CN102172776A - Method for preparing metal palladium powder - Google Patents
Method for preparing metal palladium powder Download PDFInfo
- Publication number
- CN102172776A CN102172776A CN2011100273842A CN201110027384A CN102172776A CN 102172776 A CN102172776 A CN 102172776A CN 2011100273842 A CN2011100273842 A CN 2011100273842A CN 201110027384 A CN201110027384 A CN 201110027384A CN 102172776 A CN102172776 A CN 102172776A
- Authority
- CN
- China
- Prior art keywords
- metal palladium
- salting liquid
- solution
- palladium powder
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a method for preparing metal palladium powder. In the method, ascorbic acids or hydrazine hydrates are used as reducing agents, and the reducing agent is directly mixed with a palladium solution so as to obtain palladium powder with uniform size and high purity. The size of the palladium powder can be regulated and controlled within the range of 300-800 nm. The method provided by the invention does not use any other surfactants or alkali, has simple equipment requirement and low cost, is easy to operate, and easy for industrialization.
Description
Technical field
The invention belongs to technical field of material, relate to a kind of metal material preparation method, especially a kind of preparation method of Metal Palladium powder.
Background technology
Superfine metal palladium powder is the main component of palladium-silver electrocondution slurry commonly used in the electronics industry.The palladium powder occupies 60% above cost of electrocondution slurry, and consumption is big.And the wet chemical technology for preparing the palladium powder at present often need use surfactant to control particle diameter, controls the pH value of reaction system with acid or alkali, and this just causes the purity of palladium powder not high, and the step complexity, is difficult to washing and separates the rising of production cost.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of preparation method of Metal Palladium powder is provided, this method neither needs to use surfactant, does not also need to control the solution pH value with acid or alkali, and reaction speed is fast, method is simple, the rate of recovery is high, resulting palladium powder purity height, and have monodispersity, devices needed is simpler and easy, is easy to control, good reproducibility is highly susceptible to suitability for industrialized production.
The objective of the invention is to solve by the following technical programs:
The preparation method of first kind of Metal Palladium powder that the present invention proposes may further comprise the steps:
1) Metal Palladium salt and ethanolic solution are mixed and made into the Metal Palladium salting liquid; The concentration of Metal Palladium is 0.01g/mL-0.1g/mL in the described Metal Palladium salting liquid, and the volumetric concentration of ethanol is 10%-50%;
2) reducing agent is dissolved in the distilled water, makes the reductant solution that mass concentration is 0.1g/mL-0.3g/mL; Described reducing agent is ascorbic acid or hydrazine hydrate;
3) under 20-70 degree centigrade reaction temperature be that Metal Palladium salting liquid 0.1-1 reductant solution doubly joins in the Metal Palladium solution fast with volume;
4) react completely, treat that ageing 15 minutes to 2 hours, isolates supernatant liquor, will precipitate clean, oven dry, obtain the Metal Palladium powder.
The preparation method of second kind of Metal Palladium powder that the present invention proposes may further comprise the steps:
1) Metal Palladium salt and water are mixed and made into the Metal Palladium salting liquid; The concentration of Metal Palladium is 0.01g/mL-0.1g/mL in the described Metal Palladium salting liquid;
2) reducing agent is dissolved in the distilled water, makes the reductant solution that mass concentration is 0.1g/mL-0.3g/mL; Described reducing agent is ascorbic acid or hydrazine hydrate;
3) under 20-70 degree centigrade reaction temperature be that Metal Palladium salting liquid 0.1-1 reductant solution doubly joins in the Metal Palladium solution fast with volume;
4) react completely, treat that ageing 15 minutes to 2 hours, isolates supernatant liquor, will precipitate clean, oven dry, obtain the Metal Palladium powder.
More than in two kinds of methods: Metal Palladium salt is H2PdCl4 or Pd (NO3) 2; In step 1), can be 10-100mL with described Metal Palladium salting liquid constant volume; In step 3), adopt the water-bath temperature control, magnetic agitation; In step 4), the Metal Palladium powder that obtains is of a size of 300nm-800nm.
Than prior art, the present invention has following beneficial effect:
(1) method of the present invention need not to use surfactant, is easy to separating, washing, reduces cost.
