CN108723380A - A kind of preparation method of rare earth-iron base pre-alloyed powder - Google Patents
A kind of preparation method of rare earth-iron base pre-alloyed powder Download PDFInfo
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- CN108723380A CN108723380A CN201810582384.0A CN201810582384A CN108723380A CN 108723380 A CN108723380 A CN 108723380A CN 201810582384 A CN201810582384 A CN 201810582384A CN 108723380 A CN108723380 A CN 108723380A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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Abstract
The present invention discloses a kind of preparation method of rare earth-iron base pre-alloyed powder, preparation process ferric nitrate, copper nitrate, stannous chloride, nickel nitrate, ammonium metatungstate, nitric acid rare earth, polyethylene glycol are add to deionized water to obtain mixing salt solution, spray-dried, calcining, hydrogen reducing by certain quality proportioning, and pre-alloyed powder is made.The ultimate constituent mass ratio of gained pre-alloyed powder is：24.6-35.7%Cu, 1-2.5%Sn, 0.5-3%Ni, 1-15%W, 0.05-0.5%REO, surplus Fe.This method preparation method is simple for process, and yield is high, and the rare earth-iron base pre-alloyed powder ingredient of gained is uniform, mobility and good moldability, the diamond tool high mechanical properties prepared using the powder, long lifespan.
Description
Technical field
The present invention relates to diamond tool field, in particular to a kind of preparation methods of rare earth-iron base pre-alloyed powder.
Background technology
China's rock material resource is abundant, various in style.Currently, application of the lithotome in building trade is more and more common,
Demand rises year by year.Under this market demand, processing of stone industry is quickly grown in recent years, and processing of stone technology constantly changes
Into the manufacturing level of processing of diamond tool has large increase.Due to China start to walk in terms of processing of stone research evening,
Research foundation is thin, and processing technology level falls behind, and the production scale of stone product is small, processing efficiency is low, product specification is low, stone material money
Source utilization rate is low, and waste is serious.In order to shorten the gap with Foreign Advanced Lerel, meet market of the people to various stone products
Demand, for processing of stone technology and all urgently further research and the raisings of diamond tool manufacturing technology.
The present invention starts with from powder raw material, proposes a kind of preparation method of rare earth-iron base pre-alloyed powder, solves iron-based gold
The problem of hard rock tool hold is low, poor toughness, short life.
Invention content
It is an object of the present invention in view of the above technical problems, provide a kind of preparation side of rare earth-iron base pre-alloyed powder
Method.
The preparation method step is by ferric nitrate, copper nitrate, stannous chloride, nickel nitrate, ammonium metatungstate, nitric acid rare earth, gathers
Ethylene glycol is add to deionized water by certain quality proportioning, while adding a small amount of surfactant, is stirred evenly, and plastic is matched
Liquid solution；Colloidal solution is spray-dried on spray dryer to be put into calcining furnace after mixing salt powder is made and is calcined；Finally
It is restored to obtain rare earth-iron base pre-alloyed powder in hydrogen reducing furnace.
Further, the mixing salt solution is grouped as by the group of following mass fraction：400-460 parts of ferric nitrate, copper nitrate
110-125 parts, 2.5-4.2 parts of stannous chloride, 4-8.4 parts of nickel nitrate, 5.7-11.1 parts of ammonium metatungstate, nitric acid rare earth 0.2-1.05
Part, 0.35-0.65 parts of polyethylene glycol, 1400-1600 parts of deionized water.
Further, the ultimate constituent mass ratio of obtained pre-alloyed powder is：24.6-35.7%Cu, 1-2.5%Sn,
0.5-3%Ni, 1-15%W, 0.05-0.5%REO, surplus Fe；Wherein REO is one kind or several in La2O3, CeO2, Y2O3
Kind；
Further, a concentration of 100-400g/L of mixing salt solution；Surfactant is the poly- second of mass fraction 0.1-2%
Glycol；
Further, the inlet air temperature of its spray-drying process of colloidal solution is 150-350 DEG C, air outlet temperature 80-100
℃。
Further, mixing salt powder its calcination temperature be 200-600 DEG C, calcination time 0.5-8h.
Further, hydrogen reduction reduction temperature be 250-800 DEG C, soaking time 1-6h, hydrogen flowing quantity 5-
100L/min。
The advantages and positive effects of the present invention are embodied in：
1. rare earth-iron base pre-alloyed powder Oxygen potential prepared by the present invention is higher, mobility and mouldability are preferable.
2. rare earth-iron base pre-alloyed powder ingredient prepared by the present invention is uniform, granularity is tiny, purity is high, thus has pole
Good sintering character.
