CN104190935B - The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body - Google Patents

The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body Download PDF

Info

Publication number
CN104190935B
CN104190935B CN201410437077.5A CN201410437077A CN104190935B CN 104190935 B CN104190935 B CN 104190935B CN 201410437077 A CN201410437077 A CN 201410437077A CN 104190935 B CN104190935 B CN 104190935B
Authority
CN
China
Prior art keywords
powder
granularity
nickel powder
sintering
nickel
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.)
Active
Application number
CN201410437077.5A
Other languages
Chinese (zh)
Other versions
CN104190935A (en
Inventor
高麟
汪涛
焦鹏鹤
吴磊
王韬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Intermet Technology Chengdu Co Ltd
Original Assignee
Intermet Technology Chengdu Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Intermet Technology Chengdu Co Ltd filed Critical Intermet Technology Chengdu Co Ltd
Priority to CN201410437077.5A priority Critical patent/CN104190935B/en
Publication of CN104190935A publication Critical patent/CN104190935A/en
Application granted granted Critical
Publication of CN104190935B publication Critical patent/CN104190935B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Powder Metallurgy (AREA)

Abstract

The preparation method of the powder sintered porous body of formed body rhegma probability and the pre-molding body of the sintered body is prepared the invention discloses a kind of aperture size for being capable of the powder sintered porous body of easy and effective control, and when can reduce pressure forming.The method is:Step includes dispensing, shaping and sinters, during dispensing shape, the first powder and the second powder of different sizes are used for the basic material powder for preparing the porous body, first powder is smaller compared to the second powder granularity and briquettability when being molded is more preferable, and the first powder accounts for the 10~90% of the basic material powder gross mass.Because the first powder has briquettability preferable, the sintering less feature of back aperture, the characteristics of second powder has sintering back aperture larger, after above-mentioned first powder and the second powder are sufficiently mixed, first powder can be filled in the space formed between the second powder, on the one hand play a part of material aperture after control sintering, on the one hand improve the briquettability of mixed powder.