(2) the present invention need not the acid-base value of conditioned reaction system, needn't introduce some sodium salts, sylvite, helps improving product purity and reduces cost.
(3) the direct rapid mixing of reducing agent of the present invention and metal salt solution needn't be used the reinforced control appliance of liquid of peristaltic pump and so on, and method is simple.
(4) the Metal Palladium powder particles size of method generation of the present invention is easy to precipitate and separate in the sub-micron rank.
(5) reducing agent of the present invention and salting liquid rapid mixing, reaction speed is fast, has reduced repeatedly the particle uneven phenomenon that nucleation causes, and gained Metal Palladium particle size is even, good dispersion.
(6) in reaction system of the present invention, add the dispersiveness that a certain amount of ethanol can help improving gained palladium powder, help metallic particles and solution separate and subsequent drying is handled.
(7) among the preparation method of the present invention, Metal Palladium powder footpath is controlled, and the particle diameter of palladium powder can be controlled by the concentration and the temperature of salting liquid and reducing agent.
In sum, synthesis step of the present invention is simple, and reducing agent and salt solution mix get final product, and equipment requires simple, does not need high-end devices, is easy to industrialization, and cost is low.
The specific embodiment
Come explained in detail the present invention below in conjunction with concrete case study on implementation:
Embodiment 1
The preparation method of the Metal Palladium powder of present embodiment specifically may further comprise the steps:
1) Metal Palladium salt and ethanolic solution are mixed and made into the Metal Palladium salting liquid; Wherein the concentration of Metal Palladium is 0.01g/mL in the Metal Palladium salting liquid, and the volumetric concentration of ethanol is 50%; In the present embodiment, Metal Palladium salt is selected H
2PdCl
4And with Metal Palladium salting liquid constant volume is 10mL.
2) ascorbic acid is dissolved in the distilled water as reducing agent, makes the reductant solution that mass concentration is 0.1g/mL;
3) adopt the water-bath temperature control, magnetic agitation under 70 degrees centigrade reaction temperature is that the reductant solution of 0.1 times of Metal Palladium salting liquid joins in the Metal Palladium solution fast with volume;
4) react completely, treated ageing 2 hours, isolate supernatant liquor, will precipitate and clean, dry, obtain being of a size of the Metal Palladium powder of 300nm-800nm.
Embodiment 2
The preparation method of the Metal Palladium powder of present embodiment specifically may further comprise the steps:
1) Metal Palladium salt and ethanolic solution are mixed and made into the Metal Palladium salting liquid; Wherein the concentration of Metal Palladium is 0.1g/mL in the Metal Palladium salting liquid, and the volumetric concentration of ethanol is 10%; In the present embodiment, Metal Palladium salt is selected Pd (NO
3)
2And with Metal Palladium salting liquid constant volume is 100mL.
2) ascorbic acid is dissolved in the distilled water as reducing agent, makes the reductant solution that mass concentration is 0.3g/mL;
3) adopt the water-bath temperature control, magnetic agitation under 20 degrees centigrade reaction temperature is that the reductant solution of 1 times of Metal Palladium salting liquid joins in the Metal Palladium solution fast with volume;
4) react completely, treated ageing 15 minutes, isolate supernatant liquor, will precipitate and clean, dry, obtain being of a size of the Metal Palladium powder of 300nm-800nm.
Embodiment 3
The preparation method of the Metal Palladium powder of present embodiment specifically may further comprise the steps:
1) Metal Palladium salt and ethanolic solution are mixed and made into the Metal Palladium salting liquid; Wherein the concentration of Metal Palladium is 0.05g/mL in the Metal Palladium salting liquid, and the volumetric concentration of ethanol is 20%; In the present embodiment, Metal Palladium salt is selected H
2PdCl
4And with Metal Palladium salting liquid constant volume is 80mL.
2) hydrazine hydrate is dissolved in the distilled water as reducing agent, makes the reductant solution that mass concentration is 0.2g/mL;
3) adopt the water-bath temperature control, magnetic agitation under 50 degrees centigrade reaction temperature is that the reductant solution of 0.5 times of Metal Palladium salting liquid joins in the Metal Palladium solution fast with volume;
4) react completely, treated ageing 1 hour, isolate supernatant liquor, will precipitate and clean, dry, obtain being of a size of the Metal Palladium powder of 300nm-800nm.
