CN108405881A - A kind of preparation method of high pure spherical ruthenium powder - Google Patents
A kind of preparation method of high pure spherical ruthenium powder Download PDFInfo
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- CN108405881A CN108405881A CN201810108737.3A CN201810108737A CN108405881A CN 108405881 A CN108405881 A CN 108405881A CN 201810108737 A CN201810108737 A CN 201810108737A CN 108405881 A CN108405881 A CN 108405881A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
Abstract
The invention discloses a kind of preparation method of high pure spherical ruthenium powder, step includes：(1) it dissolves：With dissolving with hydrochloric acid, ruthenium hydrochloride solution is obtained；(2) ion exchange purification and impurity removal obtains pure ruthenium solution；(3) prepared by presoma：The initial pH value of ruthenium solution obtained by set-up procedure (2), is added precipitation initiator, ageing, and heating stirring generates ruthenium powder presoma --- spherical hydrous ruthenium；(4) calcined dehydration hydrogen reducing：Presoma obtained by step (3) is placed in tube furnace and first carries out calcined dehydration, then is passed through hydrogen and carries out high temperature reduction, obtains spherical metal ruthenium powder；(5) nitration mixture is boiled to wash and is separated by filtration, and is fully washed with deionized water, after vacuum drying, obtains high pure spherical ruthenium powder.The method of the present invention is simple for process, and impurity content is less than 10ppm in the ruthenium powder of preparation, and ruthenium powder microscopic appearance is spherical shape, and granularity is less than 5 μm, can be used as the raw material of ruthenium base sputtering target material.
Description
Technical field
The present invention relates to the preparation of noble metal powder, more particularly to a kind of preparation method of high pure spherical ruthenium powder.
Background technology
Hard disc of computer memory material target ruthenium powder has special index request, it is necessary to very strictly control impurity and powder
Last pattern, purity then must 99.999% or more, microscopic appearance requires spherical or spherical.
The preparation method of country's ruthenium powder generally uses secondary oxidation to distill at present, and absorbing liquid condensing crystallizing obtains RuCl3It forges
Annealing in hydrogen atmosphere reduction prepares ruthenium powder, or ruthenium absorbed, chloride precipitation is added after liquid oxidation, calcining, hydrogen reduction prepare ruthenium powder.The method
The ruthenium powder particles of gained are thick and uneven, and impurity content is high, it is impossible to be used in the production of ruthenium target.
Chinese patent ZL200580006772.5 discloses high-purity Ru powder, sputtering target, film and high-purity Ru powder
Manufacturing method, comprise the concrete steps that and make anode with the Ru raw materials of purity 99.9%, in the solution electrolytic refining, can get
99.99% or more pure ruthenium powder, the wherein content of each alkali metal such as Na, K in 10ppm hereinafter, the content of Al be 1~50ppm,
Suitably form the capacitor electrode material of semiconductor memory.
Chinese patent ZL200610106338.0 discloses the method for preparing ruthenium powder, and this method is in calcining chlordene ruthenic acid
Ammonium was prepared in the step of ruthenium powder, the obtained thick ruthenium of ammonium hexachlororuthenate will be calcined at 500~800 DEG C and crushed, then 800~
It is calcined again at 1000 DEG C, it is 100ppm or following thus to make the chlorinity in ruthenium powder.
Chinese patent ZL200810109294.6 discloses the manufacturing method and chlordene ruthenic acid of ammonium hexachlororuthenate and ruthenium powder
Ammonium, ammonium chloride is added in the hydrochloric acid solution of ruthenium and manufactured ammonium hexachlororuthenate is burnt into prepare ruthenium powder.Specific steps
After being hydrochloric acid solution 3 hours for keeping ruthenium at 80~95 DEG C or more, make on one side the revolution of blender reach 200 turns per minute with
On be stirred ammonium chloride be added on one side, kept while being stirred 1 hour or more at 85~95 DEG C, generate ammonium hexachlororuthenate
Precipitation, by the way that the crystal that moisture content is 10% ammonium hexachlororuthenate below is obtained by filtration.
