CN1297485C - Preparation of rare earth ammonium bimolybdate - Google Patents
Preparation of rare earth ammonium bimolybdate Download PDFInfo
- Publication number
- CN1297485C CN1297485C CNB2004100734143A CN200410073414A CN1297485C CN 1297485 C CN1297485 C CN 1297485C CN B2004100734143 A CNB2004100734143 A CN B2004100734143A CN 200410073414 A CN200410073414 A CN 200410073414A CN 1297485 C CN1297485 C CN 1297485C
- Authority
- CN
- China
- Prior art keywords
- nitrate
- preparation
- solution
- ammonium
- rare earth
- 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.)
- Expired - Fee Related
Links
Abstract
The present invention discloses a preparation method of rare earth ammonium dimolybdate, which has the advantages of improvement on the processing and service performance of material, simultaneous reduction of production cost and reduction of environment pollution. A solution mixed by soft water and ammonia water with the proportion of (4 to 5L): 1L is added to a crystallization tank and stirred, then ammonium tetramolybdate is added in batches according to the proportion that ammonium tetramolybdate: soft water: ammonia water = 1kg: (4 to 5 L): 1L. The mixed solution is heated and stirred to obtain a mother solution with a pH value regulated to 7 to 8.5, and one of cerium nitrate, lanthanum nitrate and yttrium nitrate, or the compound of two or all of cerium nitrate, lanthanum nitrate and yttrium nitrate, which accounts for not more than 2.5 mass% of ammonium dimolybdate, is slowly added to the mother solution. The mixed solution is heated and evaporated for 2 to 6 hours at a heating temperature of 100 to 130 DEG C until the solution is clarified, and the solution with material discharged is drawn, filtered and dried for 6 to 8 hours at a heating temperature of 110 to 150 DEG C to prepare rare earth ammonium dimolybdate.
Description
Technical field
The present invention relates to the molybdenum alloy preparation field, particularly a kind of preparation technology of rare earth ammonium dimolybdate.
Background technology
Molybdenum has very important purposes with its good high-temperature performance at row such as national defence, electronics, metallurgy, machinery, illuminations, therefore becomes the rare metal with strategic value.But because characteristics such as the anti-oxidant and low temperature brittleness of molybdenum are difficult to satisfy higher performance requriements, for this reason, the material expert by dispersion-strengthened, melt mechanism such as reinforcement, precipitation strength admittedly, constantly improve the performance of molybdenum material.For the alloy preparation of above-mentioned strengthening mechanism, its prerequisite all is the homogeneity that requirement improves alloying constituent, and promptly alloying constituent is tiny, is evenly distributed.Rare earth element has higher activity, has purification at the molybdenum alloy material, strengthens crystal boundary, and the effect of pinning dislocation becomes one of key component of preparation high-quality molybdenum alloy material.Current, rare earth molybdenum alloy has become and anotherly after the TZM alloy has had a very alloy material of potentiality, and development prospect is good.China is molybdenum big producing country, also is rare earth metal big producing country, has the advantageous advantage of the rare earth molybdenum of first developing metal alloy, to the development regional economy, promotes the China molybdenum product restructuring to have very important realistic meaning.
In molybdenum metal powder metallurgical production process, the deamination material that high-purity three oxidations are ammonium molybdates.And ammonium molybdate is the critical process that purifies the purification molybdenum, and molybdenum compound is to exist with the solution form before this operation ammonium molybdate crystallization, and after this compound of molybdenum occurs with the powder particle form.High-purity molybdic oxide is the material that only is dissolved in ammonia, carry out liquid-liquid and mix, also only after ammonia is molten, just can carry out, and ammonia nitrogen is the environmental pollution thing that is difficult to handle, and be to be limited therefore in Europe.Foreign side shows the strict quality requirement of the high-purity molybdic oxide of import and relevant technical literature, the solid adding mode of foreign side's production high-performance molybdenum alloy second phase composition with solid-with liquid-solid carrying out.But no matter take which type of mode, all can not reach the adulterated effect of molecular level.
By domestic and international identical molybdenum alloy product tissue and composition analysis, the refinement of the second phase particle and homogenize are to improve the key of material property.
Summary of the invention
The object of the invention provides a kind of preparation technology who can be used in the rare earth oxide ammonium dimolybdate of scale operation, refinement, the homogenize molybdenum alloy second phase particle size, and the processing and the use properties of raising material reduce production costs simultaneously, reduce environmental pollution.
