the ammoniacal liquor, settled solution;
(2) use general nitrogen spray gun, above-mentioned settled solution is dispersed in pre-freeze in the general liquid nitrogen;
(3) scars after the pre-freeze in the above-mentioned liquid nitrogen are placed freeze dryer carry out vacuum drying and obtain presoma;
(4) above-mentioned dried presoma is carried out the secondary hydrogen reducing, hydrogen flowing quantity is 0.1 cubic metre/hour～0.3 cubic metre/hour, for the first time 100 ℃～160 ℃ reduction, is incubated 1 hour～7 hours; For the second time be heated to 140 ℃～200 ℃, be incubated 2 hours～6 hours, obtain sodium rice nickel powder.
The described nitrogen spray gun of step (2), its pressure are 2 atmospheric pressure～5 atmospheric pressure; The described vacuum drying of step (3), wherein the performing a programme of freeze dryer is: the operating pressure in 0 minute～2500 minutes is that 300 millitorrs～400 millitorrs, temperature are-20 ℃-12 ℃; Operating pressure in 2500 minutes～3700 minutes is that 150 millitorrs～180 millitorrs, temperature are-11 ℃～-7 ℃; Operating pressure in 3700 minutes～4500 minutes is that 80 millitorrs～100 millitorrs, temperature are-3 ℃～0 ℃; Operating pressure in 4500 minutes～4700 minutes is that 0 millitorr～10 millitorrs, temperature are 15 ℃～25 ℃.
Wherein the technical parameter of spray gun pressure and freeze-drying program requires and can adjust accordingly according to initial concentration of solution and quantity.
The present invention adopts liquid nitrogen pre-freeze-freeze-drying, can prevent the segregation and the crystallization of solution component, obtains amorphous powder simultaneously.By twice reduction of low temperature, obtain the nickel powder of the crystallite dimension of sodium meter level again.
Can know that from the X diffracting spectrum of Fig. 1 the thing phase composition of final products only has nickel.
From the image of the field emission scanning electron microscope of Fig. 2 as can be seen, the powder size distribution that adopts the method for liquid nitrogen pre-freeze-freeze drying-hydrogen reducing to obtain is even, and particle is about the powder of 50nm.
Hence one can see that, and with the obvious refinement of powder crystal grain of desivac preparation, size reaches the sodium meter level, thereby can improve surface-active, surperficial purity, specific area, has great skin effect and bulk effect.
Description of drawings
Fig. 1: the sodium ground rice body X diffracting spectrum of preparation method's example 1 of the present invention;
Fig. 2: the sodium ground rice body FESEM picture of preparation method's example 1 of the present invention;
The specific embodiment
Example 1: get nickel nitrate green crystal [Ni (NO
3)
26H
2O] powder 50 gram is dissolved in 100 ml distilled waters and gets green settled solution; In addition with sodium carbonate [Na
2CO
3] powder 10 gram is dissolved in 50 ml distilled waters and gets colorless cleared solution; After treating two kinds of solution clarifications, mix both to such an extent that light green color precipitates.With sediment with distilled water washing 4 times after, be dissolved in 90 milliliters of ammoniacal liquor, the navy blue settled solution.Use the nitrogen spray gun, spray gun pressure is 5 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0～2500 minute is that 300 millitorrs, temperature are-12 ℃; Operating pressure in 2500～3700 minutes is that 150 millitorrs, temperature are-11 ℃; Operating pressure in 3700～4500 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 4500～4700 minutes is that 0 millitorr, temperature are 15 ℃; Presoma to freeze-drying is carried out secondary reduction.Adopt hydrogen reducing, hydrogen flowing quantity is 0.3 cubic metre/hour, for the first time 100 ℃ of reduction, is incubated 7 hours; For the second time be heated to 200 ℃, be incubated 4 hours, obtaining crystallite dimension is the sodium rice nickel powder of 73.5nm.