Chinese patent 201310112626.7 discloses a kind of method preparing target ruthenium powder, is realized by step：Dissolving,
Precipitation centrifugal filtration, drying, is crushed, calcines, restoring, powder processed.Iron, carbon, sodium, the Determination of Potassium of ruthenium powder are respectively smaller than
10ppm, nitrogen, content of Cl element are respectively smaller than 50ppm, and total impurities do not include elemental gas and are less than 100ppm.Ruthenium Powder Particle Size is less than 4
μm, pattern is in regular spherical shape, 3.2~4.0g/cm of tap density3, 2~2.6g/cm of apparent density3。
The technique that Japanese enterprises produce high-purity ruthenium powder：With the potassium hydroxide and potassium nitrate melting salt oxidation and dissolving ruthenium gold of melting
Belong to, it is made to be changed into soluble ruthenate.With water dissolution extract ruthenium salt, heat and be passed through chlorine make ruthenium ion oxidation distillation at
RuO4, then with the mixed liquor of dilute hydrochloric acid and ethyl alcohol absorb RuO4, solution is being passed through oxygen later through being dried to obtain solid ruthenium trichloride
High-temperature roasting under conditions of gas makes ruthenium salt become RuO2, under final high temperature hydrogen reduction obtain ruthenium powder.But in the ruthenium powder produced
The impurity contents such as Na, K, Fe, Cl are higher.
A kind of methods preparing target ruthenium powder with ruthenium trichloride of Chinese patent ZL 201410540106.0, by solid three
Ruthenic chloride dissolving with hydrochloric acid obtains ruthenium hydrochloride solution, and solution removes cation impurity by ion exchange resin, molten toward pure ruthenium
Alkali is added in liquid and generates hydroxide ruthenium precipitation, continues to add deionized water pulp, be placed in autoclave, heat, be passed through hydrogen
It keeps certain hydrogen partial pressure to restore, obtains pure ruthenium powder.Ruthenium powder impurity content is low (being less than 100ppm), and ruthenium powder microscopic appearance is ball
Shape, 2~5 μm of granularity.
Invention content
The purpose of the present invention is overcome the deficiencies in the prior art, the side that a kind of short route prepares high pure spherical ruthenium powder has been invented
Method.
The method of the present invention is divided into five steps：(1) it dissolves；(2) ion exchange purification and impurity removal；(3) before prepared by precipitation from homogeneous solution
Drive body；(4) calcining-hydrogen reducing；(5) nitration mixture, which boils, washes.
(1) it dissolves：By solid ruthenium trichloride dissolving with hydrochloric acid, ruthenium hydrochloride solution is obtained；
(2) ion exchange purification and impurity removal：Ruthenium solution obtained by step (1) is cleaned using cation exchange resin, is obtained
Obtain pure ruthenium solution；
(3) prepared by presoma：Ruthenium solution pH value obtained by set-up procedure (2) is added precipitation initiator, is aged, heating stirring,
Hydrolytic precipitation reaction is brought it about, spherical precursor --- ruthenium oxide hydration is generated；
(4) calcined dehydration-hydrogen reducing：Spherical hydrous ruthenium obtained by step (3) is placed in tube furnace and is first forged
Dehydration is burnt, then is passed through hydrogen and carries out high temperature reduction, obtains spherical metal ruthenium powder；
(5) nitration mixture, which boils, washes：Ruthenium powder obtained by step (4) is boiled and washed using chloroazotic acid+hydrofluoric acid mixed solution, is separated by filtration, is used
Deionized water is fully washed, and after vacuum drying, obtains high pure spherical ruthenium powder.
