CN103223493B - Method for preparing target-used Ru (ruthenium) powder - Google Patents
Method for preparing target-used Ru (ruthenium) powder Download PDFInfo
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Abstract
The invention provides a method for preparing target-used Ru powder and relates to the technical field of precious metal powder production. The method for preparing the target-used Ru powder comprises the steps as follows; 1) solvation, 2) precipitation, 3) centrifugal filtration, 4) drying, 5) crushing, 6) calcination, 7) reduction and 8) powder preparation. Through the inventive method, the iron, carbon, sodium and potassium element contents of the Ru powder are respectively smaller than 10ppm, the nitrogen and chlorine element contents are respectively smaller than 50ppm, and the total impurity which does not contain gas elements is smaller than 100ppm. The Ru powder has the granularity smaller than 4mum, a standard spherical shape, the tap density ranging from 3.2 to 4.0g/cm<3>, and the apparent density raging from 2 to 2.6g/cm<3>. The (NH4)2RuCl6(IV) is separated from impurities, and the purity of the (NH4)2RuCl6(IV) is improved.
Description
Technical field
The present invention relates to the production of noble metal powder, more specifically relate to the production of the special ruthenium powder of target.
Background technology
Along with the develop rapidly of information and computer technology, the demand of hard disc of computer memory material target ruthenium powder is increasing.Target ruthenium powder has special index request, and iron carbon sodium and kalium element content is less than 10ppm respectively, and nitrogen content of Cl element is less than 50ppm respectively, and total impurities not air inclusion element is less than 100ppm.Ruthenium Powder Particle Size is less than 4um, and pattern is regular spherical, tap density 3.2 ~ 4.0g/cm
3, apparent density 2 ~ 2.6g/cm
3.
Current domestic general employing H
2sO
4+ NaClO
3twice oxidation distillation, absorbing liquid condensing crystallizing obtains RuCl
3calcining hydrogen reduction RuCl
3crystal production ruthenium powder, the ruthenium powder particles produced is thick, and uneven, can not be used for the production of target.
Patent CN1926252A discloses a kind of preparation method of high-purity Ru powder, each alkali-metal content such as ruthenium powder Na, K of preparation are all at below 10ppm, the content of Al is 1 ~ 50ppm, method makes anode by purity at 3N (99.9%) Ru raw material below, electrolytic refining in the solution, the pure ruthenium powder of more than 4N (99.99%) can be prepared, be applicable to the capacitor electrode material forming semiconductor memory.The method is only applicable to the electrorefining of thick ruthenium powder, and object mainly removes Na, K and Al impurity, can not change granularity and the pattern of ruthenium powder.
Patent CN1911572A discloses a kind of method preparing the ruthenium powder of high-quality from the solution containing ruthenium efficiently, the method prepares in the step of ruthenium powder at calcining ammonium hexachlororuthenate, pulverize calcining the thick ruthenium that ammonium hexachlororuthenate obtains at 500 ~ 800 DEG C, then again calcine at 800 ~ 1000 DEG C, make the chlorinity in ruthenium powder be 100 ppm or following thus.Utilize ammonium chloride Direct precipitation Ru (III), produce (NH
4)
3ruCl
6, calcining reduction (NH
4)
3ruCl
6obtain ruthenium powder, the ruthenium powder obtained like this is thinner, and need through twice high-temperature calcination, complicated operation cost also increases; And (NH
4)
3ruCl
6water-soluble very large, not exclusively, the rate of recovery of ruthenium is not high, the most important thing is the higher production that can not be used for target of impurity content for precipitation.
Patent CN101289229A discloses manufacture method and the ammonium hexachlororuthenate of a kind of ammonium hexachlororuthenate and ruthenium powder, its problem is that the ammonium hexachlororuthenate made adding ammonium chloride in the hydrochloric acid solution of ruthenium burns till when manufacturing ruthenium powder, makes moisture content be reduced to degree no problem comminuted.The present invention keeps the hydrochloric acid solution of ruthenium after more than 3 hours at 80 ~ 95 DEG C, make the revolution of mixer reach more than 200 turns per minute and carry out stirring while add ammonium chloride, while stir maintenance in more than 1 hour at 85 ~ 95 DEG C, generating the precipitation of ammonium hexachlororuthenate, obtaining by filtering the crystal that moisture content is the ammonium hexachlororuthenate of less than 10%.The tap density being prepared powder by this method is little, does not reach the requirement of target ruthenium powder.