Example 2: get nickel nitrate green crystal [Ni (NO
3)
26H
2O] powder 50 gram is dissolved in 100 ml distilled waters and gets green settled solution; In addition with sodium carbonate [Na
2CO
3] powder 10 gram is dissolved in 50 ml distilled waters and gets colorless cleared solution; After treating two kinds of solution clarifications, mix both to such an extent that light green color precipitates.With sediment with distilled water washing 4 times after, be dissolved in 90 milliliters of ammoniacal liquor, the navy blue settled solution.Use the nitrogen spray gun, spray gun pressure is 4 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0～2500 minute is that 350 millitorrs, temperature are-20 ℃; Operating pressure in 2500～3700 minutes is that 180 millitorrs, temperature are-10 ℃; Operating pressure in 3700～4500 minutes is that 100 millitorrs, temperature are-3 ℃; Operating pressure in 4500～4700 minutes is that 8 millitorrs, temperature are 25 ℃; Presoma to freeze-drying is carried out secondary reduction.Adopt hydrogen reducing, hydrogen flowing quantity is 0.2 cubic metre/hour, for the first time 120 ℃ of reduction, is incubated 4 hours; For the second time be heated to 140 ℃, be incubated 6 hours, obtaining crystallite dimension is the sodium rice nickel powder of 35.8nm.
Example 3: get nickel nitrate green crystal [Ni (NO
3)
26H
2O] powder 50 gram is dissolved in 100 ml distilled waters and gets green settled solution; In addition with sodium carbonate [Na
2CO
3] powder 10 gram is dissolved in 50 ml distilled waters and gets colorless cleared solution; After treating two kinds of solution clarifications, mix both to such an extent that light green color precipitates.With sediment with distilled water washing 4 times after, be dissolved in 90 milliliters of ammoniacal liquor, the navy blue settled solution.Use the nitrogen spray gun, spray gun pressure is 2 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0～2500 minute is that 400 millitorrs, temperature are-15 ℃; Operating pressure in 2500～3700 minutes is that 170 millitorrs, temperature are-7 ℃; Operating pressure in 3700～4500 minutes is that 90 millitorrs, temperature are-1 ℃; Operating pressure in 4500～4700 minutes is that 5 millitorrs, temperature are 20 ℃; Presoma to freeze-drying is carried out secondary reduction.Adopt hydrogen reducing, hydrogen flowing quantity is 0.1 cubic metre/hour, for the first time 140 ℃ of reduction, is incubated 3 hours; For the second time be heated to 160 ℃, be incubated 3 hours, obtaining crystallite dimension is the sodium rice nickel powder of 47.8nm.
Example 4: get nickel nitrate green crystal [Ni (NO
3)
26H
2O] powder 50 gram is dissolved in 100 ml distilled waters and gets green settled solution; In addition with sodium carbonate [Na
2CO
3] powder 10 gram is dissolved in 50 ml distilled waters and gets colorless cleared solution; After treating two kinds of solution clarifications, mix both to such an extent that light green color precipitates.With sediment with distilled water washing 4 times after, be dissolved in 90 milliliters of ammoniacal liquor, the navy blue settled solution.Use the nitrogen spray gun, spray gun pressure is 3 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0～2500 minute is that 350 millitorrs, temperature are-18 ℃; Operating pressure in 2500～3700 minutes is that 160 millitorrs, temperature are-9 ℃; Operating pressure in 3700～4500 minutes is that 95 millitorrs, temperature are-2 ℃; Operating pressure in 4500～4700 minutes is that 10 millitorrs, temperature are 20 ℃; Presoma to freeze-drying is carried out secondary reduction.Adopt hydrogen reducing, hydrogen flowing quantity is 0.2 cubic metre/hour, for the first time 160 ℃ of reduction, is incubated 1 hour; For the second time be heated to 180 ℃, be incubated 2 hours, obtaining crystallite dimension is the sodium rice nickel powder of 62.5nm.
Claims (3)
1, a kind of preparation method of nano-nickel powder is characterized in that, it may further comprise the steps:
(1) nickel nitrate solution is mixed with sodium carbonate solution can obtain the precipitation, with its washing after, be dissolved in the ammoniacal liquor, settled solution;
(2) use general nitrogen spray gun, above-mentioned settled solution is dispersed in pre-freeze in the liquid nitrogen;
(3) scars after the pre-freeze in the above-mentioned liquid nitrogen are placed freeze dryer carry out vacuum drying and obtain presoma;
(4) above-mentioned dried presoma is carried out the secondary hydrogen reducing, hydrogen flowing quantity is 0.1 cubic metre/hour～0.3 cubic metre/hour, for the first time 100 ℃～160 ℃ reduction, is incubated 1 hour～7 hours; For the second time be heated to 140 ℃～200 ℃, be incubated 2 hours～6 hours, obtain nano-nickel powder.
