CN100427399C - Method for preparing neodymium hexaboride - Google Patents
Method for preparing neodymium hexaboride Download PDFInfo
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- CN100427399C CN100427399C CNB200610026088XA CN200610026088A CN100427399C CN 100427399 C CN100427399 C CN 100427399C CN B200610026088X A CNB200610026088X A CN B200610026088XA CN 200610026088 A CN200610026088 A CN 200610026088A CN 100427399 C CN100427399 C CN 100427399C
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Abstract
The present invention relates to a method for preparing neodymium hex boride, and belongs to the field of preparation technique of material section. The method of the present invention comprises the following specific steps of drying neodymium oxide powder and boron carbide powder at a temperature of 200 to 400 DEG C for 2 to 4 hours, evenly mixing 1 mol of neodymium oxide powder and 3 mol of boron carbide powder by a V-shaped mixer, a ball mill, etc., preparing the obtained mixed powder into a green body with a predetermined shape by a mold pressing method, a cold isostatic pressure molding method, etc., putting the green body into a vacuum sintering furnace to be sintered under the sintering conditions of a sintering temperature of 1400 DEG C to 1800 DEG C, the vacuum degree of 1*10<-1> Pa to 1*10 <-3> Pa and the sintering time of 2 to 8 hours, and cooling the sintered green body along with the furnace to obtain neodymium hex boride. The present invention can easily and quickly prepare the neodymium hex boride powder with high purity in low cost and high efficiency, and the present invention has the advantages of short production period, low price of required production equipment, and simple operation, and is suitable for industrialization mass production.
Description
Technical field
The present invention relates to a kind of method of technical field of material, specifically, that relate to is a kind of preparation method of neodymium hexaboride.
Background technology
Neodymium hexaboride (NdB
6) possess special crystalline structure, as CaB
6The simple cubic body structure that type is the same: the Nd atom occupies cubical each drift angle, and the B atom that regular octahedron is arranged is positioned at the cubes center.NdB
6The preparation method comprise: pure element synthesis method, compound reduction sintering process, B reduction sintering process, zone melting method, solvent method, vapour deposition process etc.The pure element synthesis method is to be raw material with Nd simple substance and B simple substance, carries out high temperature sintering according to 1: 6 mol ratio and directly obtains NdB
6, this method reaction sintering time generally all surpasses 10 hours, and the temperature of reaction height, is difficult to use on suitability for industrialized production.B reduction sintering process is the effect that replaces the reductibility compound to play restoring the Nd atom with B simple substance and generates NdB with its reaction
6, but because B powder price is higher, required cost also increases, and is not suitable for scale operation.By zone melting method, solvent method and vapour deposition process, though can obtain the highly purified NdB of high quality
6Material, but owing to the required preparation equipment requirements of these methods is higher, and running cost is not low, is adding the little deficiency that waits of output, and zone melting method, solvent method and vapour deposition process generally are applied to high-quality NdB
6The preparation aspect of monocrystal material.Under the protection of rare gas element, can be divided into again according to the different zones smelting process of type of heating: radio frequency heating method, electron beam heating, electric-arc heating method and LASER HEATING method etc.; Solvent method also is preparation monocrystalline NdB
6Common method, be divided into two kinds of aluminium flux method and rare earth solvent methods, utilize young brilliantly as guiding, from solution, slowly separate out NdB
6Vapour deposition process is to utilize gaseous substance to carry out chemical reaction in the subrange on the solid-state material surface, and as the need complete reaction, this synthetic method required time is longer.
