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CN108129729A - A kind of preparation process of the novel plastic type magnetron based on permanent-magnet material - Google Patents

A kind of preparation process of the novel plastic type magnetron based on permanent-magnet material Download PDF

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Publication number
CN108129729A
CN108129729A CN201711388427.3A CN201711388427A CN108129729A CN 108129729 A CN108129729 A CN 108129729A CN 201711388427 A CN201711388427 A CN 201711388427A CN 108129729 A CN108129729 A CN 108129729A
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Prior art keywords
reactor
catalyst
polyethylene
permanent
magnet material
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CN201711388427.3A
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Inventor
朱小英
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Ningbo City Yinzhou Zhi Companion Mdt Infotech Ltd
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Ningbo City Yinzhou Zhi Companion Mdt Infotech Ltd
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Priority to CN201711388427.3A priority Critical patent/CN108129729A/en
Publication of CN108129729A publication Critical patent/CN108129729A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0843Cobalt
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/085Copper
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0856Iron
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/18Applications used for pipes

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)

Abstract

The invention discloses a kind of preparation processes of the novel plastic type magnetron based on permanent-magnet material, are prepared by following steps:R, Co, Fe, Cu, Zr are pressed into Sm (CoFeCuZrR)zThe proportioning of (Z=7.4~8.3) is put in after being configured in electric arc furnaces, is evacuated down to 10‑3Pa or more then passes to the high purity argon of 0.8~1.2 atmospheric pressure, under the protection of argon gas melt back obtain the uniform alloy cast ingot of ingredient 34 times.The melting in vacuum induction furnace by gained alloy, the vacuum degree of melting are 10 3Pa, water cooled copper mould cast, obtained alloy pig, under nitrogen, argon gas protection through coarse crushing, in broken, milling to 36 μm.Make vinyl polymerization in the presence of antigravity system in the reactor, to form polyethylene, wherein the antigravity system includes the first catalyst and the second catalyst;And the required combination of target melt flow ratio (MFR) and molecular weight distribution (MWD) with forming distribution (CD) based on the polyethylene.

