CN108372293A - A kind of method of metal powder gel injection molding catalysis degumming - Google Patents
A kind of method of metal powder gel injection molding catalysis degumming Download PDFInfo
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- CN108372293A CN108372293A CN201810179594.5A CN201810179594A CN108372293A CN 108372293 A CN108372293 A CN 108372293A CN 201810179594 A CN201810179594 A CN 201810179594A CN 108372293 A CN108372293 A CN 108372293A
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- China
- Prior art keywords
- degumming
- metal powder
- catalysis
- gel injection
- injection molding
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Classifications
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
- B22F3/1025—Removal of binder or filler not by heating only
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
A kind of method of metal powder gel injection molding catalysis degumming, belongs to gel injection-moulding metal parts molding field.The low temperature degumming of gel injection moulding blank is realized in the present invention using catalyzed gas, pass through reacting for catalyzed gas and the organic volume grid of macromolecule, then gas molecules can be changed at a lower temperature by making high polymer long chain that cracking occur, compared with the hot scouring processes of tradition, gel is easier green body, to improve degumming efficiency.Meanwhile 200 DEG C or less low temperature degummings can effectively control active metal oxygenation carburetting situation, prevent the metal powder under high temperature degumming from reacting with the macromolecule organic in gel rubber system.In addition, degumming is uniform, it will not decline because of intensity during dumping and planted agent's force effect issues raw cracking so that gel injection-moulding product has good institutional framework and performance.
Description
Technical field
The invention belongs to gel injection-moulding metal parts molding fields, provide a kind of metal powder gel injection molding catalysis degumming
New method.
Background technology
Gel casting (Gelcasting) technology is initially people to solve the near net of complicated shape ceramic component
Size Problems in forming and propose, start later applied to complicated shape metal parts molding completely.Gel casting
Core to be organic monomer occur polymerisation under gel reaction effect forms reticular structure and wrap up ceramics or metal-powder,
As the green body shaped by macromolecular network.Green body obtains densification product through drying, dumping, sintering.
Gel injection-moulding equipment is simple, forming green body component is uniform, even density, defect is few, is unlikely to deform, easily shapes complexity
Outstanding advantages of Shape Parts and very strong usability.Due to only having 10%~20% (matter in the polymer-solvent of lateral connection
Measure score) polymer, thus, it is easy to pass through drying steps remove gel member in solvent.Simultaneously as the cross of polymer
To connection, polymer cannot be with Solvent migration in the drying process.And since the liquid of flowing filling mold is solidified with slurry
Step detaches, and therefore, gel casting overcomes some major defects of injection moulding.In addition, not with casting method
Together, the green strength of gel casting is high, can be reprocessed.
Currently, since the organic monomer used in gel injection-moulding is easily decomposes, generally directly used without special degumming step
Degumming is thermally decomposed, and uses the degumming temperature of thermal decomposition degumming generally between 500-650 DEG C.But to some active metals
For gel casting, the temperature drift of degumming is thermally decomposed, many adverse effects are generated to metal in its scouring processes.Example
It is a large amount of to introduce if the organic matter decomposed in hot scouring processes can cause oxygenation carburetting in metal serious under hot degumming temperature condition
The impurity of the interstitial elements such as carbon, nitrogen, oxygen.On the other hand it is that certain metal powder sintered temperature are sufficiently close to degumming temperature,
Cause to begin to enter sintering stage completely in the also non-degumming of metal powder, has seriously affected the tissue of metal gel injection molded article
And performance.Therefore, when preparing the structural member of some active metals using gel injection-moulding, how to realize low temperature degumming be prepare it is high-strength
Spend one of the key of high-performance metal structural member.In order to solve this problem, the present invention uses a kind of metal powder gel injection molding
It is catalyzed the new method of degumming, degumming temperature can not only be controlled at 200 DEG C or less；Green body is put into catalysis atmosphere,
Pass through reacting for catalyzed gas and the organic volume grid of macromolecule, moreover it is possible to make high polymer long chain that cracking occur then at a lower temperature
Gas molecules can be changed into and be easier green body, it is not easy to strain cracking.
