CN108152355A - A kind of rare earth pyrophoric alloy Standard Reference Materials for Determination and preparation method thereof - Google Patents
A kind of rare earth pyrophoric alloy Standard Reference Materials for Determination and preparation method thereof Download PDFInfo
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- CN108152355A CN108152355A CN201711063371.4A CN201711063371A CN108152355A CN 108152355 A CN108152355 A CN 108152355A CN 201711063371 A CN201711063371 A CN 201711063371A CN 108152355 A CN108152355 A CN 108152355A
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- alloy
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
The invention belongs to chemometric techniques fields.Using cerium system rare earth alloy as matrix, the modifying element of grade doping desired amount, cover rare earth pyrophoric alloy element species and content range.Certified Reference Material Homogeneity is solved the problems, such as using intermediate alloy secondary smelting technology.The present invention relates to rare earth pyrophoric alloy Standard Reference Materials for Determination, are the alloy powder that rare earth element and modifying element simple substance form, by the sample composition of 3~5 graded elementals；The quality group of element becomes lanthanum 18.5%~22.5%, cerium 29.5%~40%, praseodymium 3%~4.5%, neodymium 12%~14%, iron 18.5%~23%, magnesium 2%~3%, copper 1%~2.5%, zinc 0.5%~2.5%.The present invention relates to rare earth pyrophoric alloy Standard Reference Materials for Determination, ingredient designability is strong, controllability is good, uniformity, stability are good, diameter of particle and Elemental redistribution are uniform, element broad covered area, and the content distribution of elements is reasonable, suitable for the calibrating and calibration of elemental analysis equipment and instrument, the preparation especially suitable for Standard Reference Materials for Determination.
Description
Technical field
The invention belongs to chemometric techniques field, be related to chemical composition amount analysis measuring technique, more particularly to chemistry into
Divide standard matter preparing technology.
Background technology
Rare earth pyrophoric alloy, also known as rare earth pyrophoric metal, are with mixed rare earth alloy（Cerium constituent element element based on cerium）It mixes
The alloy that miscellaneous iron and a small amount of magnesium, zinc, copper are prepared has the characteristics that have and is under fire that efficient, hardness is big, corrosion-resistant and wear-resisting,
It is widely used in each field such as daily life and national defense industry.
Tradition prepares rare earth pyrophoric alloy mainly using melting once method, i.e., is once added to after all raw material is crushed
It is prepared in vaccum sensitive stove.
CN102787357 A " a kind of mixed rare-earth pyrophoric metal and preparation method thereof " using by lanthanum, cerium, iron, zinc,
Manganese and aluminium score by weight weigh raw material and cut into fritter, and each component is put into smelting furnace together, carry out high temperature melting
Refining.
The ignition quality of existing literature report concern rare earth pyrophoric alloy material, uniformity, stability to sample have no
Report.Up to the present, rare earth pyrophoric alloy Standard Reference Materials for Determination is there are no in the standard substance issued both at home and abroad.
Invention content
The present invention is intended to provide it is a kind of simultaneously containing lanthanum, cerium, praseodymium, neodymium, iron, magnesium, copper, Zn-ef ficiency rare earth pyrophoric alloy into
Divide analytical standard substance and preparation method thereof, to solve the problems, such as that rare earth pyrophoric alloy composition detection lacks standard sample.This hair
Preparation method bright while that the standard substance is provided.
The object of the present invention is achieved like this, using cerium system rare earth alloy as matrix, the modified member of grade doping desired amount
Element, cover rare earth pyrophoric alloy element species and content range.Using intermediate alloy secondary smelting technology solution award of bid
Quasi- substance homogeneity question.
Preparation process is operated using anoxybiotic, solves the problems, such as that rare earth element is oxidizable, while realizes standard substance ingredient standard
Really control.Standard substance is crushed by granulating using vacuum ball mill, it is ensured that the stability of standard substance process.
The present invention relates to rare earth pyrophoric alloy Standard Reference Materials for Determination, are that rare earth element and modifying element simple substance form
Alloy powder, by the sample composition of 3~5 graded elementals；The quality group of element become lanthanum 18.5%~22.5%, cerium 29.5%~
40%, praseodymium 3%~4.5%, neodymium 12%~14%, iron 18.5%~23%, magnesium 2%~3%, copper 1%~2.5%, zinc 0.5%~2.5%.
The present invention relates to rare earth pyrophoric alloy Standard Reference Materials for Determination, it is characterised in that：Diameter of particle is less than 60 mesh.