Description

A kind of preparation process of the novel plastic type magnetron based on permanent-magnet material
Technical field
The present invention relates to a kind of magnetrons, and in particular to a kind of preparation of the novel plastic type magnetron based on permanent-magnet material Technique.
Background technology
Magnetron is a kind of electron tube for being used for generating microwave energy.Substantially one be placed in stationary magnetic field two Pole pipe.Under the control of orthogonal stationary magnetic field and steady electric field with electromagnetic field of high frequency phase interaction occurs for electronics in pipe With energy conversion is obtained from steady electric field into microwave energy, so as to achieve the purpose that generate microwave energy.Meanwhile magnetron It is a kind of consumables, easy aging and demagnetization, magnetron is usually operated at π moulds, microwave electric field at two neighboring resonator accent Phase just differs 180 °, i.e. microwave electric field direction is exactly the opposite (2).Although this microwave field is stationary field, in π moulds In the case of, it is equivalent to two identical microwave fields and circumferentially moves in opposite direction, the phase velocity value of two fields is equal.From The electronics that emission of cathode goes out makees wheel cycloid motion under crossed electric and magnetic field effect.DC voltage and stationary magnetic field are adjusted, makes electronics The phase velocity v of move in the direction microwave field is exactly equal to (in formula in the average drift velocity v=E/B of circumferencial direction E is the DC electric field average value that DC voltage is generated in interaction space, and B is axial constant magnetic induction intensity), electronics can To be synchronized with the movement with microwave field.During being synchronized with the movement, part electronics in microwave decelerating field is in by the straight of oneself Stream potential energy gradually gives microwave field, and draw close to anode, finally for collected by anode.This part electronics shifts energy to microwave field Amount, is conducive to establish stable microwave oscillation in magnetron, therefore referred to as favorable electron, and existing magnetron is not only easily old Change and demagnetization, and plasticity is very poor, and when being processed, difficulty is quite high.
Invention content
Present invention aims at a kind of preparation process of the novel plastic type magnetron based on permanent-magnet material is provided, to solve Existing magnetron not only easy aging and demagnetization, and plasticity is very poor, the quite high problem of difficulty when being processed.
In order to solve the above technical problem, the present invention provides following technical solutions:
The present invention provides a kind of preparation processes of the novel plastic type magnetron based on permanent-magnet material, pass through following steps It is prepared:
Step 1:R, Co, Fe, Cu, Zr are pressed into Sm (CoFeCuZrR)zThe proportioning of (Z=7.4~8.3) is put in after being configured In electric arc furnaces, it is evacuated down to 10-3Pa or more then passes to the high purity argon of 0.8~1.2 atmospheric pressure, in the protection of argon gas Lower melt back obtains ingredient uniform alloy cast ingot 3-4 times.
Step 2:By gained alloy melting in vacuum induction furnace in step 1), the vacuum degree of melting is 10-3Pa, water Cold copper mould casting, obtained alloy pig, under nitrogen, argon gas protection through coarse crushing, in broken, milling to 3-6 μm.
Step 3:Make vinyl polymerization in the presence of antigravity system in the reactor, to form polyethylene, wherein described urge Agent system includes the first catalyst and the second catalyst;And the target melt flow ratio (MFR) based on the polyethylene With molecular weight distribution (MWD) and the required combination of composition distribution (CD), the institute of reactor described in reactor condition and feed-in is adjusted The amount of the second catalyst is stated, to control the melt index of the polyethylene (MI) and density, is reacted after 15-45min in 150- It is stirred at a temperature of 200 DEG C.
Step 4:Alloy powder obtained in step 2) is uniformly sprinkled upon on stirring thing in whipping process, is continued after being sprinkled into Stir 5-10min.
Step 5:Object after stirring evenly is put into injection molding in mold.
As a preferred technical solution of the present invention, formed by following raw material proportioning:The R of 23~27wt%, 3.5~ The Cu of 5wt%, the Fe of 19~25wt%, the Zr of 1.5~3wt% of 1.5~3wt%, the Co of 18~26wt% and 12- The polyethylene of 58wt%.
As a preferred technical solution of the present invention, the element R is at least rare earth element containing Sm.
As a preferred technical solution of the present invention, first catalyst includes bis- (n-propyl cyclopentadienyl groups) two Methylcyclopentadienyl hafnium.
As a preferred technical solution of the present invention, second catalyst includes two (1- ethyl-indenyls) dimethyl Zirconium.
As a preferred technical solution of the present invention, second catalyst is added to as fine tuning catalyst will be described In the slurry of reactor described in first catalyst feed-in.
As a preferred technical solution of the present invention, the adjustment reactor condition includes the behaviour for adjusting the reactor Make temperature, adjustment reactor condition is also comprising the comonomer concentration adjusted in the reactor in polyblend;Adjustment is anti- Answer device condition also comprising the density of hydrogen adjusted in the reactor in polyblend;Reactor condition is adjusted also comprising tune Reactant concentration in the whole reactor in polyblend is to meet the polyethylene in the range of the MFR of the polyethylene MI targets;Adjustment reactor condition, which also includes, adjusts the reactant concentration in the reactor in polyblend to meet The density targets of the polyethylene in the range of the MFR of the polyethylene.