Find through literature search prior art, people such as Xudong Zhao are at " Journal of Alloys andCompounds " (alloy cpd), 249 (1997) 247-250 write articles " New route for thesynthesis of boron-rich rare-earth boride NdB
6Under high pressure andhigh temperature (novel method that the down synthetic rich boronation rare earth of high-temperature and high-pressure conditions is a neodymium hexaboride) "; this article has been introduced the method for preparing neodymium hexaboride under a kind of high-temperature and high-pressure conditions; having explored neodymium hexaboride prepares the possibility of industrialization, for later research has indicated direction.But the method that this article adopted is under the condition of High Temperature High Pressure, synthesizes neodymium hexaboride with neodymium sesquioxide and boron powder as raw material.In actual production process, High Temperature High Pressure synthesis condition difficulty reaches, and then can increase the cost of neodymium hexaboride greatly as raw material with the boron powder.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of neodymium hexaboride is provided, make it have advantages such as with low cost, that condition is simple and easy, the reaction times is short, the reaction product single phase property is good, be fit to the synthetic neodymium hexaboride of scale.
The present invention is achieved by the following technical solutions, and the present invention selects Nd for use
2O
3And B
4C is a raw material, under the high-temperature vacuum condition, and solid phase synthesis neodymium hexaboride powder.Specifically comprise the steps:
(1) with raw material Nd
2O
3(neodymium sesquioxide) powder and B
4C (norbide) powder places baking oven, dries to handle 2～4 hours under 200～400 ℃ of temperature, need not in the treating processes to add shielding gas or vacuumize in baking oven.
(2) Nd of drying according to mol ratio weighing in 1: 3
2O
3Powder and B
4The C powder.Adopt blending meanss such as V-Mixer, ball mill that above-mentioned powder mixes is even, adopt a kind of known blending means, need not to take special measure, just can obtain the equally distributed mixed powder of various powder particles.
(3) the uniform mixing powder with the above-mentioned steps gained adopts methods such as compression molding, cold isostatic compaction to make green compact.The big I of green body shapes is selected voluntarily.
(4) green compact are placed vacuum sintering furnace carry out high temperature sintering, sintering temperature is 1400 ℃～1800 ℃, and vacuum tightness is 1 * 10
-1Pa～1 * 10
-3Pa, sintering time be about 2 hours～and 8 hours, furnace cooling can obtain neodymium hexaboride.
The present invention pulverizes the neodymium hexaboride that obtains, and makes finished product.Reaction equation of the present invention is:
Nd
2O
3+3B
4C＝2NdB
6+3CO(g)
Principal feature of the present invention is that generated time is short.According to the calculation of thermodynamics and the actually operating situation of reaction equation, under the sintering condition of high-temperature vacuum, help reaction and carry out.Temperature of reaction is high more, vacuum tightness is more little, and the required time that reacts completely is also just short more.Usually adopt the synthetic method of chemical combination reduction preparation neodymium hexaboride, required generated time is all more than 10 hours, take synthetic method of the present invention according to the shortest need of different sintering conditions of being taked 2 hours, the longest need can obtain the neodymium hexaboride powder of based on very high purity in 8 hours.
What the present invention adopted is compound reduction sintering process, and the sintering condition of being taked reaches easily, and is not high to equipment requirements.Compare with chemistry or floating region flux synthesis procedure, the present invention can be simple and direct, low-cost, prepare highly purified neodymium hexaboride powder expeditiously, and with short production cycle, required production unit is cheap, simple to operate, suitable industrialized mass.
Embodiment
Embodiment 1
With raw material Nd
2O
3Powder and B
4The C powder places baking oven, dries to handle 4 hours under 200 ℃ of temperature, need not in the treating processes to add shielding gas or vacuumize in baking oven.Nd wherein
2O
3Powder purity is greater than 99%, B
4C powder purity is greater than 97% (massfraction).
The Nd that weighing is dried
2O
3Powder and B
4C powder (mol ratio 1: 3).Adopt V-Mixer to mix in above-mentioned powder, the method that adopts compression molding then is the mixed powder compression moulding in the above-mentioned steps, obtains cylindric base sample (Φ 38mm * 30mm).
The base sample is placed the vacuum sintering furnace sintering, and sintering temperature is 1500 ℃, and vacuum tightness is 10
-1Pa, sintering time are 4 hours, and furnace cooling can obtain neodymium hexaboride; The neodymium hexaboride that obtains is ground.