Advantageous effect of the present invention：
Method provided by the invention is to exchange ruthenium solution by cation to remove cation impurity, then toward purified ruthenium
Urea is added in solution as precipitation initiator, by controlling suitable condition, make urea uniform decomposition release hydroxyl from
Precipitation reaction occurs for son, to achieve the purpose that control particle growth speed, microscopic appearance, granularity, obtains spherical forerunner
Body --- ruthenium oxide hydration；The pattern of ruthenium oxide hydration has conclusive influence, ruthenium oxide hydration calcining de- the pattern of ruthenium powder
Ruthenium-oxide is generated after water, then during carrying out high-temperature hydrogen reduction, precursor spherical particle has heredity on pattern and granularity
Property, to obtain spherical ruthenium powder；Ruthenium powder is boiled using chloroazotic acid+hydrofluoric acid mixed solution washes that further to remove Fe, Si, noble metal etc. micro-
Impurity is measured, high pure spherical ruthenium powder is obtained.Present invention process is simple, and gained ruthenium powder impurity content is low (being less than 10ppm), and ruthenium powder is microcosmic
Pattern is spherical shape, and 2~5 μm of granularity accords with the production requirement of ruthenium target.
Description of the drawings
Attached drawing 1 is the process flow diagram of the present invention.
Fig. 2, Fig. 3 are respectively presoma and ruthenium powder microscopic appearance figure prepared by the present invention.
Specific implementation mode
Invention is further described in detail with specific example below in conjunction with the accompanying drawings.
Embodiment 1, referring to attached drawing 1, by solid ruthenium trichloride top grade pure hydrochloric acid+deionized water dissolving, gained ruthenium solution
Cation impurity is removed by cation exchange resin, obtains pure ruthenium solution, it is 5 to adjust the ruthenium solution pH value, by ruthenium:Urea
Molar ratio 1:8 are added top pure grade urea, and solution for 24 hours, is then heated to 90 DEG C, constant temperature is stirred to react 4h, hydrolyzes by ageing
Precipitation reaction generates spherical ruthenium powder presoma --- and ruthenium oxide hydration is separated by filtration, washs, dries；Presoma is placed in tubular type
Calcining at constant temperature is dehydrated 1h at a temperature of 300 DEG C in stove, is continuously heating to 600 DEG C, is passed through high-purity hydrogen, and constant temperature restores 4h, then
It is passed through nitrogen to be cooled to room temperature, obtains ruthenium powder；Gained ruthenium powder is boiled in polytetrafluoroethylene beaker using nitric acid+hydrofluoric acid again
It washes, is separated by filtration, fully washed with deionized water, after gained ruthenium powder is dried in vacuo at a temperature of 100 DEG C, obtain high pure spherical ruthenium
Powder.
Embodiment 2, referring to attached drawing 1, by solid ruthenium trichloride top grade pure hydrochloric acid+deionized water dissolving, gained ruthenium solution
Cation impurity is removed by cation exchange resin, obtains pure ruthenium solution；It is 5 to adjust ruthenium solution pH value, by ruthenium:Urea rubs
That ratio 1:6 are added top pure grade urea, and solution for 24 hours, is then heated to 90 DEG C by ageing, and constant temperature is stirred to react 4h, and it is heavy that hydrolysis occurs
Forming sediment and react, generate spherical ruthenium powder presoma --- ruthenium oxide hydration is separated by filtration, washs, dries；Presoma is placed in tube furnace
In at a temperature of 350 DEG C calcining at constant temperature be dehydrated 2h, be continuously heating to 650 DEG C, be passed through high-purity hydrogen, constant temperature restores 3h, then leads to
Enter nitrogen to be cooled to room temperature, obtains ruthenium powder；Gained ruthenium powder is boiled in polytetrafluoroethylene beaker using nitric acid+hydrofluoric acid again and is washed,
It is separated by filtration, is fully washed with deionized water, after gained ruthenium powder is dried in vacuo at a temperature of 100 DEG C, obtain high pure spherical ruthenium powder.