Technical scheme of the present invention is to solve like this:
1) preparation of nitrate solution:
A. the preparation of lanthanum nitrate or yttrium nitrate solution:
Get lanthanum trioxide, yttrium oxide, in the ratio of lanthanum trioxide or yttrium oxide: nitric acid=1kg: 2～2.5L, heated and stirred, Heating temperature are 100 ℃～200 ℃, promptly can be made into lanthanum nitrate or yttrium nitrate solution up to the solution clarification; Or
B. the preparation of cerous nitrate solution, at first according to cerium oxide: soft water=1kg: 2～3L ratio is mixed with suspension, is hydrogen peroxide with hydrogen peroxide again: suspension is that 1: 3～5 ratios add according to volume ratio, and manual the stirring forms mixing solutions; Then, according to nitric acid: cerium oxide=2～3L: the 1kg ratio joins in the mixing solutions, stirs, and 200 ℃-300 ℃ of Heating temperatures can be made into cerous nitrate solution until clarification;
2) preparation of mother liquor: the ratio of soft water and ammoniacal liquor is that 4～5L: 1L adds in the crystallizer tank, stir, add ammonium tetramolybdate then in batches, ammonium tetramolybdate: soft water: ammoniacal liquor=1kg: 4-5L: 1L, heated and stirred, 90 ℃～150 ℃ of Heating temperatures, stirring velocity is 100～120r/min, form mother liquor, the pH value of mother liquor is adjusted between 7～8.5, density is 1.25～1.35g/cm
3Between;
3) in mother liquor, slowly add cerous nitrate, lanthanum nitrate or Yttrium trinitrate or its make up or three kinds of combinations in twos, its cerous nitrate, lanthanum nitrate or Yttrium trinitrate or its make up in twos or the total mass percentage composition of three kinds of combinations is no more than 2.5% of ammonium dimolybdate total mass, when it makes up or three kinds of whens combination in twos, in total mass is no more than 2.5% scope of ammonium dimolybdate total mass, each component content can be arbitrarily than, heating evaporation 2.0～6.0 hours, 100 ℃～130 ℃ of Heating temperatures, till the solution clarification, material is emitted suction filtration, oven dry, bake out temperature is 110～150 ℃, 6～8 hours time, moisture less than 2～5.0%, promptly get the rare earth ammonium dimolybdate.
Described nitric acid mass percent concentration is 65-68%.
The present invention mixes by liquid liquid between rare earths salt and the solvable molybdenum salts solution, realizes molecular level doping effect.By the projection electron microscopy observation, the rare earth molybdenum alloy second phase particle size for preparing by the rare earth ammonium dimolybdate reaches 80 nanometers, is far superior to the level of liquid-solid doping 300～500 nanometers.The material microhardness descends 30% and 25% respectively than the rare earth molybdenum bar base of the same content that solid and liquid-solid method are produced.Materials processing and use properties are had significantly raising, and the line cutting silk life-span improves more than 2 times.
So the present invention has stopped liquid simultaneously the pollution problem that doped molybdenum exists in producing, prepare to have that the particle crystalline form is complete, yardstick is big, and non-reunion, the ammonium dimolybdate of distribution normal state guarantees the molybdenum powder good processing properties.
Specific embodiment
Embodiment one
The preparation of nitrate solution: in the ratio of lanthanum trioxide: nitric acid=1kg: 2.5L, the 742g lanthanum trioxide is placed in the beaker, adding 1.5L mass percent concentration is 65% nitric acid, heated and stirred, Heating temperature is 140 ℃, and suitably manual the stirring can make lanthanum nitrate up to the solution clarification;
The preparation of mother liquor: add soft water and ammoniacal liquor earlier and stir, add ammonium tetramolybdate then in batches, its ammonium tetramolybdate: soft water: ammoniacal liquor=1kg: 4L: 1L, heated and stirred, 110 ℃ of Heating temperatures, stirring velocity are 120r/min, form mother liquor.Adjust mother liquor pH value 7.4 by adding ammoniacal liquor, density is 1.26g/cm
3Between.
Slowly add lanthanum nitrate in mother liquor, the total mass percentage composition is no more than 2.5% of ammonium dimolybdate total mass, continues stirring heating 4.5 hours, feed liquid is poured out, suction filtration, oven dry, bake out temperature is 110 ℃, form the rare earth ammonium dimolybdate, 6 hours time, promptly get the rare earth ammonium dimolybdate.