The present invention relates to the preparation methods of rare earth pyrophoric alloy Standard Reference Materials for Determination, including intermediate alloy melting, wait
Select object alloy melting, granulation, packaging and definite value process, it is characterised in that：
Intermediate alloy melting：By lanthanum, cerium, praseodymium, neodymium, iron melting, intermediate alloy is obtained；
Candidate alloy melting：Intermediate alloy and magnesium, copper, Zinc smelting are obtained into candidate alloy；
It is granulated：It is crushed using vacuum or noble gas protection ball-milling technology, obtains candidate alloy powder.
The present invention relates to the preparation methods of rare earth pyrophoric alloy Standard Reference Materials for Determination, including intermediate alloy melting, wait
Select object alloy melting, granulation, packaging and definite value process, it is characterised in that：Candidate alloy melting process, magnesium excessive 5%~10%.
The present invention relates to the preparation methods of rare earth pyrophoric alloy Standard Reference Materials for Determination, including intermediate alloy melting, wait
Select object alloy melting, granulation, packaging and definite value process, it is characterised in that：Raw metal used is simple substance, and purity is not less than 99%.
The present invention relates to the preparation method of rare earth pyrophoric alloy Standard Reference Materials for Determination, including intermediate alloy melting, most
Whole alloy melting, granulation, packaging and definite value process, it is characterised in that：Noble gas described in granulation process is argon gas.
The present invention relates to the preparation method of rare earth pyrophoric alloy Standard Reference Materials for Determination, including intermediate alloy melting, most
Whole alloy melting, granulation, packaging and definite value process, it is characterised in that：Packaging process carries out in vacuum glove box.
The present invention relates to rare earth pyrophoric alloy Standard Reference Materials for Determination, and ingredient designability is strong, and controllability is good, uniformly
Property, stability it is good, diameter of particle and Elemental redistribution are uniform, element broad covered area, and the content distribution of elements is reasonable, suitable for element point
The calibrating and calibration of analysis equipment and instrument, the preparation especially suitable for Standard Reference Materials for Determination.
Specific embodiment
The technical solution being related to reference to specific embodiment to invention is described further, but is related to not as to invention
And the limitation of the particular content of technical solution.
Embodiment one
For preparing 2kg rare earth pyrophoric alloy Standard Reference Materials for Determination, preparation method is as follows：
Weigh cerium（Purity is 99.2%）0.8 kg, lanthanum（Purity is 99.5%）0.4 kg, praseodymium（Purity is 99.2%）0.06 kg, neodymium
（Purity is 99.1%）0.24 kg, iron（Purity is 99.5%）0.45 kg is put into magnesia crucible, is evacuated to 10 Pa, so
After be filled with nitrogen as protective gas, be warming up to after material all melts, be uniformly mixed using electromagnetic agitation, after keeping the temperature 5min,
It is crushed after casting cooling, intermediate alloy is made.
Weigh magnesium（Purity is 99.5%）0.04 kg, copper（Purity is 99.5%）0.02 kg, zinc（Purity is 99.4%）0.02
Kg is put into after crushing in the magnesia crucible for filling intermediate alloy, is evacuated to 10 Pa, is filled with nitrogen as protection gas
Body after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, and after keeping the temperature 5min, candidate is made in casting after cooling
Alloy.
It is broken into the fritter of 4cm × 4cm.Fritter is put into ball grinder, inflated with nitrogen screws lid postposition as protective atmosphere
In ball mill, sieving is taken out after ball milling 4h, sieving granularity is 60 mesh, and candidate alloy powder is made.
Candidate alloy powder is sub-packed in clean tool plug vial in vacuum glove box.
Definite value is carried out using inductively coupled plasma emission spectrography.Constituent content is：Lanthanum 18.6%, cerium 39.6%, praseodymium
3.0%, neodymium 11.8%, magnesium 1.8%, iron 22.5%, copper 1.0%, zinc 0.95%.
Embodiment two
For preparing 2kg rare earth pyrophoric alloy Standard Reference Materials for Determination, preparation method is as follows：
Weigh cerium（Purity is 99.2%）0.65 kg, lanthanum（Purity is 99.5%）0.43 kg, praseodymium（Purity is 99.2%）0.08 kg、
Neodymium（Purity is 99.1%）0.25 kg, iron（Purity is 99.5%）0.43 kg is put into magnesia crucible, is evacuated to 10 Pa,
Nitrogen is then charged with as protective gas, after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, keeps the temperature 5 min
Afterwards, it is crushed after casting cooling, intermediate alloy is made.
Weigh magnesium（Purity is 99.5%）0.06 kg, copper（Purity is 99.5%）0.05 kg, zinc（Purity is 99.4%）0.05
Kg is put into after crushing in the magnesia crucible for filling intermediate alloy, is evacuated to 10 Pa, is filled with nitrogen as protection gas
Body after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, and after keeping the temperature 5 min, casting is made candidate after cooling
Object alloy.