Embodiment 4
The preparation method of the Metal Palladium powder of present embodiment specifically may further comprise the steps:
1) Metal Palladium salt and ethanolic solution are mixed and made into the Metal Palladium salting liquid; Wherein the concentration of Metal Palladium is 0.08g/mL in the Metal Palladium salting liquid, and the volumetric concentration of ethanol is 30%; In the present embodiment, Metal Palladium salt is selected Pd (NO
3)
2And with Metal Palladium salting liquid constant volume is 40mL.
2) ascorbic acid is dissolved in the distilled water as reducing agent, makes the reductant solution that mass concentration is 0.15g/mL;
3) adopt the water-bath temperature control, magnetic agitation under 60 degrees centigrade reaction temperature is that the reductant solution of 0.6 times of Metal Palladium salting liquid joins in the Metal Palladium solution fast with volume;
4) react completely, treated ageing 1.5 hours, isolate supernatant liquor, will precipitate and clean, dry, obtain being of a size of the Metal Palladium powder of 300nm-800nm.
Embodiment 5
The preparation method of the Metal Palladium powder of present embodiment specifically may further comprise the steps:
1) Metal Palladium salt and water are mixed and made into the Metal Palladium salting liquid; Wherein the concentration of Metal Palladium is 0.01g/mL in the Metal Palladium salting liquid; In the present embodiment, Metal Palladium salt is selected H
2PdCl
4And with Metal Palladium salting liquid constant volume is 10mL.
2) hydrazine hydrate is dissolved in the distilled water as reducing agent, makes the reductant solution that mass concentration is 0.1g/mL;
3) adopt the water-bath temperature control, magnetic agitation under 20 degrees centigrade reaction temperature is that the reductant solution of 0.1 times of Metal Palladium salting liquid joins in the Metal Palladium solution fast with volume;
4) react completely, treated ageing 15 minutes, isolate supernatant liquor, will precipitate and clean, dry, obtain being of a size of the Metal Palladium powder of 300nm-800nm.
Embodiment 6
The preparation method of the Metal Palladium powder of present embodiment specifically may further comprise the steps:
1) Metal Palladium salt and water are mixed and made into the Metal Palladium salting liquid; Wherein the concentration of Metal Palladium is 0.1g/L in the Metal Palladium salting liquid; In the present embodiment, Metal Palladium salt is selected Pd (NO
3)
2And with Metal Palladium salting liquid constant volume is 100mL.
2) ascorbic acid is dissolved in the distilled water as reducing agent, makes the reductant solution that mass concentration is 0.3g/mL;
3) adopt the water-bath temperature control, magnetic agitation under 70 degrees centigrade reaction temperature is that the reductant solution of 1 times of Metal Palladium salting liquid joins in the Metal Palladium solution fast with volume;
4) react completely, treated ageing 2 hours, isolate supernatant liquor, will precipitate and clean, dry, obtain being of a size of the Metal Palladium powder of 300nm-800nm.
Embodiment 7
The chlorine palladium acid solution that will contain 1 part of palladium joins in the 100mL beaker, is settled to 20mL with distilled water, adds the 10mL absolute ethyl alcohol again, and magnetic agitation, mixing speed are 200 rev/mins, and it is 40 degrees centigrade that the water-bath temperature control makes anti-liquid temp.
3 parts of ascorbic acid are joined in the 50mL beaker, and constant volume is in 10mL water; The ascorbic acid solution that configures was joined in 2 seconds in the chlorine palladium acid solution fast, the very fast blackening of solution, continue to stir 30 minutes, upper solution is poured out in the clarification of solution upper strata, with distilled water and ethanol mixed solvent washing by soaking 3 times repeatedly, refilter at last, with the ethanol washing, it is too dried that the palladium powder can not be filtered, in case catch fire, the palladium powder vacuum 50 of wet condition is spent dry 12 hours can obtain the palladium powder that average-size is the favorable dispersibility of 400 nanometers.The disposable rate of recovery is greater than 94%.