Invention content
It is an object of the invention to provide a kind of methods that metal powder gel injection molding is catalyzed degumming, and this method is by being catalyzed gas
Body is reacted with the organic volume grid of macromolecule, then gas can be changed at a lower temperature by making high polymer long chain that cracking occur
Small molecule, it is easier to deviate from green body.Degumming efficiency can be not only improved, degumming temperature control oxygenation carburetting feelings can also be reduced
Condition, prevent at high temperature metal powder react with the macromolecule organic in gel rubber system.In addition, degumming is uniform, arranging
It will not decline because of intensity during glue and planted agent's force effect issues raw cracking.
In order to obtain the new method that above-mentioned metal powder gel injection molding is catalyzed degumming, present invention employs following technical sides
Case：
(1) it is proportionally added into gelator in organic solvent and is hybridly prepared into premixed liquid；
(2) metal powder of 20-85vol% is added in premixed liquid, and the dispersant that 0.01-1vol.% is added is adjusted
The mobility of slurry and the antifoaming agent of 0.01-0.08vol.%, are put into after stirring evenly in ball mill, and ball milling speed is
100r/min-250r/min, ratio of grinding media to material 4:1-7:1, ball milling 5-15min obtain gel-casting slurry；
(3) slurry is injected in mold and is shaped, be put into 60-90 DEG C of dry 60-180min in drying box, then note gel
Die body is removed from the molds；
(4) green body is put into atmosphere catalysis degreasing stove and carries out degumming process, it is nitrogen and catalyzed gas, nitrogen to be passed through gas
It is 90-150ml/min that gas, which is passed through rate, and the rate that is passed through of catalyzed gas is 0.01-2ml/min, usually time 20-
600min, degumming temperature are 80-200 DEG C；
(5) gel injection moulding blank after degumming is put into vacuum drying oven and is sintered, 600-1350 DEG C of sintering temperature, sintering time
45-150min, vacuum degree 10-1-10-3Pa。
Further, the organic solvent described in step (1) is one kind or several in toluene, acetone, dimethylbenzene or ethyl alcohol
Kind.
Further, the gelator described in step (1) is one or more of water base or non-water base gel rubber system.
Aqueous gel system, it is characterised in that：Solvent is water, crosslinking agent N, N '-methylene-bisacrylamide (MBAM), organic monomer
For one or more of acrylamide (AM), Methacrylamide (MAM).Non- water base gel rubber system, it is characterised in that：Solvent
Mainly there are dibasic ester, higher boiling gasoline, long-chain alcohol, toluene, the tert-butyl alcohol, dichloromethane etc..Organic monomer (adhesive) can use three
In three acrylates of methylpropane (TMPTA), ethyl methacrylate (HEMA) or 1,6 ethylene glycol divinyls sour (HDODA)
It is one or more of.
Further, the metal powder described in step (2) be titanium or titanium alloy, aluminium and aluminium alloy, copper and copper alloy or
One or more of magnesium and magnesium alloy powder, powder diameter are 5-50 μm.
Further, the dispersant described in step (2) is in oleic acid, ammonium citrate, stearmide or polyethylene etc.
It is one or more of.
Further, the antifoaming agent described in step (2) is isooctanol or isoamyl alcohol.
Further, the catalyzed gas described in step (4) is one kind in nitric acid gas, oxalic acid gas or HCl gas
Or it is several.
Advantages of the present invention：
1, it is easier to make macromolecule organism that green body be discharged using gas catalysis degumming, to improve degumming efficiency.
2, degumming temperature is reduced, oxygenation carburetting situation is controlled, is prevented in active metal powder at high temperature and gel rubber system
Macromolecule organic react.
3, degumming is uniform, will not decline because of intensity during dumping and planted agent's force effect issues raw cracking.
4, there is good institutional framework and performance using the metal gel injection molded article of gas catalysis degumming.
