CN105271783B - A kind of glass powder and preparation method thereof for 3D printing - Google Patents

A kind of glass powder and preparation method thereof for 3D printing Download PDF

Info

Publication number
CN105271783B
CN105271783B CN201510685392.4A CN201510685392A CN105271783B CN 105271783 B CN105271783 B CN 105271783B CN 201510685392 A CN201510685392 A CN 201510685392A CN 105271783 B CN105271783 B CN 105271783B
Authority
CN
China
Prior art keywords
glass
printing
pbo
powder
glass powder
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
CN201510685392.4A
Other languages
Chinese (zh)
Other versions
CN105271783A (en
Inventor
李宏
卓永
许旭佳
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.)
Wuhan University of Technology WUT
Original Assignee
Wuhan University of Technology WUT
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 Wuhan University of Technology WUT filed Critical Wuhan University of Technology WUT
Priority to CN201510685392.4A priority Critical patent/CN105271783B/en
Publication of CN105271783A publication Critical patent/CN105271783A/en
Application granted granted Critical
Publication of CN105271783B publication Critical patent/CN105271783B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Glass Compositions (AREA)

Abstract

The invention belongs to 3D printing Material Fields, and in particular to a kind of glass powder and its preparation and be used for 3D printing molding.A kind of glass powder for 3D printing, which is characterized in that with PbO-B2O3‑V2O5System glass powder is main material, mixes the epoxy resin powder of 8-12wt% outside.The PbO-B2O3‑V2O5System glass, which is characterized in that its primary raw material includes PbO, V2O5、B2O3, mass percent shared by each component are as follows: PbO 40%-80%, V2O58%-52%, B2O38%-12%.The present invention is that 3D printing industry adds a kind of new glass printed material, pushes the development of 3D printing technique.