Description

The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body
Technical field
The present invention relates to powder sintered porous body preparation method and prepare the pre-molding body of the sintered body.
Background technology
Applicant concentrates on the extension in materials application field, material to the research emphasis of powder sintered porous filter material at present Expect several aspects such as improvement, the optimization probed into preparation technology of pore formation mechanism of performance.In sintered porous filtering material application In the extension in field, courageously propose and develop and can correspondingly meet this for some specific and relatively harsher applied environments Chemical stability (such as corrosion resistance) under applied environment is required and with the new material of good strainability.Its meaning is, If such new material is once succeeded in developing, it becomes possible to bring secondary filter technology into corresponding field, thus change the field Conventional process flow, its result is often the very big improvement of environmental pollution and long-term economic benefit and social benefit Lifting.But, in the development process of new material, in addition to the research to material composition, usually can also face sintered porousization Problems in journey, for example:The excessive influence permeance property of the meander factor, material aperture are difficult after sintering densification, sintering With control etc..Therefore, the successful exploitation of a kind of new material often can accordingly be related at aspects such as pore formation mechanism, preparation technologies Innovation.
The content of the invention
The present invention is intended to provide several (refer to the substance system that thing to be filtered is formed, can be liquid for particular filter system Body system or gas system) show excellent chemical stability and good strainability powder sintered porous filtering alloy, The preparation method of the alloy and prepare the pre-molding body of the alloy.
The first powder sintered porous filtering alloy of the invention, it is substantially by by mass percentage 26~30% Mo, 0~2% Fe, 0~0.1% Cr, 0~0.02% C, 0~0.1% Si, 0~1% Mn, 0~5% Al, 0 ~1.5% Ti and the Ni of surplus are constituted;Its average pore size is not more than 20 μm and relative infiltration is when being filtered as liquid Number is not less than 0.2m3/m2Kpah, its average pore size is not more than 60 μm and relative permeability is not small during as gas filtration In 80m3/m2·kpa·h.It is to be understood that above-mentioned term " substantially by ... constituted ", specifically containing in the present invention Justice refers to:The powder sintered porous filtering alloy only can be made up of above-mentioned these elements;The unit can also mainly included Add that other are micro, will not substantially change the element of alloy property, such as Nb, V, W, Y, Ta, Zr, Co etc. on the basis of element. And the concrete meaning on " relative coefficient of permeability " and " relative permeability " will be illustrated in a specific embodiment.
The characteristics of above-mentioned the first powder sintered porous filtering alloy is:First, the powder sintered porous filtering alloy needle To complete reduction system, (i.e. non-oxidative ion is present, such as Fe3+、Cu2+Deng) corrosion resistance is very superior;Secondly, it is resistant to normal Pressure any temperature, the corrosion of any concentration hydrochloric acid;Additionally, non-oxidizable sulfuric acid in non-aerating intermediate concentration, various dense There is excellent corrosion resisting property in organic acid, bromic acid and the hydrogen chloride gas such as degree phosphoric acid, high temperature acetic acid, formic acid;Also it is resistance in addition The corrosion of halogen family catalyst.Described the first powder sintered porous filtering alloy is relatively specific for oil, the chemical industry of various harshnesses The distillation of process, such as hydrochloric acid, concentration;In the production process such as the alkylation of ethylbenzene and low-pressure carbonyl synthesized acetate.
In above-mentioned the first powder sintered porous filtering alloy, Cr, C, Si, Mn, Al, Ti are optional component.Wherein Cr, C, Si, Mn can be added to improve the chemical stability of alloy according to the specific residing filtration system of alloy.The major significance of Al It is that can to a certain extent drop low-alloyed tortuosity after adding.When alloy disclosure satisfy that filtration permeability requirement, can To be added without Al;But in the case where Al is added, because Al can be changed into liquid phase and enter in the high-temperature sintering process for prepare alloy And promote the flowing of powder particle, so that the duct that sintering is formed is more round and smooth, thus low-alloyed tortuosity drops.For The purpose of filtration permeability is improved, the weight/mass percentage composition of the Al elements is preferably 1~5%, can also be more preferably 3~ 5%.In addition, the addition of Ti can improve the high temperature hot strength of alloy.When high temperature filtration system may be faced (such as 300~ 800 DEG C of high temperature air filtration) weight/mass percentage composition of Ti elements is preferably 0.2~1%, more preferably 0.5~1%.
The preparation method of above-mentioned the first powder sintered porous filtering alloy, its step includes:1) by each element powder according to The ratio of above-mentioned setting is mixed, and wherein Ni powder uses the first nickel powder and the second nickel powder, and first nickel powder is strip, institute The second nickel powder is stated for spherical or near-spherical, the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and by The ratio that one nickel powder accounts for the 10~90% of Ni powder gross masses is added;2) above-mentioned mixed powder is granulated, dried and is pressed successively Power is molded, and drying temperature is set as into 40~60 DEG C, and drying time is set as 4~8 hours, then carries out pressure forming, pressure During shaping under 120~200MPa briquetting pressures pressurize 20~80 seconds, pre-molding body is obtained after pressure forming;3) to being pressed into advance Type body is sintered, and process comprises at least following two stages:The degreasing stage:Sintering temperature rises to 350~450 DEG C from room temperature, And it is incubated 60~300 minutes;The high temperature sintering stage:Sintering temperature is risen to 1050~1280 DEG C, and is incubated 60~180 minutes; Cooling obtains the porous filtering alloy.In the above method, the powder sintered porous filtering alloy that liquid is filtered is used as when preparing, It is granulating agent preferably to use stearic acid when then granulating, and stearic addition is the 2~8% of mixed powder gross mass;Work as system The standby powder sintered porous filtering alloy for making gas filtration, then it is granulating agent preferably use urea when granulating, and urea adds It is the 5~20% of mixed powder gross mass to enter amount.In addition, first nickel powder is also further excellent with the ratio between the granularity of the second nickel powder Elect 1 as:(2~4).Briquetting pressure during pressure forming can also be more preferably 120~150MPa.
Formed body rhegma problem when above-mentioned preparation method can be good at avoiding sintering densification problem and pressure forming, And material aperture can be control effectively.First, the method is creative will constitute the raw material powder (Ni of the infrastructure elements Ni of alloy Powder) it has been divided into the first nickel powder and the second nickel powder, wherein the first nickel powder is strip, the second nickel powder is spherical or near-spherical, first The ratio between granularity of nickel powder and the second nickel powder is 1:(1.2~5) (preferably 1:(2~4)), and the first nickel powder accounts for Ni powder gross masses 10~90%, so, because the first nickel powder is the less strip nickel powder of granularity, with briquettability, preferably (formed body is difficult to split Damage), sinter the less feature of back aperture, and the second nickel powder is the larger spherical or near-spherical nickel powder of granularity, with briquettability compared with Difference (the easy rhegma of formed body), the characteristics of sintering back aperture is larger, after above-mentioned first nickel powder and the second nickel powder are sufficiently mixed, the One nickel powder can be filled in the space formed between the second nickel powder, on the one hand play a part of material aperture (root after control sintering Adjust the ratio of the first nickel powder according to the pore diameter range for needing, such as 30%, 50%, 70%), on the one hand improve the mixed of mixed powder Powder pressing is closed, formed body rhegma probability when reducing pressure forming;In addition, the first nickel powder granularity increases the whole of Ni powder compared with I Body activity, so as to reduce sintering temperature, promotes the flowing and development of crystal grain in Powder during Sintering Process, and prevent to a certain extent Sintering densification.Secondly, the briquettability for specific blend powder is further optimized by the selection of pressure forming parameter, is entered One step improves the qualification rate of pressure forming.Also, according to material composition, sintering temperature rises to 1050 by the high temperature sintering stage~ 1280 DEG C and it is incubated the special setting of 60~180 minutes and can ensures the generation of a small amount of liquid phase during sintering, sintering is avoided well Densification problem.
The resulting pre-molding body for preparing powder sintered porous filtering alloy during the implementation above method, Ni powder uses the first nickel powder and the second nickel powder in constituting the powder particle of the pre-molding body, and first nickel powder is strip, Second nickel powder is spherical or near-spherical, and the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and the One nickel powder accounts for the 10~90% of Ni powder gross masses.The ratio between granularity of first nickel powder and the second nickel powder more preferably 1:(2 ~4).
Second powder sintered porous filtering alloy of the invention, it is substantially by by mass percentage 14~17% Cr, 15~17% Mo, 0~7% Fe, 0~4.5% W, 0~2.5% Co, 0~0.08% C, 0~1% Si, 0 ~1% Mn, 0~0.35% V, 0~0.04% P, 0~0.03% S, 0~5% Al, 0~1.5% Ti and The Ni of surplus is constituted;Its average pore size is not more than 20 μm and relative coefficient of permeability is not less than 0.2m when being filtered as liquid3/m2· Kpah, its average pore size is not more than 60 μm and relative permeability is not less than 80m during as gas filtration3/m2·kpa·h。 The concrete meaning of above-mentioned term " substantially by ... constituted " refers to:The powder sintered porous filtering alloy can only by above-mentioned These elements are constituted;Can also add that other are micro, will not substantially change alloy on the basis of mainly the element is included Element of performance, such as Nb, Y, Ta, Zr etc..
