CN106277724B - The method that laser selective sintering prepares glassware - Google Patents
The method that laser selective sintering prepares glassware Download PDFInfo
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- CN106277724B CN106277724B CN201610710134.1A CN201610710134A CN106277724B CN 106277724 B CN106277724 B CN 106277724B CN 201610710134 A CN201610710134 A CN 201610710134A CN 106277724 B CN106277724 B CN 106277724B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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Abstract
The present invention relates to a kind of methods that laser selective sintering prepares glassware comprising following steps: 1) being in mass ratio that 90-99:1-10 progress mixing granulation obtains pelletizing by parent glass material and binder；2) curing agent powder is added in pelletizing, stirring obtains mixed-powder；3) mixed-powder is subjected to tiling by preformed shape and laser selective is sintered, it melts the curing agent in mixed-powder and pelletizing therein links together, Glass body is obtained, the process that tiling and laser selective are sintered is carried out continuously n times, and tiling is every time with a thickness of 50-500 μm；4) Glass body is subjected to dumping, and is sintered at 300-900 DEG C, obtain glassware.It using method of the invention, solves the defect that glass powder is easy to reunite, mobility is bad, most of glass powders can be prepared into glassware by required shape.
Description
Technical field
The present invention relates to a kind of preparation methods of glass, prepare glassware more particularly to a kind of laser selective sintering
Method.
Background technique
Currently, the method that glassware mainly passes through molding is prepared.Mould pressing method requires height to mold, and there are sizes
The problems such as precision is low, the loss of difficult forming, mold is big, at high cost.
Preparing glassware by laser selective sintering is a kind of preparation method relatively new at present.This method be by
Powdered glass raw material is prepared into glass material product of various shapes by layer-by-layer powdering, layer-by-layer selective sintering；However,
Common glass powder is easy to reunite, poor fluidity, therefore cannot be directly used to layer-by-layer powdering and laser selective sintering, common
Solution be by glass powder processing be prepared into glass microballoon, by rule spheric granules, realize preferable mobility and
Powdering uniformity, but this method high production cost, and performance is limited to by glass ingredient, is only applicable to a small number of glass materials, because
This, prepares glassware with significant limitation by laser selective sintering in the prior art.
Summary of the invention
It is a primary object of the present invention to, a kind of method that novel laser selective sintering prepares glassware is provided,
The technical problem to be solved is that make the glass powder of various systems can be transferred through laser selective be sintered to obtain it is of different shapes
Glassware, thus more suitable for practical.
The object of the invention to solve the technical problems adopts the following technical solutions to realize.It proposes according to the present invention
The laser selective sintering method for preparing glassware comprising following steps:
It 1) is in mass ratio that 90-99:1-10 progress mixing granulation obtains pelletizing by parent glass material and binder；
2) curing agent powder is added in the pelletizing, stirring obtains mixed-powder, wherein the curing agent contains
Amount is the 2wt%-45%wt of the mixed-powder；
3) mixed-powder is carried out tiling and laser selective sintering by preformed shape makes consolidating in mixed-powder
Agent melts and pelletizing therein links together, and obtains Glass body, wherein the tiling and laser selective is burnt
The process of knot is carried out continuously n times, and tiling is every time with a thickness of 50-500 μm；
4) Glass body is subjected to dumping, and is sintered at 300-900 DEG C, obtain glassware；
Wherein, the value of the n is the preset thickness and the ratio of each tiling thickness of the glassware,
N is positive integer.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the method that laser selective sintering above-mentioned prepares glassware, wherein the parent glass material
Partial size is 5-80 μm.
Preferably, the method that laser selective sintering above-mentioned prepares glassware, wherein the parent glass material packet
Include parent glass powder and functional material powder, the mass ratio of the parent glass powder and functional material powder is greater than 1.
Preferably, the method that laser selective sintering above-mentioned prepares glassware, wherein the organic adhesion agent is
Any one in polyvinyl alcohol, polyethylene glycol, paraffin and dextrin.
Preferably, the method that laser selective sintering above-mentioned prepares glassware, wherein the partial size of the pelletizing
It is 10-200 μm.