Embodiment 8
The chlorine palladium acid solution that will contain 1 part of palladium joins in the 100mL round-bottomed flask, is settled to 20mL with distilled water, adds the 10mL absolute ethyl alcohol again, and magnetic agitation, mixing speed are that to make anti-liquid temp be 40 degrees centigrade to 200 rev/mins of water-bath temperature controls.
3 parts of hydrazine hydrates are joined in the 50mL beaker, and constant volume is in 10mL water; The hydrazine hydrate solution that configures was joined in 2 seconds in the chlorine palladium acid solution fast, solution bubbling and very fast blackening, continue to stir 30 minutes, upper solution is poured out in the clarification of solution upper strata, with distilled water and ethanol mixed solvent washing by soaking 3 times repeatedly, refilter at last, with the ethanol washing, it is too dried that the palladium powder can not be filtered, in case catch fire, the palladium powder vacuum 50 of wet condition is spent dry 12 hours can obtain the palladium powder that average-size is the favorable dispersibility of 300 nanometers.The disposable rate of recovery is greater than 98%.
Embodiment 9
The palladium nitrate solution that will contain 1 part of palladium joins in the 100mL beaker, is settled to 20mL with distilled water, adds the 10mL absolute ethyl alcohol again, and magnetic agitation, mixing speed are 200 rev/mins, and it is 40 degrees centigrade that the water-bath temperature control makes anti-liquid temp.
3 parts of ascorbic acid are joined in the 50mL beaker, constant volume is in 10mL water, the ascorbic acid solution that configures was joined in 2 seconds in the chlorine palladium acid solution fast, the very fast blackening of solution, continue to stir 30 minutes, the clarification of solution upper strata, pour out upper solution, with distilled water and ethanol mixed solvent washing by soaking 3 times repeatedly, refilter at last, with the ethanol washing, it is too dried that the palladium powder can not be filtered, in case catch fire, the palladium powder vacuum 50 of wet condition is spent dry 12 hours can obtain the palladium powder that average-size is the favorable dispersibility of 460 nanometers.The disposable rate of recovery is greater than 94%.
Embodiment 10
The chlorine palladium acid solution that will contain 10 parts of palladiums joins in the 100mL beaker, is settled to the 30mL magnetic agitation with distilled water, and mixing speed is 200 rev/mins, and it is 40 degrees centigrade that the water-bath temperature control makes anti-liquid temp.
30 parts of ascorbic acid are joined in the 50mL beaker, and constant volume is in 10mL water; The ascorbic acid solution that configures was joined in 2 seconds in the chlorine palladium acid solution fast, the very fast blackening of solution, continue to stir 30 minutes, upper solution is poured out in the clarification of solution upper strata, with distilled water and ethanol mixed solvent washing by soaking 3 times repeatedly, refilter at last, with the ethanol washing, it is too dried that the palladium powder can not be filtered, in case catch fire, 50 degrees centigrade of dryings of palladium powder vacuum of wet condition can be obtained the palladium powder (as Fig. 1) that average-size is the favorable dispersibility of 650 nanometers in 12 hours.The disposable rate of recovery is greater than 94%
The characteristics of the inventive method are: reducing agent mixes with the Quick uniform of slaine, and the even nucleation of solution suppresses the mode of growth and controls the granularity of palladium powder particles, so that do not add the particle that still can obtain small size in the situation of surfactant. And the method gained particle dispersion is good, size uniform.
Claims (6)
1. the preparation method of a Metal Palladium powder is characterized in that, may further comprise the steps:
1) Metal Palladium salt and ethanolic solution are mixed and made into the Metal Palladium salting liquid; The concentration of Metal Palladium is 0.01g/mL-0.1g/mL in the described Metal Palladium salting liquid, and the volumetric concentration of ethanol is 10%-50%;
2) reducing agent is dissolved in the distilled water, makes the reductant solution that mass concentration is 0.1g/mL-0.3g/mL; Described reducing agent is ascorbic acid or hydrazine hydrate;
3) under 20-70 degree centigrade reaction temperature be that Metal Palladium salting liquid 0.1-1 reductant solution doubly joins in the Metal Palladium solution fast with volume;
4) react completely, treat that ageing 15 minutes to 2 hours, isolates supernatant liquor, will precipitate clean, oven dry, obtain the Metal Palladium powder.
2. the preparation method of a Metal Palladium powder is characterized in that, may further comprise the steps:
1) Metal Palladium salt and water are mixed and made into the Metal Palladium salting liquid; The concentration of Metal Palladium is 0.01g/mL-0.1g/mL in the described Metal Palladium salting liquid;
2) reducing agent is dissolved in the distilled water, makes the reductant solution that mass concentration is 0.1g/mL-0.3g/mL; Described reducing agent is ascorbic acid or hydrazine hydrate;
3) under 20-70 degree centigrade reaction temperature be that Metal Palladium salting liquid 0.1-1 reductant solution doubly joins in the Metal Palladium solution fast with volume;
4) react completely, treat that ageing 15 minutes to 2 hours, isolates supernatant liquor, will precipitate clean, oven dry, obtain the Metal Palladium powder.
3. the preparation method of Metal Palladium powder according to claim 1 and 2 is characterized in that, described Metal Palladium salt is H
2PdCl
4Or Pd (NO
3)
2
4. the preparation method of Metal Palladium powder according to claim 1 and 2 is characterized in that, in the step 1), is 10-100mL with described Metal Palladium salting liquid constant volume.
5. the preparation method of Metal Palladium powder according to claim 1 and 2 is characterized in that, in the step 3), adopts the water-bath temperature control, magnetic agitation.
6. the preparation method of Metal Palladium powder according to claim 1 and 2 is characterized in that, in the step 4), the Metal Palladium powder that obtains is of a size of 300nm-800nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100273842A CN102172776A (en) | 2011-01-25 | 2011-01-25 | Method for preparing metal palladium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100273842A CN102172776A (en) | 2011-01-25 | 2011-01-25 | Method for preparing metal palladium powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102172776A true CN102172776A (en) | 2011-09-07 |
Family
ID=44516123
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100273842A Pending CN102172776A (en) | 2011-01-25 | 2011-01-25 | Method for preparing metal palladium powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102172776A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107052362A (en) * | 2017-06-15 | 2017-08-18 | 西安宏星电子浆料科技有限责任公司 | High-specific surface area ultrafine palladium powder and preparation method thereof |
| CN107663583A (en) * | 2016-07-30 | 2018-02-06 | 湖北永绍科技股份有限公司 | A kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste |
| CN108608003A (en) * | 2016-12-12 | 2018-10-02 | 昆明仁旺科技有限公司 | A kind of preparation method of ultra-thin gold foil and goldleaf powder |
| CN108889962A (en) * | 2018-07-10 | 2018-11-27 | 黑龙江大学 | A kind of preparation method of spherical shape gold/palladium bimetallic alloy assembly |
| CN110539003A (en) * | 2019-08-09 | 2019-12-06 | 无锡英特派金属制品有限公司 | Production method of palladium powder for removing palladium mirror |
| CN112809015A (en) * | 2020-12-29 | 2021-05-18 | 有研亿金新材料有限公司 | Preparation method of low-apparent-density micron palladium powder |
| CN113941712A (en) * | 2021-10-21 | 2022-01-18 | 昆明理工大学 | Preparation method of nano-scale spherical palladium powder |
| CN113953526A (en) * | 2021-10-25 | 2022-01-21 | 昆明理工大学 | Preparation method of superfine palladium powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1248503A (en) * | 1998-09-11 | 2000-03-29 | 株式会社村田制作所 | Metal power and its preparation process and electric conductivity paste |
| CN1623889A (en) * | 2003-12-04 | 2005-06-08 | 中国科学院兰州化学物理研究所 | Process for preparation metal nano partical |
| CN101020243A (en) * | 2007-03-16 | 2007-08-22 | 中国科学院长春应用化学研究所 | Nanometer Pd material and its prepn process |
-
2011
- 2011-01-25 CN CN2011100273842A patent/CN102172776A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1248503A (en) * | 1998-09-11 | 2000-03-29 | 株式会社村田制作所 | Metal power and its preparation process and electric conductivity paste |
| CN1623889A (en) * | 2003-12-04 | 2005-06-08 | 中国科学院兰州化学物理研究所 | Process for preparation metal nano partical |