Summary of the invention
For overcoming the above-mentioned deficiency of prior art, the invention provides a kind of technology maturation, process conditions less demanding production ruthenium target ruthenium powder producing method, object is that the iron carbon sodium and kalium element content realizing ruthenium powder is less than 10ppm respectively, nitrogen content of Cl element is less than 50ppm respectively, and total impurities not air inclusion element is less than 100ppm.Ruthenium Powder Particle Size is less than 4um, and pattern is regular spherical, tap density 3.2 ~ 4.0g/cm
3, apparent density 2 ~ 2.6g/cm
3.
The technical solution adopted for the present invention to solve the technical problems, a kind of method preparing target ruthenium powder, adopts following steps to realize:
1. dissolving: with the dissolving with hydrochloric acid solid ruthenium trichloride of 8 ~ 12mol/L, the amount adding hydrochloric acid makes the concentration of ruthenium at 45 ~ 55 grams per liters, generating (NH to containing adding ammonium chloride saturated solution in ruthenium solution
4)
3ruCl
6(III) amount of the ammonium chloride, added is 1.3 ~ 1.4 times of theoretical amount.
2. precipitate: heated solution reaches 90 ~ 100 DEG C, and the chlorine passing into 0.8 ~ 1 liter/min is oxidized, stir and obtain ruthenium hydrochloride ammonium (IV) precipitation, mixing speed is 60 ~ 90 revs/min, logical chlorine oxidation 1 ~ 4 hour, until ruthenium hydrochloride ammonium (IV) precipitation completely.
3. centrifugal filtration: above-mentioned sediment (NH
4)
2ruCl
6(IV) put into centrifuge centrifugal filtration 10 ~ 30 minutes, the rotating speed of centrifuge is 900 ~ 1000 revs/min.
4. dry: centrifugal anhydrate after (NH
4)
2ruCl
6(IV) oven dry is carried out 16 ~ 18 hours at 150 ~ 200 DEG C.
5. broken: (the NH of oven dry
4)
2ruCl
6(IV) in planetary ball mill, keep rotating speed 380 ~ 410 revs/min, broken 15 ~ 25 minutes, it was 18 ~ 22 minutes that the time is more optimized in fragmentation; Described planetary ball mill adopts ball grinder material to be polyurethane, and ball-milling medium is zirconia ball, ratio of grinding media to material 2.5 ~ 3.5:1.
6. calcine: (the NH after fragmentation
4)
2ruCl
6(IV) first 435 ~ 460 DEG C of temperature lower calcinations 2.5 ~ 3.5 hours, increase the temperature to 630 ~ 660 DEG C and continue calcinings 2.5 ~ 3.5 hours, then increase the temperature to 730 ~ 770 DEG C of calcinings 1.5 ~ 2.5 hours.
7. reduce: at 730 ~ 760 DEG C of temperature, logical hydrogen reduction 0.5 ~ 1.5 hour.
8. powder process: finally obtain pure ruthenium powder with planetary ball mill crusher machine again, keep rotating speed 380 ~ 410 revs/min of fragmentations 4 ~ 6 minutes in planetary ball mill.
Beneficial effect: the present invention carries out oxidation reaction by Ru(in solution by chlorine
) be oxidized to Ru(
), control the concentration of ruthenium at 45 ~ 55g/L, concentration of hydrochloric acid controls at 8 ~ 12mol/L simultaneously, and it is 60 ~ 90 revs/min that oxidizing temperature controls at 90 ~ 100 DEG C and mixing speed, can make (NH in solution under these conditions
4)
2ruCl
6(
) 99.9% can be precipitated out.Achieve (NH
4)
2ruCl
6(
) and magazins' layout, improve (NH
4)
2ruCl
6(
) purity.