It is broken into the fritter of the cm of 4 cm × 4.Fritter is put into ball grinder, inflated with nitrogen is as protective atmosphere, after screwing lid
It is placed in ball mill, sieving is taken out after ball milling 4h, sieving granularity is 60 mesh, and candidate alloy powder is made.
Candidate alloy powder is sub-packed in clean tool plug vial in vacuum glove box.
Definite value is carried out using inductively coupled plasma emission spectrography.Constituent content is：Lanthanum 21.7%, cerium 31.9%, praseodymium
3.6%, neodymium 12.2%, magnesium 2.3%, iron 20.8%, copper 2.5%, zinc 2.0%.
Embodiment three
For preparing 2kg rare earth pyrophoric alloy Standard Reference Materials for Determination, preparation method is as follows：
Weigh cerium 0.69（Purity is 99.3%）Kg, lanthanum（Purity is 99.6%）0.41 kg, praseodymium（Purity is 99.3%）0.08 kg、
Neodymium（Purity is 99.2%）0.28 kg, iron（Purity is 99.6%）0.42 kg is put into magnesia crucible, is evacuated to 10 Pa,
Nitrogen is then charged with as protective gas, after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, keeps the temperature 5 min
Afterwards, it is crushed after casting cooling, intermediate alloy is made.
Weigh magnesium（Purity is 99.4%）0.055 kg, copper（Purity is 99.4%）0.04 kg, zinc（Purity is 99.5%）
0.03 kg is put into after crushing in the magnesia crucible for filling intermediate alloy, is evacuated to 10 Pa, is filled with nitrogen as guarantor
Gas is protected, after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, after keeping the temperature 5 min, casting is made after cooling
Candidate alloy.
It is broken into the fritter of the cm of 4 cm × 4.Fritter is put into ball grinder, inflated with nitrogen is as protective atmosphere, after screwing lid
It is placed in ball mill, sieving is taken out after ball milling 4h, sieving granularity is 40 mesh, and candidate alloy powder is made.
Candidate alloy powder is sub-packed in clean tool plug vial in vacuum glove box.
Definite value is carried out using inductively coupled plasma emission spectrography.Constituent content is：Lanthanum 20.9%, cerium 34.6%, praseodymium
3.9%, neodymium 13.1%, magnesium 2.0%, iron 20.4%, copper 2.0%, zinc 1.8%.
Example IV
For preparing 2kg rare earth pyrophoric alloy Standard Reference Materials for Determination, preparation method is as follows：
Weigh cerium（Purity is 99.0%）0.73 kg, lanthanum（Purity is 99.6%）0.39 kg, praseodymium（Purity is 99.3%）0.1 kg、
Neodymium（Purity is 99.2%）0.28 kg, iron（Purity is 99.6%）0.39 kg is put into magnesia crucible, is evacuated to 10 Pa,
Nitrogen is then charged with as protective gas, after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, keeps the temperature 4 min
Afterwards, it is crushed after casting cooling, intermediate alloy is made.
Weigh magnesium（Purity is 99.4%）0.074 kg, copper（Purity is 99.4%）0.02 kg, zinc（Purity is 99.5%）
0.02 kg is put into after crushing in the magnesia crucible for filling intermediate alloy, is evacuated to 10 Pa, is filled with nitrogen as guarantor
Gas is protected, after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, after keeping the temperature 4 min, casting is made after cooling
Candidate alloy.
It is broken into the fritter of the cm of 4 cm × 4.Fritter is put into ball grinder, inflated with nitrogen is as protective atmosphere, after screwing lid
It is placed in ball mill, sieving is taken out after ball milling 4h, sieving granularity is 40 mesh, and candidate alloy powder is made.
Candidate alloy powder is sub-packed in clean tool plug vial in vacuum glove box.
Definite value is carried out using inductively coupled plasma emission spectrography.Constituent content is：Lanthanum 19.6%, cerium 26.2%, praseodymium
4.3%, neodymium 13.5%, magnesium 2.5%, iron 19.5%, copper 1.0%, zinc 0.6%.
Embodiment five
For preparing 2kg rare earth pyrophoric alloy Standard Reference Materials for Determination, preparation method is as follows：
Weigh cerium（Purity is 98.8%）0.62 kg, lanthanum（Purity is 98.7%）0.45 kg, praseodymium（Purity is 98.2%）0.11 kg、
Neodymium（Purity is 98.2%）0.29 kg, iron（Purity is 98.5%）0.37 kg is put into magnesia crucible, is evacuated to 10 Pa,
Nitrogen is then charged with as protective gas, after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, keeps the temperature 3 min
Afterwards, it is crushed after casting cooling, intermediate alloy is made.
