CN101972852A - Method for preparing complex molybdenum part - Google Patents
Method for preparing complex molybdenum part Download PDFInfo
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- CN101972852A CN101972852A CN 201010555936 CN201010555936A CN101972852A CN 101972852 A CN101972852 A CN 101972852A CN 201010555936 CN201010555936 CN 201010555936 CN 201010555936 A CN201010555936 A CN 201010555936A CN 101972852 A CN101972852 A CN 101972852A
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Abstract
The invention discloses a method for preparing a complex molybdenum part, which comprises: mixing an organic monomer and a cross-linking agent according to a certain volume ratio; adding the mixture into water to prepare 8 to 38 weight percent pre-mixed solution; adding molybdenum powder subjected to surface modification by silane or titanate and a small amount of dispersant; and preparing uniform and high-liquidity slurry containing 48 to 60 volume percent of powder; adding a proper amount of initiator and a proper amount of catalyst, uniformly stirring under vacuum at a high speed and degassing; filling into the cavity of a complex mold, initializing a cure reaction under certain conditions and obtaining a blank with a certain strength; and drying the blank, removing binder, sintering at 1,850 to 2,400 DEG C and directly preparing the complex molybdenum part with a density ranging from 95 to 98.8 percent. In the method, the process is simple, the material utilization rate is high, the cost is low, the product performance is high, the batch preparation of the complex molybdenum part can be realized easily, and the product is expected to be widely used in fields of aerospace, electronics and the like.
Description
Technical field
The present invention relates to a kind of method for preparing molybdenum part, particularly relating to a kind of is the method that raw material directly prepares the big-size complicated shape molybdenum part with the powder.
Background technology
Molybdenum is as a kind of rare refractory metal (2610 ℃ of fusing points), have high heat conduction, low thermal coefficient of expansion, high elastic modulus and elevated temperature strength advantages of higher, as electrode, high-temperature structural material etc., be widely used in fields such as metallurgy, chemical industry, national defence, Aero-Space, atomic energy and electronics industry.For example, engine trunnion, nozzle and valve in the aerospace field, the base plate for packaging of electronic tube grid in the electronics industry and anode-supported material, high-power microwave tubes hot cathode structural detail, transistor etc. and heat sink material etc.
PM technique is the main machining method of Mo and part, but the molybdenum product performance of traditional powder compaction-SINTERING PRODUCTION technology preparation is lower, precision is not high, part shape is simple, need methods such as following adopted machining, pressure processing to prepare the molybdenum part of complicated shape and high dimensional accuracy, but because the temperature-room type plasticity and the processing characteristics of molybdenum is relatively poor, so processing cost height, waste of raw materials big, produce in enormous quantities difficult.In addition, though adopt powder injection forming can prepare the molybdenum part of complicated shape, it only is confined to very tiny part, and is then powerless to large scale or cross dimensions variation complex parts greatly.
The gel casting technology is as a kind of novel near-net-shape new technology, overcome the defective of powder injection forming technology, as it is long etc. to add the special degreasing process of a large amount of binding agents, needs and time, prepare in enormous quantities in low cost and to have special advantages aspect the high-performance complicated shape part, and obtained application at ceramic field.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of technology is simple, cost is low, stock utilization is high, and is easy to realize the method for preparing the complicated shape molybdenum part produced in enormous quantities.
In order to solve the problems of the technologies described above, the method for preparing the complicated shape molybdenum part provided by the invention, realize by following steps:
(1), molybdenum powder surface modification treatment:
With purity 〉=99%, granularity is that fine pure molybdenum powder or the trace rare earth oxides doped molybdenum of 2～10 μ m is raw material; Silane or titanate esters that employing accounts for powder gross weight 0.2～1.0wt% are modifier, by mechanical mixture or chemical coating method the raw material molybdenum powder are carried out surface modification treatment, improve the powder dispersiveness;
(2), premixed liquid preparation:
With the organic monomer and crosslinking agent 20～150: 1 mixing mutually by volume of selecting for use, and the adding deionized water is mixed with the premixed liquid that concentration is 8～38wt%;
(3), high-volume fractional pulp preparation:
The molybdenum powder and the mass ratio thereof that add in premixed liquid through surface modification are the dispersant of 0.5～2wt%, and add ammoniacal liquor and regulate pH value to 8.5～10, through mechanical ball milling prepare powder volume than be 48～60% evenly, stablize and flowability slurry preferably;
(4), casting and curing:
The initator and the catalyst that in the slurry for preparing, add 0.1～2wt%, 0.1 the n-octyl alcohol defoamer of～0.4wt%, and mix fast in a vacuum, reach the purpose of degasification simultaneously, slowly inject rubber, plastics, metal or the glass mold of required product shape then, and under 50～80 ℃ of temperature, leave standstill 2～30min, make it to solidify fully, obtain solidifying base, solidify base and have higher intensity this moment;
(5), dry and necessary reprocessing:
After will solidifying the base taking-up, also can reprocess to modify to its shape in case of necessity and handle, solidify base with postposition and protect in vacuum or inert atmosphere, dry 30～180min solidifies moisture in the base with eliminating under 90～110 ℃ of temperature;
(6), binder removal and sintering:
With dried curing base, speed with 6～15 ℃/min under vacuum or hydrogen atmosphere is warming up to 400～550 ℃, and be incubated 15～45min, with the organic matter that adds in the abundant eliminating curing base or curing reaction generates, be rapidly heated subsequently to 1850～2400 ℃, and be incubated 90～360min, obtain that shape and size all meet the requirements, density is 95%～98.8% molybdenum part.