3. rare earth-iron base pre-alloyed powder sintering strength height, good toughness prepared by the present invention, are added after diamond particles by force
Degree loss is small.
4. present invention process is simple, it is easy to volume production, is suitble to industrialized production.
Specific implementation mode
The present invention will be further described in detail with reference to the specific embodiments.
Case study on implementation 1：
Weigh nine water ferric nitrates of 445.7g, 117.1g nitrate trihydrates copper, 2.9g stannous chloride dihydrates, six water nickel nitrates of 5g,
6.7g ammonium metatungstates, 0.68g yttrium nitrate hexahydrates, 0.4g polyethylene glycol, are poured into 2L plastic cups, after 1500g deionized waters are added
It stirs evenly, for use.
The mixing salt solution of above-mentioned preparation is spray-dried on spray dryer, spray art parameter is into wind-warm syndrome
300 DEG C of degree, 80 DEG C of leaving air temp, spray velocity 3kg/h.
The powder collected on spray dryer is put into Muffle furnace and is calcined, calcination temperature is 450 DEG C, time 3h.
Powder dress boat after calcining is put into reduction furnace, reducing process parameter is 300 DEG C of heat preservation 1h, and 650 DEG C keep the temperature 2h,
800 DEG C of heat preservations 1h, hydrogen flowing quantity 10L/min.
Finally the mass ratio of obtained rare earth-iron base pre-alloyed powder is：30.8%Cu, 1.5%Sn, 1%Ni, 5%W,
0.2%Y2O3,61.5%Fe.
Case study on implementation 2：
Weigh nine water ferric nitrates of 419.6g, 117.1g nitrate trihydrates copper, 3.8g stannous chloride dihydrates, six water nitric acid of 7.4g
Nickel, 10.1g ammonium metatungstates, 0.25g cerium nitrate hexahydrates, 0.68g yttrium nitrate hexahydrates, 0.6g polyethylene glycol, are poured into 2L plastic cups,
It is stirred evenly after 1500g deionized waters are added, for use.
The mixing salt solution of above-mentioned preparation is spray-dried on spray dryer, spray art parameter is into wind-warm syndrome
320 DEG C of degree, 90 DEG C of leaving air temp, spray velocity 4kg/h.
The powder collected on spray dryer is put into Muffle furnace and is calcined, calcination temperature is 400 DEG C, time 4h.
Powder dress boat after calcining is put into reduction furnace, reducing process parameter is 350 DEG C of heat preservation 1h, and 700 DEG C keep the temperature 2h,
800 DEG C of heat preservations 1.5h, hydrogen flowing quantity 15L/min.
Finally the mass ratio of obtained rare earth-iron base pre-alloyed powder is：30.8%Cu, 2%Sn, 1.5%Ni, 7.5%W,
0.1%CeO2,0.2%Y2O3,61.5%Fe.
The present embodiment is the exemplary embodiment of the present invention, for those skilled in the art, in the present invention
On the basis of disclosing application process and principle, it is easy to make various types of improvement or deformation, be not limited solely to the present invention
Method or structure described in above-mentioned specific implementation mode, therefore previously described mode is preferred embodiment, and and do not have
Restrictive meaning, it is every according to equivalence changes made by the present invention and modification, all protected in the range of claims of the present invention
In range.
Claims (7)
1. a kind of preparation method of rare earth-iron base pre-alloyed powder, which is characterized in that preparation process is：
1) ferric nitrate, copper nitrate, stannous chloride, nickel nitrate, ammonium metatungstate, nitric acid rare earth, polyethylene glycol are pressed into certain quality
Proportioning is add to deionized water to obtain mixing salt solution, while adding a small amount of surfactant, stirs evenly, it is molten to be configured to colloid
Liquid；
2) it is spray-dried, calcines：Colloidal solution is spray-dried, mixing salt powder is made, is put into calcining furnace and calcine；
3) hydrogen reducing：It is finally restored in hydrogen reducing furnace, obtains rare earth-iron base pre-alloyed powder.
2. a kind of preparation method of rare earth-iron base pre-alloyed powder as described in claim 1, which is characterized in that the mixing
Salting liquid is grouped as by the group of following mass fraction：400-460 parts of ferric nitrate, 110-125 parts of copper nitrate, stannous chloride 2.5-
4.2 parts, 4-8.4 parts of nickel nitrate, 5.7-11.1 parts of ammonium metatungstate, 0.2-1.05 parts of nitric acid rare earth, polyethylene glycol 0.35-0.65
Part, 1400-1600 parts of deionized water.