Embodiment two
With 38g cerium oxide and soft water ratio is that the ratio of 1Kg: 2L is mixed with suspension, and again with hydrogen peroxide: suspension is that 1: 4 ratio adds according to volume ratio, and manual the stirring forms mixing solutions; Then, according to nitric acid: cerium oxide is that the ratio of 1kg: 2.5L joins in the mixing solutions, and the nitric acid mass percent concentration is 66%, stirs, and Heating temperature is 260 ℃, promptly can be made into cerous nitrate up to the solution clarification;
Is that the ratio of 4L: 1L adds respectively in the crystallizer tank with 40L soft water and 10L ammoniacal liquor according to volume ratio, stirs, and adds ammonium tetramolybdate 20kg then, heated and stirred, and 120 ℃ of Heating temperatures, stirring velocity are 120r/min, form mother liquor.The pH value of mother liquor is adjusted between 7.2, and density is 1.3g/cm
3Between.
Slowly add cerous nitrate solution in mother liquor, the quality percentage composition of cerous nitrate is no more than 4%, heating evaporation 6.0 hours, 120 ℃ of Heating temperatures, till the solution clarification, material is emitted suction filtration, oven dry, bake out temperature is 115 ℃, 6 hours time, promptly gets the rare earth ammonium dimolybdate.
Embodiment three
With yttrium oxide 60g, according to the ratio adding beaker of yttrium oxide: nitric acid=1kg: 2L, heated and stirred, Heating temperature are 130 ℃, promptly can be made into yttrium nitrate solution up to the solution clarification; The nitric acid mass percent concentration is 67%.
With 40L soft water and 8L ammoniacal liquor according to 5L: the 1L ratio adds crystallizer tank respectively, stirs, and adds ammonium tetramolybdate 20kg then, heated and stirred, 120 ℃ of Heating temperatures, stirring velocity are 120r/min, form mother liquor.Adjust pH value to 7.8, density is at 1.25g/cm
3The time.
In mother liquor, slowly add yttrium nitrate solution, the total mass percentage composition of yttrium nitrate solution is no more than 2.5% of ammonium dimolybdate total mass, can be with any than mixing, evaporative crystallization, the time is 3.0 hours, 110 ℃ of Heating temperatures, when density reaches 1.48, blowing through centrifugal fall dried, the oven dry treatment temp be 120,7 hours time, form the rare earth ammonium dimolybdate.
Embodiment four
Get lanthanum trioxide, each 20g of yttrium oxide puts into beaker, in lanthanum trioxide and yttrium oxide: nitric acid=1kg: it is 65% nitric acid that the 2.5L ratio is added mass percent concentration, the manual stirring, hot plate heating then, 140 ℃ of Heating temperatures, 5 hours time,, promptly can be made into lanthanum nitrate and Yttrium trinitrate mixing solutions up to the solution clarification;
Soft water 50L and ammoniacal liquor 10L is first according to 5L: the 1L ratio adds respectively in the crystallizer tank, adds ammonium tetramolybdate 15kg then, and 140 ℃ of Heating temperatures, stirring velocity are 120r/min, and dissolving forms mother liquor fully.The pH value of mother liquor is adjusted in 8.5, and density is 1.30g/cm
3
In mother liquor, slowly add lanthanum nitrate and Yttrium trinitrate mixing solutions, the total mass percentage composition is no more than 2.5% of ammonium dimolybdate total mass, can be with any than mixing heating evaporation 4.0 hours, 140 ℃ of Heating temperatures, evaporation time 4h, material is emitted, suction filtration, oven dry, bake out temperature is 120 ℃, 8 hours time, promptly get the compound ammonium dimolybdate of rare earth lanthanum oxide and yttrium oxide.
Embodiment five
The preparation method makes lanthanum nitrate hexahydrate with embodiment 2 with the 38g lanthanum trioxide.
Get the 20g cerium oxide and put into beaker, according to cerous nitrate: soft water=1kg: 2～3L ratio adds soft water and is mixed with suspension, adds hydrogen peroxide (H while stirring
2O
2), volume is 0.2～0.3 of a suspension vol.React the post-heating that finishes, Heating temperature is 140 ℃ then, 1 hour time.Then according to nitric acid: cerium oxide=2L: 1kg ratio adding mass percent concentration is 68% nitric acid, continues heating, can be made into cerous nitrate solution until clarification;
Above-mentioned two kinds of solution are mixed, obtain the mixing solutions of lanthanum nitrate and cerous nitrate.
