CN100503090C - Method for preparing nylon coating film metal powder material - Google Patents
Method for preparing nylon coating film metal powder material Download PDFInfo
- Publication number
- CN100503090C CN100503090C CNB2007100517959A CN200710051795A CN100503090C CN 100503090 C CN100503090 C CN 100503090C CN B2007100517959 A CNB2007100517959 A CN B2007100517959A CN 200710051795 A CN200710051795 A CN 200710051795A CN 100503090 C CN100503090 C CN 100503090C
- Authority
- CN
- China
- Prior art keywords
- nylon
- antioxidant
- powder
- gram
- microns
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000843 powder Substances 0.000 title claims abstract description 76
- 239000004677 Nylon Substances 0.000 title claims abstract description 65
- 229920001778 nylon Polymers 0.000 title claims abstract description 65
- 239000002184 metal Substances 0.000 title claims abstract description 46
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 33
- 239000011248 coating agent Substances 0.000 title claims abstract description 18
- 238000000576 coating method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 25
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 31
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 25
- 229920005989 resin Polymers 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 238000012216 screening Methods 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 239000012046 mixed solvent Substances 0.000 claims description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920000571 Nylon 11 Polymers 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 7
- 229920000299 Nylon 12 Polymers 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 150000002989 phenols Chemical class 0.000 claims description 6
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 150000008301 phosphite esters Chemical class 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 229920003189 Nylon 4,6 Polymers 0.000 claims description 2
- 229920002292 Nylon 6 Polymers 0.000 claims description 2
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 2
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 2
- 229920000572 Nylon 6/12 Polymers 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000000110 selective laser sintering Methods 0.000 description 17
- 229920000642 polymer Polymers 0.000 description 13
- 239000007767 bonding agent Substances 0.000 description 12
- 239000002131 composite material Substances 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 4
- 238000012805 post-processing Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910002482 Cu–Ni Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000007493 shaping process Methods 0.000 description 3
- 229920006125 amorphous polymer Polymers 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- QZPBMYUQHNTUHM-UHFFFAOYSA-N 2-tert-butyl-4-methylphenol methane Chemical compound C.CC1=CC=C(C(=C1)C(C)(C)C)O QZPBMYUQHNTUHM-UHFFFAOYSA-N 0.000 description 1
- -1 3,5-di-tert-butyl-hydroxy phenyl Chemical group 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical class OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N phthalic acid di-n-butyl ester Natural products CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940080818 propionamide Drugs 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a making method of nylon cover membrane metallic powder material, first heating mixture of nylon resin, solvent, metallic powder and antioxidant in the closing container, dissolving the nylon in the solvent, then gradually cooling, making the nylon as nucleus of metal granular, and gradually crystaling and coating on the surface of metal granular, by vacuum drying, ball milling, screening to select powder distributing by certain particle diameter namely the nylon cover membrane metallic powder material. The material made by the invention has superior sintering performance and good flow characteristics, without containing impurity difficult to remove by after-treatment process. The material has less nylon content, but the SLS original blank has higher accuracy and intensity. Thereby the invention is adapted to SLS indirect making metalwork.
Description
Technical field
The wood invention belongs to the field of material preparation in the advanced manufacturing fast, be specifically related to a kind of preparation method of nylon coating film metal powder material, the prepared nylon coating film metal powder material of this method is particularly useful for selective laser sintering (SLS) and makes metalwork fast indirectly.
Technical background
Selective laser sintering uses pressed powder (as polymer, pottery, precoated metal etc.) as moulding material, cad model slice information according to prototype, utilize computer control laser sintering successively, after the stack that successively is shaped, finally formed required prototype or part.It is wide that this method has moulding material, and manufacture process is not limited by the part complexity, manufacturing efficient height, the characteristics that cost is low.