Preferably, the method that laser selective sintering above-mentioned prepares glassware, wherein the curing agent powder is
Any one in polyethylene, polystyrene, polyethylene glycol, polycarbonate, epoxy resin and phenolic resin.
Preferably, the method that laser selective sintering above-mentioned prepares glassware, wherein the laser selective is burnt
The power of knot is 10-100W, and scanning speed 1000-8000mm/s, laser beam focus is having a size of 0.01-0.1mm.
Preferably, the method that laser selective sintering above-mentioned prepares glassware, wherein the temperature of the dumping is
250-650℃。
By above-mentioned technical proposal, the method that laser selective sintering of the present invention prepares glassware at least has following excellent
Point:
1, any mold is not needed using method of the invention, reduced costs, preparation method is simple, shortens product
Production cycle.
2, most of glass powders can be prepared by required shape by glassware using method of the invention, this
Invention joined curing agent in pelletizing, by laser selective sintering by curing agent curing molding, wherein laser selective
Sintering is curing agent, and the present invention leads to that its is easy to reunite, mobility is bad without the concern for different due to glass powder composition,
And the problem of laser sintering process complexity, therefore method of the invention is suitable for the glass powder of various composition systems.
3, by the way that various functional material powder are added in glass powder of the invention, such as pigment, metal powder, ceramic powder
End etc. can arbitrarily adjust the physical properties such as color, the coefficient of expansion, the electric conductivity of glass.
4, glassware its formed precision height prepared using method of the invention.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, with presently preferred embodiments of the present invention, detailed description is as follows below.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to laser selective sintering proposed according to the present invention prepare the method for glassware its specific embodiment,
Feature and its effect, detailed description is as follows.In the following description, what different " embodiment " or " embodiment " referred to is not necessarily
The same embodiment.In addition, the special characteristic or feature in one or more embodiments can be combined by any suitable form.
One embodiment according to the present invention proposes a kind of method that laser selective sintering prepares glassware comprising
Following steps:
It 1) is in mass ratio that 90-99:1-10 progress mixing granulation obtains pelletizing by parent glass material and binder；
Parent glass material in the present embodiment can choose the frit of any system, it is not limited to certain special compositions
Frit, parent glass material be glassware main body；Binder links together parent glass material as auxiliary material
Pelletizing is obtained eventually by granulation.
Preferably, the parent glass material and organic adhesion agent in the present embodiment are 92-96:4-8 in mass ratio, using the model
The glassware precision size Du Genggao that the ratio enclosed is prepared, if the binder being added may excessively make to glue during dumping
Knot agent can not exclude completely, influence the performance of glassware, and the organic binders of addition excessively cause to be granulated incomplete.
Preferably, the partial size of parent glass material is 5-80 μm in the present embodiment；Wherein the partial size of parent glass material crosses senior general
Cause the partial size of pelletizing excessive, pelletizing partial size is excessive, it will to cause final mixed-powder to tile uneven；
Preferably, parent glass material includes parent glass powder and functional material powder, the basis in the present embodiment
The mass ratio of glass powder and functional material powder is greater than 1；Wherein functional material powder changes the physical property of glassware, for gold
Belong to powder, ceramic powders, colorant etc.；The glass with various physical properties can be prepared by the way that different functionalities material powder is added
Glass product；If the very few glassware intensity for causing finally to prepare of parent glass powder being added is low；Preferably, the present embodiment
Middle organic adhesion agent is any one in polyvinyl alcohol, polyethylene glycol, paraffin and dextrin；Polyvinyl alcohol, polyethylene glycol, paraffin
It is good with the adhesive property of dextrin, and volatility is low, is easy to exclude during dumping.
Preferably, the mixing granulation of the present embodiment is granulated using mist projection granulating or by hand；It is made by prepared by mist projection granulating
Grain powder is the spherical shape of regular shape, and the effect of tiling is good uniform, suitable for largely preparing pelletizing；It is granulated by hand and is suitble to micro make
The preparation of grain powder saves resource relative to mist projection granulating.