The characteristics of above-mentioned second powder sintered porous filtering alloy is:First, the powder sintered porous filtering alloy exists In oxidisability and reproducibility system, superior rotproofness is shown;Secondly, main moisture-proof chlorine, various oxidisability chlorides, chlorine Salt dissolving solution, sulfuric acid and oxidisability salt;Additionally, having good corrosion resisting property in low temperature with the acid of middle thermohaline.Therefore, the powder Sintered porous filtering alloy ratio is relatively adapted to should in the industrial circle such as chemical industry, petrochemical industry, flue gas desulfurization, paper pulp and papermaking, environmental protection With.
In above-mentioned second powder sintered porous filtering alloy, Fe, Co, W, C, Si, Mn, V, P, S, Al, Ti are optional group Point.Wherein Co, C, Si, Mn, V, P, S can be added steady to improve the chemistry of alloy according to the specific residing filtration system of alloy It is qualitative.The weight/mass percentage composition of W can be more preferably 3~4.5%, can so improve resistance to reduction dielectric corrosion, such as office Portion's spot corrosion, crevice corrosion;The weight/mass percentage composition of Fe can be more preferably 4~7%.The major significance of Al is can after adding Low-alloyed tortuosity drops to a certain extent.When alloy disclosure satisfy that filtration permeability requirement, Al can be added without;But In the case where Al is added, because Al can be changed into liquid phase and then promote powder particle in the high-temperature sintering process for prepare alloy Flowing so that sintering formed duct it is more round and smooth, thus low-alloyed tortuosity drops.For raising filtration permeability Purpose, the weight/mass percentage composition of the Al elements is preferably 1~5%, can also be more preferably 3~5%.In addition, Ti Addition can improve the high temperature hot strength of alloy.When that may face high temperature filtration system, the weight/mass percentage composition of Ti elements is preferred It is 0.2~1%, more preferably 0.5~1%.
The preparation method of above-mentioned second powder sintered porous filtering alloy, its step includes:1) by each element powder according to The ratio of above-mentioned setting is mixed, and wherein Ni powder uses the first nickel powder and the second nickel powder, and first nickel powder is strip, institute The second nickel powder is stated for spherical or near-spherical, the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and by The ratio that one nickel powder accounts for the 10~90% of Ni powder gross masses is added;2) above-mentioned mixed powder is granulated, dried and is pressed successively Power is molded, and drying temperature is set as into 40~60 DEG C, and drying time is set as 4~8 hours, then carries out pressure forming, pressure During shaping under 120~200MPa briquetting pressures pressurize 20~80 seconds, pre-molding body is obtained after pressure forming;3) to being pressed into advance Type body is sintered, and process comprises at least following two stages:The degreasing stage:Sintering temperature rises to 350~450 DEG C from room temperature, And it is incubated 60~300 minutes;The high temperature sintering stage:Sintering temperature is risen to 1150~1280 DEG C, and is incubated 60~180 minutes; Cooling obtains the porous filtering alloy.In the above method, the powder sintered porous filtering alloy that liquid is filtered is used as when preparing, It is granulating agent preferably to use stearic acid when then granulating, and stearic addition is the 2~8% of mixed powder gross mass;Work as system The standby powder sintered porous filtering alloy for making gas filtration, then it is granulating agent preferably use urea when granulating, and urea adds It is the 5~20% of mixed powder gross mass to enter amount.In addition, first nickel powder is also further excellent with the ratio between the granularity of the second nickel powder Elect 1 as:(2~4).Briquetting pressure during pressure forming can be more preferably 120~150MPa.
Formed body rhegma problem when above-mentioned preparation method can be good at avoiding sintering densification and pressure forming, and can Material aperture is control effectively.First, the method is creative will constitute the raw material powder (Ni powder) of the infrastructure elements Ni of alloy The first nickel powder and the second nickel powder have been divided into it, the first nickel powder is strip, the second nickel powder is spherical or near-spherical, the first nickel powder and the The ratio between granularity of two nickel powders is 1:(1.2~5), and the first nickel powder accounts for the 10~90% of Ni powder gross masses, so, due to the first nickel Powder is the less strip nickel powder of granularity, with briquettability preferably, sinters the less feature of back aperture, and the second nickel powder is granularity Larger spherical or near-spherical nickel powder, it is poor with briquettability, the characteristics of sintering back aperture is larger, by above-mentioned first nickel powder and the After two nickel powders are sufficiently mixed, the first nickel powder can be filled in the space formed between the second nickel powder, on the one hand play control sintering Afterwards material aperture effect (ratio of the nickel powder of aperture adjustment first as needed, such as 30%, 50%, 70%), on the one hand Improve mixed powder mixed powder briquettability, reduce pressure forming when formed body rhegma probability, in addition, the first nickel powder granularity compared with I increases the overall activity of Ni powder, so as to reduce sintering temperature, promotes the flowing and development of crystal grain in Powder during Sintering Process, and Sintering densification is prevented to a certain extent.Secondly, further optimized for specific mixed by the selection of pressure forming parameter The briquettability of powder is closed, the qualification rate of pressure forming is further improved.Also, according to material composition, the high temperature sintering stage will Sintering temperature rises to 1150~1280 DEG C and is incubated the special setting of 60~180 minutes, sintering densification is avoided well and is asked Topic.
The resulting pre-molding body for preparing powder sintered porous filtering alloy during the implementation above method, Ni powder uses the first nickel powder and the second nickel powder in constituting the powder particle of the pre-molding body, and first nickel powder is strip, Second nickel powder is spherical or near-spherical, and the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and the One nickel powder accounts for the 10~90% of Ni powder gross masses.The ratio between granularity of first nickel powder and the second nickel powder is further 1:(2~ 4)。
The third powder sintered porous filtering alloy that the present invention is provided, substantially by by mass percentage 21~23.5% Cr, 6~8% Mo, 18~21% Fe, 0~1.5% W, 0~2.5% Co, 0~0.05% C, 0~1% The Ni of Si, 0~2% Mn, 0~2.5% Ta or/and Nb, 0~5% Al, 0~1.5% Ti and surplus is constituted;With Its average pore size is not more than 20 μm and relative coefficient of permeability is not less than 0.2m when making liquid filtering3/m2Kpah, as gas Its average pore size is not more than 60 μm and relative permeability is not less than 80m during filtering3/m2·kpa·h.Above-mentioned term is " substantially By ... constituted " concrete meaning refer to:The powder sintered porous filtering alloy only can be made up of above-mentioned these elements;When The right powder sintered porous filtering alloy can also add other micro, Bu Huiming on the basis of mainly the element is included The aobvious element for changing alloy property, such as V, Y, Zr etc..
The characteristics of above-mentioned the third powder sintered porous filtering alloy is:The powder sintered porous filtering alloy needle is to strong oxygen Changing gonosome system has splendid resistance;Especially resistance to phosphoric acid, sulfuric acid, sulfate etc..
In above-mentioned the third powder sintered porous filtering alloy, W, Co, C, Si, Mn, Ta, Nb, Al, Ti are optional component. Wherein W, Co, C, Si, Mn, Ta, Nb can be added steady to improve the chemistry of alloy according to the specific residing filtration system of alloy It is qualitative.The weight/mass percentage composition of Mn can be more preferably 1.5~2.5%, and the red brittleness of material can be so obviously reduced;Ta Or/and the weight/mass percentage composition of Nb can be more preferably 1~2%, material resistance local corrosion can be so significantly improved Effect, while improve material heat endurance.The major significance of Al is that can to a certain extent drop low-alloyed after adding Tortuosity.When alloy disclosure satisfy that filtration permeability requirement, Al can be added without;But in the case where Al is added, due to Al can be changed into liquid phase and then promote the flowing of powder particle in the high-temperature sintering process for prepare alloy, so that sintering is formed Duct it is more round and smooth, thus low-alloyed tortuosity drops.For the purpose for improving filtration permeability, the matter of the Al elements Amount percentage composition is preferably 1~5%, can also be more preferably 3~5%.In addition, the addition of Ti can improve the high temperature of alloy Calorific intensity.When that may face high temperature filtration system, the weight/mass percentage composition of Ti elements is preferably 0.2~1%, further preferably It is 0.5~1%.
The preparation method of above-mentioned the third powder sintered porous filtering alloy, its step includes:1) by each element powder according to The ratio of above-mentioned setting is mixed, and wherein Ni powder uses the first nickel powder and the second nickel powder, and first nickel powder is strip, institute The second nickel powder is stated for spherical or near-spherical, the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and by The ratio that one nickel powder accounts for the 10~90% of Ni powder gross masses is added;2) above-mentioned mixed powder is granulated, dried and is pressed successively Power is molded, and drying temperature is set as into 40~60 DEG C, and drying time is set as 4~8 hours, then carries out pressure forming, pressure During shaping under 120~200MPa briquetting pressures pressurize 20~80 seconds, pre-molding body is obtained after pressure forming;3) to being pressed into advance Type body is sintered, and process comprises at least following two stages:The degreasing stage:Sintering temperature rises to 350~450 DEG C from room temperature, And it is incubated 60~300 minutes;The high temperature sintering stage:Sintering temperature is risen to 1150~1310 DEG C, and is incubated 60~180 minutes; Cooling obtains the porous filtering alloy.In the above method, the powder sintered porous filtering alloy that liquid is filtered is used as when preparing, It is granulating agent preferably to use stearic acid when then granulating, and stearic addition is the 2~8% of mixed powder gross mass;Work as system The standby powder sintered porous filtering alloy for making gas filtration, then it is granulating agent preferably use urea when granulating, and urea adds It is the 5~20% of mixed powder gross mass to enter amount.In addition, first nickel powder is also further excellent with the ratio between the granularity of the second nickel powder Elect 1 as:(2~4).Briquetting pressure during pressure forming can be more preferably 120~150MPa.