Embodiment 2
With raw material Nd
2O
3Powder and B
4The C powder places baking oven, dries to handle 2 hours under 400 ℃ of temperature, need not in the treating processes to add shielding gas or vacuumize in baking oven.Nd wherein
2O
3Powder purity is greater than 99%, B
4C powder purity is greater than 97% (massfraction).
The Nd that weighing is dried
2O
3Powder and B
4C powder (mol ratio 1: 3).Adopt ball mill to mix in above-mentioned powder, the method that adopts compression molding then is the mixed powder compression moulding in the above-mentioned steps, obtains cylindric base sample (Φ 30mm * 20mm).
The base sample is placed the vacuum sintering furnace sintering, and sintering temperature is 1400 ℃, and vacuum tightness is 10
-2Pa, sintering time are 6 hours, and furnace cooling can obtain neodymium hexaboride; The neodymium hexaboride that obtains is ground.
Embodiment 3
With raw material Nd
2O
3Powder and B
4The C powder places baking oven, dries to handle 3 hours under 300 ℃ of temperature, need not in the treating processes to add shielding gas or vacuumize in baking oven.Nd wherein
2O
3Powder purity is greater than 99%, B
4C powder purity is greater than 97% (massfraction).
The Nd that weighing is dried
2O
3Powder and B
4C powder (mol ratio 1: 3).Adopt ball mill to mix in above-mentioned powder, the method that adopts isostatic cool pressing then is the mixed powder compression moulding in the above-mentioned steps, obtains cylindric base sample (Φ 40mm * 15mm).
The base sample is placed the vacuum sintering furnace sintering, and sintering temperature is 1800 ℃, and vacuum tightness is 10
-1Pa, sintering time are 2 hours, and furnace cooling can obtain neodymium hexaboride; The neodymium hexaboride that obtains is ground.
Embodiment 4
With raw material Nd
2O
3Powder and B
4The C powder places baking oven, dries to handle 4 hours under 300 ℃ of temperature, need not in the treating processes to add shielding gas or vacuumize in baking oven.Nd wherein
2O
3Powder purity is greater than 99%, B
4C powder purity is greater than 97% (massfraction).
The Nd that weighing is dried
2O
3Powder and B
4C powder (mol ratio 1: 3).Adopt V-Mixer to mix in above-mentioned powder, the method that adopts isostatic cool pressing then is the mixed powder compression moulding in the above-mentioned steps, obtains cylindric base sample (Φ 25mm * 20mm).
The base sample is placed the vacuum sintering furnace sintering, and sintering temperature is 1450 ℃, and vacuum tightness is 10
-3Pa, sintering time are 3 hours, and furnace cooling can obtain neodymium hexaboride; The neodymium hexaboride that obtains is ground.
Embodiment 5
With raw material Nd
2O
3Powder and B
4The C powder places baking oven, dries to handle 4 hours under 350 ℃ of temperature, need not in the treating processes to add shielding gas or vacuumize in baking oven.Nd wherein
2O
3Powder purity is greater than 99%, B
4C powder purity is greater than 97% (massfraction).
The Nd that weighing is dried
2O
3Powder and B
4C powder (mol ratio 1: 3).Adopt ball mill to mix in above-mentioned powder, the method that adopts isostatic cool pressing then is the mixed powder compression moulding in the above-mentioned steps, obtains cylindric base sample (Φ 38mm * 15mm).
The base sample is placed the vacuum sintering furnace sintering, and sintering temperature is 1500 ℃, and vacuum tightness is 10
-3Pa, sintering time are 2 hours, and furnace cooling can obtain neodymium hexaboride; The neodymium hexaboride that obtains is ground.