The preparation of mother liquor: 50L soft water and 10L ammoniacal liquor is first according to 4L: the 1L ratio adds in the crystallizer tank, adds ammonium tetramolybdate 15kg then, heated and stirred, and 130 ℃ of Heating temperatures, stirring velocity are 120r/min, form mother liquor.The pH value of mother liquor is adjusted in 8.0, and density is 1.28g/cm
3
The mixing solutions that in mother liquor, slowly adds lanthanum nitrate and cerous nitrate, the total mass percentage composition is no more than 2.5% of ammonium dimolybdate total mass, can be with any than mixing, 130 ℃ of Heating temperatures, stirring velocity are 100r/min, heating evaporation 5.0 hours, material is emitted, suction filtration, oven dry, bake out temperature is 110 ℃, 6 hours time, promptly get the rare earth ammonium dimolybdate.
Embodiment six
According to embodiment 4 the 40g yttrium oxide is configured to yttrium nitrate solution, the preparation method is configured to cerous nitrate solution with embodiment 5 with the 20g cerium oxide, then both is mixed, and forms cerous nitrate and Yttrium trinitrate mixing solutions.
The preparation of mother liquor: soft water 45L and 10L ammoniacal liquor is first according to 4.5L: the 1L ratio adds in the crystallizer tank, stirs, and adds ammonium tetramolybdate 15kg then, heated and stirred, and 120 ℃ of Heating temperatures, stirring velocity are 120r/min, form mother liquor.The pH value of mother liquor is adjusted in 8.0, and density is 1.26g/cm
3
In mother liquor, slowly add cerous nitrate and Yttrium trinitrate mixing solutions, the total mass percentage composition is no more than 2.5% of ammonium dimolybdate total mass, can be with any than mixing heating evaporation 5.0 hours, 120 ℃ of Heating temperatures, stirring velocity is 120r/min, and heating evaporation 4.0 hours is emitted material, suction filtration, oven dry, bake out temperature is 130 ℃, 8 hours time, promptly gets cerium oxide and yttrium oxide compound rare-earth ammonium dimolybdate.
Embodiment seven
Respectively 20g lanthanum trioxide, cerium oxide, yttrium oxide are made nitrate solution, mix forming mixing solutions then.
The preparation of mother liquor: 50L soft water and 10L ammoniacal liquor is first according to 5L: the 1L ratio adds in the crystallizer tank, adds ammonium tetramolybdate 20kg then, heated and stirred, and 110 ℃ of Heating temperatures, stirring velocity are 100r/min, form mother liquor.The pH value of mother liquor is adjusted in 7.4, and density is 1.32g/cm
3
In mother liquor, slowly add three kinds of nitrate mixed solutions, the total mass percentage composition is no more than 2.5% of ammonium dimolybdate total mass, can be with any than mixing heating evaporation 5.0 hours, 120 ℃ of Heating temperatures, stirring velocity is 100r/min, and crystallization time 5.5 hours is emitted material, suction filtration, oven dry, bake out temperature is 110 ℃, 8 hours time, promptly gets the rare earth ammonium dimolybdate.
Claims (2)
1, preparation of rare earth ammonium bimolybdate is characterized in that,
1) preparation of nitrate solution: the preparation of a. lanthanum nitrate or yttrium nitrate solution:
Get lanthanum trioxide, yttrium oxide, in the ratio of lanthanum trioxide or yttrium oxide: nitric acid=1kg: 2～2.5L, heated and stirred, Heating temperature are 100 ℃～200 ℃, promptly can be made into lanthanum nitrate or yttrium nitrate solution up to the solution clarification; Or
B. the preparation of cerous nitrate solution:
At first according to cerium oxide: soft water=1kg: 2～3L ratio is mixed with suspension, is hydrogen peroxide with hydrogen peroxide again: suspension is that 1: 3～5 ratios add according to volume ratio, and manual the stirring forms mixing solutions; Then, according to nitric acid: cerium oxide=2～3L: the 1kg ratio joins in the mixing solutions, stirs, and 200 ℃-300 ℃ of Heating temperatures can be made into cerous nitrate solution until clarification;
2) preparation of mother liquor: the ratio of soft water and ammoniacal liquor is that 4～5L: 1L adds in the crystallizer tank, stir, add ammonium tetramolybdate then in batches, ammonium tetramolybdate: soft water: ammoniacal liquor=1kg: 4-5L: 1L, heated and stirred, 90 ℃～150 ℃ of Heating temperatures, stirring velocity is 100～120r/min, form mother liquor, the pH value of mother liquor is adjusted between 7～8.5, density is 1.25～1.35g/cm
3Between;
3) in mother liquor, slowly add cerous nitrate, lanthanum nitrate or Yttrium trinitrate or it makes up or three kinds of combinations in twos, its cerous nitrate, lanthanum nitrate or Yttrium trinitrate or its make up in twos or the total mass percentage composition of three kinds of combinations is no more than 2.5% of ammonium dimolybdate total mass, heating evaporation 2.0～6.0 hours, 100 ℃～130 ℃ of Heating temperatures till the solution clarification, are emitted material, suction filtration, oven dry, bake out temperature is 110～150 ℃, 6～8 hours time, promptly gets the rare earth ammonium dimolybdate.