Formed body rhegma problem when above-mentioned preparation method can be good at avoiding sintering densification and pressure forming, and can Material aperture is control effectively.First, the method is creative will constitute the raw material powder (Ni powder) of the infrastructure elements Ni of alloy The first nickel powder and the second nickel powder have been divided into it, the first nickel powder is strip, the second nickel powder is spherical or near-spherical, the first nickel powder and the The ratio between granularity of two nickel powders is 1:(1.2~5), and the first nickel powder accounts for the 10~90% of Ni powder gross masses, so, due to the first nickel Powder is the less strip nickel powder of granularity, with briquettability preferably, sinters the less feature of back aperture, and the second nickel powder is granularity Larger spherical or near-spherical nickel powder, it is poor with briquettability, the characteristics of sintering back aperture is larger, by above-mentioned first nickel powder and the After two nickel powders are sufficiently mixed, the first nickel powder can be filled in the space formed between the second nickel powder, on the one hand play control sintering Afterwards material aperture effect (ratio of the nickel powder of aperture adjustment first as needed, such as 30%, 50%, 70%), on the one hand Improve mixed powder mixed powder briquettability, reduce pressure forming when formed body rhegma probability, in addition, the first nickel powder granularity compared with I increases the overall activity of Ni powder, so as to reduce sintering temperature, promotes the flowing and development of crystal grain in Powder during Sintering Process, and Sintering densification is prevented to a certain extent.Secondly, further optimized for specific mixed by the selection of pressure forming parameter The briquettability of powder is closed, the qualification rate of pressure forming is further improved.Also, according to material composition, the high temperature sintering stage will Sintering temperature rises to 1150~1310 DEG C and is incubated the special setting of 60~180 minutes, sintering densification is avoided well and is asked Topic.
The resulting pre-molding body for preparing porous filtering alloy, constitutes this pre- during the implementation above method Ni powder uses the first nickel powder and the second nickel powder in the powder particle of molded body, and first nickel powder is strip, described second Nickel powder is spherical or near-spherical, and the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and the first nickel powder accounts for The 10~90% of Ni powder gross masses.The ratio between granularity of first nickel powder and the second nickel powder is further 1:(2~4).
4th kind of powder sintered porous filtering alloy of the invention, it is substantially by by mass percentage 14~17% Cr, 6~10% Fe, 0~0.15% C, 0~0.5% Si, 0~1% Mn, 0~0.05% Cu, 0~5% Al, 0~1.5% Ti and the Ni of surplus are constituted, and its average pore size is not more than 60 μm and relative permeability is not less than 80m3/ m2·kpa·h.It is to be understood that above-mentioned term " substantially by ... constituted ", concrete meaning refers to:This is powder sintered Porous filtering alloy only can be made up of above-mentioned these elements;Other can also be added on the basis of mainly the element is included Micro, element that is will not substantially changing alloy property, such as Nb, V, W, Y, Ta, Zr, Co etc..
Above-mentioned 4th kind of powder sintered porous filtering alloy has good resistance to chlorine, the characteristic of hydrogen chloride gas corrosion (particularly under the high temperature conditions), is particularly suited for the gas solid separation filtering under high temperature chlorine, chlorination hydrogen system.
In above-mentioned 4th kind of powder sintered porous filtering alloy, C, Si, Mn, Cu, Al, Ti are optional component.Wherein Cr, C, Si, Mn, Cu can be added to improve the chemical stability of alloy according to the specific residing filtration system of alloy.The main meaning of Al Justice is that can to a certain extent drop low-alloyed tortuosity after adding.When alloy disclosure satisfy that filtration permeability requirement, Al can be added without;But in the case where Al is added, because Al can be changed into liquid phase in the high-temperature sintering process for prepare alloy And then the flowing of promotion powder particle, so that the duct that sintering is formed is more round and smooth, thus low-alloyed tortuosity drops.Go out In the purpose for improving filtration permeability, the weight/mass percentage composition of the Al elements is preferably 1~5%, can also be more preferably 3 ~5%.In addition, the addition of Ti can improve the high temperature hot strength of alloy.When high temperature filtration system may be faced (such as 300 ~800 DEG C of high temperature air filtration) Ti elements weight/mass percentage composition be preferably 0.2~1%, more preferably 0.5~ 1%.
The preparation method of above-mentioned 4th kind of powder sintered porous filtering alloy, its step includes:1) by each element powder according to The ratio of above-mentioned setting is mixed, and wherein Ni powder uses the first nickel powder and the second nickel powder, and first nickel powder is strip, institute The second nickel powder is stated for spherical or near-spherical, the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and by The ratio that one nickel powder accounts for the 10~90% of Ni powder gross masses is added;2) above-mentioned mixed powder is granulated, dried and is pressed successively Power is molded, and drying temperature is set as into 40~60 DEG C, and drying time is set as 4~8 hours, then carries out pressure forming, pressure During shaping under 120~220MPa briquetting pressures pressurize 20~80 seconds, pre-molding body is obtained after pressure forming;3) to being pressed into advance Type body is sintered, and process comprises at least following two stages:The degreasing stage:Sintering temperature rises to 350~450 DEG C from room temperature, And it is incubated 60~300 minutes;The high temperature sintering stage:Sintering temperature is risen to 1200~1320 DEG C, and is incubated 120~300 minutes; Cooling obtains the porous filtering alloy.In the above method, it is granulating agent, the addition of urea preferably to use urea during granulation It is the 5~20% of mixed powder gross mass.In addition, the ratio between first nickel powder and granularity of the second nickel powder are still further preferably 1:(2~4).Briquetting pressure during pressure forming can also be more preferably 150~200MPa.
Formed body rhegma problem when above-mentioned preparation method can be good at avoiding pressure forming, and material aperture can be entered Row effectively control.First, the method is creative has been divided into the first nickel by the raw material powder (Ni powder) for constituting the infrastructure elements Ni of alloy Powder and the second nickel powder, wherein the first nickel powder is strip, the second nickel powder is spherical or near-spherical, the first nickel powder and the second nickel powder The ratio between granularity is 1:(1.2~5) (preferably 1:(2~4)), and the first nickel powder accounts for the 10~90% of Ni powder gross masses, so, by In the first nickel powder be the less strip nickel powder of granularity, with briquettability preferably (formed body is difficult rhegma), sintering back aperture compared with Small the characteristics of, and the second nickel powder is the larger spherical or near-spherical nickel powder of granularity, with briquettability, poor (formed body easily splits Damage), sintering back aperture it is larger the characteristics of, after above-mentioned first nickel powder and the second nickel powder are sufficiently mixed, the first nickel powder can be filled in In the space formed between second nickel powder, on the one hand play a part of material aperture (aperture model as needed after control sintering Enclose adjustment the first nickel powder ratio, such as 30%, 50%, 70%), on the one hand improve mixed powder mixed powder briquettability, Formed body rhegma probability when reducing pressure forming;In addition, the first nickel powder granularity increases the overall activity of Ni powder compared with I, so as to drop Sintering temperature and low, promotes the flowing and development of crystal grain in Powder during Sintering Process, and prevents sintering densification to a certain extent.Separately Outward, the briquettability for specific blend powder is further optimized by the selection of pressure forming parameter, further improves pressure The qualification rate of power shaping.
The resulting pre-molding body for preparing powder sintered porous filtering alloy during the implementation above method, Ni powder uses the first nickel powder and the second nickel powder in constituting the powder particle of the pre-molding body, and first nickel powder is strip, Second nickel powder is spherical or near-spherical, and the ratio between granularity of first nickel powder and the second nickel powder is 1:(1.2~5), and the One nickel powder accounts for the 10~90% of Ni powder gross masses.The ratio between granularity of first nickel powder and the second nickel powder more preferably 1:(2 ~4).It can also be more preferably 15~50% that first nickel powder accounts for Ni powder gross mass.
In sum, main the having in common that of four kinds of powder sintered porous filtering alloys is Ni based alloys above, and Raw material powder (Ni powder) for the infrastructure elements Ni for constituting the alloy in preparation technology takes special technological means.Shen Ask someone during the above-mentioned powder sintered porous filtering alloy of first three is developed, prepared by the conventional powder metallurgic method of discovery burns The technique for tying porous material has that sintering densification, infiltration rate be relatively low, tortuosity, thus cannot far reach Its average pore size is not more than 20 μm and relative coefficient of permeability is not less than 0.2m when being filtered as liquid3/m2Kpah, is used as Its average pore size is not more than 60 μm and relative permeability is not less than 80m during gas filtration3/m2The technical requirements of kpah.It is logical Above-mentioned a series of measures is crossed, the powder sintered porous filtering alloy obtained by making can either show excellent for particular filter system Different chemical stability, while having reached good strainability again.Developing above-mentioned 4th kind of powder sintered porous filtering alloy During, sintering densification problem is not protruded, but low qualified during discovery pressure forming, and pre-compaction forming body easily splits Damage, after the treatment measures to Ni powder are taken, pre-compaction forming body qualification rate can be greatly improved.