Because metal parts is of a great variety, superior performance is widely used, thereby adopts the SLS technology directly or indirectly to make the focus that metal parts is the research of various countries, the world today fast.The method of making metal parts with SLS has two kinds of direct method and indirect methods.Direct method is used high power laser exactly, and sintering melts single shaping of metal powders and goes out metalwork, but because direct method still has some technical barriers such as nodularization, easy warpage etc. not to solve, thereby do not obtain wide popularization and application as yet; Indirect method is a bonding agent with low-melting-point metal or polymer exactly, the bonding shaping of matrix material (refractory metal powder), the initial shape base after the shaping just becomes the metal function spare with certain intensity by aftertreatment technologys such as degreasing, high temperature secondary sintering, metallic cementations again by SLS.The advantage of indirect method be with in, the low power laser cost reduces, control easily is shaped, especially with the polymer method that the SLS of bonding agent makes metalwork indirectly, can use low power laser, greatly reduce cost, thereby become one of method of the SLS manufacturing metalwork that is most widely used at present.
Make indirectly in the method for metalwork at the SLS that with the polymer is bonding agent, polymer bonding agent/metal composite powder powder material produces decisive role to intensity, precision and the final metalwork performance of the initial shape base of SLS.The principal element of impact polymer bonding agent/composite metal powder material property has: the kind of polymer bonding agent, addition manner and addition etc.Polymer bonding agent commonly used at present mostly is amorphous polymer, as polymethyl methacrylate and derivative thereof, amorphism PUR etc., because the intensity of the SLS drip molding of amorphous polymer is less, thereby polymer bonding agent consumption (volume content is usually about 20%) that need be bigger, could satisfy the requirement of post processing to initial shape base intensity, and a large amount of polymer bonding agent meetings produces very adverse influence to the final performance of post processing and metal parts, shape base easy deformation during as degreasing and high temperature secondary sintering, subside, shrink to increase and cause precise decreasing etc.; Bonding agent addition manner commonly used has two kinds: mixing method and method with plastic film, mixing method promptly is by mixing apparatus binder powder simply to be mixed with metal dust, and the overlay film rule is by certain special process, and the polymer bonding agent is coated on the metal powder granulates outer surface, forms the overlay film powder.When bonding agent content was identical, the intensity of the initial shape base of overlay film powder and precision all were higher than the initial shape base of mixed-powder.And preparation technology's more complicated of present overlay film powder requires very high to equipment.
In addition, polymer coating film metal powder grain shape by present known method preparation is irregular, mobile relatively poor, need a certain amount of inorganic filler of adding such as Nano carbon white to wait and improve its flowability, and these inorganic powders are difficult to remove in last handling process, thereby final metalwork performance is had a negative impact.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nylon coating film metal powder material, good, the good fluidity of material sintering character that this method is prepared does not contain the impurity that aftertreatment technology is difficult to remove.
The preparation method of nylon coating film metal powder material provided by the invention, its step comprises:
(1) with metal dust, nylon resin, mixed solvent and antioxidant in following ratio composition mixture material, join in the closed container, vacuumize, logical inert gas shielding, wherein,
The particle diameter of metal dust is distributed between 10 microns～50 microns, and grain shape is subsphaeroidal;
The consumption of nylon resin is: per 100 gram metal dusts, and the consumption of nylon resin is 1～3 gram;
The consumption of mixed solvent is: per 100 gram nylon resins, and the mixed solvent consumption is: 500～800 grams; The composition of mixed solvent and mass ratio are: ethanol: 70～85%, and distilled water: 0.1～5%, ethylene glycol: 0.1～20%, propane diols: 0.1～10%;
The consumption of antioxidant is: per 100 gram nylon resins, and the amount of antioxidant is: 0.1 gram～0.5 gram; The composition of antioxidant and mass ratio are: Hinered phenols antioxidant, 60～80%, phosphite ester kind antioxidant, 20～40%;
(2) with the speed of 1～2 ℃/min, the said mixture material is warmed up to 150～160 ℃ gradually, nylon resin is dissolved in the solvent fully, again heat-insulation pressure keeping 2h～3h;
(3) under stirring fast, be cooled to room temperature gradually, form nylon coating film metal powder suspension with 2～4 ℃/min speed;
(4) carry out decompression distillation, chilled suspension is carried out solid-liquid separate, obtain powder aggregates;
(5) powder aggregates that obtains is carried out vacuum drying, carry out ball milling and screening again, select particle diameter to be distributed in 10 microns～50 microns powder, promptly get nylon coating film metal powder material.