(NH
4)
2ruCl
6(
) volume comparatively large, moisture higher, be difficult to moisture pump with ordinary porcelain funnel, cause impurity higher.Adopt centrifuge to filter the moisture content that can reduce ammonium salt as much as possible, reduce carrying secretly of impurity, also favourable to the oven dry of a rear step.
(NH
4)
2ruCl
6(IV) precipitation must dry ability fragmentation, and bake out temperature is moderate, and bake out temperature is too high, and ruthenium hydrochloride ammonium (IV) decomposes, and ruthenium powder ball gathers, can not be broken.Bake out temperature is too low, and ruthenium hydrochloride ammonium (IV) can stick on zirconia ball, and affect ball milling effect, drying time is long, and production efficiency is low.
By control ruthenium hydrochloride ammonium (
) to dry and the condition of twice fragmentation can reach target ruthenium powder to the requirement of granularity pattern, ruthenium hydrochloride ammonium (
) be that a kind of compound crystal is easier to fragmentation, so first carry out primary fragmentation before calcining, effectively reduce calcining heat, and make the ruthenium powder after calcining thinner, thus powder process crush strength after alleviating calcining, be just not easy to bring new impurity in powder crushing process process.The present invention's point syllogic controls calcining heat just can better obtain thinner ruthenium powder ball like this, because calcining heat is lower, ruthenium metal is not sintered, highly beneficial to follow-up flouring technology, the requirement that just can reach target ruthenium powder can not be pulverized because of needing high strength, thus can not again bring new impurity into.
Accompanying drawing explanation
Fig. 1 is process chart;
Fig. 2 is the shape appearance figure that embodiment 1 obtains ruthenium powder;
Fig. 3 is the shape appearance figure that embodiment 2 obtains ruthenium powder;
Fig. 4 is the shape appearance figure that embodiment 3 obtains ruthenium powder.
Detailed description of the invention
embodiment 1
As shown in Figure 1, get solid ruthenium trichloride 1000 grams, containing ruthenium 370 grams, by following technological operation:
1. dissolving: the solid ruthenium trichloride dissolving with hydrochloric acid of 7.4 liters of 8mol/L, makes the concentration of ruthenium at 50 grams per liters, generating (NH to containing adding ammonium chloride saturated solution in ruthenium solution
4)
3ruCl
6(III) amount of the ammonium chloride, added is 1.3 times of theoretical amount.
2. precipitate: heated solution, temperature 90 DEG C, the chlorine passing into 1 liter/min carries out being oxidized, stir and obtain (NH
4)
2ruCl
6(IV) precipitate, mixing speed is 80 revs/min, and the logical chlorine oxidation time is 2 hours, until ruthenium hydrochloride ammonium (IV) precipitation completely, filter to obtain ruthenium hydrochloride ammonium (IV) sediment, analyze mother liquor containing ruthenium 0.7 gram, the rate of deposition of ruthenium is 99.8%.
3. centrifugal filtration: above-mentioned sediment is put into centrifuge dehydration 20 minutes, the rotating speed of centrifuge is 950 revs/min.The volume that ruthenium hydrochloride ammonium (IV) precipitates is comparatively large, moisture higher, is difficult to moisture pump, causes impurity higher with ordinary porcelain funnel.Adopt centrifuge to filter the moisture content that can reduce ammonium salt as much as possible, reduce carrying secretly of impurity.Also favourable to the oven dry of a rear step.
4. dry: centrifugal anhydrate after ruthenium hydrochloride ammonium (IV) be deposited in 180 DEG C and carry out, dries 16 hours, acquisition (NH
4)
2ruCl
6(IV) 1223 grams are precipitated.
5. broken: the material of oven dry keeps rotating speed 400 revs/min of fragmentations 20 minutes in planetary ball mill, described planetary ball mill adopts ball grinder material to be polyurethane, ball-milling medium is zirconia ball, ratio of grinding media to material 3:1, and after broken, ruthenium hydrochloride ammonium (IV) is less than 80 orders.