In addition, can also further summarize showing that one kind being capable of the easy and effective powder sintered porous body of control by the above Aperture size, and when can reduce pressure forming the powder sintered porous body of formed body rhegma probability preparation method and system The pre-molding body of the standby sintered body.The preparation method of i.e. this powder sintered porous body is:Step includes dispensing, shaping and burns Knot, shape, the first powder and the second powder of different sizes, institute are used during dispensing for the basic material powder for preparing the porous body Briquettability when stating the first powder smaller compared to the second powder granularity and shaping is more preferable, and the first powder accounts for the basic material powder The 10~90% of gross mass.If porous body is Ni based alloys, the first powder is the first nickel powder, and the second powder is the second nickel powder. Because the first powder has briquettability preferably, the sintering less feature of back aperture (because the first powder granularity is smaller), and the second powder The characteristics of body has sintering back aperture larger (because the second powder granularity is larger), above-mentioned first powder and the second powder are fully mixed After conjunction, the first powder can be filled in the space formed between the second powder, on the one hand play material aperture after control is sintered Effect (ratio of the powder of aperture adjustment first as needed, such as 30%, 50%, 70%), on the one hand improve mixed powder Briquettability, formed body rhegma probability when reducing pressure forming, in addition, the first powder granularity increases basic material powder compared with I Overall activity, so as to reduce sintering temperature, promotes the flowing and development of crystal grain in Powder during Sintering Process, and prevent to a certain extent Only sintering densification.
A kind of preferred concrete mode in the preparation method of the powder sintered porous body is:First powder is strip Shape, second powder is spherical or near-spherical, and the ratio between granularity of first powder and the second powder is 1:(1.2~5).Its First powder of middle strip is the characteristics of briquettability is more preferable when having shaping, and the accumulation of spherical or near-spherical the second powder Space is larger, and sintering porosity is higher;The ratio between granularity by the first powder and the second powder is set as 1:(1.2~5), can be more preferable The briquettability for ensuring mixed powder and pore size control accuracy.Wherein the ratio between granularity of the first powder and the second powder enters one Step is preferably 1:(2~4).Additionally, the first powder can use electrolytic powder (shape of electrolytic powder is strip), the second powder can Using atomized powder (shape of atomized powder is spherical or near-spherical).Certainly, the first powder of strip not can only be using electricity Solution mode is obtained, and the first powder of strip can be also obtained by other Preparation Technique of Powders (such as oxidation-reduction method);It is spherical Or the second powder of near-spherical can only not be obtained using atomizing type, can also be obtained by other known Preparation Technique of Powders Second powder.
The resulting pre-molding body for preparing powder sintered porous body during the implementation above method, constituting should Basic material powder in the powder particle of pre-molding body uses shape, the first powder and the second powder of different sizes, described First powder is smaller compared to the second powder granularity and briquettability during shaping more preferably, and the first powder to account for the basic material powder total The 10~90% of quality.Wherein, it is further that first powder is strip, second powder is spherical or class ball The ratio between granularity of shape, first powder and the second powder is 1:(1.2~5).
With reference to specific embodiment, the present invention will be further described.The additional aspect of the present invention and advantage will be under The description middle part in face is given out, partly will become apparent from the description below, or is recognized by practice of the invention.
Specific embodiment
Below by four groups of experimental examples to the preparation side of above-mentioned several powder sintered Ni bases porous filtering alloys of the invention Method and it is specifically described by the powder sintered Ni bases porous filtering alloy that these methods are obtained.Illustrated by these, this area Technical staff clearly can recognize the outstanding feature that powder sintered Ni bases porous filtering alloy of the invention has.Hereinafter relate to And experimental example numbering with correspondence " sample " numbering it is consistent.
<Battery of tests>
The material composition and content (by percentage to the quality) of first group of experimental example 1 to 12 of test example are shown in Table 1.Wherein, Material applications A refers to that the powder sintered porous filtering alloy of preparation is filtered as liquid;Material applications B refers to the powder sintered many of preparation Hole filtering alloy is used as gas filtration.In the experimental example 1 to 12 of battery of tests, each experimental example also includes 5 identical realities Example.
Table 1 --- the material composition and content of experimental example 1 to 12 in first group of test example
Note:"×" represents no this item in table.
In above-mentioned experimental example 1 to 12, Ni powder has used the first nickel powder and the second nickel powder.Wherein, the first nickel powder choosing The electrolytic nickel powder of strip is selected, granularity is 10~25 μm;The second nickel powder selection is spherical or near-spherical atomization nickel powder, grain Spend is 35~45 μm.The particle diameter of remaining the raw material powder in addition to Ni powder is -400 mesh.Above-mentioned particle diameter is standby powder sintered according to drawing up The design aperture of Ni base porous filtering alloys and pore-size distribution determine that what those skilled in the art can be according to aperture situation will Ask and be adjusted.In addition, in test example 1-4, the first nickel powder accounts for the 35% of Ni powder gross masses, in test example 5-7,9-11 One nickel powder accounts for the 55% of Ni powder gross masses, and first nickel powder accounts for the 20% of Ni powder gross masses in test example 8,12.
As listed by table 1, the raw material to experimental example 1 to 12 mixes respectively.After being sufficiently mixed, then to experimental example 1 to 12 Powder granulated, be dried again after granulation, drying temperature is set as 55 DEG C, and drying time is set as 6 hours.Test example It is granulating agent to use stearic acid when being granulated in 1-7,9-11, and stearic addition is the 5% of mixed powder gross mass.Herein It is from stearic effect and advantage:1) it is agglomerated powder granules, prevents component segregation, secondly, makees with certain lubrication With, that is, suppress easy-formation and easy mold release;2) stearic acid is easily decomposed, and 360-370 DEG C is decomposed completely, and catabolite be CO2, CO, H2O etc., easily overflows noresidue, is granulating agent with urea is used during granulation in the reactionless test example 8,12 of matrix material, urea Addition is the 12% of mixed powder gross mass.Effect and advantage from urea herein be:1) as foaming agent, material is improved Porosity;2) decomposition temperature is low (160 DEG C), and catabolite is ammonia and cyanic acid, and hole position is left after sending out, and formation is opened Hole.
Afterwards, the powder of experimental example 1 to 12 is fitted into the isostatic pressing mold of unified specification respectively, then by these Mould is respectively placed in cold isostatic compaction machine, pressurize 60 seconds under 150MPa briquetting pressures, and it is 1 to 12 to be made numbering after the demoulding Tubulose pre-molding body.Above-mentioned isostatic pressing the results are shown in Table 2.From Table 2, it can be seen that the only example 3 of experimental example 12 Pre-molding body find rhegma, without rhegma, isostatic pressing qualification rate is significantly better than existing situation for remaining pre-molding body.
Table 2 --- isostatic pressing qualification rate
Experimental example is numbered Example 1 Example 2 Example 3 Example 4 Example 5
1
2
3
4
5
6
7
8
9
10
11
12 ×
Note:"×" represents that pre-molding body has rhegma in table, unqualified;" √ " represents pre-molding body without rhegma in table, It is qualified.
Then, the pre-molding body of one of example in experimental example 1 to 12 is chosen respectively and loads sintering boat, then this A little sintering boats are placed in sintering furnace and are sintered, and furnace cooling after sintering finally obtains sample 1 to 12 from each sintering boat again. The sintering schedule of experimental example 1 to 12 includes following two stages.First stage is the degreasing stage:Sintering temperature rises to from room temperature 400 DEG C, and it is incubated 180 minutes;Second stage is the high temperature sintering stage:Sintering temperature is risen to 1150 DEG C, and is incubated 120 points Clock;Cooling obtains the porous filtering alloy.
The strainability test such as table 3 of sample 1 to 12.Wherein, the measure of material porosity and average pore size uses bubble Method;Relative coefficient of permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under water lead to Amount;Relative permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under air Flux;The test of Tensile strength is led to after sample 1 to 12 is processed as into standard specimen by CNS GB7963-87 Overstretching machine is measured.
Table 3 --- result of the test
Note:"×" represents no this item in table.
The chemical stability test such as table 3 of sample 1 to 12.Wherein, erosion test 1 is with the salt that mass fraction is 10% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in acid solution;Erosion test 2 is with the hydrochloric acid that mass fraction is 80% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in solution;Erosion test 3 is with molten in the phosphoric acid that mass fraction is 60% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in liquid;Erosion test 4 is with the sulfuric acid solution that mass fraction is 60% Weight-loss ratio (%) of the middle soaking at room temperature after 60 days is characterized;Erosion test 5 is with the formic acid solution that mass fraction is 60% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized;Erosion test 5 is with the weightlessness after being used 60 days in hydrogen chloride gas Rate (%) is characterized.
Table 4 --- result of the test
Note:"×" represents no this item in table.
<Second group of experiment>
The material composition and content (by percentage to the quality) of second group of experimental example 1 to 12 of experiment are shown in Table 5.Wherein, material Material purposes A refers to that the powder sintered porous filtering alloy of preparation is filtered as liquid;Material applications B refers to the powder sintered porous of preparation Filtering alloy is used as gas filtration.In second group of experimental example 1 to 12 of experiment, each experimental example only has an example.
Table 5 --- the material composition and content of experimental example 1 to 12 in second group of test example
Note:"×" represents no this item in table.