| CN101020243A (en) * | 2007-03-16 | 2007-08-22 | 中国科学院长春应用化学研究所 | Nanometer Pd material and its prepn process |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107663583A (en) * | 2016-07-30 | 2018-02-06 | 湖北永绍科技股份有限公司 | A kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste |
| CN108608003A (en) * | 2016-12-12 | 2018-10-02 | 昆明仁旺科技有限公司 | A kind of preparation method of ultra-thin gold foil and goldleaf powder |
| CN108608003B (en) * | 2016-12-12 | 2021-09-17 | 昆明仁旺科技有限公司 | Preparation method of ultrathin gold foil sheet and gold foil powder |
| CN107052362A (en) * | 2017-06-15 | 2017-08-18 | 西安宏星电子浆料科技有限责任公司 | High-specific surface area ultrafine palladium powder and preparation method thereof |
| CN108889962A (en) * | 2018-07-10 | 2018-11-27 | 黑龙江大学 | A kind of preparation method of spherical shape gold/palladium bimetallic alloy assembly |
| CN110539003A (en) * | 2019-08-09 | 2019-12-06 | 无锡英特派金属制品有限公司 | Production method of palladium powder for removing palladium mirror |
| CN112809015A (en) * | 2020-12-29 | 2021-05-18 | 有研亿金新材料有限公司 | Preparation method of low-apparent-density micron palladium powder |
| CN113941712A (en) * | 2021-10-21 | 2022-01-18 | 昆明理工大学 | Preparation method of nano-scale spherical palladium powder |
| CN113941712B (en) * | 2021-10-21 | 2024-03-19 | 昆明理工大学 | Preparation method of nanoscale spherical palladium powder |
| CN113953526A (en) * | 2021-10-25 | 2022-01-21 | 昆明理工大学 | Preparation method of superfine palladium powder |
| CN113953526B (en) * | 2021-10-25 | 2024-03-15 | 昆明理工大学 | Preparation method of superfine palladium powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102172776A (en) | Method for preparing metal palladium powder | |
| WO2016023461A1 (en) | Method for preparation of a metal powder | |
| CN104174864B (en) | The preparation method of a kind of nanometer or submicron order Argent grain powder | |
| CN104211053A (en) | Preparation method of modified graphene aqueous dispersion | |
| CN105234426B (en) | Preparation method of ultrafine nano silver | |
| CN105252014A (en) | Method for preparing superfine silver powder in alkalic system | |
| CN105817641A (en) | Preparation method for producing metal powder through induction of newly-generated nanometer seed crystals | |
| CN104743613A (en) | Method for continuously preparing large-particle-size spherical cobalt carbonate | |
| CN103111306A (en) | Magnetic load type nanometer palladium/iron grain catalyst and preparation method and application thereof | |
| CN105148854A (en) | Preparation method of mesoporous silica solidified laccase printing and dyeing wastewater decolorizer | |
| CN108247077B (en) | Method for preparing copper powder by micro-reaction | |
| CN102977009B (en) | A kind of synthetic method of 2-trifluoromethyl-3-fluorine pyridine | |
| CN103881675A (en) | Long-acting active sand-controlling oil washing agent and preparation method thereof | |
| CN104478699A (en) | Preparation method of high-purity superfine cobalt oxalate powder | |
| CN103521273B (en) | Preparation method of micro-nano metal nickel-coated silicon dioxide catalyst | |
| CN102962470B (en) | Method for preparing spherical ultrafine nickel powder at room temperature | |
| CN102676164B (en) | Spherical calcium molybdate-base red phosphor and preparation method thereof | |
| CN101406963B (en) | Method for preparing nano silver powder | |
| CN104418333A (en) | Method for preparing mesoporous silica hollow spheres | |
| CN106513706B (en) | A kind of preparation method for being used for Nano Silver nucleus in ball shape silver powder production technology | |
| CN104211121A (en) | Preparation method of water soluble sodium tantalate quantum dot with low cost | |
| CN103204554B (en) | Method for preparing spherical nickel hydroxide | |
| CN102441667B (en) | La (Lanthanum) doped TiO2 powder body of coreshell structure and preparation method thereof | |
| CN107098374A (en) | Dispersed bulk morphologies carbonic acid cerium crystal and preparation method thereof | |
| CN106635007B (en) | A kind of preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110907 |