Description

A kind of glass powder and preparation method thereof for 3D printing
Technical field
The invention belongs to 3D printing Material Fields, and in particular to a kind of glass powder and its preparation and be used for 3D printing at Type.
Background technique
3D printing is successively to increase material by 3D printing equipment to manufacture three-dimensional objects according to designed 3D model Technology.3D printing combines many necks such as digital modeling techniques, Electromechanical Control technology, information technology, material science and chemistry The cutting edge technology in domain is one kind of rapid shaping technique, is known as the core technology of " the third time industrial revolution ".With it is conventionally manufactured Technology is compared, and 3D printing need not manufacture mold in advance, it is not necessary to a large amount of material is removed in the fabrication process, also without going through complexity Forging technology can be obtained by final products, therefore, may be implemented in production structure optimization, save material and save energy Source.3D printing technique is suitable for new product development, quick-acting single and parts in small batch manufacture, the manufacture of complicated shape part, mould Design and manufacture of tool etc., are also suitable for manufacture, configuration design inspection, assembly test of difficult-to-machine material etc..Therefore, 3D printing Industry receives concern more and more extensive both at home and abroad, will become next tool rising industry with broad prospects for development.
Currently, 3D printing has been applied to the fields such as product prototype, mold manufacture, art creation product, jewelry-making, can replace The conventional fine processing technology relied on for these fields.3D printing can largely promote the efficiency and precision of production Degree.In addition to this, in the fields such as bioengineering and medicine, building, clothes, the introducing of 3D printing technique has also been opened up more for it Wide development space.Based on the strategic height of 21 century manufacturing industry competition, the U.S., Europe and Japan are all to rapid prototyping technology A large amount of research has been put into, 3D printing technique is rapidly developed.In national defence, European and American developed countries pay much attention to 3D The application of printing technique, and put into huge fund and develop increasing material manufacturing metal parts, especially push increases material manufacturing technology to exist energetically Application in the manufacture of the high values material components such as titanium alloy.
3D printing material is the important material base of 3D printing technique development, and to a certain extent, the development of material determines 3D printing can have the problem of broader applications.Currently, 3D printing material mainly includes engineering plastics, photosensitive resin, rubber Class material, metal material and ceramic material etc., in addition to this, coloured plaster material, artificial bone meal, cell biological raw material and sand The food materials such as sugar are also applied in 3D printing field.These raw material used in 3D printing are all specific to 3D printing Equipment and technique and research and develop, and different froms such as common plastics, gypsum, resin, form generally have it is powdered, Filamentous, The mouths such as lamellar, liquid.In general, used powdered 3D is beaten according to the type of printing device and the difference of operating condition The partial size of print material, which is 1~100 μm, to be differed, and in order to make powder keep good mobility, generally require powder that there is height Sphericity.This greatly restricts the development of 3D printing technique.
In order to expand the use scope of 3D printing material, researchers carry out the lower glass powder of glass transformation temperature It probes into.The lower molding for being conducive to glass of glass transformation temperature, the PbO-V for urging bamboo et al. to prepare2O5-TeO2Its glass of system glass Glass transition temperature has reached 270 DEG C or so;Chinese patent (patent publication No.: CN102190442A) discloses a kind of vacuum glass Sealing-in low melting point glass powder and preparation method thereof, which belongs to B2O3-V2O5-P2O5System glass, Glass Transition temperature Degree has also reached 260 DEG C.Although lead vanadium tellurium system glass mobility of particle is fine, it volatilizees in temperature-rise period very tight Weight, this has seriously affected the heat treatment process after product molding;And alum phosphorus boron system glass can not then expire on mobility of particle Sufficient 3D printing material requirements, and the phosphate in glass can also make the glass powder moisture absorption.PbO-B2O3-V2O5The glass of system glass Glass transition temperature is low, while being also able to satisfy mobility of particle and the Post isothermal treatment requirement of material, so the system glass can be used In 3D printing.
Currently, although the use of flint glass can all cause certain damage, PbO-B to human body, environment2O3- V2O5The properties of system glass have all reached the requirement of 3D printing material, and also demonstrating it by experiment is that can use In 3D printing.Therefore, as long as we while carrying out discarded in experiment, production and in use, careful use leaded substance Recovery processing work afterwards, so that it may leaded substance be avoided to damage to human body, environment bring.
Summary of the invention
Object of the present invention is to provide a kind of glass for 3D printing for deficiency existing for current 3D printing glass material Glass powder and preparation method thereof adds a kind of new glass printed material for 3D printing industry, pushes the development of 3D printing technique.
To achieve the above object, the technical scheme adopted by the invention is that: a kind of glass powder for 3D printing, feature It is, with PbO-B2O3-V2O5System glass powder is main material, mixes epoxy resin powder (the i.e. epoxy resin powder of 8-12wt% outside Additional amount be PbO-B2O3-V2O5The 8-12wt% of system glass silty amount).
The molding mode that 3D printing selects is selective laser sintering, and scanning speed 800-1400m/s, forming temperature is room Temperature, laser power 8-14W.
PbO-B of the present invention2O3-V2O5System glass, which is characterized in that its main component includes PbO, V2O5、 B2O3, mass percent shared by each component are as follows:
PbO 40%-80%,
V2O58%-52%,
B2O38%-12%.
PbO-B of the present invention2O3-V2O5System glass, which is characterized in that its component also includes Al2O3、SiO2、R2O、 RO, mass percent shared by each component are as follows:
The R2O is Li2O、Na2O、K2One or more of O press any proportion mixture, RO ZnO, CuO, One or more of MgO, BaO press the mixture of any proportion.
PbO is introduced by lead oxide;V2O5It is introduced by ammonium metavanadate;B2O3It is introduced by boric acid;R2O is introduced by carbonate;RO by Oxide introduces;Al2O3It is introduced by aluminium oxide;SiO2It is introduced by silica.
The preparation method of above-mentioned a kind of glass powder for 3D printing, it is characterised in that include the following steps:
1) by mass percent shared by each component are as follows: PbO:40%-80%, V2O5: 8%-52%, B2O3: 8%-12%, Al2O3: 0%-3%, SiO2: 0%-5%, R2O:0%-2%, RO:0%-10%;Weigh PbO, NH4VO3、H3BO3、Al2O3、 SiO2、R2CO3(R2For Li2、Na2、K2) and RO raw material for standby;The R2O is Li2O、Na2O、K2One or more of O is by any The mixture of proportion, one or more of RO ZnO, CuO, MgO, BaO press the mixture of any proportion;R2O is by carbonate It introduces;
2) by weighed PbO, NH4VO3、H3BO3、Al2O3、SiO2、R2CO3It is fully ground, mixes in mortar with RO raw material It is melted after uniformly, 1100 DEG C -1200 DEG C of fusion temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding;
5) by obtained glass powder, the epoxy resin of 8-12wt% is mixed outside, is sufficiently mixed, obtain the glass for 3D printing Glass powder.
Using: it is room temperature in forming temperature, scanning speed 800-1400m/s, laser power is that will mix under 8-14W The mode of the glass powder selective laser sintering for 3D printing afterwards successively prints, can obtain complicated glass Product.
Obtained PbO-B2O3-V2O5The glass transition temperature Tg of system glass is 279.9-381.0 DEG C.
When processing, powder is preheating to the temperature of slightly less than its fusing point first, then by powder under the action of striking off rod End is paved;Laser beam is selectively sintered according to layering cross section information under the control of the computer, is carried out again after the completion of one layer Next layer of sintering, removes extra powder after being all sintered, then can be obtained by the part sintered.
The epoxy resin mixed outside moment at a high temperature of laser issues melts, to play adhesive in forming process Effect.
The molding mode that 3D printing selects is selective laser sintering.Glass powder and epoxy resin are sufficiently mixed, at Type temperature is that room temperature, laser are kept under certain output power, by layer-by-layer printing, it is preferable that molding can be made Glassware.Glass powder is used for 3D printing, has expanded the scope of application of 3D printing, make its consumptive material be not limited solely to ceramics, The fields such as plastics, metal also provide a kind of new molding mode for glassware, and solving glass material and being difficult to prepare has The problems such as accurate labyrinth object.
The present invention has following major advantage: 1) by PbO-B2O3-V2O5System glass is formed for 3D printing, is beaten for 3D Print industry adds a kind of new glass printed material, pushes the development of 3D printing industry;2) it is formed using 3D printing, is PbO- B2O3-V2O5System glass provides a kind of new molding mode, can quick close complex devices of preparation structure, expand PbO-B2O3-V2O5The application field of system glass;3) selective laser sintering and moulding PbO-B is used2O3-V2O5When system glass, It can carry out at room temperature, to keep forming process more simple and efficient, simultaneously the requirement of forming temperature when reducing 3D printing Also forming cost is greatly reduced.
Detailed description of the invention
Fig. 1 is 1 glass powder DSC test result figure of embodiment.
Fig. 2 is 5 glass powder DSC test result figure of embodiment.
Fig. 3 is 14 glass powder DSC test result figure of embodiment.
Fig. 4 is 14 results of sample preparation figure of embodiment, and a is top view, and b is side view.
Specific embodiment
For a better understanding of the present invention, below with reference to the example content that the present invention is furture elucidated, but the present invention is not only It is limited only to the following examples.
Embodiment 1:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 8wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 800m/s, molding Temperature is room temperature, laser power 8W.
The PbO-B2O3-V2O5System glass, primary raw material include PbO, V2O5、B2O3, quality hundred shared by each component Score is 80%, 12%, 8%.
Table 1
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 1 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder (i.e. PbO-B with 400 mesh sieve after glass breaking, grinding2O3-V2O5System glass Glass powder), DSC test result is 373.6-381.0 DEG C, as shown in Figure 1;
5) by obtained glass powder, the epoxy resin of 8wt% is mixed outside, is sufficiently mixed and (is obtained the glass for 3D printing Glass powder);
It 6) is room temperature in forming temperature, scanning speed 800m/s, laser power is to use mixed glass powder under 8W The mode of selective laser sintering successively prints, can obtain complicated glassware.
Embodiment 2:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 9wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 800m/s, molding Temperature is room temperature, laser power 10W.
Table 2
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 2 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 368.6-370.3℃;
5) by obtained glass powder, the epoxy resin of 9wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 800m/s, laser power is under 10W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 3:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 10wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1000m/s, at Type temperature is room temperature, laser power 12W.
Table 3
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 3 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 362.7-366.2℃;
5) by obtained glass powder, the epoxy resin of 10wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1000m/s, laser power is under 12W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 4:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 11wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1000m/s, at Type temperature is room temperature, laser power 10W.
Table 4
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 4 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 280.1-286.8℃;
5) by obtained glass powder, the epoxy resin of 11wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1000m/s, laser power is under 10W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 5:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 12wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1000m/s, at Type temperature is room temperature, laser power 8W.
Table 5