Specific implementation mode
Case study on implementation 1：
A kind of new method of sized spherical titanium powder gel injection-moulding catalysis degumming：
(1) organic monomer hydroxyethyl methacrylate (HEMA) and peroxidating (two) benzoyl is added in solvent toluene
BPO is 40 according to volume ratio:40:1 ratio is mixed and stirred for uniformly preparing premixed liquid；
(2) the 68% spherical pure titanium valve of aerosolization is weighed by volume, grain size is 45 μm, is then added in premixed liquid, and
0.05% dispersant oleic acid is added, 0.02% antifoaming agent isooctanol is put into after stirring evenly in ball mill, and ball milling speed is
120r/min, ratio of grinding media to material 5:1, Ball-milling Time 8min obtains gel-casting slurry；
(3) titanium valve slurry is injected in mold and is shaped, 60 DEG C of dry 60min in drying box are put into, then by gel injection-moulding
Green body is removed from the molds；
(4) green body is put into atmosphere catalysis degreasing stove and carries out degumming process, it is nitrogen and oxalic acid gas, nitrogen to be passed through gas
It is 110ml/min that gas, which is passed through rate, and the rate that is passed through of catalyzed gas is 0.06ml/min, usually time 30min, degumming temperature
It is 150 DEG C；
(5) the gel injection-moulding titanium green body after degumming is put into vacuum drying oven and is sintered, 1320 DEG C of sintering temperature, sintering time
90min, vacuum degree 10-3Pa finally obtains pure titanium gel injection molded article.
Case study on implementation 2：
A kind of new method of copper alloy powder gel injection-moulding catalysis degumming：
(1) water base acrylamide gels system is used, AM, MBAM are dissolved in deionized water with debita spissitudo, are made dense
Spend homogeneous and transparent premixed liquid；
(2) 55% copper alloy powder is weighed by volume, and grain size is 20 μm, is then added in premixed liquid, and be added
0.04% dispersant ammonium citrate, 0.05% antifoaming agent isooctanol, is put into after stirring evenly in ball mill, and ball milling speed is
100r/min, ratio of grinding media to material 4:1, Ball-milling Time 6min obtains gel-casting slurry；
(3) slurry is injected into mold, is put into 70 DEG C of dry 80min in drying box, then by gel injection moulding blank from mold
Middle taking-up；
(4) green body is put into atmosphere catalysis degreasing stove and carries out degumming process, it is nitrogen and HCl gas, nitrogen to be passed through gas
It is 100ml/min that gas, which is passed through rate, and the rate that is passed through of catalyzed gas is 0.05ml/min, usually time 50min, degumming temperature
For 100 DEG C of green bodies；
(5) the gel injection-moulding copper alloy green body after degumming is put into vacuum drying oven and is sintered, 1000 DEG C of sintering temperature, when sintering
Between 60min, vacuum degree 10-2Pa is finally obtained and is obtained copper alloy gel injection-moulding product.
Claims (7)
1. a kind of method of metal powder gel injection molding catalysis degumming, which is characterized in that prepare as follows：
(1) premixed liquid is prepared：The gelator that 20-75vol.% is added in a solvent is hybridly prepared into premixed liquid；
(2) slurry is prepared：The metal powder of 20-85vol% is added in premixed liquid, and the dispersant of 0.01-1vol.% is added
The mobility of slurry and the antifoaming agent of 0.01-0.08vol.% are adjusted, is put into ball mill after stirring evenly, ball milling speed
For 100r/min-250r/min, ratio of grinding media to material 4:1-7:1, ball milling 5-15min obtain gel-casting slurry；
(3) casting：Slurry is injected in mold and is shaped, and is put into 60-90 DEG C of dry 60-180min in vacuum drying chamber,
Then gel injection moulding blank is removed from the molds；
(4) it is catalyzed degumming：Green body is put into atmosphere catalysis degreasing stove and carries out degumming process, it is nitrogen and catalysis gas to be passed through gas
Body, it is 90-150ml/min that nitrogen, which is passed through rate, and the rate that is passed through of catalyzed gas is 0.01-2ml/min, usually time 20-
600min, degumming temperature are 80-200 DEG C；
(5) vacuum-sintering：Gel injection moulding blank after degumming is put into vacuum drying oven and is sintered, 600-1250 DEG C of sintering temperature is burnt
Tie time 45-150min, vacuum degree 10-1-10-3Pa。
2. a kind of method of metal powder gel injection molding catalysis degumming according to claim 1, it is characterised in that：Step
(1) organic solvent described in is one or more of toluene, acetone, dimethylbenzene or ethyl alcohol.