The nylon coating film metal powder material that the inventive method is prepared, compare with existing known polymer coating film metal powder and to have the following advantages:
(1), thereby do not need in advance preparation technology has been simplified in the processing that organises of metal dust surface because nylon itself and metal have bonding interface preferably.
(2) well-known, the intensity of the SLS drip molding of semicrystalline polymeric nylon is higher, thereby under the required certain initial shape base intensity of post processing, the nylon amount of required interpolation is less, and this raising to post processing and final metal parts performance is very favorable.
(3) the present invention is that nylon by dissolving is when slow cooling, homogeneously crystallizedly be coated on spherical or subsphaeroidal metal powder granulates surface prepares, thereby the overlay film powder particles shape that obtains also has subglobose feature, flowability and discreteness are very good, need not add lubricated and flow promortor, thereby can not introduce the impurity that last handling process is difficult to remove.
In a word, nylon content is few in the prepared material of the inventive method, utilizes the initial shape base of SLS of its preparation to possess degree of precision and intensity, is very suitable for SLS and makes metalwork indirectly.
The specific embodiment
The present invention heats the mixture of nylon resin, solvent, metal powder and antioxidant in closed container, nylon resin is dissolved in the solvent, cooling gradually then, making nylon is nuclear with the metallic particles, crystallization is coated on surface of metal particles gradually, through solvent recovery, vacuum drying, ball milling, screening selects the powder of certain grain size distribution to be nylon coating film metal powder material.Concrete implementation step of the present invention comprises:
(1) nylon resin, solvent, metal powder and antioxidant are dropped in the closed reaction vessel in proportion, vacuumize, logical inert gas shielding.
Nylon resin is a semicrystalline polymeric, and its melt viscosity is less, can make the initial shape base of SLS of preparation have the advantages that density is big, intensity is high, form accuracy is good.
The preferable range of nylon resin is: nylon 6, nylon 46, nylon 66, NYLON610, nylon 612, nylon 1010, nylon 11, nylon 12, nylon 1212, one or more in the nylon 1313, its further preferable range is that fusing point is lower than 200 ℃ nylon, preheat temperature when material melting point is hanged down laser sintering (SLS) requires also low, and sintering is controlled easily.The consumption of nylon is: per 100 gram metal powders, the consumption of nylon is 1～3 gram.
Solvent is a mixed solvent, and its composition and mass ratio are: 70～85% ethanol, 0.1～5% distilled water, 0.1～20% ethylene glycol, 0.1～10% propane diols.The consumption of mixed solvent is: per 100 gram nylon, the consumption of solvent is: 500～800 grams.
Metal dust can be average grain diameter between 10 microns～50 microns, the powder particle shape is spherical or the subglobose SLS of can be used for makes all metal powder materials of metalwork indirectly, as ferrous alloy, nickel-base alloy, Al alloy powder etc.
Antioxidant is selected the composite antioxidant of being made up of Hinered phenols and phosphorous acid esters for use, and its composition and mass ratio are: Hinered phenols antioxidant 60～80%, phosphite ester kind antioxidant: 20～40%.Hinered phenols antioxidant can preferably following material: 1,3,5-trimethyl-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6-di-t-butyl-4-methyl-phenol, N, N '-two (3,5-di-tert-butyl-hydroxy phenyl propionamide), 2,2 '-two (4-methyl-6-tert butyl-phenol) methane, 2,2 '-two (the 4-ethyl-6-tert-butyl group-phenol) methane etc.Phosphite ester kind antioxidant can preferably following material: 2, and 2 '-ethylenebis (4, the 6-di-tert-butyl-phenyl) fluorophosphite and four (2, the 4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite etc.The consumption of antioxidant: per 100 gram nylon, the amount of antioxidant is: 0.1 gram～0.5 gram.
(2) with the speed of 1～2 ℃/min, be warmed up to 150～160 ℃ gradually, make nylon be dissolved in the solvent heat-insulation pressure keeping 2h～3h fully.
(3) under stirring fast, be cooled to room temperature gradually with 2～4 ℃/min speed, making nylon is nuclear with the metal powder granulates gradually, and crystallization is coated on surface of metal particles, forms nylon coating film metal powder suspension.
(4) carry out decompression distillation, chilled suspension is carried out solid-liquid separate, obtain powder aggregates, the solvent of separating can repeat to recycle.