Preferably, the partial size of the pelletizing in the present embodiment is 10-200 μm；If partial size is excessive to will affect mixed-powder
Laying, paving it is uneven, lead to the glassware poor dimensional precision prepared；
2) curing agent powder is added in the pelletizing, stirring obtains mixed-powder, wherein the curing agent contains
Amount is the 2wt%-45%wt of the mixed-powder；
The present invention joined curing agent in pelletizing, is sintered by laser selective by curing agent sinter molding, wherein
Laser selective sintering is curing agent, the present invention cause without the concern for different due to glass powder composition its is easy to reunite,
Mobility is bad and the defect problem of laser sintering process complexity, therefore method of the invention is suitable for various composition systems
Glass powder；Curing agent cannot exclude completely during the curing dose of addition will lead to final dumping too much；
Preferably, curing agent powder is polyethylene, polystyrene, polyethylene glycol, polycarbonate, epoxy resin, phenolic aldehyde tree
Any one in rouge；Polyethylene, polystyrene, polyethylene glycol, polycarbonate, epoxy resin, phenolic resin curing effect are good,
And volatility is lower, is easy to exclude during dumping.
3) mixed-powder is carried out tiling and laser selective sintering by preformed shape makes consolidating in mixed-powder
Agent melts and pelletizing therein links together, and obtains Glass body, wherein the tiling and laser selective is burnt
The process of knot is carried out continuously n times, and tiling is every time with a thickness of 50-500 μm；
Wherein, if the thickness to tile every time is greater than 500 μm, laser selective sintering is uneven, the glass system prepared
Product dimensional accuracy is low；
4) Glass body is subjected to dumping, and is sintered at 300-900 DEG C, obtain glassware；
Wherein, the value of the n is the preset thickness and the ratio of each tiling thickness of the glassware,
N is positive integer.It at such a temperature can be by the powder sintered curing molding of parent glass in glass idiosome.
Dumping carries out in heating furnace, by dumping be discharged glassware in organic adhesion agent and curing agent, continue by
The powder sintered curing molding of parent glass, obtains glassware.Preferably, the power that the laser selective in the present embodiment is sintered
For 10-100W, scanning speed 1000-8000mm/s, laser beam focus is having a size of 0.01-0.1mm.
Preferably, the temperature of the dumping in the present embodiment is 250-650 DEG C, can exclude in Glass body at such a temperature
Organic binder and curing agent, and do not influence the structure of parent glass material.
By means of the present invention, it is with high accuracy various that glassware, glass devices equidimension can be prepared according to demand
Glassware.
Embodiment 1
1) wherein, the PbO-ZnO-B that 100g partial size is 5-20 μm2O3The silver of parent glass powder and 95g partial size less than 20 μm
Powder is uniformly mixed, and obtains parent glass material, and the paraffin of parent glass material and 20g are mixed, and heating stirring, granulation are simultaneously sieved, and is made
Obtain the pelletizing that partial size is 5-38 μm；PbO-ZnO-B used in it2O3Glass powder is grouped as by the group of following mass fraction:
64%PbO, 21%ZnO, 9%B2O3, 6% other ingredients；
2) the above-mentioned pelletizing of 100g is taken, the Polystyrene powder of 25g is added, stirs, obtains mixed-powder；
3) mixed-powder obtained is carried out continuously 30 tilings by each tiling with a thickness of 100 μm by required shape
It is sintered with laser selective；Wherein laser selective sintering is sintered the Polystyrene powder in the mixed-powder, obtains
To Glass body；Laser selective sintering uses CO2Laser, while being sintered and being carried out under heating plate heat transfer, when laser sintered
Power be 20W, scanning speed 1000mm/s, focal beam spot 0.1mm, the temperature of heating plate is 100 DEG C；
4) Glass body is put into heating furnace and excludes paraffin and polystyrene in 300 DEG C of heat preservation 1h, continue slowly heating
To 450 DEG C, 20min is kept the temperature, allows glass particle to be sufficiently sintered, after last slow cooling, obtains glassware.
Glassware manufactured in the present embodiment does not need mold, reduces the molding difficulty of complicated shape glassware；Silver
Powder has excellent electric conductivity, can reduce the insulation resistance of glassware manufactured in the present embodiment.