Embodiment 3, referring to attached drawing 1, by solid ruthenium trichloride top grade pure hydrochloric acid+deionized water dissolving, gained ruthenium solution
Cation impurity is removed by cation exchange resin, obtains pure ruthenium solution, adjustment ruthenium solution pH value is 5, by ruthenium:Urea rubs
That ratio 1:6 are added top pure grade urea, and solution for 24 hours, then is heated to boiling by ageing, and constant temperature is stirred to react 4h, and it is heavy that hydrolysis occurs
Forming sediment and react, generate spherical ruthenium powder presoma --- ruthenium oxide hydration is separated by filtration, washs, dries；Presoma is placed in tube furnace
In at a temperature of 350 DEG C calcining at constant temperature be dehydrated 2h, be continuously heating to 650 DEG C, be passed through high-purity hydrogen, constant temperature restores 3h, then leads to
Enter nitrogen to be cooled to room temperature, obtains ruthenium powder；Gained ruthenium powder is boiled in polytetrafluoroethylene beaker using nitric acid+hydrofluoric acid again and is washed,
It is separated by filtration, is fully washed with deionized water, after gained ruthenium powder is dried in vacuo at a temperature of 100 DEG C, obtain high pure spherical ruthenium powder.
The ruthenium powder prepared to the present invention is analyzed using GDMS, as a result as shown in table 1 below.
1 ruthenium powder GDMS impurity analysis results of table
Total impurities constituent content is less than 10ppm, purity in the ruthenium powder prepared by the present invention it can be seen from table 1 and Fig. 3
More than 99.999%, granularity is less than 5 μm, and pattern is spherical in shape, can be as the ingredient requirement of ruthenium base sputtering target material.
Claims (5)
1. a kind of preparation method of high pure spherical ruthenium powder, it is characterised in that complete according to the following steps：
(1) it dissolves：By solid ruthenium trichloride dissolving with hydrochloric acid, ruthenium hydrochloride solution is obtained；
(2) ion exchange purification and impurity removal：Ruthenium solution obtained by step (1) is cleaned using cation exchange resin, is obtained pure
Net ruthenium solution；
(3) prepared by presoma：The initial pH value of ruthenium solution obtained by set-up procedure (2), is added precipitation initiator, ageing, and heating is stirred
It mixes, brings it about hydrolytic precipitation reaction, generate ruthenium powder presoma --- spherical hydrous ruthenium；
(4) calcined dehydration-hydrogen reducing：Presoma obtained by step (3) is placed in tube furnace and is first calcined, then is passed through hydrogen
High temperature reduction is carried out, spherical metal ruthenium powder is obtained；
(5) nitration mixture, which boils, washes：Ruthenium powder obtained by step (4) is boiled and is washed using chloroazotic acid+hydrofluoric acid mixed solution, is separated by filtration, spend from
Sub- water fully washs, and after vacuum drying, obtains high pure spherical ruthenium powder.
2. a kind of preparation method of high pure spherical ruthenium powder according to claim 1, it is characterised in that the tune described in step (3)
Whole solution initial pH value is 3~5.
3. a kind of preparation method of high pure spherical ruthenium powder according to claim 1, it is characterised in that heavy described in step (3)
Shallow lake initiator is top pure grade urea, ruthenium:Urea mol ratio is 1:5~8, digestion time 12~for 24 hours, 80~100 DEG C of reaction temperature,
2~4h of reaction time.
4. a kind of preparation method of high pure spherical ruthenium powder according to claim 1, it is characterised in that forging described in step (4)
Burn dehydration conditions：250~350 DEG C of temperature, 1~2h of soaking time.