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 5 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 279.9-285.6 DEG C, as shown in Figure 2;
5) by obtained glass powder, the epoxy resin of 12wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1000m/s, laser power is under 8W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 6:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 11wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, at Type temperature is room temperature, laser power 10W.
Table 6
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 6 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 280.4-286.2℃;
5) by obtained glass powder, the epoxy resin of 11wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 10W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 7:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 10wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, at Type temperature is room temperature, laser power 8W.
Table 7
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 7 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 368.3-370.0℃;
5) by obtained glass powder, the epoxy resin of 10wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 8W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 8:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 9wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, molding Temperature is room temperature, laser power 12W.
Table 8
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 8 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 329.1-331.5℃;
5) by obtained glass powder, the epoxy resin of 9wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 12W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 9:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 8wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, molding Temperature is room temperature, laser power 14W.
Table 9
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 9 each component of table4VO3And H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3And H3BO3Raw material is fully ground in mortar, is melted after mixing, is melted Change 1100 DEG C -1200 DEG C of temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 283.3-284.7℃;
5) by obtained glass powder, the epoxy resin of 8wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 14W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 10:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 9wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1000m/s, molding Temperature is room temperature, laser power 14W.
Table 10
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 10 each component of table4VO3、H3BO3、Al2O3、SiO2And Li2CO3Raw material It is spare;
2) by weighed PbO, NH4VO3、H3BO3、Al2O3、SiO2And Li2CO3Raw material is fully ground in mortar, and mixing is equal It is melted after even, 1100 DEG C -1200 DEG C of fusion temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 291.7-292.1℃;
5) by obtained glass powder, the epoxy resin of 9wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 12W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 11:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 10wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, at Type temperature is room temperature, laser power 12W.
Table 11
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 11 each component of table4VO3、H3BO3、ZnO、CuO、MgO、SiO2And Na2CO3Raw material for standby;
2) by weighed PbO, NH4VO3、H3BO3、ZnO、CuO、MgO、SiO2And Na2CO3Raw material is sufficiently ground in mortar Mill, is melted, 1100 DEG C -1200 DEG C of fusion temperature after mixing, is kept the temperature 1-2 hours, is obtained glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 303.9-305.0℃;
5) by obtained glass powder, the epoxy resin of 10wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 12W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 12:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 11wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, at Type temperature is room temperature, laser power 12W.
Table 12
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 12 each component of table4VO3、H3BO3、ZnO、CuO、Al2O3, MgO and K2CO3Raw material for standby;
2) by weighed PbO, NH4VO3、H3BO3、ZnO、CuO、Al2O3, MgO and K2CO3Raw material is fully ground in mortar, It is melted after mixing, 1100 DEG C -1200 DEG C of fusion temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 295.8-297.2℃;
5) by obtained glass powder, the epoxy resin of 11wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 12W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 13:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 12wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, at Type temperature is room temperature, laser power 12W.
Table 13
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 12 each component of table4VO3、H3BO3, ZnO, CuO, MgO raw material for standby;
2) by weighed PbO, NH4VO3、H3BO3, ZnO, CuO, MgO raw material be fully ground in mortar, after mixing It is melted, 1100 DEG C -1200 DEG C of fusion temperature, keeps the temperature 1-2 hours, obtain glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, DSC test result is 295.0-297.4℃;
5) by obtained glass powder, the epoxy resin of 12wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 12W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.
Embodiment 14:
A kind of glass powder for 3D printing, it is with PbO-B2O3-V2O5System glass powder is main material, is mixed outside The epoxy resin powder of 10wt%.The molding mode that 3D printing selects is selective laser sintering, scanning speed 1200m/s, at Type temperature is room temperature, laser power 12W.
Table 14
Specific preparation process is as follows:
1) PbO, NH are weighed by mass percent shared by 14 each component of table4VO3、H3BO3、ZnO、CuO、MgO、Al2O3、SiO2 And K2CO3Raw material for standby;
2) by weighed PbO, NH4VO3、H3BO3、ZnO、CuO、MgO、Al2O3、SiO2And K2CO3Raw material is abundant in mortar Grinding, is melted, 1100 DEG C -1200 DEG C of fusion temperature after mixing, is kept the temperature 1-2 hours, is obtained glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 It anneals 1-2 hours at DEG C, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding, Glass Transition carried out to glass powder Temperature test, DSC test result are 295.2-300.0 DEG C, as shown in Figure 3;
5) by obtained glass powder, the epoxy resin of 10wt% is mixed outside, is sufficiently mixed;
It 6) is room temperature in forming temperature, scanning speed 1200m/s, laser power is under 12W, by mixed glass powder With the mode of selective laser sintering, successively prints, complicated glassware can be obtained.In order to test conveniently selection Simple bowl structure, as shown in Figure 4.
The bound of each raw material cited by the present invention and each raw material of the present invention, section value and technological parameter Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.

