CN106248517A - The analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track - Google Patents
The analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track Download PDFInfo
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- CN106248517A CN106248517A CN201610550482.7A CN201610550482A CN106248517A CN 106248517 A CN106248517 A CN 106248517A CN 201610550482 A CN201610550482 A CN 201610550482A CN 106248517 A CN106248517 A CN 106248517A
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- single track
- sample
- nanometer copper
- jet printing
- copper slurry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/16—Investigating or analyzing materials by the use of thermal means by investigating thermal coefficient of expansion
Abstract
The present invention relates to metal parts manufacture, a kind of analysis method particularly to physical characteristic based on Nanometer Copper slurry 3D jet printing single track, including using paraffin and copper nanoparticle configuration Nanometer Copper slurry, Nanometer Copper slurry is injected 3D jet printer and prints single track, and measure the width of single track；Progressively heating single track sample, heating rate when controlling heating is 8 12 DEG C/min, single track sample is carried out thermogravimetric analysis, obtains the temperature of single track sample and the variation relation of weight；Single track sample carries out the sintering that heats up, and heating rate when controlling sintering is 8 12 DEG C/min, observes the microstructure regularity of distribution of single track sample；Measure the width of single track sample in sintering process, calculate the shrinkage factor of single track sample, obtain the variation relation between the temperature of single track sample and the shrinkage factor of single track sample.The analysis method of the physical characteristic based on Nanometer Copper slurry 3D jet printing single track that the present invention provides, it is achieved that effective analysis of Nanometer Copper slurry 3D jet printing single track physical characteristic.
Description
Technical field
The present invention relates to metal parts manufacture, particularly to a kind of physics based on Nanometer Copper slurry 3D jet printing single track
The analysis method of characteristic.
Background technology
Metal parts 3D printing technique, as forefront and most potential technology in 3D printing system, is advanced manufacture skill
The important development direction of art.Microminiature components and parts are had huge by the high-tech areas such as Advanced Equipment, unmanned plane and Aero-Space
The market demand, especially metal material enjoys pass with its excellent mechanical performance and processing characteristics in Micro-manufacturing field
Note, its processing and forming manufacturing method have become study hotspot.Fine turnning and milling based on material removal process brill mill, ultrasound wave are micro-
The technology such as fining-off, electrochemical micromachining is difficult to shaping of labyrinth microminiature part, and there is cost height, cycle
The shortcomings such as length, versatility are the strongest.3D prints the digitized as a kind of advanced person and increases material manufacturing technology, with personalized, can short-term training soon
The advantages such as shape labyrinth, provide thinking for microminiature metal structure manufacture.Based on metal paste 3D jet printing principle, gold
The single track shaping belonging to slurry is the basis that metal three dimensional structure shapes.Single track reaction-injection moulding may determine that size performance is to formability
Impact, and how affect single track width by clear and definite print parameters, metal 3 D stereo is formed with the strongest guidance meaning
Justice.Analysis method currently for the physical characteristic of Nanometer Copper slurry 3D jet printing single track does not also occur.
Summary of the invention
The present invention, by providing a kind of analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track, solves
Prior art of having determined is difficult to analyze the technical problem of the physical characteristic of Nanometer Copper slurry 3D jet printing single track, it is achieved that nanometer
The temperature of copper slurry 3D jet printing single track sample and the variation relation of weight, the microstructure regularity of distribution of single track sample, list
Effective analysis of the physical parameters such as the variation relation between temperature and the shrinkage factor of single track sample of road sample, for 3D metallic print
Provide theoretical basis.
The invention provides a kind of analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track, described
Method includes:
Use paraffin and copper nanoparticle configuration Nanometer Copper slurry, described Nanometer Copper slurry is injected 3D jet printer and prints
Single track, and measure the width of described single track；
Progressively heating single track sample, heating rate when controlling heating is 8-12 DEG C/min, enters described single track sample
Row thermogravimetric analysis, obtains the temperature of described single track sample and the variation relation of weight；
Described single track sample carries out the sintering that heats up, and heating rate when controlling sintering is 8-12 DEG C/min, observes described
The microstructure regularity of distribution of single track sample；
Measure the width of single track sample described in sintering process, calculate the shrinkage factor of described single track sample, obtain described list
Variation relation between temperature and the shrinkage factor of single track sample of road sample.