6. calcine: ruthenium hydrochloride ammonium (IV) after fragmentation first 450 DEG C of temperature lower calcinations 3 hours, increases the temperature to 650 DEG C and continues calcinings 3 hours, then increase the temperature to 750 DEG C of calcinings 2 hours, obtain powdery ruthenium black.
7. reduce: at 750 DEG C of temperature, logical hydrogen reduction 1 hour, obtains sponge ruthenium powder.
8. powder process: finally obtain pure ruthenium powder with planetary ball mill crusher machine again, keep rotating speed 410 revs/min of fragmentations 5 minutes in planetary ball mill.Obtain 353.3 grams, pure ruthenium powder.Shape appearance figure as shown in Figure 2, has manufactured high performance ruthenium target with this ruthenium powder.
embodiment 2
As shown in Figure 1, get solid ruthenium trichloride 3000 grams, containing ruthenium 1110 grams, by following technological operation:
1. dissolving: the solid ruthenium trichloride dissolving with hydrochloric acid of 24.66 liters of 10mol/L, makes the concentration of ruthenium at 45 grams per liters, generating (NH to containing adding ammonium chloride saturated solution in ruthenium solution
4)
3ruCl
6(III) the ammonium chloride amount of being, added is 1.3 times of theoretical amount.
2. precipitate: heated solution, temperature 95 DEG C, the chlorine passing into 0.8 liter/min carries out being oxidized, stir and obtain (NH
4)
2ruCl
6(IV) precipitate, mixing speed is 70 revs/min, and the logical chlorine oxidation time is 2.5 hours, until ruthenium hydrochloride ammonium (IV) precipitation completely, filter to obtain ruthenium hydrochloride ammonium (IV) sediment, analyze mother liquor of precipitation of ammonium containing ruthenium 5.12 grams, rate of deposition is 99.5%.
3. centrifugal filtration: above-mentioned sediment is put into centrifuge dehydration 10 minutes, the rotating speed of centrifuge is 1000 revs/min.
4. dry: centrifugal anhydrate after ruthenium hydrochloride ammonium (IV) be deposited in 160 DEG C and carry out, dries 18 hours, acquisition (NH
4)
2ruCl
6(IV) 3362 grams are precipitated.(NH
4)
2ruCl
6(IV) precipitation must dry ability fragmentation.
5. broken: the material of oven dry keeps rotating speed 410 revs/min of fragmentations 18 minutes in planetary ball mill, described planetary ball mill adopts ball grinder material to be polyurethane, ball-milling medium is zirconia ball, ratio of grinding media to material 2.8:1, and after broken, ruthenium hydrochloride ammonium (IV) is less than 80 orders.
6. calcine: ruthenium hydrochloride ammonium (IV) after fragmentation first 440 DEG C of temperature lower calcinations 3.3 hours, improves temperature and continues calcinings 2.8 hours to 630 DEG C, then improve temperature to 730 DEG C of calcinings 1.7 hours, obtain powdery ruthenium black.
7. reduce: at 730 DEG C of temperature, logical hydrogen reduction 1.5 hours, obtains sponge ruthenium powder.
8. powder process: finally obtain pure ruthenium powder with planetary ball mill crusher machine again, keep rotating speed 380 revs/min of fragmentations 6 minutes in planetary ball mill.Obtain 1074.4 grams, ruthenium powder, shape appearance figure as shown in Figure 3, has manufactured high performance ruthenium target with this ruthenium powder.
embodiment 3
As shown in Figure 1, get solid ruthenium trichloride 6000 grams, containing ruthenium 2220 grams, by following technological operation:
1. dissolving: the solid ruthenium trichloride dissolving with hydrochloric acid of 40.36 liters of 8mol/L, makes the concentration of ruthenium at 55 grams per liters, generating (NH to containing adding ammonium chloride saturated solution in ruthenium solution
4)
3ruCl
6(III) amount of the ammonium chloride, added is 1.4 times of theoretical amount.