In technical scheme of the present invention, the Cu of R, 3.5~5wt% containing 23~27wt%, the Fe of 19~25wt%, The Zr of 1.5~3wt%, remaining be Co and polyethylene, wherein, element R is at least rare earth element containing Sm, wherein, it is described dilute Native cobalt permanent magnetism volume density is 8.15~8.39g/cm3, and the rare earthcobalt permanent magnet metal structure includes the born of the same parents containing Sm2Co17 phases Phase and around born of the same parents' phase and containing the cell wall of SmCo5 phases, the rare earthcobalt permanent magnet average crystal grain diameter for 40~ 100 μm, in the cell wall, the half breadth of the content of Cu is 10nm hereinafter, catalyst finely tunes ratio, polymer reactor temperature It can change under less constant density of pe and MI (I-2) with polymer reactor hydrogen and comonomer concentration Obtain MFR ranges.The technology can advantageously provide the MI of wide scope under given catalyst system.In addition, in embodiment In, MI controls can be controlled generally with MFR and are detached from.For the antigravity system of feed-in polymer reactor, polymer MI, MFR, Density and CD can be by changing reactor condition, such as temperature, density of hydrogen and comonomer (such as 1- hexenes, butylene) Concentration controls, and the combination of permanent-magnet material and polyethylene is realized by above-mentioned means, and make it have good plasticity.
Beneficial effects of the present invention:The Cu of R, 3.5~5wt% containing 23~27wt%, the Fe of 19~25wt%, 1.5 The Zr of~3wt%, remaining be Co and polyethylene, wherein, element R is at least rare earth element containing Sm, wherein, the rare earth Cobalt permanent magnetism volume density is 8.15~8.39g/cm3, and the rare earthcobalt permanent magnet metal structure includes the born of the same parents containing Sm2Co17 phases Phase and around born of the same parents' phase and containing the cell wall of SmCo5 phases, the rare earthcobalt permanent magnet average crystal grain diameter for 40~ 100 μm, in the cell wall, the half breadth of the content of Cu is 10nm hereinafter, not only having by magnetron made from this technique The performance of permanent magnetism, ductility and plasticity are splendid, are not only convenient for processing, and with the good market competitiveness.
Other than objects, features and advantages described above, the present invention also has other objects, features and advantages. Below by embodiment, the present invention is described in further detail.
Specific embodiment
Embodiment 1
The present invention provides a kind of preparation process of the novel plastic type magnetron based on permanent-magnet material, by following raw material proportioning It forms:The polyethylene of the Co and 50wt% of Zr, 20wt% of Fe, 2wt% of Cu, 20wt% of R, 4wt% of 23wt%.
It is prepared by following steps:
Step 1:R, Co, Fe, Cu, Zr are pressed into Sm (CoFeCuZrR)zThe proportioning of (Z=7.4~8.3) is put in after being configured In electric arc furnaces, it is evacuated down to 10-3Pa or more then passes to the high purity argon of 0.8~1.2 atmospheric pressure, in the protection of argon gas Lower melt back obtains ingredient uniform alloy cast ingot 3-4 times.
Step 2:By gained alloy melting in vacuum induction furnace in step 1), the vacuum degree of melting is 10-3Pa, water Cold copper mould casting, obtained alloy pig, under nitrogen, argon gas protection through coarse crushing, in broken, milling to 3-6 μm.
Step 3:Make vinyl polymerization in the presence of antigravity system in the reactor, to form polyethylene, wherein described urge Agent system includes the first catalyst and the second catalyst;And the target melt flow ratio (MFR) based on the polyethylene With molecular weight distribution (MWD) and the required combination of composition distribution (CD), the institute of reactor described in reactor condition and feed-in is adjusted The amount of the second catalyst is stated, to control the melt index of the polyethylene (MI) and density, is reacted after 15-45min in 150- It is stirred at a temperature of 200 DEG C.
Step 4:Alloy powder obtained in step 2) is uniformly sprinkled upon on stirring thing in whipping process, is continued after being sprinkled into Stir 5-10min.
Step 5:Object after stirring evenly is put into injection molding in mold.
Embodiment 2
The present invention provides a kind of preparation process of the novel plastic type magnetron based on permanent-magnet material, by following raw material proportioning It forms:The polyethylene of the Co and 25wt% of Zr, 25wt% of Fe, 3wt% of Cu, 24wt% of R, 5wt% of 27wt%.
It is prepared by following steps:
Step 1:R, Co, Fe, Cu, Zr are pressed into Sm (CoFeCuZrR)zThe proportioning of (Z=7.4~8.3) is put in after being configured In electric arc furnaces, it is evacuated down to 10-3Pa or more then passes to the high purity argon of 0.8~1.2 atmospheric pressure, in the protection of argon gas Lower melt back obtains ingredient uniform alloy cast ingot 3-4 times.
Step 2:By gained alloy melting in vacuum induction furnace in step 1), the vacuum degree of melting is 10-3Pa, water Cold copper mould casting, obtained alloy pig, under nitrogen, argon gas protection through coarse crushing, in broken, milling to 3-6 μm.
Step 3:Make vinyl polymerization in the presence of antigravity system in the reactor, to form polyethylene, wherein described urge Agent system includes the first catalyst and the second catalyst;And the target melt flow ratio (MFR) based on the polyethylene With molecular weight distribution (MWD) and the required combination of composition distribution (CD), the institute of reactor described in reactor condition and feed-in is adjusted The amount of the second catalyst is stated, to control the melt index of the polyethylene (MI) and density, is reacted after 15-45min in 150- It is stirred at a temperature of 200 DEG C.
Step 4:Alloy powder obtained in step 2) is uniformly sprinkled upon on stirring thing in whipping process, is continued after being sprinkled into Stir 5-10min.
Step 5:Object after stirring evenly is put into injection molding in mold.
Finally it should be noted that:The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic. All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's Within protection domain.