Further, the particle diameter of described copper powder is 20-100nm.
Further, described paraffin and copper nanoparticle configure according to weight ratio 1:1.
Further, described paraffin and copper nanoparticle add heater in three times and mix；Hot charging is added described in control
The temperature put is 75 DEG C；Described paraffin in described heater and copper nanoparticle are stirred 15 minutes.
Further, when described single track sample is progressively heated, use N2Atmosphere.
Further, when progressively heating described single track sample, heating rate when controlling heating is 10 DEG C/min.
Further, electronic scanner microscope is used to observe the microstructure regularity of distribution of described single track sample.
Further, also include: by analyzing the X diffracting spectrum of described single track sample, it is judged that described single track sample dewaxes
After whether remaining impurity apart from copper.
Further, when described Nanometer Copper slurry injects 3D jet printer printing single track, use pottery for printing base
The end.
Further, when observing the microstructure regularity of distribution of described single track sample, the temperature that described single track sample is corresponding
Value is 200 DEG C, 400 DEG C, 600 DEG C, 800 DEG C and 1000 DEG C.
One or more technical schemes that the present invention provides, at least possess following beneficial effect or advantage:
The analysis method of the physical characteristic based on Nanometer Copper slurry 3D jet printing single track that the present invention provides, it is achieved that receive
Temperature and the variation relation of weight of rice copper slurry 3D jet printing single track sample, the microstructure regularity of distribution of single track sample,
Effective analysis of the physical characteristics such as the variation relation between temperature and the shrinkage factor of single track sample of single track sample, beats for 3D metal
Print provides theoretical basis.
Accompanying drawing explanation
The analysis side of the physical characteristic based on Nanometer Copper slurry 3D jet printing single track that Fig. 1 provides for the embodiment of the present invention
Method flow chart；
Fig. 2 for single track sample is carried out in intensification sintering process, the list observed with electronic scanner microscope when 400 DEG C
Road sample shape appearance figure；
Fig. 3 for single track sample is carried out in intensification sintering process, the list observed with electronic scanner microscope when 600 DEG C
Road sample shape appearance figure；
Fig. 4 for single track sample is carried out in intensification sintering process, the list observed with electronic scanner microscope when 800 DEG C
Road sample shape appearance figure；
Fig. 5 for single track sample is carried out in intensification sintering process, the list observed with electronic scanner microscope when 950 DEG C
Road sample shape appearance figure；
Fig. 6 is the shrinkage factor graph of a relation with temperature of single track Nanometer Copper slurry.
Detailed description of the invention
The embodiment of the present invention is by providing the analysis of a kind of physical characteristic based on Nanometer Copper slurry 3D jet printing single track
Method, solves the technical problem being difficult to analyze the physical characteristic of Nanometer Copper slurry 3D jet printing single track in prior art, real
Temperature and the variation relation of weight, the microstructure distribution of single track sample of Nanometer Copper slurry 3D jet printing single track sample are showed
Effective analysis of the physical parameters such as the variation relation between rule, the temperature of single track sample and the shrinkage factor of single track sample, for 3D
Metallic print provides theoretical basis.
See Fig. 1, embodiments provide a kind of physical characteristic based on Nanometer Copper slurry 3D jet printing single track
Analysis method, described method includes:
Step 10, employing paraffin and copper nanoparticle configuration Nanometer Copper slurry, inject 3D jet printer by Nanometer Copper slurry
Print single track, and measure the width of single track.
The particle diameter of copper powder is 20-100nm (such as 20nm, 60nm or 100nm), and paraffin and copper nanoparticle are according to weight ratio 1:1
Configuration.Paraffin and copper nanoparticle add heater in three times and mix；The temperature controlling heater is 75 DEG C；To heating
Paraffin and copper nanoparticle in device stir 15 minutes.When Nanometer Copper slurry is injected 3D jet printer printing single track, use
Pottery is printed substrates.
Step 20, single track sample is progressively heated, heating rate when controlling heating be 8-12 DEG C/min (such as 8 DEG C/minute
Clock, 10 DEG C/min or 12 DEG C/min), single track sample is carried out thermogravimetric analysis, obtains the temperature of single track sample and the change of weight
Change relation.
When single track sample is progressively heated, use N2Atmosphere.When single track sample is progressively heated, control intensification during heating
Speed is 10 DEG C/min.