Wherein, adopting acrylamide (AM) or Methacrylamide (MAM) is organic monomer, N, N ,-methylene-bisacrylamide (MBAM), diallyl tartaric acid diamides (DATDA) or polyethylene glycol dimethacrylate (PEGDAM) any as crosslinking agent.
Wherein, described dispersant is any in ammonium citrate, the big organic boron non-ionic surface active agent of molecule, polycarboxylate (molecular weight is 2000～8000) or the herring oil.
Wherein, described initator is (AIIP) or in the hydrogen peroxide any of ammonium persulfate (APS), potassium peroxydisulfate, hydrochloric acid azo [2-imidazoline-2-propane], and catalyst is N, N, N, N-tetramethylethylenediamine (TEMED).
The invention has the advantages that:
It has broken through the defective of prior powder metallurgy technology, can direct forming and prepare the high-performance molybdenum product of large scale, complicated shape, and its technology is simple, cost is low, stock utilization is high, and is easy to realize producing in enormous quantities.In addition, its mold materials wide material sources are easy to make.Compare with the powder injection forming technology, add organic amount seldom, so need not special degreasing process, not only shortened the time of whole operation, and reduce or avoided having solved problems such as molybdenum poor in processability, large scale complex parts shaping difficulty because of adding a series of problems such as product distortion that too much organic matter causes, cracking
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1:
Referring to Fig. 1, prepare the method for complicated shape molybdenum part, realize by following steps:
(1), molybdenum powder surface modification treatment:
With purity 99.5%, granularity is that the molybdenum powder of 5 μ m is a raw material, carries out the mechanical mixture surface modification treatment with the KH550 silane of 0.3wt%;
(2), premixed liquid preparation:
With acrylamide (AM) is organic monomer, N, and N ,-methylene-bisacrylamide (MBAM) is a crosslinking agent, both mixed in 25: 1 by volume mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 30wt%;
(3), high-volume fractional pulp preparation:
Add the ammonium citrate of 0.8wt% and the molybdenum powder after the surface modification subsequently more in succession, the powder volume mark is 52VOL%, and to be adjusted to PH with ammoniacal liquor be 9, prepares uniform slurry through mechanical ball milling;
(4), casting and curing:
The ammonium persulfate and the N that in above-mentioned slurry, add 0.3wt%, N, N, N-tetramethylethylenediamine, 0.1% n-octyl alcohol defoamer, and mix fast in a vacuum, slowly inject the mould of plastics of previously prepared complicated drug-shaped cover shape then, and under 60 ℃ of temperature, leave standstill 15min, reach completely crued curing base;
(5), dry and necessary reprocessing:
After will solidifying the base taking-up, also can reprocess to modify to its shape in case of necessity and handle, solidify base with postposition and protect in vacuum, dry 30min under 110 ℃ of temperature be to get rid of moisture in the curing base;
(6), binder removal and sintering
With the dried curing base of the demoulding, the speed with 12 ℃/min is warming up to 500 ℃ under the hydrogen atmosphere in intermediate frequency furnace, and insulation 30min is rapidly heated subsequently to 2200 ℃, and insulation 150min, obtains density and be 96.2% molybdenum part.