2, preparation of rare earth ammonium bimolybdate according to claim 1 is characterized in that, described nitric acid mass percent concentration is 65%-68%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100734143A CN1297485C (en) | 2004-12-16 | 2004-12-16 | Preparation of rare earth ammonium bimolybdate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100734143A CN1297485C (en) | 2004-12-16 | 2004-12-16 | Preparation of rare earth ammonium bimolybdate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1644512A CN1644512A (en) | 2005-07-27 |
| CN1297485C true CN1297485C (en) | 2007-01-31 |
Family
ID=34869005
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100734143A Expired - Fee Related CN1297485C (en) | 2004-12-16 | 2004-12-16 | Preparation of rare earth ammonium bimolybdate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1297485C (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402682C (en) * | 2005-10-27 | 2008-07-16 | 西安交通大学 | Fine crystal rare earth oxide molybdenum alloy-doped and its preparation method |
| CN101250067B (en) * | 2008-03-20 | 2010-12-08 | 中南大学 | Method for producing chemical fertilizer by precipitating ammonium molybdate mother liquor |
| CN101643874B (en) * | 2009-09-15 | 2011-08-17 | 金堆城钼业光明（山东）股份有限公司 | Rare earth ammonium tetramolybdate preparation method |
| CN102060329A (en) * | 2010-11-01 | 2011-05-18 | 金堆城钼业股份有限公司 | Method for preparing lanthanum-doped ammonium octamolybdate |
| CN102010007B (en) * | 2011-01-12 | 2012-06-27 | 中南大学 | Method for producing industrial-grade ammonium dimolybdate by combination method |
| CN105502501B (en) * | 2015-12-02 | 2017-08-11 | 辽宁天桥新材料科技股份有限公司 | A kind of ammonium dimolybdate automates the production technology of continuous crystallisation |
| CN106115782B (en) * | 2016-06-17 | 2017-07-18 | 天津大学 | A kind of ultra-thin sheet material of the rare earth molybdate of morphology controllable and preparation method thereof |
| CN109678506B (en) * | 2019-03-06 | 2021-03-19 | 宁波大学 | Preparation method of erbium oxide transparent ceramic |
| CN109987630B (en) * | 2019-04-11 | 2020-07-28 | 西安交通大学 | Nano-grade rare earth oxide doped powder and preparation method thereof |
| CN111187958B (en) * | 2020-02-19 | 2021-01-19 | 西安交通大学 | Mo powder/MoO2Method for preparing nano lanthanum-molybdenum oxide alloy by doping with lanthanum ammonium molybdate powder |
| CN111547768A (en) * | 2020-04-26 | 2020-08-18 | 金堆城钼业股份有限公司 | Preparation method for preparing rare earth ammonium dimolybdate by nano doping |
| CN112453401B (en) * | 2020-12-04 | 2021-12-28 | 西安交通大学 | Method for reducing anisotropy of rare earth molybdenum alloy material |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0754092A (en) * | 1993-08-11 | 1995-02-28 | Tokyo Tungsten Co Ltd | Electrode for heating and pressure welding |
| US5437744A (en) * | 1993-01-28 | 1995-08-01 | Rhenium Alloys, Inc. | Molybdenum-rhenium alloy |
| JPH07242491A (en) * | 1994-03-02 | 1995-09-19 | Natl Res Inst For Metals | Dispersion strengthening molybdenum single crystal and production thereof |
| US5606141A (en) * | 1994-07-05 | 1997-02-25 | Schwarzkopf Technologies Corporation | Electrical conductor in lamps |
| CN1269426A (en) * | 1999-04-06 | 2000-10-11 | 株洲硬质合金厂 | Preparation of doped molybdenum-base alloy |
| JP2002363663A (en) * | 2001-06-13 | 2002-12-18 | Allied Material Corp | Molybdenum sheet and manufacturing method therefor |
| CN1389890A (en) * | 2002-07-24 | 2003-01-08 | 北京工业大学 | Ternary RE-Mo secondary emitting material and its prepn. |
| CN1480404A (en) * | 2003-07-22 | 2004-03-10 | 株洲硬质合金集团有限公司 | Method for preparing high pure ammonium paramolybdate |
-
2004
- 2004-12-16 CN CNB2004100734143A patent/CN1297485C/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5437744A (en) * | 1993-01-28 | 1995-08-01 | Rhenium Alloys, Inc. | Molybdenum-rhenium alloy |
| JPH0754092A (en) * | 1993-08-11 | 1995-02-28 | Tokyo Tungsten Co Ltd | Electrode for heating and pressure welding |