Step 30, single track sample is carried out heat up sintering, control sintering time heating rate be 8-12 DEG C/min (such as 8
DEG C/min, 10 DEG C/min or 12 DEG C/min), observe single track sample the microstructure regularity of distribution.
Electronic scanner microscope is used to observe the microstructure regularity of distribution of single track sample.Observe the microcosmic group of single track sample
When knitting the regularity of distribution, the temperature value that single track sample is corresponding is 200 DEG C, 400 DEG C, 600 DEG C, 800 DEG C and 1000 DEG C.
In step 40, measurement sintering process, the width of single track sample, calculates the shrinkage factor of single track sample, obtains single track sample
Temperature and the shrinkage factor of single track sample between variation relation.
Step 50, by analyzing the X diffracting spectrum of single track sample, it is judged that after the dewaxing of single track sample, remaining is apart from copper
Impurity.
The physics based on the Nanometer Copper slurry 3D jet printing single track present invention provided below in conjunction with specific embodiment
The analysis method of characteristic illustrates:
Use paraffin and copper nanoparticle configuration Nanometer Copper slurry, the particle diameter of copper powder be 20nm, paraffin and copper nanoparticle according to
Weight ratio 1:1 configures.Paraffin and copper nanoparticle add heater in three times and mix；The temperature controlling heater is 75
DEG C, the paraffin in heater and copper nanoparticle are stirred 15 minutes.Nanometer Copper slurry is injected 3D jet printer printing list
Road, and measure the width of single track, when Nanometer Copper slurry injects 3D jet printer printing single track, use pottery for printing base
The end.
Progressively heating single track sample, heating uses N2Atmosphere, heating rate when controlling heating is 8 DEG C/min, to list
Road sample carries out thermogravimetric analysis, obtains the temperature of single track sample and the variation relation of weight.Thermogravimetric analysis uses TG curve to show,
In the present embodiment, in 200 DEG C, single track sample is the most weightless, and now Nanometer Copper pulp surface is paraffin melting, produces part volatilization.
Between 200 DEG C-300 DEG C, single track sample is the most weightless, and the decomposition of paraffin mainly occurs, and is the Main Stage of paraffin removing.
After 400 DEG C, single track sample mass changes hardly.And TG curve occurs endothermic peak at 250 DEG C, show nano copper slurry
Material sintering process has begun to occur at a lower temperature.950 DEG C there is endothermic peak, and now sintering enters later stage, send out
The raw diffusion of atom and the formation of crystal boundary are moved.
Single track sample carries out the sintering that heats up, and heating rate when controlling sintering is 8 DEG C/min, uses electron scanning to show
Micro mirror observes the microstructure regularity of distribution of single track sample.When observing the microstructure regularity of distribution of single track sample, single track sample
Corresponding temperature value is 200 DEG C, 400 DEG C, 600 DEG C, 800 DEG C and 1000 DEG C.Along with sintering temperature is different, single track sample microcosmic group
The change knitted.Seeing Fig. 2, when 400 DEG C, the copper nanoparticle of single track sample is cluster-shaped distribution, sintered together preliminarily forms
Sintering neck, there is substantial amounts of hole in single track sample.Along with the rising of sintering temperature, single track sample sintering neck is gradually grown up, simultaneously
The part of each cluster-shaped moves closer to.Seeing Fig. 3, sinter steady temperature when being 600 DEG C, part copper powder has been coupled to together,
In net distribution, sample exists irregular pore simultaneously.Seeing Fig. 4, when temperature continues to increase to 800 DEG C, copper granule is
Through being fully connected to together, hole is substantially circular, and crystal grain is grown up the most completely.See Fig. 5, continue to increase temperature to 950
DEG C, circular holes before is got rid of substantially, and this just can explain that, when temperature is increased to 950 DEG C, the shrinkage factor of sample reaches
Greatly.As can be seen here, from the point of view of Nanometer Copper slurry cross-section morphology, when sintering temperature is 950 DEG C, sintering effect is preferable, and this ratio
The fusing point (1083 DEG C) of block copper is much lower, and this is owing to copper nanoparticle activity is the highest, provides burning in sintering process
The driving force of knot.