2. precipitate: heated solution, temperature 98 DEG C, the chlorine passing into 0.9 liter/min carries out being oxidized, stir and obtain (NH
4)
2ruCl
6(IV) precipitate, mixing speed is 90 revs/min, and the logical chlorine oxidation time is 3 hours, until ruthenium hydrochloride ammonium (IV) precipitation completely, filter to obtain ruthenium hydrochloride ammonium (IV) sediment, analyze mother liquor containing ruthenium 2.12 grams, the rate of deposition of ruthenium is 99.9%.
3. centrifugal filtration: above-mentioned sediment is put into centrifuge dehydration 30 minutes, the rotating speed of centrifuge is 900 revs/min.
4. dry: centrifugal anhydrate after ruthenium hydrochloride ammonium (IV) be deposited in 200 DEG C and carry out, dries 16 hours, acquisition (NH
4)
2ruCl
6(IV) 6914 grams are precipitated.(NH
4)
2ruCl
6(IV) precipitation must dry ability fragmentation.
5. broken: the material of oven dry keeps rotating speed 410 revs/min of fragmentations 22 minutes in planetary ball mill, described planetary ball mill adopts ball grinder material to be polyurethane, ball-milling medium is zirconia ball, ratio of grinding media to material 3.2:1, and after broken, ruthenium hydrochloride ammonium (IV) is less than 80 orders.
6. calcine: ruthenium hydrochloride ammonium (IV) after fragmentation first 455 DEG C of temperature lower calcinations 2.5 hours, improves temperature and continues calcinings 2.5 hours to 660 DEG C, then improve temperature to 770 DEG C of calcinings 1.5 hours, obtain powdery ruthenium black.
7. reduce: at 760 DEG C, logical hydrogen reduction 0.5 hour, obtains sponge ruthenium powder.
8. powder process: finally obtain pure ruthenium powder with planetary ball mill crusher machine again, keep rotating speed 410 revs/min in planetary ball mill, broken 4 minutes, obtain 2134.2 grams, ruthenium powder, shape appearance figure as shown in Figure 4, manufactured high performance ruthenium target with this ruthenium powder.
?
embodimentunder condition, chloride precipitation de-ferrous effect is as shown in table 1 below:
| Lot number | Iron content (being converted to ruthenium powder) ppm in solution | Iron content ppm in ruthenium powder | Clearance (%) |
| Embodiment 1 | 24.85 | 4.11 | 83.46 |
| Embodiment 2 | 28.86 | 5.24 | 81.84 |
| Embodiment 3 | 15.23 | 2.03 | 86.67 |
table 1
The ruthenium powder GDMS analysis result that embodiment obtains is as shown in table 2 below:
| Element | Embodiment 1(ppm) | Embodiment 2(ppm) | Embodiment 3(ppm) |
| Li | 0.0022 | 0.0012 | 0.0002 |
| Be | 0.0071 | 0.0032 | 0.0021 |
| B | 0.1171 | 0.0141 | 0.1151 |
| F | 0.432 | 0.032 | 0.402 |
| Na | 0.5126 | 0.2354 | 0.1263 |
| Mg | 0.1044 | 0.0140 | 0.0944 |
| Al | 8.6965 | 5.1245 | 8.6615 |
| Si | 10.0238 | 8.0280 | 4.0281 |
| P | 0.0633 | 0.0338 | 0.0033 |
| S | 5.3998 | 4.9988 | 5.3142 |
| Cl | 21.8739 | 13.3923 | 7.7394 |
| K | 0.3029 | 0.3022 | 0.3120 |
| Ca | 15.9823 | 10.9323 | 9.9232 |
| Sc | 0.0025 | 0.0005 | 0.0015 |
| Ti | 0.2869 | 0.2268 | 0.1165 |