Claims (4)
1, a kind of preparation method of neodymium hexaboride is characterized in that, comprises the steps:
(1) with raw material Nd
2O
3Powder and B
4The C powder places baking oven, dries processing;
(2) Nd of drying according to mol ratio weighing in 1: 3
2O
3Powder and B
4The C powder mixes is even;
(3) the uniform mixing powder with the above-mentioned steps gained makes green compact;
(4) green compact are placed vacuum sintering furnace carry out high temperature sintering, sintering temperature is 1400 ℃～1800 ℃, and vacuum tightness is 1 * 10
-1Pa～1 * 10
-3Pa, sintering time are 2 hours～8 hours, and furnace cooling promptly obtains neodymium hexaboride.
2, the preparation method of neodymium hexaboride as claimed in claim 1 is characterized in that, in the described step (1), dries processing, is specially: dry under 200～400 ℃ of temperature and handled 2～4 hours.
3, the preparation method of neodymium hexaboride as claimed in claim 1 is characterized in that, in the described step (2), adopts V-Mixer or ball mill method with Nd
2O
3Powder and B
4The C powder mixes is even.
4, the preparation method of neodymium hexaboride as claimed in claim 1 is characterized in that, in the described step (3), adopts compression molding or cold isostatic pressing method to make green compact.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610026088XA CN100427399C (en) | 2006-04-27 | 2006-04-27 | Method for preparing neodymium hexaboride |
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|---|---|---|---|
| CNB200610026088XA CN100427399C (en) | 2006-04-27 | 2006-04-27 | Method for preparing neodymium hexaboride |
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| Publication Number | Publication Date |
|---|---|
| CN1843929A CN1843929A (en) | 2006-10-11 |
| CN100427399C true CN100427399C (en) | 2008-10-22 |
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|---|---|---|---|
| CNB200610026088XA Expired - Fee Related CN100427399C (en) | 2006-04-27 | 2006-04-27 | Method for preparing neodymium hexaboride |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112573925B (en) * | 2021-02-22 | 2022-09-23 | 山东合创明业精细陶瓷有限公司 | High-performance electromagnetic shielding NdB 6 /SiO 2 Complex phase ceramic material and preparation method thereof |
| CN113772711B (en) * | 2021-08-09 | 2022-07-05 | 北京科技大学 | Method for preparing rare earth metal hexaboride through aluminothermic reduction |
| CN115180632B (en) * | 2022-07-15 | 2023-11-14 | 贵州交通职业技术学院 | Controllable preparation method and application of morphology of rare earth hexaboride nano powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0409717A1 (en) * | 1989-07-21 | 1991-01-23 | Rhone-Poulenc Chimie | Sintering process for rare earth boride |
| US4999176A (en) * | 1988-04-22 | 1991-03-12 | Rhone-Poulenc Chimie | Preparation of rare earth borides |
| US5176890A (en) * | 1987-11-26 | 1993-01-05 | Rhone-Poulenc Chimie | Preparation of rare earth borides |
-
2006
- 2006-04-27 CN CNB200610026088XA patent/CN100427399C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5176890A (en) * | 1987-11-26 | 1993-01-05 | Rhone-Poulenc Chimie | Preparation of rare earth borides |
| US4999176A (en) * | 1988-04-22 | 1991-03-12 | Rhone-Poulenc Chimie | Preparation of rare earth borides |
| EP0409717A1 (en) * | 1989-07-21 | 1991-01-23 | Rhone-Poulenc Chimie | Sintering process for rare earth boride |
Non-Patent Citations (4)
| Title |
|---|
| 富硼稀土硼化物NdB6的高温高压合成. 赵旭东等.高压物理学报，第10卷第3期. 1996 |
| 富硼稀土硼化物NdB6的高温高压合成. 赵旭东等.高压物理学报，第10卷第3期. 1996 * |
| 自蔓延高温合成LaB6微粉的制备及表征. 张廷安等.东北大学学报（自然科学版），第26卷第1期. 2005 |
| 自蔓延高温合成LaB6微粉的制备及表征. 张廷安等.东北大学学报（自然科学版），第26卷第1期. 2005 * |
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Granted publication date: 20081022 Termination date: 20110427 |