5. a kind of preparation method of high pure spherical ruthenium powder, it is characterised in that complete according to the following steps：
By solid ruthenium trichloride top grade pure hydrochloric acid+deionized water dissolving, gained ruthenium solution is removed by cation exchange resin
Cation impurity obtains pure ruthenium solution, and it is 5 to adjust the ruthenium solution pH value, by ruthenium:Urea mol ratio 1:8 are added top pure grade urine
Solution for 24 hours, is then heated to 90 DEG C by element, ageing, and constant temperature is stirred to react 4h, and hydrolytic precipitation reaction occurs, and generates spherical ruthenium powder
Presoma --- ruthenium oxide hydration is separated by filtration, washs, dries；Presoma is placed in tube furnace constant temperature at a temperature of 300 DEG C
Calcined dehydration 1h is continuously heating to 600 DEG C, is passed through high-purity hydrogen, and constant temperature restores 4h, then passes to nitrogen and be cooled to room temperature, obtain
To ruthenium powder；Gained ruthenium powder is boiled in polytetrafluoroethylene beaker using nitric acid+hydrofluoric acid again and is washed, is separated by filtration, uses deionized water
Fully washing after gained ruthenium powder is dried in vacuo at a temperature of 100 DEG C, obtains high pure spherical ruthenium powder.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110014165A (en) * | 2019-05-23 | 2019-07-16 | 西北有色金属研究院 | A kind of preparation method of high-purity micron-size spherical molybdenum powder |
| CN110340373A (en) * | 2019-07-09 | 2019-10-18 | 贵研铂业股份有限公司 | A kind of preparation method of High Purity Palladium powder |
| CN110893467A (en) * | 2019-12-24 | 2020-03-20 | 湖南欧泰稀有金属有限公司 | Grinding tank and preparation method of high-purity superfine ruthenium powder |
| CN111940758A (en) * | 2020-08-17 | 2020-11-17 | 昆明理工大学 | Method for preparing spherical ruthenium powder by polyol reduction method |
| CN113020615A (en) * | 2021-03-03 | 2021-06-25 | 中海油(山西)贵金属有限公司 | Method for preparing high-purity rhodium powder by using rhodium trichloride |
| CN113458407A (en) * | 2021-07-12 | 2021-10-01 | 安徽拓思贵金属有限公司 | Preparation method of high-purity ruthenium powder |
| CN114959772A (en) * | 2022-05-26 | 2022-08-30 | 浙江大学 | Long-life noble metal oxide oxygen evolution reaction electrocatalyst and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110014165A (en) * | 2019-05-23 | 2019-07-16 | 西北有色金属研究院 | A kind of preparation method of high-purity micron-size spherical molybdenum powder |
| CN110014165B (en) * | 2019-05-23 | 2020-07-17 | 西北有色金属研究院 | Preparation method of high-purity micron-sized spherical molybdenum powder |
| CN110340373A (en) * | 2019-07-09 | 2019-10-18 | 贵研铂业股份有限公司 | A kind of preparation method of High Purity Palladium powder |
| CN110893467A (en) * | 2019-12-24 | 2020-03-20 | 湖南欧泰稀有金属有限公司 | Grinding tank and preparation method of high-purity superfine ruthenium powder |
| CN111940758A (en) * | 2020-08-17 | 2020-11-17 | 昆明理工大学 | Method for preparing spherical ruthenium powder by polyol reduction method |
| CN111940758B (en) * | 2020-08-17 | 2023-01-31 | 昆明理工大学 | Method for preparing spherical ruthenium powder by polyol reduction method |
| CN113020615A (en) * | 2021-03-03 | 2021-06-25 | 中海油(山西)贵金属有限公司 | Method for preparing high-purity rhodium powder by using rhodium trichloride |
| CN113458407A (en) * | 2021-07-12 | 2021-10-01 | 安徽拓思贵金属有限公司 | Preparation method of high-purity ruthenium powder |
| CN114959772A (en) * | 2022-05-26 | 2022-08-30 | 浙江大学 | Long-life noble metal oxide oxygen evolution reaction electrocatalyst and preparation method and application thereof |
| CN114959772B (en) * | 2022-05-26 | 2023-10-03 | 浙江大学 | Long-life noble metal oxide oxygen evolution reaction electrocatalyst, preparation method and application |
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