Embodiment 2
1) wherein, Na of the 20kg partial size less than 80 μm2O-B2O3-SiO2Parent glass powder and 0.4kg red coloring material for mixing
Uniformly, parent glass material is obtained, the polyvinyl alcohol of parent glass material and 0.6kg is sent by the feeding system of granulation tower
Granulation tower carries out mist projection granulating, and is sieved, and 100 mesh pelletizing below is made；Na used in it2O-B2O3-SiO2Glass
Powder is grouped as by the group of following mass fraction: 55%SiO2, 5%B2O3, 3%CaO, 9%Na2O, 3%Al2O3, 25% is other；
2) the above-mentioned pelletizing of 10kg is taken, the polycarbonate powder of 0.2kg is added, stirs, obtains mixed-powder；
3) mixed-powder obtained is carried out continuously 50 tilings by each tiling with a thickness of 50 μm by required shape
It is sintered with laser selective；Wherein laser selective sintering is sintered the polyethylene powders in the mixed-powder, obtains
Glass body；Laser selective sintering uses optical fiber laser, and power when laser sintered is 10W, scanning speed 2000mm/
S, focal beam spot 0.01mm；
4) Glass body is put into heating furnace and excludes polyvinyl alcohol and polycarbonate in 400 DEG C of heat preservation 1h, continued slow
900 DEG C are warming up to, 20min is kept the temperature, allows glass particle to be sufficiently sintered, after last slow cooling, obtain glassware.
Red color is added in parent glass material can prepare red glass product.
Embodiment 3
1) wherein, Bi of the 200g partial size less than 70 μm2O3-ZnO-B2O3-SiO2Parent glass powder and 20g partial size are less than 30
μm negative expansion ceramic powders be uniformly mixed, obtain parent glass material, by the polyethylene glycol of parent glass material and 20g mix, add
Thermal agitation, granulation are simultaneously sieved, and 100 mesh pelletizing below is made；Bi used in it2O3-ZnO-B2O3-SiO2Glass powder by
The group of following mass fraction is grouped as: 45%Bi2O3, 30%B2O3, 10%ZnO, 10%SiO2, 5% is other；
2) the above-mentioned pelletizing of 100g is taken, the polyethylene powders of 45g are added, stirs, obtains mixed-powder；
3) mixed-powder obtained is carried out continuously 20 tilings by each tiling with a thickness of 500 μm by required shape
It is sintered with laser selective；Wherein laser selective sintering is sintered the polyethylene powders in the mixed-powder, obtains
Glass body；Laser selective sintering uses CO2Laser, power when laser sintered are 100W, scanning speed 6000mm/
S, focal beam spot 0.01mm；
4) Glass body is put into high temperature furnace and excludes polyethylene glycol and polyethylene in 250 DEG C of heat preservation 1h, continue slowly to rise
Temperature keeps the temperature 20min, allows glass particle to be sufficiently sintered, after last slow cooling, obtain glassware to 420 DEG C.
Negative expansion ceramic powders in the glassware of the present embodiment reduce the coefficient of expansion of glassware, improve glass
The mechanical property of glass.
Embodiment 4
1) wherein, CaO-Al of the 1000g partial size less than 20 μm2O3-SiO2Parent glass powder and 50g partial size are less than 30 μm
Zircon powder be uniformly mixed, obtain parent glass material, by the dextrin of parent glass material and 11g mix, then by granulation tower
Feeding system be sent into granulation tower, carry out mist projection granulating, and be sieved, 200 mesh pelletizing below is made；CaO- used in it
Al2O3-SiO2Glass powder is grouped as by the group of following mass fraction: 18%CaO, 6%Al2O3, 63%SiO2, 3%B2O3, 7%
Na2O, 3% is other；
2) the above-mentioned pelletizing of 100g is taken, the epoxy powder of 15g is added, stirs, obtains mixed-powder；
3) mixed-powder obtained is carried out continuously 50 tilings by each tiling with a thickness of 20 μm by required shape
It is sintered with laser selective；Wherein laser selective sintering is sintered the epoxy powder in the mixed-powder, obtains
To Glass body；Using optical fiber laser is used, power when laser sintered is 30W for laser selective sintering, and scanning speed is
8000mm/s, focal beam spot 0.01mm；
4) Glass body is put into heating furnace and excludes dextrin and epoxy resin in 400 DEG C of heat preservation 2h, continue slowly heating
To 780 DEG C, 20min is kept the temperature, allows glass particle to be sufficiently sintered, after last slow cooling, obtains glassware.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, this hair is still fallen within
In the range of bright technical solution.