3. a kind of method of metal powder gel injection molding catalysis degumming according to claim 1, it is characterised in that：Step
(1) gelator described in is one or more of water base or non-water base gel rubber system.
4. a kind of method of metal powder gel injection molding catalysis degumming according to claim 1, it is characterised in that：Step
(2) metal powder described in is one kind in titanium or titanium alloy, aluminium and aluminium alloy, copper and copper alloy or magnesium and magnesium alloy powder
Or it is several, powder diameter is 5-50 μm.
5. a kind of method of metal powder gel injection molding catalysis degumming according to claim 1, it is characterised in that：Step
(2) dispersant described in is one or more of oleic acid, ammonium citrate, stearmide or polyethylene.
6. a kind of method of metal powder gel injection molding catalysis degumming according to claim 1, it is characterised in that：Step
(2) antifoaming agent described in is isooctanol or isoamyl alcohol.
7. a kind of method of metal powder gel injection molding catalysis degumming according to claim 1, it is characterised in that：Step
(4) catalyzed gas described in is one or more of nitric acid gas, oxalic acid gas or HCl gas.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810179594.5A CN108372293A (en) | 2018-03-05 | 2018-03-05 | A kind of method of metal powder gel injection molding catalysis degumming |
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| CN201810179594.5A CN108372293A (en) | 2018-03-05 | 2018-03-05 | A kind of method of metal powder gel injection molding catalysis degumming |
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| CN108372293A true CN108372293A (en) | 2018-08-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114029490A (en) * | 2021-11-29 | 2022-02-11 | 深圳艾利佳材料科技有限公司 | Three-dimensional metal ceramic gradient material gel casting mould |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872458A (en) * | 2006-05-26 | 2006-12-06 | 北京科技大学 | Injection moulding method for Ti6A14V alloy gel |
| CN101279106A (en) * | 2008-05-21 | 2008-10-08 | 北京科技大学 | Preparation of gel injection molding of porous titanium-cobalt alloy medical implant article |
| CN101972852A (en) * | 2010-11-19 | 2011-02-16 | 中南大学 | Method for preparing complex molybdenum part |
| CN103447534A (en) * | 2013-09-06 | 2013-12-18 | 北京科技大学 | Organic physical gel-based gel-casting forming method |
| CN105382261A (en) * | 2015-11-24 | 2016-03-09 | 广州有色金属研究院 | Precision titanium part manufacturing method |
-
2018
- 2018-03-05 CN CN201810179594.5A patent/CN108372293A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872458A (en) * | 2006-05-26 | 2006-12-06 | 北京科技大学 | Injection moulding method for Ti6A14V alloy gel |
| CN101279106A (en) * | 2008-05-21 | 2008-10-08 | 北京科技大学 | Preparation of gel injection molding of porous titanium-cobalt alloy medical implant article |
| CN101972852A (en) * | 2010-11-19 | 2011-02-16 | 中南大学 | Method for preparing complex molybdenum part |
| CN103447534A (en) * | 2013-09-06 | 2013-12-18 | 北京科技大学 | Organic physical gel-based gel-casting forming method |
| CN105382261A (en) * | 2015-11-24 | 2016-03-09 | 广州有色金属研究院 | Precision titanium part manufacturing method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114029490A (en) * | 2021-11-29 | 2022-02-11 | 深圳艾利佳材料科技有限公司 | Three-dimensional metal ceramic gradient material gel casting mould |
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Application publication date: 20180807 |