Claims (6)

1. a kind of glass powder for 3D printing, which is characterized in that with PbO-B2O3-V2O5System glass powder is main material, outside Mix the epoxy resin powder of 8-12wt%;
The PbO-B2O3-V2O5System glass, main component include PbO, V2O5、B2O3, mass percent shared by each component Are as follows:
PbO 40%-80%,
V2O58%-52%,
B2O38%-12%;
Applied to 3D printing: being room temperature in forming temperature, scanning speed 800-1400m/s, laser power is to incite somebody to action under 8-14W The mode of the mixed glass powder selective laser sintering for 3D printing successively prints, can obtain glassware.
2. a kind of glass powder for 3D printing according to claim 1, which is characterized in that the PbO-B2O3-V2O5 System glass, which is characterized in that its component also includes Al2O3、SiO2、R2O, RO, mass percent shared by each component are as follows:
The R2O is Li2O、Na2O、K2One or more of O presses the mixture of any proportion, RO ZnO, CuO, MgO, BaO One or more of press any proportion mixture.
3. a kind of glass powder for 3D printing as described in claim 1, which is characterized in that its glass transition temperature Tg It is 279.9-381.0 DEG C.
4. a kind of glass powder for 3D printing as described in claim 1, which is characterized in that be applied to 3D printing: forming Temperature is room temperature, and scanning speed 800-1400m/s, laser power is under 8-14W, by the mixed glass for being used for 3D printing The mode of powder selective laser sintering successively prints, can obtain glassware.
5. a kind of preparation method of glass powder for 3D printing according to claim 1, it is characterised in that including as follows Step:
1) by mass percent shared by each component are as follows: PbO:40%-80%, V2O5: 8%-52%, B2O3: 8%-12% is weighed PbO、NH4VO3、H3BO3Raw material for standby;
2) by weighed PbO, NH4VO3、H3BO3Raw material is fully ground in mortar, is melted after mixing, fusion temperature 1100 DEG C -1200 DEG C, 1-2 hours are kept the temperature, glass metal is obtained;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 DEG C Annealing 1-2 hours, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding;
5) by obtained glass powder, the epoxy resin of 8-12wt% is mixed outside, is sufficiently mixed, obtain the glass for 3D printing Powder.
6. a kind of preparation method of glass powder for 3D printing according to claim 2, it is characterised in that including as follows Step:
1) by mass percent shared by each component are as follows: PbO:40%-80%, V2O5: 8%-52%, B2O3: 8%-12%, Al2O3: 0%-3%, SiO2: 0%-5%, R2O:0%-2%, RO:0%-10%;Weigh PbO, NH4VO3、H3BO3、Al2O3、SiO2、 R2CO3With RO raw material for standby;The R2O is Li2O、Na2O、K2One or more of O presses the mixture of any proportion, and RO is One or more of ZnO, CuO, MgO, BaO press the mixture of any proportion;R2O is introduced by carbonate;
2) weighed raw material is fully ground in mortar, is melted after mixing, 1100 DEG C -1200 DEG C of fusion temperature, Heat preservation 1-2 hours, obtains glass metal;
3) glass metal is poured into graphite jig and is formed, the glass that casting obtains is placed in annealing furnace, at 300 DEG C -500 DEG C Annealing 1-2 hours, obtains transparent glass after cooling to room temperature with the furnace;
4) it will be sieved to obtain glass powder with 400 mesh sieve after glass breaking, grinding;
5) by obtained glass powder, the epoxy resin of 8-12wt% is mixed outside, is sufficiently mixed, obtain the glass for 3D printing Powder.
CN201510685392.4A 2015-10-21 2015-10-21 A kind of glass powder and preparation method thereof for 3D printing Active CN105271783B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510685392.4A CN105271783B (en) 2015-10-21 2015-10-21 A kind of glass powder and preparation method thereof for 3D printing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510685392.4A CN105271783B (en) 2015-10-21 2015-10-21 A kind of glass powder and preparation method thereof for 3D printing

