CN104746056B - A kind of silver-plated method of quartz capillary inwall - Google Patents
A kind of silver-plated method of quartz capillary inwall Download PDFInfo
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- CN104746056B CN104746056B CN201410833304.6A CN201410833304A CN104746056B CN 104746056 B CN104746056 B CN 104746056B CN 201410833304 A CN201410833304 A CN 201410833304A CN 104746056 B CN104746056 B CN 104746056B
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Abstract
The present invention relates to a kind of method that quartz glass capillary inwall is silver-plated, comprise the following steps：Quartz glass capillary surface hydroxylation；Surface silanization；The deposition of palladium nano-particles；Electroless copper：By chemical bronze plating liquid with 0.032 ~ 0.034 mLmin‑1Flow velocity, capillary at least 15 min are flowed through under the conditions of 30 ~ 35 DEG C, then pass to deionized water cleaning；Chemical silvering：By chemical plating liquid with 0.32 ~ 0.34 mLmin‑1Flow velocity, capillary at least 10 min are flowed through under the conditions of 25 ~ 30 DEG C, then pass to deionized water cleaning.Its obtained plated film light is uniform, has good tack in capillary tube inner wall, difficult for drop-off, and has good albedo to laser signal.It, which is used to determine the relative peak heights of the nitrogen in air and can reach, does not fill more than 8 times of relative peak intensities value under the conditions of capillary.
Description
Technical field
The invention belongs to quartz capillary plated film field, and in particular to a kind of silver-plated method of quartz capillary inwall.
Background technology
In LR laser raman gas analyzer, the gas of sampling enters sample room after pretreatment, uses laser illumination
Generation Ramam effect, it is then as undamped as possible to signal to collect, keep signal undistorted, recycle analysis module to solve it
Analysis, so as to draw accurate measurement result.Because optical fiber can be very good transmitting laser signal and produce Raman signal, it is
It is convenient that detection under many specific conditions is provided, so we serve as sample room and signal receiving device with capillary fiber,
It is another critical component in addition to Raman spectrum analysis module.
At present, the solid core fibres for having loaded nanogold or Argent grain are mostly used for the Raman inspection of substances in liquids or solid
Survey, and seldom on the research report of gas context of detection, it is smaller and cause to produce mainly due to gas molecule scattering section
Raman signal intensity it is very weak, it is difficult to realize sensitive and accurately detect.Can land productivity very well if using capillary fiber
Under test gas is preserved with capillary cavity, while being improved the absorption of its Raman response and under test gas by means of nanoparticle coating
Property, it is possible to realize the accurate detection to gaseous sample.
Existing document report capillary fiber is silver-plated can to strengthen Raman signal.At present, foreign countries have Countries also to slap
Hold capillary tube inner wall and plate the technique of silverskin, and there are corresponding commodity, but it is generally physical method plated film, it is expensive.Thus,
Research and development are a kind of low using chemical method cost of implementation, are easy to the technique of the capillary tube inner wall plating silverskin of control to have and weigh very much
The meaning wanted.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of silver-plated method of quartz glass capillary inwall.This method
Cost is low, and technique is simply controllable, and the plated film light of preparation is uniform, has good albedo to laser signal.By its preparation
Plating membrane capillary as gas sample chamber be used for LR laser raman gas analyzer Raman test can be remarkably reinforced signal intensity.
To realize above-mentioned technical problem, the technical solution adopted in the present invention is：
The silver-plated method of quartz glass capillary inwall, comprises the following steps：
1) quartz glass capillary surface hydroxylation：By quartz glass capillary be put into plasma cleaner carry out etc. from
Subprocessing, by quartz glass capillary surface hydroxylation；
2) surface silanization：At normal temperatures, isopropanol is flowed through into the cleaning that capillary carries out capillary inner surface, then made
It is preferably that 1~2h carries out silane to it that silylating reagent flows through capillary at least 1h with 0.32~0.34mLmin-1 flow velocity
Change, then make isopropanol by capillary to remove the silylating reagent of capillary inner surface residual, last blowing air is dried, described
Silylating reagent for 9wt%~12wt% 3- aminopropyls-trimethoxy silane aqueous isopropanol；
3) deposition of palladium nano-particles：Palladium colloidal sol is flowed through into quartz glass wool with 0.32~0.34mLmin-1 flow velocity
Tubule at least 1h is preferably 1~2h；
4) electroless copper：By chemical bronze plating liquid with 0.032~0.034mLmin-1Flow velocity, under the conditions of 30~35 DEG C
It is preferably 15~20min to flow through capillary at least 15min, then passes to deionized water cleaning；
5) chemical silvering：By chemical plating liquid with 0.32~0.34mLmin-1Flow velocity, 25~30 DEG C of conditions flow down
It is preferably 10~15min through capillary at least 10min, then passes to deionized water cleaning.
In such scheme, described step 2)~5) in isopropanol, silylating reagent, palladium colloidal sol, chemical bronze plating liquid, change
Learning silver plating liquid can make it flow through quartz glass capillary in the following way：One end of quartz glass capillary and peristaltic pump are used
Flexible pipe is connected, and the other end is placed in the solution of corresponding capillary to be flowed through, and the pressure differential produced using peristaltic pump realizes phase
Answer flowing of the solution in capillary.
In such scheme, the step 2) in isopropanol with 1.5~1.7mLmin-1Flow velocity flow through capillary 3~
5min。
In such scheme, the step 3) palladium colloidal sol in 12~14nm of palladium nano-particles size.
In such scheme, the step 3) in the commercially available acquisition of palladium colloidal sol or prepared using following methods：Prepare
The deionized water solution of ammonium chloropalladite, sodium citrate and hydroxylamine hydrochloride, wherein：The content of each component is：Ammonium chloropalladite (Pd
(NH4)2Cl4) 0.08~0.09g/L, sodium citrate (Na3C6H5O7) 0.35~0.4g/L, hydroxylamine hydrochloride (NH2OH·HCl)0.08
~0.09g/L, then in 90 ± 2 DEG C, reaction at least 0.5h is preferably 0.5~1h.
In such scheme, the step 4) in the commercially available acquisition of chemical bronze plating liquid or according to formula as below voluntarily with being made
Arrive：Under normal temperature, copper sulphate (CuSO4·5H2O) 180~220g/L, sulfuric acid (H2SO4) 50~70g/L, polyethylene glycol 0.03~
0.05g/L, 2- tetrahydro-thiazoles sulphur 0.001~0.003g/L of copper, solvent is deionized water.
In such scheme, the step 5) in chemical plating liquid voluntarily prepare and obtain according to formula as below：Under normal temperature, nitric acid
Silver (AgNO3) 30~40g/L, imino-diacetic ichthyodin (HN (SO3NH4)2) 80~120g/L, ammonium sulfate ((NH4)2SO4) 100~
140g/L, ammonium citrate ((NH4)3C6H5O7) 1~5g/L, pH 8.2~9, solvent is deionized water.
In such scheme, the step 2) in blowing air drying time be 10-15min, the step 4) and 5) in
Scavenging period is 10~15min.
In such scheme, the length of the quartz glass capillary is more than 25 centimetres, and internal diameter is more than 300 microns.
In such scheme, the silver-plated method of described quartz glass capillary inwall, which is included in after chemical silvering, carries out chemistry
Gold-plated, to form one layer of golden protective layer in silver surface, step is：By chemical gold plating liquid with 0.32~0.34mLmin-1Stream
Speed, it is preferably 10~15min that capillary at least 10min is flowed through under the conditions of 25~30 DEG C, be then passed through successively deionized water and
Ethanol is carried out, and last blowing air is dried.
In such scheme, the chemical gold plating liquid is voluntarily prepared according to formula as below to be obtained：Acrylic acid, hydrogen are prepared under normal temperature
The aqueous solution of sodium oxide molybdena and gold chloride, wherein, acrylic acid 27-28.5mM, sodium hydroxide (NaOH) 55-56.5mM and gold chloride
(HAuCl4) 0.022-0.028mM, solvent is deionized water.
In such scheme, the scavenging period of deionized water and ethanol is 10~15min during the chemical gilding, and blowing air is done
The dry time is 10~15min.
The advantage of the invention is that：
The inventive method especially sets advance copper facing by the special setting of each step especially before chemical silvering, and passes through
Flow velocity when controlling copper facing and be silver-plated, temperature, the parameter such as time finally realizes the uniform plating of quartz glass capillary inside pipe wall
Silver, not only light is uniform for its obtained plated film, and has good tack in capillary tube inner wall, difficult for drop-off, uses flow velocity
10mL min-1 big flow gas, which continues through after capillary (such as 4h) for a long time and has not yet to see plated film, to come off, and to laser
Signal has good albedo.The plating membrane capillary is surveyed as gas sample chamber for LR laser raman gas analyzer Raman
Trial signal intensity is remarkably reinforced.Its relative peak heights for being used to determine the nitrogen in air, which can reach, does not fill capillary bar
More than 8 times of relative peak intensities value under part.
Further preferably plating one layer of golden protective layer in the present invention after chemical silvering can better ensure that prepared by this method
Quartz glass capillary inside pipe wall plates the service life and stability of silverskin.
The chemical reagent cost used is low, environment-friendly.
It is simple to operate, no danger.Can continuous circulate operation.
Reaction condition is gentle, and required instrumentation is simple, and whole flow process does not have the limitation of apparatus and being easily enlarged
Production, provides safeguard to realize that the part of LR laser raman gas analyzer domesticizes.
Brief description of the drawings
Fig. 1 plates the process chart of silverskin for the quartz capillary inwall of the embodiment of the present invention 1；
Fig. 2 plates the light microscope enlarged drawing of silverskin for the quartz capillary inwall of the embodiment of the present invention 1；
Fig. 3 is the Raman test signal intensity contrast figure of the embodiment of the present invention 1.
Embodiment
Embodiment 1
300 microns of internal diameter and the quartz glass capillary of 28 centimeter lengths are intercepted, with plasma cleaner (power is 200W)
5min is handled, then upper binding head is assembled in its one end, is connected with flexible pipe with peristaltic pump, the other end is placed on to be waited to flow through accordingly
In the solution of capillary, peristaltic pump is opened, isopropanol, silylating reagent and isopropanol are extracted at normal temperatures successively with peristaltic pump,
The pressure differential produced using peristaltic pump, makes isopropanol flow through capillary 3min, silanization with 1.5mLmin-1 flow velocity respectively
Reagent flows through capillary 1h with 0.32mLmin-1 flow velocity, and isopropanol flows through capillary with 1.5mLmin-1 flow velocity
3min, described silylating reagent is the aqueous isopropanol of 9wt% 3- aminopropyls-trimethoxy silane, then blowing air
Dry 10min.Continue to use apparatus above, 25~30 DEG C of extraction palladium colloidal sol, makes palladium colloidal sol with 0.32mLmin-1's at normal temperatures
Flow velocity flows through capillary 1h, then extracts chemical bronze plating liquid at 30 DEG C, makes chemical bronze plating liquid with 0.032mLmin-1Flow velocity
Capillary 15min is flowed through, deionized water cleaning 10min is then passed to.Continue 25~30 DEG C of extraction chemical plating liquids at normal temperatures,
Make chemical plating liquid with 0.32mLmin-1Flow velocity flow through capillary 10min, then pass to deionized water cleaning 10min.Most
Afterwards at normal temperatures 25~30 DEG C extraction chemical gold plating liquid, make chemical gold plating liquid with 0.32mLmin-1Flow velocity flow through capillary
10min, then passes to deionization washing 10min, and ethanol washes 10min and is air-dried 10min.
Above-mentioned palladium colloidal sol is prepared using following methods：Prepare going for ammonium chloropalladite, sodium citrate and hydroxylamine hydrochloride
Deionized water solution, wherein：The content of each component is：Ammonium chloropalladite (Pd (NH4)2Cl4) 0.08g/L, sodium citrate
(Na3C6H5O7) 0.4g/L, hydroxylamine hydrochloride (NH2OHHCl) 0.09g/L, then in 90 ± 2 DEG C, reacts 1h.
Above-mentioned chemical bronze plating liquid is voluntarily prepared according to formula as below to be obtained：Under normal temperature, copper sulphate (CuSO4·5H2O)220g/
L, sulfuric acid (H2SO4) 70g/L, polyethylene glycol (relative molecular mass 4000-6000) 0.03g/L, 2- tetrahydro-thiazoles sulphur copper
0.001g/L, solvent is deionized water.
Above-mentioned chemical plating liquid is voluntarily prepared according to formula as below to be obtained：Under normal temperature, silver nitrate (AgNO3) 40g/L, imido
Base disulfonic acid ammonium (HN (SO3NH4)2) 80g/L, ammonium sulfate ((NH4)2SO4) 140g/L, ammonium citrate ((NH4)3C6H5O7) 5g/L,
PH 9, solvent is deionized water.
Above-mentioned chemical gold plating liquid is voluntarily prepared according to formula as below to be obtained：Acrylic acid, sodium hydroxide and chlorine are prepared under normal temperature
The aqueous solution of auric acid, wherein, acrylic acid 27mM, sodium hydroxide (NaOH) 55mM and gold chloride (HAuCl4) 0.022mM, solvent is
Deionized water.
The process chart is as shown in figure 1, its plating silverskin quartz capillary light microscope enlarged drawing prepared is shown in Fig. 2 institutes
Show, surface unusual light after plated film, is advantageously implemented the reflection of light as seen from Figure 2.
After the preparation for completing silver-plated membrane capillary, we are applied to gas Raman test.First mix up LR laser raman gas
Physical examination test sample machine platform, in the case where not filling capillary, the peak value that we measure the nitrogen signal in air is 148；With this
For contrast condition, load the plating membrane capillary as gas sample chamber on LR laser raman gas analyzer, to detect that laser is drawn
Graceful gas detection Prototyping Platform is loading onto the Postcapillary scattered signal intensity change of the plated film.After measured：Load onto plated film hair
The relative peak heights that the nitrogen in air is measured on software after tubule are 1200, are not fill 8.1 be worth under the conditions of capillary
Times.Raman test signal intensity contrast figure is shown in Fig. 3.
Embodiment 2
300 microns of internal diameter and the quartz glass capillary of 28 centimeter lengths are intercepted, is handled with plasma cleaner by quartzy glass
Glass capillary surface hydroxylating, then assembles upper binding head in its one end, is connected with flexible pipe with peristaltic pump, the other end is placed on phase
In the solution for the capillary to be flowed through answered, peristaltic pump is opened, isopropanol, silylating reagent are extracted at normal temperatures successively with peristaltic pump
And isopropanol, the pressure differential produced using peristaltic pump, isopropanol is flowed through capillary with 1.6mLmin-1 flow velocity respectively
3min, silylating reagent flows through capillary 1h with 0.33mLmin-1 flow velocity, and isopropanol is with 1.5mLmin-1 flow velocity stream
Through capillary 3min, the aqueous isopropanol for 3- aminopropyls-trimethoxy silane that described silylating reagent is 12wt%, so
Blowing air dries 10min afterwards.Continue to use apparatus above, at normal temperatures 25~30 DEG C extraction palladium colloidal sol, make palladium colloidal sol with
0.32mLmin-1 flow velocity flows through capillary 2h, then extracts chemical bronze plating liquid at 35 DEG C, make chemical bronze plating liquid with
0.034mL·min-1Flow velocity flow through capillary 20min, then pass to deionized water cleaning 15min.Continue at normal temperatures 25~
30 DEG C of extraction chemical plating liquids, make chemical plating liquid with 0.34mLmin-1Flow velocity flow through capillary 10min, then pass to
Ionized water cleans 10min.Last 25~30 DEG C of extraction chemical gold plating liquids at normal temperatures, make chemical gold plating liquid with 0.34mLmin-1
Flow velocity flow through capillary 10min, then pass to deionization washing 10min, ethanol washes 10min and be air-dried 10min.
Above-mentioned palladium colloidal sol is prepared using following methods：Prepare going for ammonium chloropalladite, sodium citrate and hydroxylamine hydrochloride
Deionized water solution, wherein：The content of each component is：Ammonium chloropalladite (Pd (NH4)2Cl4) 0.09g/L, sodium citrate
(Na3C6H5O7) 0.35g/L, hydroxylamine hydrochloride (NH2OHHCl) 0.08g/L, then in 90 ± 2 DEG C, reacts 0.5h.
Above-mentioned chemical bronze plating liquid is voluntarily prepared according to formula as below to be obtained：Under normal temperature, copper sulphate (CuSO4·5H2O)180g/
L, sulfuric acid (H2SO4) 50g/L, polyethylene glycol (relative molecular mass 4000-6000) 0.05g/L, 2- tetrahydro-thiazoles sulphur copper
0.003g/L, solvent is deionized water.
Above-mentioned chemical plating liquid is voluntarily prepared according to formula as below to be obtained：Under normal temperature, silver nitrate (AgNO3) 30g/L, imido
Base disulfonic acid ammonium (HN (SO3NH4)2) 120g/L, ammonium sulfate ((NH4)2SO4) 100g/L, ammonium citrate ((NH4)3C6H5O7) 1g/L,
PH 8.2, solvent is deionized water.
Above-mentioned chemical gold plating liquid is voluntarily prepared according to formula as below to be obtained：Acrylic acid, sodium hydroxide and chlorine are prepared under normal temperature
The aqueous solution of auric acid, wherein, acrylic acid 28mM, sodium hydroxide (NaOH) 56mM and gold chloride (HAuCl4) 0.028mM, solvent is
Deionized water.
Through characterizing, coated surface smooth even prepared by this method.The plating membrane capillary is made according to the method for embodiment 1
For gas sample chamber load LR laser raman gas analyzer on, with detect LR laser raman gas detection Prototyping Platform load onto it is gold-plated
Postcapillary scattered signal intensity changes.After measured：Load onto the nitrogen measured after the plating membrane capillary on software in air
Relative peak heights be 1160.
Embodiment 3
300 microns of internal diameter and the quartz glass capillary of 28 centimeter lengths are intercepted, is handled with plasma cleaner by quartzy glass
Glass capillary surface hydroxylating, upper binding head then is assembled in its one end, is connected with flexible pipe with peristaltic pump, the other end is placed on
In the solution of corresponding capillary to be flowed through, peristaltic pump is opened, isopropanol, silanization is extracted at normal temperatures successively with peristaltic pump and tries
Agent and isopropanol, the pressure differential produced using peristaltic pump make isopropanol flow through capillary with 1.7mLmin-1 flow velocity respectively
5min, silylating reagent flows through capillary 2h with 0.34mLmin-1 flow velocity, and isopropanol is with 1.6mLmin-1 flow velocity stream
Through capillary 3min, the aqueous isopropanol for 3- aminopropyls-trimethoxy silane that described silylating reagent is 10wt%, so
Blowing air dries 10min afterwards.Continue to use apparatus above, 25~30 DEG C are extracted the palladium colloidal sol that particle diameter is 12-14nm at normal temperatures, are made
Palladium colloidal sol flows through capillary 1h with 0.32mLmin-1 flow velocity, then extracts chemical bronze plating liquid at 30 DEG C, makes electroless copper
Liquid is with 0.032mLmin-1Flow velocity flow through capillary 20min, then pass to deionized water cleaning 10min.Continue at normal temperatures
25~30 DEG C of extraction chemical plating liquids, make chemical plating liquid with 0.32mLmin-1Flow velocity flow through capillary 15min, Ran Houtong
Enter deionized water cleaning 15min.Last 25~30 DEG C of extraction chemical gold plating liquids at normal temperatures, make chemical gold plating liquid with 0.32mL
min-1Flow velocity flow through capillary 15min, then pass to deionization washing 15min, ethanol washes 15min and be air-dried 15min.
Above-mentioned chemical bronze plating liquid is voluntarily prepared according to formula as below to be obtained：Under normal temperature, copper sulphate (CuSO4·5H2O)200g/
L, sulfuric acid (H2SO4) 60g/L, polyethylene glycol (relative molecular mass 4000-6000) 0.04g/L, 2- tetrahydro-thiazoles sulphur copper
0.002g/L, solvent is deionized water.
Above-mentioned chemical plating liquid is voluntarily prepared according to formula as below to be obtained：Under normal temperature, silver nitrate (AgNO3) 35g/L, imido
Base disulfonic acid ammonium (HN (SO3NH4)2) 110g/L, ammonium sulfate ((NH4)2SO4) 120g/L, ammonium citrate ((NH4)3C6H5O7) 3g/L,
PH 8.5, solvent is deionized water.
Above-mentioned chemical gold plating liquid is voluntarily prepared according to formula as below to be obtained：Acrylic acid, sodium hydroxide and chlorine are prepared under normal temperature
The aqueous solution of auric acid, wherein, acrylic acid 27.5mM, sodium hydroxide (NaOH) 55.5mM and gold chloride (HAuCl4) 0.025mM, it is molten
Agent is deionized water.
Through characterizing, coated surface smooth even prepared by this method.The plating membrane capillary is made according to the method for embodiment 1
For gas sample chamber load LR laser raman gas analyzer on, with detect LR laser raman gas detection Prototyping Platform load onto it is gold-plated
Postcapillary scattered signal intensity changes.After measured：Load onto the nitrogen measured after the plating membrane capillary on software in air
Relative peak heights be 1250.
Claims (10)
1. the silver-plated method of quartz glass capillary inwall, it is characterised in that：Comprise the following steps：
1) quartz glass capillary surface hydroxylation：Quartz glass capillary is put into plasma cleaner and carried out at plasma
Reason, by quartz glass capillary surface hydroxylation；
2) surface silanization：At normal temperatures, isopropanol is flowed through into the cleaning that capillary carries out capillary inner surface, then makes silane
Change reagent flows through capillary at least 1h with 0.32~0.34mLmin-1 flow velocity and silanization is carried out to it, then leads to isopropanol
Capillary is crossed to remove the silylating reagent of capillary inner surface residual, last blowing air is dried, and described silylating reagent is
The aqueous isopropanol of 9wt%~12wt% 3- aminopropyls-trimethoxy silane；
3) deposition of palladium nano-particles：Palladium colloidal sol is flowed through into quartz glass capillary with 0.32~0.34mLmin-1 flow velocity
At least 1h；
4) electroless copper：By chemical bronze plating liquid with 0.032~0.034mLmin-1Flow velocity, flowed through under the conditions of 30~35 DEG C
Capillary at least 15min, then passes to deionized water cleaning；
5) chemical silvering：By chemical plating liquid with 0.32~0.34mLmin-1Flow velocity, flow through hair under the conditions of 25~30 DEG C
Tubule at least 10min, then passes to deionized water cleaning.
2. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：Described step 2)
~5) in isopropanol, silylating reagent, palladium colloidal sol, chemical bronze plating liquid, chemical plating liquid can flow through it in the following way
Quartz glass capillary：One end of quartz glass capillary is connected with peristaltic pump with flexible pipe, the other end is placed on to be treated accordingly
In the solution for flowing through capillary, the pressure differential produced using peristaltic pump realizes flowing of the corresponding solution in capillary.
3. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：The step 2) in
Isopropanol with 1.5~1.7mLmin-1Flow velocity flow through 3~5min of capillary.
4. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：The step 3)
12~14nm of palladium nano-particles size in palladium colloidal sol.
5. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：The step 3) in
The commercially available acquisition of palladium colloidal sol or prepared using following methods：Prepare ammonium chloropalladite, sodium citrate and hydroxylamine hydrochloride
Deionized water solution, wherein：The content of each component is：0.08~0.09g/L of ammonium chloropalladite, 0.35~0.4g/ of sodium citrate
L, 0.08~0.09g/L of hydroxylamine hydrochloride, then in 90 ± 2 DEG C, react at least 0.5h.
6. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：The step 4) in
The commercially available acquisition of chemical bronze plating liquid is voluntarily prepared according to formula as below and obtained：Under normal temperature, 180~220g/L of copper sulphate, sulfuric acid
50~70g/L, polyethylene glycol 0.03~0.05g/L, 2- tetrahydro-thiazoles sulphur 0.001~0.003g/L of copper, solvent is deionized water.
7. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：The step 5) in
Chemical plating liquid is voluntarily prepared according to formula as below and obtained：Under normal temperature, 30~40g/L of silver nitrate, imino-diacetic ichthyodin 80~
120g/L, 100~140g/L of ammonium sulfate, ammonium citrate 1~5g/L, pH 8.2~9, solvent is deionized water.
8. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：The quartz glass
The length of capillary is more than 25 centimetres, and internal diameter is more than 300 microns.
9. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：Described quartzy glass
The silver-plated method of glass capillary tube inner wall, which is included in after chemical silvering, carries out chemical gilding, to be protected in one layer of gold of silver surface formation
Layer, step is：By chemical gold plating liquid with 0.32~0.34mLmin-1Flow velocity, capillary is flowed through under the conditions of 25~30 DEG C extremely
Few 10min, is then passed through deionized water successively and ethanol is carried out, and last blowing air is dried.
10. the silver-plated method of quartz glass capillary inwall according to claim 1, it is characterised in that：The chemical plating
Golden liquid is voluntarily prepared according to formula as below to be obtained：The aqueous solution of acrylic acid, sodium hydroxide and gold chloride is prepared under normal temperature, wherein,
Acrylic acid 27-28.5mM, sodium hydroxide 55-56.5mM and gold chloride 0.022-0.028mM, solvent is deionized water.
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| CN117385346B (en) * | 2023-12-12 | 2024-02-23 | 江苏中科智芯集成科技有限公司 | Method for copper-based chemical nickel-plating palladium-gold in wafer |
| CN117405651B (en) * | 2023-12-15 | 2024-03-22 | 武汉理工大学 | Rhodium-plated metal capillary, preparation method thereof and gas Raman spectrum detection system |
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| CN104020151A (en) * | 2014-07-10 | 2014-09-03 | 苏州大学 | Preparation method of surface-enhanced Raman scattering metal nano-disc array substrate |
| CN104046968A (en) * | 2014-07-02 | 2014-09-17 | 华中师范大学 | Method for plating gold on inner wall of quartz glass capillary tube |
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| CN1944709A (en) * | 2006-09-21 | 2007-04-11 | 复旦大学 | Method for depositing continuous metal layer on capillary tube inner wall |
| CN101649477A (en) * | 2009-09-11 | 2010-02-17 | 中国工程物理研究院激光聚变研究中心 | Preparation method of metal carbon aerogel composite material |
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