(5) powder aggregates that obtains ball milling, sieves after vacuum drying, selects particle diameter to be distributed in 10 microns～50 microns powder, promptly gets nylon coating film metal powder material.
Embodiment 1:
(1) gets that 1000 gram particles directly distribute between 10 microns～50 microns, powder particle is shaped as subglobose Fe-Cu-Ni alloy powder, nylon 12 resins 20 grams, mixed solvent 160 grams and composite antioxidant 0.02 gram drop in the stainless steel 50L reactor of strap clamp cover, and reactor is sealed, vacuumize logical N
2Gas shiled.The proportioning of mixed solvent is: 85% ethanol, 1% distilled water, 10% ethylene glycol, 4% propane diols.The proportioning of composite antioxidant is: 1,3, and 5-trimethyl-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene is 80%, four (2, the 4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite is 20%.
(2) with the speed of 1 ℃/min, be warmed up to 150 ℃ gradually, make nylon 12 be dissolved in the solvent heat-insulation pressure keeping 2h fully.
(3) under vigorous stirring, be cooled to room temperature gradually with 2 ℃/min speed, making nylon 12 is nuclear with the alloy powder particle, crystallization is coated on the alloy powder particle surface gradually, forms nylon 12 overlay film Fe-Cu-Ni alloy powder suspension.
(4) in reactor, by decompression distillation, chilled suspension is carried out solid-liquid separate, the solvent that obtains can repeat to recycle.
(5) powder aggregates that obtains after vacuum drying, ball milling, screening, the powder of selecting particle diameter to be distributed in 10 microns～50 microns promptly gets nylon 12 overlay film Fe-Cu-Ni alloy powder materials.
Embodiment 2:
(1) gets that 1000 gram particles directly are distributed between 10 microns～50 microns, powder particle is shaped as subglobose 00Cr17Ni14Mo2 powder of stainless steel, particle diameter distributes between 10 microns～50 microns, powder particle is shaped as subsphaeroidal nylon 11 resin 16 grams, mixed solvent 128 grams and composite antioxidant 0.048 gram drop in the stainless steel 50L reactor of strap clamp cover, reactor is sealed, vacuumize logical N
2Gas shiled.The proportioning of mixed solvent is: 80% ethanol, 2% distilled water, 15% ethylene glycol, 3% propane diols.The proportioning of composite antioxidant is: 1,3, and 5-trimethyl-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene is 80%, four (2, the 4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite is 20%.
(2) with the speed of 2 ℃/min, be warmed up to 150 ℃ gradually, make nylon 11 be dissolved in the solvent heat-insulation pressure keeping 3h fully.
(3) under vigorous stirring, be cooled to room temperature gradually with 4 ℃/min speed, making nylon 11 is nuclear with the powder particle, crystallization is coated on the powder of stainless steel particle surface gradually, forms nylon 11 overlay film 00Cr17Ni14Mo2 powder of stainless steel suspension.
(4) in reactor, by decompression distillation, chilled suspension is carried out solid-liquid separate, the solvent that obtains can repeat to recycle.
(5) powder aggregates that obtains after vacuum drying, ball milling, screening, the powder of selecting particle diameter to be distributed in 10 microns～50 microns promptly gets nylon 11 overlay film 00Cr17Ni14Mo2 powder of stainless steel.
Embodiment 3:
(1) gets that 1000 gram particles directly distribute between 10 microns～50 microns, powder particle is shaped as subglobose copper powders may, nylon 11 resin 8 grams, nylon 1212 resin 8 grams, mixed solvent 128 grams and composite antioxidant 0.032 gram drop in the stainless steel 50L reactor of strap clamp cover, reactor is sealed, vacuumize logical N
2Gas shiled.The proportioning of mixed solvent is: 80% ethanol, 2% distilled water, 15% ethylene glycol, 3% propane diols.The proportioning of composite antioxidant is: 1,3, and 5-trimethyl-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene is 80%, four (2, the 4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite is 20%.
(2) with the speed of 2 ℃/min, be warmed up to 160 ℃ gradually, make nylon 11 and nylon 1212 be dissolved in the solvent heat-insulation pressure keeping 3h fully.