Publications (2)

Publication Number Publication Date
CN105271783A CN105271783A (en) 2016-01-27
CN105271783B true CN105271783B (en) 2019-03-08

Family

ID=55141708

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510685392.4A Active CN105271783B (en) 2015-10-21 2015-10-21 A kind of glass powder and preparation method thereof for 3D printing

Country Status (1)

Country Link
CN (1) CN105271783B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105669208A (en) * 2016-03-07 2016-06-15 武汉理工大学 Phenolic resin coated ceramic powder for laser 3D printing and preparation method thereof
CN106587643B (en) * 2016-12-01 2019-03-15 天津理工大学 Heat fusing lamination 3D printing glass wire rod and its preparation method and application
CN107417127A (en) * 2017-08-01 2017-12-01 安徽原动力生产力促进中心有限公司 A kind of 3D printing glass powder, preparation method thereof
CN110316943B (en) * 2018-03-28 2021-12-17 许浒 Integral vacuum glass manufacturing method and integral vacuum glass
CN110316946B (en) * 2018-03-28 2021-12-17 许浒 Integral hollow glass manufacturing method and integral hollow glass
CN114044631B (en) * 2021-11-15 2022-11-11 海南大学 Preparation method and application of active substance glass powder

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3375450B2 (en) * 1995-03-02 2003-02-10 松下電器産業株式会社 Dielectric porcelain composition
CN104647760B (en) * 2015-02-12 2017-03-08 华中科技大学 A kind of 3D printing manufacture method of short fiber reinforced thermosetting resin joint product

Also Published As

Publication number Publication date
CN105271783A (en) 2016-01-27

Similar Documents

Publication Publication Date Title
CN105271783B (en) A kind of glass powder and preparation method thereof for 3D printing
CN108059351A (en) A kind of method that sintering process prepares rich iron lead skim devitrified glass
CN112624608B (en) Borosilicate glass curing substrate and preparation method and application thereof
CN103626398B (en) A kind of crystallization type lead-free low-temperature seal glass and preparation thereof and using method
CN102603191A (en) Method for manufacturing glass ceramic by titanium-containing melting blast furnace slag
CN108328932A (en) A kind of gear division devitrified glass that Ce, Er, Tb, Y are co-doped with and its preparation and application
CN104193171A (en) Silicon manganese alloy slag glass ceramic and preparation method thereof
CN103232164B (en) Coffee microcrystal glass plate and production method thereof
CN103288351A (en) Diopside phase glass ceramic and preparation method thereof
CN108947255A (en) A kind of polycrystalline phase devitrified glass and preparation method thereof
CN106116161A (en) A kind of method utilizing yellow phosphorus furnace slag and chromium slag to prepare devitrified glass
CN105130196A (en) Process for the preparation of ceramic glass material in the form of sheets, sheets thus obtained and use thereof
CN107417127A (en) A kind of 3D printing glass powder, preparation method thereof
CN104478219B (en) Nano-scale spinel glass ceramic and preparation method thereof
CN106630636A (en) Ceramic glass with lanthanum disilicate as principal crystalline phase, preparation method and application
CN103253867B (en) A kind of molten state yellow phosphorus furnace slag prepares the Technology of devitrified glass
CN105271762A (en) Composition and method for preparing lithium disilicate glass ceramics
CN101844869B (en) Method for preparing fluorine amphibole glass ceramic by using reactive crystallization-sintering method
CN104909562A (en) High-refractivity environment-friendly ruby glass and preparation method thereof
CN101125735A (en) Method for preparing yellow phosphorus ore slag microcrystalline glass by hot-casting method
CN106927681B (en) A kind of gear division devitrified glass that lithium sodium potassium is co-doped with and its preparation and application
CN110436778A (en) A kind of orthopaedics reparation bioactive glass material preparation method
CN108585511A (en) A kind of preparation method of high-performance devitrified glass
CN102249539A (en) Method for preparing aventurine fluoride-free opal glass
CN103011603A (en) Low-corrosion microcrystal jade ware and manufacturing 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
GR01 Patent grant