3. a kind of preparation method of rare earth-iron base pre-alloyed powder as described in claim 1, which is characterized in that obtained dilute
The ultimate constituent mass ratio of soil-iron-based prealloyed powder is：24.6-35.7%Cu, 1-2.5%Sn, 0.5-3%Ni, 1-15%
W, 0.05-0.5%REO, surplus Fe；Wherein REO is one or more of La2O3, CeO2, Y2O3.
4. a kind of preparation method of rare earth-iron base pre-alloyed powder as described in claim 1, which is characterized in that in step 1
A concentration of 100-400g/L of mixing salt solution；Surfactant is the polyethylene glycol of mass fraction 0.1-2%.
5. a kind of preparation method of rare earth-iron base pre-alloyed powder as described in claim 1, which is characterized in that in step 2
Being spray-dried design parameter is：Inlet air temperature is 150-350 DEG C, and air outlet temperature is 80-100 DEG C.
6. a kind of preparation method of rare earth-iron base pre-alloyed powder as described in claim 1, which is characterized in that in step 2
Calcination temperature is 200-600 DEG C, calcination time 0.5-8h.
7. a kind of preparation method of rare earth-iron base pre-alloyed powder as described in claim 1, which is characterized in that in step 3
Reduction temperature is 250-800 DEG C, soaking time 1-6h, hydrogen flowing quantity 5-100L/min.
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Citations (9)
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|---|---|---|---|---|
| CN1373237A (en) * | 2001-02-28 | 2002-10-09 | 北京科技大学 | Process for preparing W-Ni-Fe alloy with superfine grains and high specific weight |
| CN1565782A (en) * | 2003-06-12 | 2005-01-19 | 中南大学 | Method for preparing nano-grade tungsten-based composite powder by sol-spray drying-thermal reduction |
| CN1593819A (en) * | 2004-06-29 | 2005-03-16 | 北京科技大学 | Preparation method of nanometer sized superfine ferro nickel alloy powder |
| CN101230427A (en) * | 2008-02-22 | 2008-07-30 | 中南大学 | Method for preparing grain-refining W-Ni-Fe alloy containing rare earth |
| CN101234430A (en) * | 2008-02-22 | 2008-08-06 | 中南大学 | Method for preparing ultrafine molybdenum powder and ultrafine molybdenum powder doped with rare earth |
| JP4737046B2 (en) * | 2006-11-21 | 2011-07-27 | 日立金属株式会社 | Iron-based rare earth permanent magnet and method for producing the same |
| CN103394702A (en) * | 2013-07-17 | 2013-11-20 | 河北工程大学 | Method for uniformly and efficiently manufacturing pre-alloyed powder for nano-structured oxide-dispersion-strengthened iron-based alloy |
| CN104148640A (en) * | 2014-07-24 | 2014-11-19 | 华侨大学 | Diamond cutting disc with rare-earth modified tungsten-based binding agents and method for manufacturing diamond cutting disc |
| KR20150067546A (en) * | 2013-12-10 | 2015-06-18 | 손우창 | Metal iron granule and the manufacturing method of the same |
-
2018
- 2018-06-07 CN CN201810582384.0A patent/CN108723380A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1373237A (en) * | 2001-02-28 | 2002-10-09 | 北京科技大学 | Process for preparing W-Ni-Fe alloy with superfine grains and high specific weight |
| CN1565782A (en) * | 2003-06-12 | 2005-01-19 | 中南大学 | Method for preparing nano-grade tungsten-based composite powder by sol-spray drying-thermal reduction |
| CN1593819A (en) * | 2004-06-29 | 2005-03-16 | 北京科技大学 | Preparation method of nanometer sized superfine ferro nickel alloy powder |
| JP4737046B2 (en) * | 2006-11-21 | 2011-07-27 | 日立金属株式会社 | Iron-based rare earth permanent magnet and method for producing the same |
| CN101230427A (en) * | 2008-02-22 | 2008-07-30 | 中南大学 | Method for preparing grain-refining W-Ni-Fe alloy containing rare earth |
| CN101234430A (en) * | 2008-02-22 | 2008-08-06 | 中南大学 | Method for preparing ultrafine molybdenum powder and ultrafine molybdenum powder doped with rare earth |
| CN103394702A (en) * | 2013-07-17 | 2013-11-20 | 河北工程大学 | Method for uniformly and efficiently manufacturing pre-alloyed powder for nano-structured oxide-dispersion-strengthened iron-based alloy |
| KR20150067546A (en) * | 2013-12-10 | 2015-06-18 | 손우창 | Metal iron granule and the manufacturing method of the same |
| CN104148640A (en) * | 2014-07-24 | 2014-11-19 | 华侨大学 | Diamond cutting disc with rare-earth modified tungsten-based binding agents and method for manufacturing diamond cutting disc |
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Application publication date: 20181102 |