| V | 1.0294 | 0.0274 | 0.0246 |
| Element | Embodiment 1(ppm) | Embodiment 2(ppm) | Embodiment 3(ppm) |
| Cr | 0.752 | 0.524 | 0.732 |
| Mn | 0.0958 | 0.0586 | 0.0825 |
| Fe | 4.11 | 5.24 | 2.03 |
| Co | 0.7086 | 0.4085 | 0.0208 |
| Ni | 8.9543 | 8.3531 | 4.5434 |
| Cu | 0.311 | 0.301 | 0.323 |
| Zn | 0.0717 | 0.0212 | 0.0413 |
| Ga | 0.0144 | 0.0102 | 0.0121 |
| Ge | 0.0207 | 0.0107 | 0.0102 |
| As | 0.0889 | 0.0869 | 0.0821 |
| Se | 0.0018 | 0.0008 | 0.0009 |
| Br | 0.0381 | 0.0281 | 0.0189 |
| Rb | 0.0011 | 0.0001 | 0.0020 |
| Sr | 0.4535 | 0.1535 | 0.2509 |
| Y | 0.0773 | 0.0243 | 0.0258 |
| Zr | 8.224 | 4.214 | 9.222 |
| Nb | 0.0003 | 0.0003 | 0.0003 |
| Mo | 0.0108 | 0.0098 | 0.0057 |
| Rh | 0.0799 | 0.0394 | 0.0556 |
| Pd | 1.1404 | 1.0402 | 0.1204 |
| Ag | 0.4338 | 0.2332 | 0.1738 |
| Cd | 0.1461 | 0.0431 | 0.0764 |
| In | 0.0691 | 0.0631 | 0.0292 |
| Sb | 0.1252 | 0.0262 | 0.1052 |
| Te | 0.0256 | 0.0052 | 0.0057 |
| I | 0.0008 | 0.0005 | 0.0003 |
| Cs | 0.0001 | 0.0001 | 0.0001 |
| Nd | 0.0061 | 0.0021 | 0.0042 |
| Sm | 0.0041 | 0.0046 | 0.0001 |
| Eu | 0.0038 | 0.0072 | 0.0040 |
| Gd | 0.0011 | 0.0012 | 0.0008 |
| Tb | 0 | 0 | 0 |
| Dy | 0 | 0 | 0 |
| Ho | 0 | 0 | 0 |
| Er | 0 | 0 | 0 |
| Tm | 0.0001 | 0.0001 | 0.0001 |
| Yb | 0 | 0 | 0 |
| Lu | 0 | 0 | 0 |
| Hf | 0.7197 | 0.6157 | 0.7295 |
| Ta | 0.0001 | 0.0001 | 0.0001 |
| W | 0.008 | 0.002 | 0.004 |
| Re | 0 | 0 | 0 |
| Os | 0 | 0 | 0 |
| Ir | 0.0189 | 0.0109 | 0.0122 |
| Pt | 0.0048 | 0.0005 | 0.0043 |
| Au | 0.0008 | 0.0008 | 0.0008 |
| Hg | 0 | 0 | 0 |
| Tl | 0 | 0 | 0 |
| Pb | 0.1429 | 0.1320 | 0.1123 |
| Bi | 0.0013 | 0.0010 | 0.0007 |
| Th | 0.0001 | 0.0001 | 0.0001 |
| U | 0.0002 | 0.0002 | 0.0002 |
| C* | 2.13 | 3.36 | 2.08 |
| Add up to | 93.834 | 68.4011 | 57.7884 |
| Element | Embodiment 1(ppm) | Embodiment 2(ppm) | Embodiment 3(ppm) |
| Ru | 999906.166 | 999931.5989 | 999942.2116 |
(
note:c* is carbon sulphur instrument testing result.）
table 2
The analysis of table 3 ruthenium powder tap density, apparent density analysis and processing characteristics
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Tap density is analyzed | 3.24 g/cm 3 | 3.88g/cm 3 | 3.76g/cm 3 |
| Apparent density is analyzed | 2.24g/cm 3 | 2.32g/cm 3 | 2.28g/cm 3 |
| Target processing characteristics | Well | Well | Well |
table 3
Can be found out by upper table 2 and table 3 and Fig. 2, Fig. 3 and Fig. 4, the iron carbon sodium and kalium element content realizing ruthenium powder is less than 10ppm respectively, and nitrogen content of Cl element is less than 50ppm respectively, and total impurities not air inclusion element is less than 100ppm.Ruthenium Powder Particle Size is less than 4um, and pattern is regular spherical, tap density 3.2 ~ 4.0g/cm
3, apparent density 2 ~ 2.6g/cm
3.The ruthenium Powder Particle Size, pattern and the impurity that obtain meet the requirement manufacturing ruthenium target; The ruthenium powder processing characteristics manufactured with this ruthenium powder is good.