(3) under stirring fast, be cooled to room temperature gradually with 4 ℃/min speed, making nylon 11 and nylon 1212 is nuclear with the powder particle, and crystallization is coated on the powder of stainless steel particle surface gradually, forms nylon 11 and nylon 1212 overlay film copper powder suspension.
(4) in reactor, by decompression distillation, chilled suspension is carried out solid-liquid separate, the solvent that obtains can repeat to recycle.
(5) powder aggregates that obtains after vacuum drying, ball milling, screening, the powder of selecting particle diameter to be distributed in 10 microns～50 microns promptly gets nylon 11 and nylon 1212 overlay film copper powders may material.
Claims (5)
1, a kind of preparation method of nylon coating film metal powder material, its step comprises:
(1) with metal dust, nylon resin, mixed solvent and antioxidant in following ratio composition mixture material, join in the closed container, vacuumize, logical inert gas shielding, wherein,
The particle diameter of metal dust is distributed between 10 microns～50 microns, and grain shape is subsphaeroidal;
The consumption of nylon resin is: per 100 gram metal dusts, and the consumption of nylon resin is 1～3 gram;
The consumption of mixed solvent is: per 100 gram nylon resins, and the mixed solvent consumption is: 500～800 grams; The composition of mixed solvent and mass ratio are: ethanol: 70～85%, and distilled water: 0.1～5%, ethylene glycol: 0.1～20%, propane diols: 0.1～10%;
The consumption of antioxidant is: per 100 gram nylon resins, and the amount of antioxidant is: 0.1 gram～0.5 gram; The composition of antioxidant and mass ratio are: Hinered phenols antioxidant, 60～80%, phosphite ester kind antioxidant, 20～40%;
(2) with the speed of 1～2 ℃/min, the said mixture material is warmed up to 150～160 ℃ gradually, nylon resin is dissolved in the solvent fully, again heat-insulation pressure keeping 2h～3h;
(3) under stirring fast, be cooled to room temperature gradually, form nylon coating film metal powder suspension with 2～4 ℃/min speed;
(4) carry out decompression distillation, chilled suspension is carried out solid-liquid separate, obtain powder aggregates;
(5) powder aggregates that obtains is carried out vacuum drying, carry out ball milling and screening again, select particle diameter to be distributed in 10 microns～50 microns powder, promptly get nylon coating film metal powder material.
2, preparation method according to claim 1 is characterized in that: nylon resin is: nylon 6, nylon 46, nylon 66, NYLON610, nylon 612, nylon 1010, nylon 11, nylon 12, the mixing of one or more in nylon 1212 or the nylon 1313.
3, preparation method according to claim 1 is characterized in that: nylon resin is a fusing point smaller or equal to 200 ℃ nylon resin.
4, according to claim 1,2 or 3 described preparation methods, it is characterized in that: described Hinered phenols antioxidant is: 1,3, and 5-trimethyl-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene.
5, according to claim 1,2 or 3 described preparation methods, it is characterized in that: described phosphite ester kind antioxidant is: four (2, the 4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100517959A CN100503090C (en) | 2007-04-04 | 2007-04-04 | Method for preparing nylon coating film metal powder material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100517959A CN100503090C (en) | 2007-04-04 | 2007-04-04 | Method for preparing nylon coating film metal powder material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101036944A CN101036944A (en) | 2007-09-19 |
| CN100503090C true CN100503090C (en) | 2009-06-24 |
Family
ID=38888238
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100517959A Expired - Fee Related CN100503090C (en) | 2007-04-04 | 2007-04-04 | Method for preparing nylon coating film metal powder material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100503090C (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140246A (en) * | 2010-12-21 | 2011-08-03 | 湖南华曙高科技有限责任公司 | Method for preparing nylon powder for selective laser sintering |
| CN104668553B (en) * | 2015-01-30 | 2016-08-17 | 成都新柯力化工科技有限公司 | A kind of alloyed powder printing metal parts for direct 3D and preparation method thereof |