| JPH07242491A (en) * | 1994-03-02 | 1995-09-19 | Natl Res Inst For Metals | Dispersion strengthening molybdenum single crystal and production thereof |
| US5606141A (en) * | 1994-07-05 | 1997-02-25 | Schwarzkopf Technologies Corporation | Electrical conductor in lamps |
| CN1269426A (en) * | 1999-04-06 | 2000-10-11 | 株洲硬质合金厂 | Preparation of doped molybdenum-base alloy |
| JP2002363663A (en) * | 2001-06-13 | 2002-12-18 | Allied Material Corp | Molybdenum sheet and manufacturing method therefor |
| CN1389890A (en) * | 2002-07-24 | 2003-01-08 | 北京工业大学 | Ternary RE-Mo secondary emitting material and its prepn. |
| CN1480404A (en) * | 2003-07-22 | 2004-03-10 | 株洲硬质合金集团有限公司 | Method for preparing high pure ammonium paramolybdate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1644512A (en) | 2005-07-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1297485C (en) | Preparation of rare earth ammonium bimolybdate | |
| CN1027890C (en) | Process for preparing rare earth ammonium double oxalate and use for preparing rare earth oxidate | |
| CN103182302B (en) | Rare earth Zr based composite oxide with nucleocapsid structure and its preparation method and application | |
| CN111276688B (en) | Cerium-zirconium co-doped porous structure cathode material and preparation method thereof | |
| JP5754416B2 (en) | Method for producing nickel cobalt composite hydroxide | |
| CN108456331A (en) | A kind of metal-organic framework materials are the preparation method of the vulcanizing activator of carrier | |
| CN1280200C (en) | Prepn process of nano silver iodide powder | |
| CN103011240A (en) | Bulky-grain rare earth carbonate and preparation method and application of carbonate | |
| CN107629482B (en) | Preparation method of nano bismuth vanadate orange inorganic pigment | |
| CN102627454A (en) | Preparation method for indium tin oxide (ITO) powder and preparation method for ITO sintering body | |
| CN101342597A (en) | Process for producing nano-scale W-Cu composite powder with even dispersion | |
| CN109928510B (en) | ZVI reduction coupling microorganism-based Schwerner mineral preparation method | |
| CN113385138A (en) | Preparation method and application of Schneider mineral | |
| CN111017994B (en) | Preparation method of nano green-phase bismuth yellow vanadate powder | |
| CN113562782A (en) | Tungsten and lanthanum double-doped co-coated ternary positive electrode precursor and preparation method thereof | |
| CN117247092A (en) | Fluorine removing agent for fluorine-containing wastewater treatment and preparation method thereof | |
| CN113571693A (en) | Modified ternary positive electrode material precursor of lithium ion battery and preparation method thereof | |
| CN108557792A (en) | A kind of preparation method of cladded type iron manganese phosphate | |
| CN1364730A (en) | Method for preparing super-fine nanometer ferric oxide powder | |
| CN112591801A (en) | Preparation method of Z-shaped hexaferrite ultrafine powder | |
| CN113336304B (en) | Preparation method and application of high-purity silver-doped bismuth tungstate nano antibacterial fiber membrane | |
| CN106635007B (en) | A kind of preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor | |
| CN105800688B (en) | A kind of method that solid phase roasting prepares vanadic sulfate | |
| CN111730063B (en) | Preparation method of lead nanowire | |
| JP5967264B2 (en) | Method for producing positive electrode active material for non-aqueous electrolyte secondary battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160414 Address after: 276017, building 308, third floor, innovation building, hi tech Zone, Shandong, Linyi Patentee after: Linyi Kechuang Material Co. Ltd. Address before: 710049 Xianning Road, Shaanxi, China, No. 28, No. Patentee before: Xi'an Jiaotong University |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070131 Termination date: 20171216 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |