CN105669047A - Preparation method of mechanosensitive conductive glass - Google Patents

Preparation method of mechanosensitive conductive glass Download PDF

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Publication number
CN105669047A
CN105669047A CN201610022506.1A CN201610022506A CN105669047A CN 105669047 A CN105669047 A CN 105669047A CN 201610022506 A CN201610022506 A CN 201610022506A CN 105669047 A CN105669047 A CN 105669047A
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glass
ion exchange
potassium
preparation
molten salt
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何峰
宋培煜
谢峻林
梅书霞
金明芳
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3607—Coatings of the type glass/inorganic compound/metal
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/154—Deposition methods from the vapour phase by sputtering
    • C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a preparation method of mechanosensitive conductive glass. The preparation method comprises the following steps: heating an ion exchange furnace to 430-480 DEG C, putting raw glass and a first-step ion exchange fused salt component into the furnace, and exchanging to obtain primary ion exchange glass; putting the primary ion exchange glass and a second-step ion exchange fused salt component into the furnace, and exchanging to obtain secondary ion exchange glass; selecting a SiO2 target material, and preparing a SiO2 film of 40-100 nm on the surface of the secondary ion exchange glass; selecting pure gold as a target material, and preparing a metallic film of 7-11 nm on the surface of the SiO2 film so as to obtain the target product. The problem that breaking strength distribution of general chemical ion exchange glass is not centralized is solved. According to the mechanosensitive glass prepared by a low-temperature two-step ion exchange method, ion exchange intensity is guaranteed, and the mechanosensitive glass has great breaking centrality. In addition, sensitivity is extremely high, and it can be ensured that the product can be broken completely when being slammed.

Description

A kind of preparation method of mechanics sensitive conductive glass
Technical field
The invention belongs to field of material engineering technology, be specifically related to a kind of mechanics sensitive conductive method for glass preparation.
Background technology
Silicate glass has a lot of excellent physical property, and as light transmission is good, machine-shaping operation is simple, has the good characteristic such as high intensity, high rigidity thus can have a wide range of applications in fields such as building, automobile, space flight. But, along with application and industry development, silicate glass requirement in intensity, anti-thermal shock etc. is more and more higher. And the functional limitations such as the fragility that glass material itself has, the insulating properties demand for development of its material property. The glass theoretical strength drawn by the Theoretical Calculation that chemical bond is strong is about 7000MPa, and in reality, the actual strength of glass is less than 100MPa, differs 2-3 the order of magnitude. This biggest factor wherein affecting strength of glass is the micro-crack existed in glass, under stressing conditions, the brittleness of glass makes micro-crack by dislocation, micro-crack can not be carried out pinning or Stress Release as metal, and stress concentrates on micro-crack tip so that rapid crack. This needs to manufacture a kind of glass thus improving its tensile strength, we term it chemcor glass. And tensile strength horizontal homogeneous in order to reach chemcor glass is consistent, it is possible to obtain mechanics sensing glass by the mode of two-step solution. But mechanics sensing glass only has the performance such as high intensity, high transmission rate and do not have electric conductivity, it is difficult to be applied to the semiconductor applications such as photoelectron, a kind of mechanics sensitive conductive glass can be obtained then through the plated film mode of magnetron sputtering for this. This mechanics sensitive conductive glass, can exist as the electronic component in semiconductor instrument, primarily serve the purpose of conductance property, transmit electric current. When instrument is subject to general shock, owing to its tensile strength is relatively big, survivable; But when instrument is subject to actively strike or severe impact beyond tensile strength, owing to it has more consistent tensile strength level, sensing glass can crush by complete rupture, loses electric conductivity, thus serving the effect of protection instrument host.
The tensile strength of glass can be improved by glass being carried out the mode of chemical ion exchange. Chemical tempering, i.e. chemical ion exchange, be dipped in fused salt to keep steady temperature and the tempering processing mode of certain swap time by glass. Owing to the fragility characteristic of glass makes the comprcssive strength of glass material own greatly, tensile strength is little, the drawing stress on surface that broken, the micro-crack both from its glass surface that ruptures of glass bears, extension is started, so that broken or fracture phenomenon occurs in glass along crack tip place. And chemical ion exchange process will make glass surface obtain a degree of compressive stress in fused salt in advance, its principle is due to the less metal ion (M of glass Ionic Radius+, M2+, such as Na+) with the bigger metal ion (M of fused salt Ionic Radius+, M2+, such as K+) phase counterdiffusion exchanges, the ion that in fused salt, radius is bigger occupies the ion position that radius in glass is less, creates " jammed " effect so that surface layer of glass density increases, and produces internal pressure stress. When glass material is once again subjected to extraneous tension, first having to overcome glass surface compressive stress, just may occur in which tensile stress state, namely surface pre-compression stress can improve the extraneous tension size that glass bears, and improves the tensile strength of glass.
And it is inadequate for only improving glass surface compressive stress, due to the existence of micro-crack so that the weakest link of glass itself is at the most advanced and sophisticated place of micro-crack. Micro-crack degree of depth ginseng is time uneven, and some glass crack degree of depth are shallower, and have may reach distance glass surface 50 μ m place, and and non-glass outermost surface. The compressive stress of its outermost surface institute pre-add of glass after primary ions exchange processes is maximum, and along with the increase of thickness of glass, internal layer compressive stress is more and more less, almost nil to 70 μ m places. Through the glass sample that same chemical ion exchange process system processes, the difference of its final tensile strength may be caused due to the difference of each of which sample micro-crack degree of depth, therefore maximum crushing stress value need to be moved to inside glass, guarantee has bigger value of compressive stress at micro-crack tip place, thus it is basically identical to ensure that identical chemical ion exchange process processes its tensile strength of glass specimen obtained.
Here introducing the concept of Weibull modulus, Weibull modulus characterizes uniformity and the reliability of the strength of materials, and Weibull modulus is more big, and intensity discreteness is more little, and the coefficient of variation is more little, and reliability is more good. Although the glass tensile strength after primary ions exchange processes significantly increases, but its Weibull modulus is not greatly improved.
And general glass belongs to insulating properties object at present, does not have electric conductivity. Conventional magnetron sputtering technology is not distributed in glass at engineering stress and carries out coating process. Can current existing technology not accomplish to lose electric conductivity when producing electric conductivity when being not affected by clashing into and be subject to clashing into. And engineering stress is distributed after glass carries out plated film and can obtain a lot of good characteristics, it is possible to make glass material can obtain the mechanical property such as electric conductivity, high light transmittance and high intensity and high Weibull modulus simultaneously. So it is very necessary for inventing a kind of electro-conductive glass with mechanics sensitivity characteristic.
Summary of the invention
Present invention aim at providing a kind of High anti bending strength, Weibull modulus is high, has the electro-conductive glass system of mechanics sensitivity characteristic, it is possible to meet mechanics and electricity dual property, and provide the preparation method preparing this mechanics sensitive conductive glass.
The present invention solves that the technical scheme that problem set forth above adopts is:
The preparation method of a kind of mechanics sensitive conductive glass, comprises the following steps:
1) first step ion-exchange treatment process: ion exchanging furnace is warming up to 430-480 DEG C, exchanges in the separated stove of components of molten salt by the former sheet glass of surface preparation and first step ion, preheats 1-2.5h; After fused salt component melts, glass is immersed in components of molten salt, is incubated 25-48h; Exchange quickly cools down with the rate of temperature fall of 10-15 DEG C after terminating, and obtains primary ions exchange glass;
Wherein, first step ion exchange components of molten salt is as follows in parts by weight: potassium nitrate 90-94%, potassium fluoride 0.5-1%, potassium silicate 1.4-2.5%, potassium phosphate 1.1-2.3%, aluminium oxide 0.2-0.8%, potassium hydroxide 0.1-0.5%, potassium carbonate 0.5-1%, kieselguhr 1.7-2.5%;
2) second step ion-exchange treatment process: ion exchanging furnace is warming up to 380-450 DEG C, exchanges primary ions in glass and the second step ion exchange separated stove of components of molten salt, preheats 1-2.5h; After fused salt component melts, primary ions is exchanged glass and is immersed in components of molten salt, be incubated 15-60min; Exchange is rapidly heated 50 DEG C after terminating, and is incubated 2-5min, then quickly cools down with the rate of temperature fall of 10-15 DEG C, obtain Two-step ion-exchanging glass;
Wherein, second step ion exchange components of molten salt is as follows in parts by weight: potassium fluoride 0.5-0.7%, potassium silicate 1.0-1.6%, potassium phosphate 1.3-2.1%, aluminium oxide 0.2-0.8%, potassium hydroxide 0.1-0.5%, potassium carbonate 0.5-0.7%, kieselguhr 1.0-2.5%, above component accounts for the 6.5% of whole components of molten salt. All the other 93.5% are potassium nitrate and sodium nitrate composition, and proportionally the ratio of 7:3 carries out proportioning, then potassium nitrate accounts for 65.45%, and sodium nitrate accounts for 28.05%.
3)SiO2The preparation of thin film: use radio-frequency sputtering technology, selects SiO2Target, coating chamber atmosphere selects the logical argon of evacuation and oxygen, prepares the SiO of 40-100nm at Two-step ion-exchanging glass surface2Thin film;
4) preparation of metallic film: using radio-frequency sputtering technology, selection proof gold is target, coating chamber atmosphere selects the logical argon of evacuation, at SiO2Film surface prepares the metallic film of 7-11nm, obtains target product.
By such scheme, described first step ion exchange components of molten salt and second step ion exchange components of molten salt use front ground and mixed, by 300-400 mesh sieve, tail over less than 0.5-0.8wt%.
By such scheme, described former sheet glass surface preparation process is: polishing, polishing, and ultrasonic cleaning is dried.
By such scheme, prepare SiO2The radio-frequency sputtering speed of thin film is 2-4nm/min, and argon pressure is 0.5-1Pa, and sputtering power is 180-220W, and the plated film time is 20-25min.
By such scheme, the sputter rate preparing metallic film is 10-20W, argon pressure 0.1-0.2Pa, and the plated film time is 100-130s, and the resistance value between farthest 2 of length direction is less than 90-100 Ω.
Compared with prior art, the invention has the beneficial effects as follows:
(1) present invention employs chemical ion exchanged form and prepare mechanics sensing glass, its tensile strength is compared former sheet glass and is significantly increased, and the experimental data according to the present invention can prepare the chemcor glass of a series of tensile strength from low to high, can prepare the chemcor glass of specific tensile strength according to practical situation demand, market prospect is extensive.
(2) the invention solves the fracture strength of general chemistry chemcor glass and be distributed the problem do not concentrated, adopt the mechanics sensing glass prepared by low temperature two-step solution method while ensureing its ion exchange intensity, be provided with good fracture set neutral;Weibull is between 40-50, and sensitivity is high. Ensure that when being subject to clashing, can crush by complete rupture.
(3) a large amount of micro-crack is produced before the mechanics sensitive conductive glass breakage that prepared by the present invention; it is made to lose electric conductivity; thus playing system cut-off; play forewarning function; after fracture is broken simultaneously, fragment is fine particle shape; it is all obtuse angle state, without acute angle, it is possible to play the effect that protection instrument internal element is not damaged.
(4) chemical ion exchange process and magnetron sputtering method are combined by the present invention; on the basis of prepared mechanics sensing glass; the electric conductivity not available for traditional glass is realized again through evaporation double-layer films; can be applicable to semiconductor applications, military field; the instrument of specific function has protected host, the effect of Support Equipment safety.
Detailed description of the invention
Following example explain technical scheme further, but not as limiting the scope of the invention.
Embodiment 1
(1) in first step ion exchange fused salt, the mass percent of each component is potassium nitrate 90%, potassium fluoride 1.0%, potassium silicate 2.5%, potassium phosphate 2.3%, aluminium oxide 0.8%, potassium hydroxide 0.4%, potassium carbonate 0.5%, kieselguhr 2.5%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(2) former sheet glass cuts in inner circle cutting machine, make long 25mm, cross-sectional area is the foursquare match stick shape glass of 3mm, with mould, glass is positioned in polished machine, surface after cutting is towards polished machine, experience the grinding process of 1000 orders, 1500 orders, 2000 orders, 2500 orders, 3000 orders, 3500 orders, 5000 order carborundum papers successively, by fine for cutting surfaces polishing, polishing then through polishing cloth, every one procedure carries out about 1 hour, afterwards glass is carried out ultrasonic cleaning, dry, wait that next step processes.
(3) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min1, temperature is 430 DEG C, the former sheet glass anticipated and first step ion is exchanged component formula and places respectively in stove, preheating 2h, waits that first step ion exchange component all becomes after fused salt state through high temperature, by glass submergence components of molten salt, close fire door, be incubated 25h. Again the chemcor glass exchanged is taken out, and the glass that ion is exchanged after terminating by the rate of temperature fall of 15 DEG C/min quickly cools down, ultrasonic cleaning, dry, wait that next step processes.
(4) in second step ion exchange fused salt, the mass percent of each component is potassium nitrate 65.45%, sodium nitrate 28.05%, potassium fluoride 0.5%, potassium silicate 1.2%, potassium phosphate 2%, aluminium oxide 0.5%, potassium hydroxide 0.1%, potassium carbonate 0.5%, kieselguhr 1.7%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(5) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min2Temperature is 420 DEG C, the chemcor glass anticipated and second step ion are exchanged component formula place respectively in stove, preheating 2h, waits that second step ion exchange component all becomes after fused salt state through high temperature, by chemcor glass submergence components of molten salt, close fire door, insulation 15min, exchange is rapidly heated higher than T after terminating2The temperature spot of temperature 50 C, is incubated 3min, then is taken out by the chemcor glass exchanged, and the glass after then ion being exchanged with the rate of temperature fall of 15 DEG C quickly cools down.Ultrasonic cleaning, dry, wait that next step processes.
(6) JGC-40 magnetron sputtering coater plated film is used. Use radio-frequency sputtering technology, glass is fixed on chip bench, select SiO2Target. Close vent valve, open main valve, start mechanical pump and vacuometer, after pressure to 10Pa, start molecular pump, open fine vacuum after below 0.1Pa and measure, treat that vacuum reaches 10-3After Pa, turn main valve down, open effusion meter, pass into argon and oxygen. Starting sputtering, sputter rate is 2.5nm/min, and argon pressure is 0.5Pa, and sputtering power is 180W, and the plated film time is 20min. Prepare the SiO of 50nm thickness2Thin film.
(7) d.c. sputtering technology is used. SiO will be carried out2Glass substrate after plated film is once again secured on chip bench, and selection proof gold is target. Close vent valve, open main valve, start mechanical pump and vacuometer, after pressure to 10Pa, start molecular pump, open fine vacuum after below 0.1Pa and measure, treat that vacuum reaches 10-3After Pa, turn main valve down, open effusion meter, pass into argon. Starting sputtering, sputtering power is 10W, argon pressure 0.1Pa, and the plated film time is 100s. Prepare the gold thin film of 7nm thickness.
Obtained mechanics sensitive conductive glass, rupture strength has reached 470MPa, Weibull modulus and has reached more than 20. Transmitance after plated film is more than 85%, and the resistance value between farthest 2 of length direction is less than 90 Ω, and surface roughness is less.
Embodiment 2
(1) in first step ion exchange fused salt, the mass percent of each component is potassium nitrate 91%, potassium fluoride 0.6%, potassium silicate 1.6%, potassium phosphate 2.2%, aluminium oxide 0.8%, potassium hydroxide 0.3%, potassium carbonate 1.0%, kieselguhr 2.5%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(2) former sheet glass is cut in inner circle cutting machine, make long 28mm, cross-sectional area is the foursquare match stick shape glass of 1.3mm, with mould, glass is positioned in polished machine, surface after cutting is towards polished machine, experience the grinding process of 1000 orders, 1500 orders, 2000 orders, 2500 orders, 3000 orders, 3500 orders, 5000 order carborundum papers successively, by fine for cutting surfaces polishing, polishing then through polishing cloth, every one procedure carries out about 1 hour, afterwards glass is carried out ultrasonic cleaning, dry, wait that next step processes.
(3) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min1, temperature is 440 DEG C, the former sheet glass anticipated and first step ion is exchanged component formula and places respectively in stove, preheating 2h, wait that first step ion exchange component all becomes after fused salt state through high temperature, in glass submergence components of molten salt, fire door will be closed, insulation 32h, again the chemcor glass exchanged is taken out, and the glass that ion is exchanged after terminating by the rate of temperature fall of 15 DEG C/min quickly cools down, ultrasonic cleaning, dry, wait that next step processes.
(4) in second step ion exchange fused salt, the mass percent of each component is potassium nitrate 65.45%, sodium nitrate 28.05%, potassium fluoride 0.7%, potassium silicate 1.3%, potassium phosphate 2%, aluminium oxide 0.2%, potassium hydroxide 0.2%, potassium carbonate 0.5%, kieselguhr 1.6%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(5) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min2Temperature is 420 DEG C, the chemcor glass anticipated and second step ion are exchanged component formula place respectively in stove, preheating 2h, waits that second step ion exchange component all becomes after fused salt state through high temperature, by chemcor glass submergence components of molten salt, close fire door, insulation 60min, exchange is rapidly heated higher than T after terminating2The temperature spot of temperature 50 C, is incubated 3min, then is taken out by the chemcor glass exchanged, and the glass after then ion being exchanged with the rate of temperature fall of 15 DEG C quickly cools down, ultrasonic cleaning, dry, waits that next step processes.
(6) JGC-40 magnetron sputtering coater plated film is used. Use radio-frequency sputtering technology, glass is fixed on chip bench, select SiO2Target. Close vent valve, open main valve, start mechanical pump and vacuometer, after pressure to 10Pa, start molecular pump, open fine vacuum after below 0.1Pa and measure, treat that vacuum reaches 10-3After Pa, turn main valve down, open effusion meter, pass into argon and oxygen. Starting sputtering, sputter rate is 2.5nm/min, and argon pressure is 0.75Pa, and sputtering power is 200W, and the plated film time is 20min. Prepare the SiO of 55nm thickness2Thin film.
(7) d.c. sputtering technology is used. SiO will be carried out2Glass substrate after plated film is once again secured on chip bench, and target selects metal targets. Close vent valve, open main valve, start mechanical pump and vacuometer, after pressure to 10Pa, start molecular pump, open fine vacuum after below 0.1Pa and measure, treat that vacuum reaches 10-3After Pa, turn main valve down, open effusion meter, pass into argon. Starting sputtering, sputtering power is 15W, argon pressure 0.2Pa, and the plated film time is 100s. Prepare the gold thin film of 9nm thickness.
Obtained mechanics sensitive conductive glass, rupture strength has reached 460MPa, Weibull modulus and has reached more than 30, and the transmitance after plated film is more than 85%, and the resistance value between farthest 2 of length direction is less than 95 Ω, and surface roughness is less.
Embodiment 3
(1) in first step ion exchange fused salt, the mass percent of each component is potassium nitrate 92%, potassium fluoride 0.5%, potassium silicate 1.9%, potassium phosphate 1.5%, aluminium oxide 0.5%, potassium hydroxide 0.1%, potassium carbonate 1.0%, kieselguhr 2.5%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(2) identical with embodiment 1 step 2.
(3) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min1, temperature is 460 DEG C, is incubated 38h, and all the other steps are identical with embodiment 1 step 3.
(4) in second step ion exchange fused salt, the mass percent of each component is potassium nitrate 65.45%, sodium nitrate 28.05%, potassium fluoride 0.6%, potassium silicate 1.6%, potassium phosphate 1.7%, aluminium oxide 0.8%, potassium hydroxide 0.3%, potassium carbonate 0.5%, kieselguhr 1.0%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(5) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min2, temperature is 420 DEG C, and temperature retention time is 60min, and all the other steps are identical with embodiment 1 step 5.
(6) JGC-40 magnetron sputtering coater plated film is used. Using radio-frequency sputtering technology, sputter rate is 2.0nm/min, and argon pressure is 1Pa, and sputtering power is 220W, and the plated film time is 20min, and all the other steps are identical with embodiment 1 step 6.Prepare the SiO of 40nm thickness2Thin film.
(7) d.c. sputtering technology is used. Sputtering power is 20W, argon pressure 0.1Pa, and the plated film time is 120s, and all the other steps are identical with embodiment 1 step 7. Prepare the gold thin film of 10nm thickness.
Obtained mechanics sensitive conductive glass, rupture strength has reached 450MPa, Weibull modulus and has reached more than 40. Transmitance after plated film is more than 85%, and the resistance value between farthest 2 of length direction is less than 100 Ω, and surface roughness is less.
Embodiment 4
(1) in first step ion exchange fused salt, the mass percent of each component is potassium nitrate 93%, potassium fluoride 0.5%, potassium silicate 1.4%, potassium phosphate 2%, aluminium oxide 0.5%, potassium hydroxide 0.4%, potassium carbonate 0.5%, kieselguhr 1.7%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(2) identical with embodiment 1 step 2.
(3) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min1, temperature is 470 DEG C, temperature retention time 42h, and all the other steps are identical with embodiment 1 step 3.
(4) in second step ion exchange fused salt, the mass percent of each component is potassium nitrate 65.45%, sodium nitrate 28.04%, potassium fluoride 0.5%, potassium silicate 1.1%, potassium phosphate 2.1%, aluminium oxide 0.2%, potassium hydroxide 0.4%, potassium carbonate 0.7%, kieselguhr 1.5%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(5) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min2, temperature is 430 DEG C, temperature retention time 60min, and all the other steps are identical with embodiment 1 step 5.
(6) JGC-40 magnetron sputtering coater plated film is used. Use radio-frequency sputtering technology. Sputter rate is 4.0nm/min, and argon pressure is 0.75Pa, and sputtering power is 200W, and the plated film time is 25min, and all the other steps are identical with embodiment 1 step 6. Prepare the SiO of 100nm thickness2Thin film.
(7) d.c. sputtering technology is used. Sputtering power is 20W, argon pressure 0.1Pa, and the plated film time is 130s, and all the other steps are identical with embodiment 1 step 7. Prepare the gold thin film of 11nm thickness.
Obtained mechanics sensitive conductive glass, rupture strength has reached 430MPa, Weibull modulus and has reached more than 30, and the transmitance after plated film is more than 85%, and the resistance value between farthest 2 of length direction is less than 100 Ω, and surface roughness is less.
Embodiment 5
(1) in first step ion exchange fused salt, the mass percent of each component is potassium nitrate 94%, potassium fluoride 0.5%, potassium silicate 1.4%, potassium phosphate 1.1%, aluminium oxide 0.2%, potassium hydroxide 0.5%, potassium carbonate 0.6%, kieselguhr 1.7%. Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(2) identical with embodiment 1 step 2.
(3) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min1, temperature is 480 DEG C, temperature retention time 48h, and all the other steps are identical with embodiment 1 step 3.
(4) in second step ion exchange fused salt, the mass percent of each component is potassium nitrate 65.45%, sodium nitrate 28.04%, potassium fluoride 0.5%, potassium silicate 1.0%, potassium phosphate 1.3%, aluminium oxide 0.2%, potassium hydroxide 0.5%, potassium carbonate 0.5%, kieselguhr 2.5%.Being placed by above-mentioned formula and be ground with interpolation agate ball in corundum ball grinder, duration is 2 hours. It is ground to by 300 mesh sieves, tails over less than 0.5wt%.
(5) ion exchanging furnace is warming up to T according to the heating rate of 5 DEG C/min2, temperature is 450 DEG C, temperature retention time 15min, and all the other steps are identical with embodiment 1 step 5.
(6) use JGC-40 magnetron sputtering coater plated film, use radio-frequency sputtering technology. Sputter rate is 2.5nm/min, and argon pressure is 0.75Pa, and sputtering power is 200W, and the plated film time is 23min, and all the other steps are identical with embodiment 1 step 6. Prepare the SiO of 57.5nm thickness2Thin film.
(7) d.c. sputtering technology is used. Sputtering power is 20W, argon pressure 0.1Pa, and the plated film time is 120s, and all the other steps are identical with embodiment 1 step 7. Prepare the gold thin film of 10nm thickness.
Obtained mechanics sensitive conductive glass, rupture strength has reached 420MPa, Weibull modulus and has reached more than 20, and the transmitance after plated film is more than 85%, and the resistance value between farthest 2 of length direction is less than 100 Ω, and surface roughness is less.

Claims (5)

1. the preparation method of a mechanics sensitive conductive glass, it is characterised in that comprise the following steps:
1) first step ion-exchange treatment process: ion exchanging furnace is warming up to 430-480 DEG C, exchanges in the separated stove of components of molten salt by the former sheet glass of surface preparation and first step ion, preheats 1-2.5h; After fused salt component melts, glass is immersed in components of molten salt, is incubated 25-48h; Exchange quickly cools down with the rate of temperature fall of 10-15 DEG C after terminating, and obtains primary ions exchange glass;
Wherein, first step ion exchange components of molten salt is as follows in parts by weight: potassium nitrate 90-94%, potassium fluoride 0.5-1%, potassium silicate 1.4-2.5%, potassium phosphate 1.1-2.3%, aluminium oxide 0.2-0.8%, potassium hydroxide 0.1-0.5%, potassium carbonate 0.5-1%, kieselguhr 1.7-2.5%;
2) second step ion-exchange treatment process: ion exchanging furnace is warming up to 380-450 DEG C, exchanges primary ions in glass and the second step ion exchange separated stove of components of molten salt, preheats 1-2.5h; After fused salt component melts, primary ions is exchanged glass and is immersed in components of molten salt, be incubated 15-60min; Exchange is rapidly heated 50 DEG C after terminating, and is incubated 2-5min, then quickly cools down with the rate of temperature fall of 10-15 DEG C, obtain Two-step ion-exchanging glass;
Wherein, second step ion exchange components of molten salt is as follows in parts by weight: potassium fluoride 0.5-0.7%, potassium silicate 1.0-1.6%, potassium phosphate 1.3-2.1%, aluminium oxide 0.2-0.8%, potassium hydroxide 0.1-0.5%, potassium carbonate 0.5-0.7%, kieselguhr 1.0-2.5%, above component accounts for the 6.5% of whole components of molten salt. All the other 93.5% are potassium nitrate and sodium nitrate composition, and proportionally the ratio of 7:3 carries out proportioning, then potassium nitrate accounts for 65.45%, and sodium nitrate accounts for 28.05%.
3)SiO2The preparation of thin film: use radio-frequency sputtering technology, selects SiO2Target, coating chamber atmosphere selects the logical argon of evacuation and oxygen, prepares the SiO of 40-100nm at Two-step ion-exchanging glass surface2Thin film;
4) preparation of metallic film: using radio-frequency sputtering technology, selection proof gold is target, coating chamber atmosphere selects the logical argon of evacuation, at SiO2Film surface prepares the metallic film of 7-11nm, obtains target product.
2. the preparation method of mechanics sensitive conductive glass as claimed in claim 1, it is characterised in that described first step ion exchange components of molten salt and second step ion exchange components of molten salt use front ground and mixed, by 300-400 mesh sieve, tail over less than 0.5-0.8wt%.
3. the preparation method of mechanics sensitive conductive glass as claimed in claim 1, it is characterised in that described former sheet glass surface preparation process is: polishing, polishing, ultrasonic cleaning is dried.
4. the preparation method of mechanics sensitive conductive glass as claimed in claim 1, it is characterised in that preparation SiO2The radio-frequency sputtering speed of thin film is 2-4nm/min, and argon pressure is 0.5-1Pa, and sputtering power is 180-220W, and the plated film time is 20-25min.
5. the preparation method of mechanics sensitive conductive glass as claimed in claim 1, it is characterized in that the sputter rate preparing metallic film is 10-20W, argon pressure 0.1-0.2Pa, the plated film time is 100-130s, and the resistance value between farthest 2 of length direction is less than 90-100 Ω.
CN201610022506.1A 2016-01-13 2016-01-13 Preparation method of mechanosensitive conductive glass Pending CN105669047A (en)

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CN110330237A (en) * 2019-06-19 2019-10-15 南京航空航天大学 One kind being based on chemcor glass substrate film deposition method
CN110482876A (en) * 2019-09-23 2019-11-22 醴陵旗滨电子玻璃有限公司 Chemical strengthening composition, chemical strengthening method and chemically reinforced glass
CN113501670A (en) * 2021-07-20 2021-10-15 海南海控特玻科技有限公司 Chemical strengthening and film-covering strengthening process for ultrathin high-aluminum glass

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CN110330237A (en) * 2019-06-19 2019-10-15 南京航空航天大学 One kind being based on chemcor glass substrate film deposition method
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CN110482876B (en) * 2019-09-23 2021-04-13 醴陵旗滨电子玻璃有限公司 Chemical strengthening composition, chemical strengthening method and chemically strengthened glass
CN113501670A (en) * 2021-07-20 2021-10-15 海南海控特玻科技有限公司 Chemical strengthening and film-covering strengthening process for ultrathin high-aluminum glass
CN113501670B (en) * 2021-07-20 2022-05-31 海南海控特玻科技有限公司 Chemical strengthening and film-covering strengthening process for ultrathin high-aluminum glass

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