Embodiment 2:
Referring to Fig. 1, prepare the method for complicated shape molybdenum part, realize by following steps:
(1), molybdenum powder surface modification treatment:
With purity 99.5%, granularity is that the molybdenum powder of 3 μ m is a raw material, carries out the mechanical mixture surface modification treatment with the KH550 silane of 0.9wt%;
(2), premixed liquid preparation:
Mixed mutually in 40: 1 by volume with Methacrylamide (MAM) and polyethylene glycol dimethacrylate (PEGDAM), and the adding deionized water is mixed with the premixed liquid that concentration is 18wt%;
(3), high-volume fractional pulp preparation:
Add herring oil and the modification molybdenum powder of 2wt% subsequently more in succession, the powder addition is 60VOL%, and to be adjusted to PH with ammoniacal liquor be 9.5, prepares uniform slurry through mechanical ball milling;
(4), casting and curing:
The hydrochloric acid azo [2-imidazoline-2-propane] and the N that in above-mentioned slurry, add 1.5wt%, N, N, N-tetramethylethylenediamine, 0.3% n-octyl alcohol defoamer, and mix fast in a vacuum, slowly inject the metal die of the aero-engine trunnion of previously prepared complicated shape then, and under 80 ℃ of temperature, leave standstill 8min, reach completely crued curing base;
(5), dry and necessary reprocessing:
After will solidifying the base taking-up, also can reprocess to modify to its shape in case of necessity and handle, solidify base with postposition and protect in inert atmosphere, dry 30min under 110 ℃ of temperature be to get rid of moisture in the curing base;
(6), binder removal and sintering
With the dried curing base of the demoulding, the speed with 10 ℃/min is warming up to 550 ℃ under the hydrogen atmosphere in intermediate frequency furnace, and insulation 20min is rapidly heated subsequently to 2350 ℃, and insulation 300min, obtains density and be 97.5% molybdenum part.
Embodiment 3:
Referring to Fig. 1, prepare the method for complicated shape molybdenum part, realize by following steps:
(1), molybdenum powder surface modification treatment:
Is purity 99.5%, granularity the molybdenum powder of 10 μ m and the La of 0.8wt%
2O
3Prepare the doped with rare-earth oxide molybdenum powder that granularity is 4 μ m in the mechanical alloying mode, and carry out the mechanical mixture surface modification treatment with the NDZ201 titanate esters of 0.5wt%;
(2), premixed liquid preparation:
Mixed mutually in 100: 1 by volume with Methacrylamide (MAM) and diallyl tartaric acid diamides (DATDA), and the adding deionized water is mixed with the premixed liquid that concentration is 35wt%;
(3), high-volume fractional pulp preparation:
Add doped molybdenum after the organic boron non-ionic surface active agent of big molecule of 1.2wt% and the modification subsequently more in succession, the powder volume mark is 56VOL%, and to be adjusted to PH with ammoniacal liquor be 9, prepares uniform slurry through mechanical ball milling;
(4), casting and curing:
The hydrogen peroxide and the N that in above-mentioned slurry, add 0.8wt%, N, N, N-tetramethylethylenediamine, 0.2% n-octyl alcohol defoamer, and mix fast in a vacuum, slowly inject the rubber mold of previously prepared complicated shape then, and under 60 ℃ of temperature, leave standstill 20min, reach completely crued curing base;
(5), dry and necessary reprocessing:
After will solidifying the base taking-up, also can reprocess to modify to its shape in case of necessity and handle, solidify base with postposition and protect in vacuum, dry 60min under 100 ℃ of temperature be to get rid of moisture in the curing base;
(6), binder removal and sintering
Solidify base and further process, to obtain net shape, then in intermediate frequency furnace under the hydrogen atmosphere speed with 10 ℃/min be warming up to 500 ℃, insulation 30min, be rapidly heated subsequently to 2350 ℃, and insulation 360min, density obtained and be 98.4% high-performance rare-earth doping molybdenum part.
If be rapidly heated in vacuum drying oven earlier to 550 ℃ of insulation 20min degreasing solidifying a base, placing SPS discharge plasma sintering stove sintering 5min under 1650 ℃, 40MPa pressure can obtain density again is 98.8% high-performance rare-earth doping molybdenum part.