Claims (7)

1. a kind of preparation process of the novel plastic type magnetron based on permanent-magnet material, which is characterized in that by following steps system It is standby to form:
Step 1:R, Co, Fe, Cu, Zr are pressed into Sm (CoFeCuZrR)zThe proportioning of (Z=7.4~8.3) is put in electric arc furnaces after being configured It is interior, it is evacuated down to 10-3Pa or more then passes to the high purity argon of 0.8~1.2 atmospheric pressure, under the protection of argon gas repeatedly Melting obtains ingredient uniform alloy cast ingot 3-4 times.
Step 2:By gained alloy melting in vacuum induction furnace in step 1), the vacuum degree of melting is 10-3Pa, water-cooled copper Mould is poured into a mould, obtained alloy pig, under nitrogen, argon gas protection through coarse crushing, in broken, milling to 3-6 μm.
Step 3:Make vinyl polymerization in the presence of antigravity system in the reactor, to form polyethylene, wherein the catalyst System includes the first catalyst and the second catalyst;And target melt flow ratio (MFR) based on the polyethylene and point The required combination of son amount distribution (MWD) and composition distribution (CD) adjusts described the of reactor described in reactor condition and feed-in The amount of two catalyst to control the melt index of the polyethylene (MI) and density, is reacted after 15-45min in 150-200 DEG C of temperature It is stirred under degree.
Step 4:Alloy powder obtained in step 2) is uniformly sprinkled upon on stirring thing in whipping process, continues to stir after being sprinkled into 5-10min。
Step 5:Object after stirring evenly is put into injection molding in mold.
2. a kind of preparation process of novel plastic type magnetron based on permanent-magnet material according to claim 1, feature It is, is formed by following raw material proportioning:The R of 23~27wt%, the Cu of 3.5~5wt%, the Fe of 19~25wt%, 1.5~ The polyethylene of the Zr of 3wt%, the Co of 18~26wt% and 12-58wt%.
3. a kind of preparation process of novel plastic type magnetron based on permanent-magnet material according to claim 1, feature It is, the element R is at least rare earth element containing Sm.
4. a kind of preparation process of novel plastic type magnetron based on permanent-magnet material according to claim 2, feature It is, first catalyst includes bis- (n-propyl cyclopentadienyl group) dimethyl hafniums.
5. a kind of preparation process of novel plastic type magnetron based on permanent-magnet material according to claim 2, feature It is, second catalyst includes two (1- ethyl-indenyls) zirconium dimethyls.
6. a kind of preparation process of novel plastic type magnetron based on permanent-magnet material according to claim 1-5, special Sign is that second catalyst is added to as fine tuning catalyst by the slurry of reactor described in the first catalyst feed-in In.
7. a kind of preparation process of novel plastic type magnetron based on permanent-magnet material according to claim 1-6, special Sign is that the adjustment reactor condition includes the operation temperature for adjusting the reactor, and adjustment reactor condition, which also includes, to be adjusted Comonomer concentration in the whole reactor in polyblend;Reactor condition is adjusted also comprising in the adjustment reactor Density of hydrogen in polyblend;Reactor condition is adjusted also comprising the reaction adjusted in the reactor in polyblend Object concentration is to meet the MI targets of the polyethylene in the range of the MFR of the polyethylene;Reactor condition is adjusted also comprising adjustment Reactant concentration in the reactor in polyblend is to meet the close of the polyethylene in the range of the MFR of the polyethylene Spend target.
CN201711388427.3A 2017-12-20 2017-12-20 A kind of preparation process of the novel plastic type magnetron based on permanent-magnet material Withdrawn CN108129729A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009161599A (en) * 2007-12-28 2009-07-23 Riken Technos Corp Ferromagnetic thermoplastic resin composition and use thereof
CN102071339A (en) * 2011-01-24 2011-05-25 宁波科星材料科技有限公司 Samarium-cobalt permanent magnet material and preparation method thereof
CN102516625A (en) * 2011-12-03 2012-06-27 广东聚缘塑料科技有限公司 Magnetic plastic produced by waste plastic
CN102952386A (en) * 2012-10-31 2013-03-06 中国计量学院 A kind of gradient magnetostrictive material and its preparation method
CN103325513A (en) * 2013-07-18 2013-09-25 湖南航天工业总公司 Samarium cobalt permanent magnetic material and preparation method thereof
CN104916382A (en) * 2014-03-11 2015-09-16 Nec东金株式会社 Rare earth-cobalt permanent magnet
CN106029712A (en) * 2014-02-11 2016-10-12 尤尼威蒂恩技术有限责任公司 Method of producing polyethylene and polyethylene thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009161599A (en) * 2007-12-28 2009-07-23 Riken Technos Corp Ferromagnetic thermoplastic resin composition and use thereof
CN102071339A (en) * 2011-01-24 2011-05-25 宁波科星材料科技有限公司 Samarium-cobalt permanent magnet material and preparation method thereof
CN102516625A (en) * 2011-12-03 2012-06-27 广东聚缘塑料科技有限公司 Magnetic plastic produced by waste plastic
CN102952386A (en) * 2012-10-31 2013-03-06 中国计量学院 A kind of gradient magnetostrictive material and its preparation method
CN103325513A (en) * 2013-07-18 2013-09-25 湖南航天工业总公司 Samarium cobalt permanent magnetic material and preparation method thereof
CN106029712A (en) * 2014-02-11 2016-10-12 尤尼威蒂恩技术有限责任公司 Method of producing polyethylene and polyethylene thereof
CN104916382A (en) * 2014-03-11 2015-09-16 Nec东金株式会社 Rare earth-cobalt permanent magnet

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Application publication date: 20180608