Claims (6)
1. a kind of method that laser selective sintering prepares glassware, it is characterised in that: itself the following steps are included:
It 1) is in mass ratio that 90-99:1-10 progress mixing granulation obtains pelletizing by parent glass material and organic binder；
2) curing agent powder is added in the pelletizing, stirring obtains mixed-powder, wherein the content of the curing agent is
The 2wt%-45wt% of the mixed-powder；
3) mixed-powder is subjected to tiling by preformed shape and laser selective is sintered, make the curing agent in mixed-powder
It melts and pelletizing therein links together, the process of the tiling and laser selective sintering is carried out continuously n times, often
Secondary tiling obtains Glass body with a thickness of 50-500 μm；
4) Glass body is subjected to dumping, the dump temperature is 250-400 DEG C；
5) it and by the Glass body after dumping at 300-900 DEG C is sintered, obtains glassware；
Wherein, the curing agent powder is polyethylene, polystyrene, polyethylene glycol, polycarbonate, epoxy resin and phenolic aldehyde tree
Any one in rouge；
The value of the n is the preset thickness of the glassware and the ratio of each tiling thickness, and n is positive whole
Number.
2. the method that laser selective sintering according to claim 1 prepares glassware, which is characterized in that the base
The partial size of plinth frit is 5-80 μm.
3. the method that laser selective sintering according to claim 1 prepares glassware, which is characterized in that the base
Plinth frit includes parent glass powder and functional material powder, the quality of the parent glass powder and functional material powder
Than being greater than 1.
4. the method that laser selective sintering according to claim 1 prepares glassware, which is characterized in that described has
Machine binder is any one in polyvinyl alcohol, polyethylene glycol, paraffin and dextrin.
5. the method that laser selective sintering according to claim 1 prepares glassware, which is characterized in that described makes
The partial size of grain powder is 10-200 μm.
6. the method that laser selective sintering according to claim 1 prepares glassware, which is characterized in that described swashs
The power of light selective sintering is 10-100W, and scanning speed 1000-8000mm/s, laser beam focus is having a size of 0.01-
0.1mm。
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| GB2570160A (en) * | 2018-01-15 | 2019-07-17 | Ortheia Ltd | Method of processing glass |
| CN109234724B (en) * | 2018-08-29 | 2020-08-14 | 中国科学院上海硅酸盐研究所 | Method for preparing porous silica glass film by laser melting |
| CN110606663B (en) * | 2019-10-18 | 2022-04-12 | 维达力实业（赤壁）有限公司 | Composite microcrystalline glass and preparation method thereof |
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|---|---|---|---|---|
| CN105254309A (en) * | 2015-09-24 | 2016-01-20 | 佛山华智新材料有限公司 | Ceramic 3D printing method |
| CN105330177A (en) * | 2015-11-27 | 2016-02-17 | 中国建筑材料科学研究总院 | Method for preparing sealing glass prefabricated part by selective laser sintering |
| CN105542468A (en) * | 2015-12-24 | 2016-05-04 | 成都新柯力化工科技有限公司 | Binder for 3D printing glass material and application of binder |
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| ITMO20030112A1 (en) * | 2003-04-18 | 2004-10-19 | C R P Technology S R L | MIXTURE OF SINTERED POWDERS FOR RAPID PROTOTYPING. |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254309A (en) * | 2015-09-24 | 2016-01-20 | 佛山华智新材料有限公司 | Ceramic 3D printing method |
| CN105330177A (en) * | 2015-11-27 | 2016-02-17 | 中国建筑材料科学研究总院 | Method for preparing sealing glass prefabricated part by selective laser sintering |
| CN105542468A (en) * | 2015-12-24 | 2016-05-04 | 成都新柯力化工科技有限公司 | Binder for 3D printing glass material and application of binder |
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