Weigh magnesium（Purity is 99.2%）0.084 kg, copper（Purity is 99.2%）0.03 kg, zinc（Purity is 99.2%）
0.05 kg is put into after crushing in the magnesia crucible for filling intermediate alloy, is evacuated to 10 Pa, is filled with nitrogen as guarantor
Gas is protected, after being warming up to material whole thawing, is uniformly mixed using electromagnetic agitation, after keeping the temperature 3 min, casting is made after cooling
Candidate alloy.
It is broken into the fritter of the cm of 4 cm × 4.Fritter is put into ball grinder, inflated with nitrogen is as protective atmosphere, after screwing lid
It is placed in ball mill, sieving is taken out after ball milling 4h, sieving granularity is 40 mesh, and candidate alloy powder is made.
Candidate alloy powder is sub-packed in clean tool plug vial in vacuum glove box.
Definite value is carried out using inductively coupled plasma emission spectrography.Constituent content is：Lanthanum 22.4%, cerium 29.4%, praseodymium
4.6%, neodymium 13.8%, magnesium 3.0%, iron 18.7%, copper 1.7%, zinc 2.3%.
Claims (7)
1. a kind of rare earth pyrophoric alloy Standard Reference Materials for Determination is the alloyed powder that rare earth element and modifying element simple substance form
Body, by the sample composition of 3~5 graded elementals；The quality group of element becomes lanthanum 18.5%~22.5%, cerium 29.5%~40%, praseodymium
3%~4.5%, neodymium 12%~14%, iron 18.5%~23%, magnesium 2%~3%, copper 1%~2.5%, zinc 0.5%~2.5%.
2. rare earth pyrophoric alloy Standard Reference Materials for Determination according to claim 1, it is characterised in that：Diameter of particle is less than 60
Mesh.
3. according to the preparation method of rare earth pyrophoric alloy Standard Reference Materials for Determination described in claims 1 or 2 any one, including
Intermediate alloy melting, candidate alloy melting, granulation, packaging and definite value process, it is characterised in that：
Intermediate alloy melting：By lanthanum, cerium, praseodymium, neodymium, iron melting, intermediate alloy is obtained；
Candidate alloy melting：Intermediate alloy and magnesium, copper, Zinc smelting are obtained into candidate alloy；
It is granulated：It is crushed using vacuum or noble gas protection ball-milling technology, obtains candidate alloy powder.
4. the preparation method of rare earth pyrophoric alloy Standard Reference Materials for Determination according to claim 3, it is characterised in that：It is candidate
Object alloy melting process, magnesium excessive 5%~10%.
5. the preparation method of rare earth pyrophoric alloy Standard Reference Materials for Determination according to claim 3, it is characterised in that：It is used
Raw metal is simple substance, and purity is not less than 99%.
6. the preparation method of rare earth pyrophoric alloy Standard Reference Materials for Determination according to claim 3, it is characterised in that：It is granulated
Noble gas described in process is argon gas.
7. the preparation method of rare earth pyrophoric alloy Standard Reference Materials for Determination according to claim 3, it is characterised in that：Packaging
Process carries out in vacuum glove box.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166589A (en) * | 2021-11-08 | 2022-03-11 | 国核宝钛锆业股份公司 | Preparation method of nuclear-grade hafnium and hafnium alloy single-point spectrum standard sample |
| WO2024027327A1 (en) * | 2022-08-01 | 2024-02-08 | 北矿检测技术股份有限公司 | Rare earth oxide standard sample, and preparation process therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820698A (en) * | 2014-03-11 | 2014-05-28 | 包头稀土研究院 | Rare earth iron intermediate alloy and application thereof |
| CN106756446A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | The hypoxemia rare earth steel preparation method of Rare-earth Iron intermediate alloy |
| CN106834860A (en) * | 2015-12-03 | 2017-06-13 | 黄波 | A kind of pyrophoric alloy of neodymium element containing cerium and preparation method thereof |
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2017
- 2017-11-02 CN CN201711063371.4A patent/CN108152355A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820698A (en) * | 2014-03-11 | 2014-05-28 | 包头稀土研究院 | Rare earth iron intermediate alloy and application thereof |
| CN106834860A (en) * | 2015-12-03 | 2017-06-13 | 黄波 | A kind of pyrophoric alloy of neodymium element containing cerium and preparation method thereof |
| CN106756446A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | The hypoxemia rare earth steel preparation method of Rare-earth Iron intermediate alloy |
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| 林河成: "稀土发火合金材料的生产、应用及市场", 《稀土》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166589A (en) * | 2021-11-08 | 2022-03-11 | 国核宝钛锆业股份公司 | Preparation method of nuclear-grade hafnium and hafnium alloy single-point spectrum standard sample |
| WO2024027327A1 (en) * | 2022-08-01 | 2024-02-08 | 北矿检测技术股份有限公司 | Rare earth oxide standard sample, and preparation process therefor |
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Application publication date: 20180612 |