Measure the width of single track sample in sintering process, calculate the shrinkage factor of single track sample, obtain the temperature of single track sample
And the variation relation between the shrinkage factor of single track sample.Along with the rising of temperature, single track sample Nanometer Copper slurry creates more
Significantly shrink.Before sintering temperature 400 DEG C, paraffin substantially completely removes, and has relatively concrete dynamic modulus, temperature between copper powder particle
Continue the internal densification process that hole eliminating and copper powder occur of elevated single track base substrate.When sintering temperature is 950 degrees Celsius
Time, single track sample can be shown in metallic luster, but single track specimen surface occurs that flatness is the highest, and possible reason is prepared slurry
The most uniformly.Fig. 6 is the shrinkage factor graph of a relation with temperature of single track single track Nanometer Copper slurry, it will be appreciated from fig. 6 that single track sample
Shrinkage factor increases with the rising of temperature.
By analyzing the X diffracting spectrum of single track sample, it is judged that the most remaining impurity apart from copper after the dewaxing of single track sample.
In the present embodiment, remaining impurity apart from copper after observing the dewaxing of single track sample by X diffracting spectrum.
One or more technical schemes that the present invention provides, at least possess following beneficial effect or advantage:
The analysis method of the physical characteristic based on Nanometer Copper slurry 3D jet printing single track that the present invention provides, it is achieved that receive
Temperature and the variation relation of weight of rice copper slurry 3D jet printing single track sample, the microstructure regularity of distribution of single track sample,
Effective analysis of the physical parameters such as the variation relation between temperature and the shrinkage factor of single track sample of single track sample, beats for 3D metal
Print provides theoretical basis.
It should be noted last that, above detailed description of the invention only in order to technical scheme to be described and unrestricted,
Although the present invention being described in detail with reference to example, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent, without deviating from the spirit and scope of technical solution of the present invention, it all should be contained
In the middle of scope of the presently claimed invention.
Claims (10)
1. the analysis method of a physical characteristic based on Nanometer Copper slurry 3D jet printing single track, it is characterised in that described side
Method includes:
Use paraffin and copper nanoparticle configuration Nanometer Copper slurry, described Nanometer Copper slurry is injected 3D jet printer printing list
Road, and measure the width of described single track；
Progressively heating single track sample, heating rate when controlling heating is 8-12 DEG C/min, and described single track sample is carried out heat
Weight analysis, obtains the temperature of described single track sample and the variation relation of weight；
Described single track sample carries out the sintering that heats up, and heating rate when controlling sintering is 8-12 DEG C/min, observes described single track
The microstructure regularity of distribution of sample；
Measure the width of single track sample described in sintering process, calculate the shrinkage factor of described single track sample, obtain the examination of described single track
Variation relation between temperature and the shrinkage factor of single track sample of sample.
2. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 1, it is special
Levying and be, the particle diameter of described copper powder is 20-100nm.
3. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 2, it is special
Levying and be, described paraffin and copper nanoparticle configure according to weight ratio 1:1.
4. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 3, it is special
Levying and be, described paraffin and copper nanoparticle add heater in three times and mix；
The temperature controlling described heater is 75 DEG C；
Described paraffin in described heater and copper nanoparticle are stirred 15 minutes.
5. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 1, it is special
Levy and be, when described single track sample is progressively heated, use N2Atmosphere.
6. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 1, it is special
Levying and be, when progressively heating described single track sample, heating rate when controlling heating is 10 DEG C/min.
7. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 1, it is special
Levy and be, use electronic scanner microscope to observe the microstructure regularity of distribution of described single track sample.
8. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 1, it is special
Levy and be, also include:
By analyzing the X diffracting spectrum of described single track sample, it is judged that remaining is apart from copper after the dewaxing of described single track sample
Impurity.
9. the analysis side of the physical characteristic based on Nanometer Copper slurry 3D jet printing single track as described in any one of claim 1-8
Method, it is characterised in that when described Nanometer Copper slurry injects 3D jet printer printing single track, using pottery is printed substrates.
10. the analysis method of physical characteristic based on Nanometer Copper slurry 3D jet printing single track as claimed in claim 1, it is special
Levy and be, when observing the microstructure regularity of distribution of described single track sample, the temperature value that described single track sample is corresponding is 200 DEG C,
400 DEG C, 600 DEG C, 800 DEG C and 1000 DEG C.
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Application publication date: 20161221 |