In above-mentioned experimental example 1 to 12, Ni powder has used the first nickel powder and the second nickel powder.Wherein, the first nickel powder choosing Select the electrolytic nickel powder of strip, 10~25 μm of granularity;The second nickel powder selection is spherical or near-spherical atomization nickel powder, granularity 35~45 μm.The particle diameter of remaining the raw material powder outside Ni powder is -400 mesh.Equally, above-mentioned particle diameter is according to the standby powder sintered Ni that draws up The design aperture of base porous filtering alloy and pore-size distribution determine that those skilled in the art can be according to the requirement of aperture situation It is adjusted.In addition, in test example 1-4, the first nickel powder accounts for the 35% of Ni powder gross masses, and the first nickel powder is accounted in test example 5-11 The 55% of Ni powder gross masses, first nickel powder accounts for the 20% of Ni powder gross masses in test example 12.
As listed by table 5, the raw material to experimental example 1 to 12 mixes respectively.After being sufficiently mixed, then to experimental example 1 to 12 Powder granulated, be dried again after granulation, drying temperature is set as 55 DEG C, and drying time is set as 6 hours.Test example It is granulating agent to use stearic acid when being granulated in 1-11, and stearic addition is the 5% of mixed powder gross mass.Test example 12 It is granulating agent that urea is used during middle granulation, and the addition of urea is the 12% of mixed powder gross mass.
Afterwards, the powder of experimental example 1 to 12 is fitted into the isostatic pressing mold of unified specification respectively, then by these Mould is respectively placed in cold isostatic compaction machine, pressurize 60 seconds under 150MPa briquetting pressures, and it is 1 to 12 to be made numbering after the demoulding Tubulose pre-molding body.These pre-molding bodies are without rhegma.
Then, by the pre-molding body in experimental example 1 to 12 and load sintering boat respectively, then these sintering boats are placed in burning It is sintered in freezing of a furnace, furnace cooling after sintering, finally obtains sample 1 to 12 from each sintering boat again.The burning of experimental example 1 to 12 Knot system includes following two stages.First stage is the degreasing stage:Sintering temperature rises to 400 DEG C from room temperature, and is incubated 180 Minute;Second stage is the high temperature sintering stage:Sintering temperature is risen to 1200 DEG C, and is incubated 120 minutes;It is to obtain respectively after cooling To sample 1 to 12.
The strainability test such as table 6 of sample 1 to 12.Wherein, the measure of material porosity and average pore size uses bubble Method;Relative coefficient of permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under water lead to Amount;Relative permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under air Flux;The test of Tensile strength is led to after sample 1 to 12 is processed as into standard specimen by CNS GB7963-87 Overstretching machine is measured.
Table 6 --- result of the test
Note:"×" represents no this item in table.
The chemical stability test such as table 7 of sample 1 to 12.Wherein, erosion test 1 is with the salt that mass fraction is 10% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in acid solution;Erosion test 2 is with the sulfuric acid that mass fraction is 10% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in solution;Erosion test 3 is with the sodium chloride that mass fraction is 10% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in solution;Erosion test 4 is with the iron chloride that mass fraction is 10% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in solution;Erosion test 5 is with the mistake after being used 60 days in moist chlorine Rate (%) is characterized again.
Table 7 --- result of the test
Note:"×" represents no this item in table.
<3rd group of experiment>
The material composition and content (by percentage to the quality) of the 3rd group of experimental example 1 to 9 of experiment are shown in Table 8.Wherein, material Purposes A refers to that the powder sintered porous filtering alloy of preparation is filtered as liquid;Material applications B refers to the powder sintered porous mistake of preparation Filter alloy is used as gas filtration.In the experimental example 1 to 9 of battery of tests, each experimental example only has an example.
Table 8 --- the material composition and content of experimental example 1 to 9 in the 3rd group of test example
Note:"×" represents no this item in table.
In above-mentioned experimental example 1 to 9, Ni powder has used the first nickel powder and the second nickel powder.Wherein, the first nickel powder selection The electrolytic nickel powder of strip, 10~25 μm of granularity;The second nickel powder selection is spherical or near-spherical atomization nickel powder, granularity 35 ~45 μm.The particle diameter of remaining the raw material powder outside Ni powder is -400 mesh.In above-mentioned test example 1-8, the first nickel powder accounts for Ni powder gross masses 55%, first nickel powder accounts for the 20% of Ni powder gross masses in test example 9.
As listed by table 8, the raw material to experimental example 1 to 9 mixes respectively.After being sufficiently mixed, then to experimental example 1 to 9 Powder is granulated, and is dried again after granulation, and drying temperature is set as 55 DEG C, and drying time is set as 6 hours.Test example It is granulating agent to use stearic acid when being granulated in 1-8, and stearic addition is the 5% of mixed powder gross mass.In test example 9 It is granulating agent that urea is used during granulation, and the addition of urea is the 12% of mixed powder gross mass.
Afterwards, the powder of experimental example 1 to 9 is fitted into the isostatic pressing mold of unified specification respectively, then by these Mould is respectively placed in cold isostatic compaction machine, pressurize 60 seconds under 150MPa briquetting pressures, and it is 1 to 9 to be made numbering after the demoulding Tubulose pre-molding body.These pre-molding bodies are without rhegma.
Then, by the pre-molding body of experimental example 1 to 9 and load sintering boat, then these sintering boats are placed in sintering furnace It is sintered, furnace cooling after sintering, finally obtains sample 1 to 9 from each sintering boat again.The sintering schedule of experimental example 1 to 9 is equal Comprising following two stages.First stage is the degreasing stage:Sintering temperature rises to 400 DEG C from room temperature, and is incubated 180 minutes;The Two-stage is the high temperature sintering stage:Sintering temperature is risen to 1200 DEG C, and is incubated 120 minutes;Sample 1 is respectively obtained after cooling To 9.
The strainability test such as table 9 of sample 1 to 9.Wherein, the measure of material porosity and average pore size uses bubble Method;Relative coefficient of permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under water lead to Amount;Relative permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under air Flux;The test of Tensile strength is led to after sample 1 to 9 is processed as into standard specimen by CNS GB7963-87 Overstretching machine is measured.
Table 9 --- result of the test
Note:"×" represents no this item in table.
The chemical stability test such as table 10 of sample 1 to 9.Wherein, erosion test 1 is with the phosphorus that mass fraction is 10% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in acid solution;Erosion test 2 is with the phosphoric acid that mass fraction is 30% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in solution;Erosion test 3 is with molten in the sulfuric acid that mass fraction is 10% Weight-loss ratio (%) of the soaking at room temperature after 60 days is characterized in liquid;Erosion test 4 is with the sulfuric acid solution that mass fraction is 30% Weight-loss ratio (%) of the middle soaking at room temperature after 60 days is characterized;Erosion test 5 is with the weightlessness after being used 60 days in dry chlorine gas Rate (%) is characterized.
Table 10 --- result of the test
Note:"×" represents no this item in table.
<4th group of experimental example>
The material composition and content (by percentage to the quality) of the 4th group of experimental example 1 to 8 of experiment are shown in Table 11.Wherein, material Material purposes B refers to that the powder sintered porous filtering alloy of preparation is used as gas filtration.In the experimental example 1 to 8 of battery of tests, each Experimental example only has an example.
Table 11 --- the material composition and content of experimental example 1 to 8 in the 4th group of test example
Note:"×" represents no this item in table.
In above-mentioned experimental example 1 to 8, Ni powder has used the first nickel powder and the second nickel powder.Wherein, the first nickel powder selection The electrolytic nickel powder of strip, 10~25 μm of granularity;The second nickel powder selection is spherical or near-spherical atomization nickel powder, granularity 35 ~45 μm.The particle diameter of remaining the raw material powder outside Ni powder is -400 mesh.In above-mentioned test example 1-8, the first nickel powder accounts for Ni powder gross masses 20%.
As listed by table 11, the raw material to experimental example 1 to 8 mixes respectively.After being sufficiently mixed, then to experimental example 1 to 8 Powder is granulated, and is dried again after granulation, and drying temperature is set as 55 DEG C, and drying time is set as 6 hours.Test example It is granulating agent that urea is used when being granulated in 1-8, and the addition of urea is the 12% of mixed powder gross mass.
Afterwards, the powder of experimental example 1 to 8 is fitted into the isostatic pressing mold of unified specification respectively, then by these Mould is respectively placed in cold isostatic compaction machine, pressurize 60 seconds under 180MPa briquetting pressures, and it is 1 to 8 to be made numbering after the demoulding Tubulose pre-molding body.These pre-molding bodies are without rhegma.
Then, by the pre-molding body of experimental example 1 to 8 and load sintering boat, then these sintering boats are placed in sintering furnace It is sintered, furnace cooling after sintering, finally obtains sample 1 to 8 from each sintering boat again.The sintering schedule of experimental example 1 to 8 is equal Comprising following two stages.First stage is the degreasing stage:Sintering temperature rises to 400 DEG C from room temperature, and is incubated 180 minutes;The Two-stage is the high temperature sintering stage:Sintering temperature is risen to 1300 DEG C, and is incubated 200 minutes;Sample 1 is respectively obtained after cooling To 8.
The strainability test such as table 12 of sample 1 to 8.Wherein, the measure of material porosity and average pore size uses bubble Method;Relative coefficient of permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under water lead to Amount;Relative permeability is specially in every square metre of filter area, in every kpa (kPa) filtration pressure difference and per hour under air Flux;The test of Tensile strength is led to after sample 1 to 8 is processed as into standard specimen by CNS GB7963-87 Overstretching machine is measured.
Table 12 --- result of the test
Note:"×" represents no this item in table.
The chemical stability test such as table 10 of sample 1 to 8.Wherein, erosion test 1 makes with 400 DEG C of dry chlorine gas Characterized with the weight-loss ratio (%) after 30 days.
Table 13 --- result of the test
Note:"×" represents no this item in table.