Embodiment 4:
Referring to Fig. 1, prepare the method for complicated shape molybdenum part, realize by following steps:
(1), molybdenum powder surface modification treatment:
With purity 99.5%, granularity is that the molybdenum powder of 2 μ m is a raw material, carries out the chemical coating method surface modification treatment with the KH550 silane of 0.2wt%;
(2), premixed liquid preparation:
With acrylamide (AM) is organic monomer, N, and N ,-methylene-bisacrylamide (MBAM) is a crosslinking agent, both mixed in 20: 1 by volume mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 30wt%;
(3), high-volume fractional pulp preparation:
The molecular weight that adds 0.5wt% subsequently more in succession is 6000 polycarboxylic acids ammonium and the molybdenum powder after the surface modification, and the powder volume mark is 50VOL%, and to be adjusted to PH with ammoniacal liquor be 8.5, prepares uniform slurry through mechanical ball milling;
(4), casting and curing:
The ammonium persulfate and the N that in above-mentioned slurry, add 1.5wt%, N, N, N-tetramethylethylenediamine, 0.2% n-octyl alcohol defoamer, and mix fast in a vacuum, slowly inject the mould of plastics of previously prepared complicated drug-shaped cover shape then, and under 80 ℃ of temperature, leave standstill 2min, reach completely crued curing base;
(5), dry and necessary reprocessing:
After will solidifying the base taking-up, also can reprocess to modify to its shape in case of necessity and handle, solidify base with postposition and protect in inert atmosphere, dry 50min under 95 ℃ of temperature be to get rid of moisture in the curing base;
(6), binder removal and sintering
With the dried curing base of the demoulding, the speed with 6 ℃/min in vacuum drying oven is warming up to 400 ℃, and insulation 45min is rapidly heated subsequently to 1850 ℃, and insulation 240min, obtains density and be 95.4% molybdenum part.
Embodiment 5:
Referring to Fig. 1, prepare the method for complicated shape molybdenum part, realize by following steps:
(1), molybdenum powder surface modification treatment:
With purity 99.5%, granularity is that the molybdenum powder of 8 μ m is a raw material, carries out the mechanical mixture surface modification treatment with the KH550 silane of 1.0wt%;
(2), premixed liquid preparation:
Mixed mutually in 80: 1 by volume with Methacrylamide (MAM) and polyethylene glycol dimethacrylate (PEGDAM), and the adding deionized water is mixed with the premixed liquid that concentration is 8wt%;
(3), high-volume fractional pulp preparation:
Add herring oil and the modification molybdenum powder of 1.0wt% subsequently more in succession, the powder addition is 48VOL%, and to be adjusted to PH with ammoniacal liquor be 10, prepares uniform slurry through mechanical ball milling;
(4), casting and curing:
The potassium peroxydisulfate and the N that in above-mentioned slurry, add 0.1wt%, N, N, N-tetramethylethylenediamine, 0.3% n-octyl alcohol defoamer, and mix fast in a vacuum, slowly inject the metal die of the aero-engine trunnion of previously prepared complicated shape then, and under 50 ℃ of temperature, leave standstill 30min, reach completely crued curing base;
(5), dry and necessary reprocessing:
After will solidifying the base taking-up, also can reprocess to modify to its shape in case of necessity and handle, solidify base with postposition and protect in vacuum, dry 120min under 110 ℃ of temperature be to get rid of moisture in the curing base;
(6), binder removal and sintering
With the dried curing base of the demoulding, the speed with 15 ℃/min is warming up to 450 ℃ under the hydrogen atmosphere in intermediate frequency furnace, and insulation 15min is rapidly heated subsequently to 2400 ℃, and insulation 90min, obtains density and be 98.3% molybdenum part.
Embodiment 6:
Referring to Fig. 1, prepare the method for complicated shape molybdenum part, realize by following steps:
(1), molybdenum powder surface modification treatment:
Is purity 99.5%, granularity the molybdenum powder of 6 μ m and the La of 0.4wt%
2O
3Prepare the doped with rare-earth oxide molybdenum powder that granularity is 4 μ m in the mechanical alloying mode, and carry out the mechanical mixture surface modification treatment with the NDZ201 titanate esters of 0.6wt%;
(2), premixed liquid preparation:
Mixed mutually in 150: 1 by volume with Methacrylamide (MAM) and diallyl tartaric acid diamides (DATDA), and the adding deionized water is mixed with the premixed liquid that concentration is 38wt%;
(3), high-volume fractional pulp preparation:
Add doped molybdenum after the organic boron non-ionic surface active agent of big molecule of 1.2wt% and the modification subsequently more in succession, the powder volume mark is 50VOL%, and to be adjusted to PH with ammoniacal liquor be 9, prepares uniform slurry through mechanical ball milling;
(4), casting and curing:
The hydrogen peroxide and the N that in above-mentioned slurry, add 2.0wt%, N, N, N-tetramethylethylenediamine, 0.4% n-octyl alcohol defoamer, and mix fast in a vacuum, slowly inject the glass mold of previously prepared complicated shape then, and under 70 ℃ of temperature, leave standstill 20min, reach completely crued curing base;
(5), dry and necessary reprocessing:
After will solidifying the base taking-up, also can reprocess to modify to its shape in case of necessity and handle, solidify base with postposition and protect in vacuum or inert atmosphere, dry 150min under 100 ℃ of temperature be to get rid of moisture in the curing base;
(6), binder removal and sintering
With the dried curing base of the demoulding, the speed with 8 ℃/min is warming up to 480 ℃ under the hydrogen atmosphere in intermediate frequency furnace, and insulation 40min is rapidly heated subsequently to 2000 ℃, and insulation 200min, obtains density and be 96.8% high-performance rare-earth doping molybdenum part.