2, Preparation Method of Nanometer nickel Ultrafine according to claim 1 is characterized in that: the described pre-freeze of step (2), and nitrogen spray gun wherein, its pressure is 2 atmospheric pressure～5 atmospheric pressure.
3, Preparation Method of Nanometer nickel Ultrafine according to claim 1, it is characterized in that: the described vacuum drying of step (3), wherein the performing a programme of freeze dryer is: the operating pressure in 0 minute～2500 minutes is that 300 millitorrs～400 millitorrs, temperature are-20 ℃～-12 ℃; Operating pressure in 2500 minutes～3700 minutes is that 150 millitorrs～180 millitorrs, temperature are-11 ℃～-7 ℃; Operating pressure in 3700 minutes～4500 minutes is that 80 millitorrs～100 millitorrs, temperature are-3 ℃～0 ℃; Operating pressure in 4500 minutes～4700 minutes is that 0 millitorr～10 millitorrs, temperature are 15 ℃～25 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100002949A CN1292866C (en) | 2005-01-10 | 2005-01-10 | Nanometer nickel powder preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100002949A CN1292866C (en) | 2005-01-10 | 2005-01-10 | Nanometer nickel powder preparing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1636655A CN1636655A (en) | 2005-07-13 |
| CN1292866C true CN1292866C (en) | 2007-01-03 |
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|---|---|---|---|
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100363134C (en) * | 2005-11-25 | 2008-01-23 | 北京科技大学 | Method for preparing nano nickel powder by precipitation-hydrogen reduction process |
| CN100374231C (en) * | 2006-04-06 | 2008-03-12 | 北京工业大学 | Preparation method of nano-cobalt powder |
| CN100441348C (en) * | 2006-05-12 | 2008-12-10 | 天津大学 | Metal nano nickel tube and preparation method thereof |
| JP5828923B2 (en) * | 2014-01-30 | 2015-12-09 | 国立大学法人高知大学 | Method for producing nickel powder |
| JP6099601B2 (en) * | 2014-02-17 | 2017-03-22 | 国立大学法人高知大学 | Method for producing nickel powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215639A (en) * | 1997-10-29 | 1999-05-05 | 中国科学院化学研究所 | Method for mfg. nm metal cluster |
| JPH11335709A (en) * | 1998-05-21 | 1999-12-07 | Sakai Chem Ind Co Ltd | Production of fine spherical powder of metal nickel |
| CN1381328A (en) * | 2001-04-18 | 2002-11-27 | 中国科学院化工冶金研究所 | Process for preparing superfine (nano) metal powder by hydrogen reduction of polyol |
| CN1387583A (en) * | 1999-11-09 | 2002-12-25 | 奥托库姆普联合股份公司 | Method for reduction of nickel from aqueous solution |
| CN1442259A (en) * | 2003-04-09 | 2003-09-17 | 北京工业大学 | Nano-rare earth tungsten powder and its preparation method |
-
2005
- 2005-01-10 CN CNB2005100002949A patent/CN1292866C/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215639A (en) * | 1997-10-29 | 1999-05-05 | 中国科学院化学研究所 | Method for mfg. nm metal cluster |
| JPH11335709A (en) * | 1998-05-21 | 1999-12-07 | Sakai Chem Ind Co Ltd | Production of fine spherical powder of metal nickel |
| CN1387583A (en) * | 1999-11-09 | 2002-12-25 | 奥托库姆普联合股份公司 | Method for reduction of nickel from aqueous solution |
| CN1381328A (en) * | 2001-04-18 | 2002-11-27 | 中国科学院化工冶金研究所 | Process for preparing superfine (nano) metal powder by hydrogen reduction of polyol |
| CN1442259A (en) * | 2003-04-09 | 2003-09-17 | 北京工业大学 | Nano-rare earth tungsten powder and its preparation method |
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|---|---|
| CN1636655A (en) | 2005-07-13 |
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