Claims (8)

1. the preparation method of powder sintered porous body, step includes dispensing, isostatic pressing and sintering, it is characterised in that:Dispensing When for prepare the porous body basic material powder use shape, the first powder and the second powder of different sizes, described first Powder is smaller compared to the second powder granularity and briquettability when being molded is more preferable, and the first powder accounts for the basic material powder gross mass 30~90%;First powder is strip, and second powder is spherical or near-spherical, first powder and second The ratio between granularity of powder is 1:(1.2~5);The granularity of first powder is 10~25 μm, the granularity of the second powder for 35~ 45 μm, and the mixed powder for obtaining batching step during isostatic pressing pressurize 20~80 under 120~200MPa briquetting pressures Second obtains pre-molding body, is then sintered pre-molding body and obtains powder sintered porous body.
2. as claimed in claim 1 powder sintered porous body preparation method, it is characterised in that:First powder and the second powder The ratio between granularity of body is 1:(2~4).
3. as claimed in claim 1 powder sintered porous body preparation method, it is characterised in that:First powder is electrolysis Powder, second powder is atomized powder.
4. as described in any one claim in claims 1 to 3 powder sintered porous body preparation method, its feature exists In:The porous body is Ni based alloys, then the first powder is the first nickel powder, and the second powder is the second nickel powder.
5. the resulting pre-molding for preparing powder sintered porous body during claim 1 methods described is implemented Body, it is characterised in that:The basic material powder constituted in the powder particle of the pre-molding body uses shape, of different sizes first Powder and the second powder, first powder is smaller compared to the second powder granularity and briquettability when being molded is more preferable, and first Powder accounts for the 30~90% of the basic material powder gross mass;First powder is strip, second powder for spherical or The ratio between granularity of near-spherical, first powder and the second powder is 1:(1.2~5);The granularity of first powder be 10~ 25 μm, the granularity of the second powder is 35~45 μm.
6. pre-molding body as claimed in claim 5, it is characterised in that:The ratio between granularity of first powder and the second powder It is 1:(2~4).
7. pre-molding body as claimed in claim 5, it is characterised in that:First powder is electrolytic powder, second powder Body is atomized powder.
8. the pre-molding body as described in any one claim in claim 5 to 7, it is characterised in that:The porous body is Ni based alloys, then the first powder is the first nickel powder, and the second powder is the second nickel powder.
CN201410437077.5A 2014-08-31 2014-08-31 The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body Active CN104190935B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410437077.5A CN104190935B (en) 2014-08-31 2014-08-31 The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410437077.5A CN104190935B (en) 2014-08-31 2014-08-31 The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body