Claims (6)
1. method for preparing the complicated shape molybdenum part, it is characterized in that: its preparation technology is:
(1), molybdenum powder surface modification treatment:
With purity 〉=99%, granularity is that fine pure molybdenum powder or the trace rare earth oxides doped molybdenum of 2～10 μ m is raw material; Silane or titanate esters that employing accounts for powder gross weight 0.2～1.0wt% are modifier, by mechanical mixture or chemical coating method the raw material molybdenum powder are carried out surface modification treatment, improve the powder dispersiveness;
(2), premixed liquid preparation:
Organic monomer and crosslinking agent are pressed 20～150: 1 mixing mutually by volume, and the adding deionized water is mixed with the premixed liquid that concentration is 8～38wt%;
(3), high-volume fractional pulp preparation:
Adding modification molybdenum powder and mass ratio thereof in premixed liquid is the dispersant of 0.5～2wt%, and regulates pH value to 8.5～10 with ammoniacal liquor, through mechanical ball milling prepare powder volume than be 48～60% evenly, stablize and flowability slurry preferably;
(4), casting and curing:
The initator and the catalyst that in slurry, add 0.1～2wt%, 0.1 the n-octyl alcohol defoamer of～0.4wt%, and mix and reach the purpose of degasification in a vacuum fast, slowly be injected into then in the die cavity of mould of required product shape, and under 50～80 ℃ of temperature, leave standstill 2～30min, make it to solidify fully, obtain solidifying base;
(5), drying:
After will solidifying back base substrate taking-up, be protected in dry 30～180min under 90～110 ℃ of temperature in vacuum or the inert atmosphere, get rid of and solidify moisture in the base with being placed on;
(6), binder removal and sintering:
With dried curing base, speed with 6～15 ℃/min under vacuum or hydrogen atmosphere is warming up to 400～550 ℃, and be incubated 15～45min, with the organic matter that adds in the abundant eliminating base substrate or curing reaction generates, be rapidly heated subsequently to 1850～2400 ℃, and be incubated 90～360min, obtain molybdenum part.
2. the method for preparing the complicated shape molybdenum part according to claim 1, it is characterized in that: the organic monomer described in the above-mentioned steps (2) is acrylamide or Methacrylamide, described crosslinking agent is N, N ,-methylene-bisacrylamide, diallyl tartaric acid diamides or polyethylene glycol dimethacrylate.
3. the method for preparing the complicated shape molybdenum part according to claim 1 and 2 is characterized in that: the dispersant described in the above-mentioned steps (3) is an ammonium citrate, the organic boron non-ionic surface active agent of molecule, molecular weight are 2000～8000 polycarboxylate or herring oil greatly.
4. the method for preparing the complicated shape molybdenum part according to claim 1 and 2, it is characterized in that: the initator described in the above-mentioned steps (4) is ammonium persulfate, potassium peroxydisulfate, hydrochloric acid azo [2-imidazoline-2-propane] or hydrogen peroxide, and described catalyst is N, N, N, the N-tetramethylethylenediamine.
5. the method for preparing the complicated shape molybdenum part according to claim 1 and 2 is characterized in that: described mould is rubber, plastics, metal or glass mold.
6. the method for preparing the complicated shape molybdenum part according to claim 1 and 2 is characterized in that: after will solidifying the base taking-up in the above-mentioned steps (5), its shape is reprocessed modification handle, can further improve product precision and complexity.
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| CN104451222A (en) * | 2014-12-30 | 2015-03-25 | 中南大学 | Preparation method of nano W-Cu composite block material |
| CN108372293A (en) * | 2018-03-05 | 2018-08-07 | 北京科技大学 | A kind of method of metal powder gel injection molding catalysis degumming |
| CN109467391A (en) * | 2018-12-11 | 2019-03-15 | 山东理工大学 | Oxide modifying full information surface silica gel mould cadmia waste material infuses solidification forming method |
| CN109467400A (en) * | 2018-12-11 | 2019-03-15 | 山东理工大学 | The modified full information surface silica gel mould boron slag waste material of aluminium powder infuses solidification forming method |
| CN109848405A (en) * | 2019-02-22 | 2019-06-07 | 北京科技大学 | Powder surface treating agent, titanium or Titanium Powder surface treatment method and composite powder |
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| CN101972852B (en) | 2012-04-25 |
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