| CN104801703B (en) * | 2015-03-26 | 2016-08-24 | 成都新柯力化工科技有限公司 | A kind of flexible metal powder for 3 D-printing and its preparation method and application method |
| CN104858422B (en) * | 2015-05-22 | 2017-05-31 | 东莞劲胜精密组件股份有限公司 | A kind of stainless steel composite powder for 3D printing and preparation method thereof |
| CN105820562B (en) * | 2016-04-28 | 2018-04-20 | 河南工程学院 | A kind of selective laser sintering electroconductive nylon composite powder and preparation method thereof |
| CN106832910B (en) * | 2016-12-16 | 2019-12-10 | 湖南华曙高科技有限责任公司 | Preparation method of nylon conductive powder for laser sintering |
| CN108015271A (en) * | 2017-12-12 | 2018-05-11 | 成都育芽科技有限公司 | A kind of 3D printing high strength and modulus composite particulate material preparation method |
| CN108788123A (en) * | 2018-05-08 | 2018-11-13 | 苏州耐思特塑胶有限公司 | A kind of preparation method of metal die dusty material |
| CN109175353B (en) * | 2018-09-13 | 2021-05-11 | 北京有研粉末新材料研究院有限公司 | Surface coating method for automatic pressing and forming of spherical powder |
| CN109517377B (en) * | 2018-11-09 | 2020-06-30 | 湖南华曙高科技有限责任公司 | Nylon polymer powder material and preparation method thereof |
| CN111269563A (en) * | 2020-04-02 | 2020-06-12 | 贵州省冶金化工研究所 | Nylon composite Sn-Bi material for 3D laser printing and manufacturing method thereof |
| CN113695567B (en) * | 2021-07-28 | 2022-10-14 | 北京科技大学 | Coated copper alloy for selective laser sintering printing and preparation and sintering method |
-
2007
- 2007-04-04 CN CNB2007100517959A patent/CN100503090C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101036944A (en) | 2007-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100503090C (en) | Method for preparing nylon coating film metal powder material | |
| CN100432019C (en) | Manufacture method for nylon tectorial membrane ceramics powder material | |
| CN111097919B (en) | Preparation method of multi-component refractory alloy spherical powder | |
| CN104191615A (en) | Preparation method of high-molecular polymer powder material applied to 3D printing | |
| CN1649688A (en) | Blended powder solid-supersolidus liquid phase sintering | |
| CN105985632A (en) | Powder material for selective laser sintering and preparation method thereof | |
| WO2016119556A1 (en) | Aluminum powder used for 3d printing, and method for preparation of said aluminum powder | |
| CN1044727C (en) | Semi-solid processed magnesium-beryllium alloys | |
| CN107052225A (en) | Spherical fused silica of special sand and its preparation method and application | |
| CN106243705B (en) | The alloy powder material preparation method of long-chain nylon and nylon 6 for SLS | |
| CN101319075A (en) | Copolymer based powdered material for selective laser sintering and preparation method thereof | |
| CN101146919B (en) | Formed articles including master alloy, and methods of making and using the same | |
| CN103394700B (en) | The prealloy diffusion method of production tin bronze powder | |
| CN110842204B (en) | 3D printing method for selective laser solidified metal | |
| CN109226742A (en) | A kind of ultra-fine cemented carbide injection moulding feeding and preparation method thereof | |
| CN108178931A (en) | Special wax wire of a kind of hot investment casting fused glass pellet 3D printing essence mould and preparation method thereof | |
| CN106810268B (en) | Ceramic 3D printing material based on selective laser sintering and preparation method thereof | |
| CN102672109A (en) | Easy-to-demould precoated sand and production process of easy-to-demould precoated sand | |
| CN103554841A (en) | Resin composite material applicable to fast prototyping technology | |
| CN106147220B (en) | For the long-chain nylon of SLS and nylon66 fiber alloy powder material preparation method | |
| CN105108134B (en) | A kind of paste metallic composite for 3D printing and preparation method thereof | |
| CN1669704A (en) | Process for preparing tungsten parts and components with complicated shape and high dimensional accuracy | |
| CN109926589A (en) | The injection moulding method and mold of ultra-fine cemented carbide CNC turning tool | |
| CN109679301B (en) | Filler model material based on graphene/polyethylene glycol terephthalate modified resin and preparation method thereof | |
| CN108192360A (en) | A kind of dental selective laser sintering 3D printing wax powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090624 |