Claims (4)
1. prepare a method for target ruthenium powder, adopt following steps to realize:
1. dissolving: with the dissolving with hydrochloric acid solid ruthenium trichloride of 8 ~ 12mol/L, add hydrochloric acid content and make the concentration of ruthenium at 45 ~ 55 grams per liters, generating (NH to containing adding ammonium chloride saturated solution in ruthenium solution
4)
3ruCl
6(III) amount of the ammonium chloride, added is 1.3 ~ 1.4 times of theoretical amount;
2. precipitate: heated solution reaches 90 ~ 100 DEG C, and the chlorine passing into 0.8 ~ 1 liter/min is oxidized, stir and obtain ruthenium hydrochloride ammonium (IV) precipitation, logical chlorine oxidation 1 ~ 4 hour, until ruthenium hydrochloride ammonium (IV) precipitation completely;
3. centrifugal filtration: above-mentioned sediment (NH
4)
2ruCl
6(IV) put into centrifuge centrifugal filtration 10 ~ 30 minutes, the rotating speed of centrifuge is 900 ~ 1000 revs/min;
4. dry: centrifugal anhydrate after (NH
4)
2ruCl
6(IV) oven dry is carried out 16 ~ 18 hours at 150 ~ 200 DEG C;
5. broken: (the NH of oven dry
4)
2ruCl
6(IV) in planetary ball mill, keep rotating speed 380 ~ 410 revs/min of fragmentations 15 ~ 25 minutes, described planetary ball mill adopts ball grinder material to be polyurethane, and ball-milling medium is zirconia ball, ratio of grinding media to material 2.2 ~ 3.7:1;
6. calcine: (the NH after fragmentation
4)
2ruCl
6(IV) first calcination 2.5 ~ 3.5 hours at 435 ~ 460 DEG C of temperature, increases the temperature to 630 ~ 660 DEG C and continues calcinings 2.5 ~ 3.5 hours, then increase the temperature to 730 ~ 770 DEG C of calcinings 1.5 ~ 2.5 hours;
7. reduce: at 730 ~ 760 DEG C of temperature, logical hydrogen reduction 0.5 ~ 1.5 hour;
8. powder process: finally obtain pure ruthenium powder with planetary ball mill crusher machine again; Rotating speed 380 ~ 410 revs/min is kept, broken 4 ~ 6 minutes in planetary ball mill.
2. a kind of method preparing target ruthenium powder as claimed in claim 1, is characterized in that: step 2. in mixing speed be 60 ~ 90 revs/min.
3. a kind of method preparing target ruthenium powder as claimed in claim 1, is characterized in that: step 5. in the broken time be 18 ~ 21 minutes.
4. a kind of method preparing target ruthenium powder as claimed in claim 2, is characterized in that: step 5. in the broken time be 18 ~ 21 minutes.
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| CN104308185B (en) * | 2014-10-14 | 2016-08-24 | 昆明贵金属研究所 | A kind of ruthenium trichloride prepares the method for target ruthenium powder |
| CN105458278B (en) * | 2015-12-08 | 2018-03-16 | 贵研铂业股份有限公司 | A kind of preparation method of high pure spherical ruthenium powder |
| CN107262732A (en) * | 2017-06-21 | 2017-10-20 | 昆明理工大学 | A kind of method that microwave one-step method prepares high-purity ruthenium powder |
| CN108405881A (en) * | 2018-02-02 | 2018-08-17 | 贵研铂业股份有限公司 | A kind of preparation method of high pure spherical ruthenium powder |
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| CN110919019A (en) * | 2019-12-02 | 2020-03-27 | 河南东微电子材料有限公司 | Preparation method of high-purity ruthenium powder |
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