Publications (2)

Publication Number Publication Date
CN104190935A CN104190935A (en) 2014-12-10
CN104190935B true CN104190935B (en) 2017-06-16

Family

ID=52076382

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410437077.5A Active CN104190935B (en) 2014-08-31 2014-08-31 The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body

Country Status (1)

Country Link
CN (1) CN104190935B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104625071B (en) * 2015-01-28 2016-09-28 东莞劲胜精密组件股份有限公司 A kind of preparation method of powder injection-molded surface pore material
CN106994512B (en) * 2017-04-18 2019-03-15 中南大学 A kind of composite bore diameter copper sintered porous material and its preparation method and application
CN112441817B (en) * 2019-08-29 2023-12-29 深圳市绎立锐光科技开发有限公司 Fluorescent ceramic, preparation method thereof and light source device

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102166651A (en) * 2011-03-29 2011-08-31 黑龙江科技学院 Method for manufacturing porous metal parts by laser scanning
CN102836997A (en) * 2011-06-22 2012-12-26 烟台龙源电力技术股份有限公司 Metal powder sintered porous body and preparation method thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3483600B2 (en) * 1993-10-26 2004-01-06 片山特殊工業株式会社 Porous metal body and method for producing the metal porous body
JP4572287B2 (en) * 2001-03-23 2010-11-04 独立行政法人産業技術総合研究所 Method for producing high strength porous body and high strength porous body
RU2200647C1 (en) * 2001-07-17 2003-03-20 Литвинцев Александр Иванович Method for making porous semifinished products of aluminium alloy powders
EP1569790A4 (en) * 2002-12-12 2006-09-20 Entegris Inc Porous sintered composite materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102166651A (en) * 2011-03-29 2011-08-31 黑龙江科技学院 Method for manufacturing porous metal parts by laser scanning
CN102836997A (en) * 2011-06-22 2012-12-26 烟台龙源电力技术股份有限公司 Metal powder sintered porous body and preparation method thereof

Also Published As

Publication number Publication date
CN104190935A (en) 2014-12-10

Similar Documents

Publication Publication Date Title
CN104195374B (en) Powder sintered porous filtering alloy, its preparation method and its pre-molding body
CN104190918B (en) Powder sintering porous filter alloy, preparation method thereof and pre-pressing molding body for preparing powder sintering porous filter alloy
CN103397256B (en) The sintering Fe-Al base alloy porous material of resistance to high temperature oxidation and filtering element
CN104190935B (en) The preparation method of powder sintered porous body and prepare the pre-molding body of the sintered body
CN103215470B (en) The preparation method of the open celled foam copper that a kind of pore structure parameter is controlled
CN103290248B (en) A kind of particle reinforce abradable porous titanium preparation method
US20090297396A1 (en) Fabrication method of alloy parts by metal injection molding and the alloy parts
CN103695689A (en) Preparation method of Fe-Al intermetallic compound porous membrane
CN103343251B (en) Sintering Ti-Al base alloy porous material, application and improve the method for its pore structure
WO2018053940A1 (en) Non-magnetic steel product and powder metallurgy manufacturing method therefor
CN102828096B (en) Metal ceramic cutting tool material and preparation method thereof
CN103409678B (en) Sintering Fe-Al base alloy porous material and apply its filtering element
CN101358304A (en) NiAl intermetallic compound porous material and preparation method thereof
CN104419841A (en) Preparation method of powdery sintered metal porous body
CN104233004B (en) Powder sintered porous filtering alloy, its preparation method and its pre-molding body
CN106191505B (en) Preparation method of high-temperature oxidation-resistant porous material
CN103397243B (en) The preparation method of sintering Fe-Al base alloy porous material
CN104419848A (en) Powdery sintered metal porous body, filter element and method for improving permeability thereof
CN104550906B (en) A kind of premixing bronze powder, preparation method and applications
CN103397244B (en) The preparation method of the sintering Fe-Al base alloy porous material of resistance to high temperature oxidation
CN105803239A (en) Preparation method for micro-pore-diameter high-porosity nickel-chrome-molybdenum porous material
CN106987740A (en) A kind of porous aluminum based composite metal material and preparation method thereof
CN103789592B (en) A kind of tungsten alloy material and preparation method thereof and the application in preparing aluminium liquid filtering table
CN104195373B (en) Powder sintered porous filter alloy, preparation method thereof and pre-compression molded body
CN107267847B (en) A kind of resistance to high temperature oxidation, iron-based porous material of caustic corrosion resistance 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
GR01 Patent grant